FINAL REPORT

Standardization

of

Materials

the

and
Volume

Test

Carbon-Phenolic

Processes
II

Methods

and

Speclflcatlons

August

31,

1988

Nasa
Marshall

Grant

NAG8-545

Space

Flight

Center

Final Report

(for

Volume

I1, Test

Methods

period

1 September

and

1985

Specifications

to

31 August

1988)

for

Standardization

of

Materials

the

and

NASA Grant

Processes

No. NAG8-545

Prepared

National
Ronald
George

Aeronautics

for

and Space

L. Nichols,

C. Marshall

Carbon-Phenollc

Admlnlstratlon

NASA Technical

Space

Flight

Prepared

Center,

Officer
Alabama

by

William B, Hall
Professor

of

Chemlcal Engineering

MIssissippi
Mississippi

State,

State

Unlverslty

Mississippi

39762

35812

PREFACE

The

test

files

methods

of

the

contained

Space

Flight

Huntsville,
Fibers,
Front

VA

CA

Ana,

CA

Inc.

Louisville,
Fiberite

methods
be

to

assistance.

MN

were

modified
on

all

KY

Corporation

Winona,

given

NASA,

Polymeric

Borden,

depending

Center,

Inc.

Santa

to

from

SC

Valencia,

need

taken

Inc.

PolyCarbon,

test

were

Inc.

Cheraw,

The

volume

AL

Royal,

Highlands,

U.S.

this

following:

Marshall

Avtex

in

made
as

as

generic

required

equipment

and

the

identities

above

by

as

other

personnel.
for

possible

and

would

laboratories
Sincere

the

appreciation

unrewarded

is

TABLE

OF

CONTENTS

MATERIALS
Resins
M-R-I

Chemical
Fillers,
Alkaline

M-R-2

Analysis
of
and
Prepregs
Earth
Metals

Percent
Broadgoods

Resins,
Fabrics,
for
Alkali
and
....................

Resin
Pickup
in Manufacture
...............................

of
8

M-R-3

Total
Resin
Solids
Content
of Liquid
Solutions
................................

M-R-4

Specific
Liquids,

M-R-5

Gravity
Solids,

viscosity
Brookfield

M-R-6

M-R-7

M-R-8

M-R-9

M-R-I

M-R-14

of
.........

Determination
by
the
Methods
.......................

Gel

Time

of

Liquid

Determination

in

an

Oil

12

16

Bath

.........................

21

Gel
Time
Determination
of
Liquid
Resins
at
132C
..........................

24

RDS
- Viscosity
at Various
Temperatures
with
Rheomatic
Dynamics
Spectrophotometer
.........................

26

Liquid
and
Determining

29

Purity

M-R-12

Determination
and
Semi
Solids

Resins

of

Gel
Permeation
Mol
Weights
Solvents

by

Chromatography
...................
Chromatography

......

Infra-Red
Spectrophotometer
Analysis
Resins
....................................

of

Moisture
Content
Photo
Volt
Unit

pH
pH

45

of Liquid
Resins
by use
of
a
Meter
..................................

Resin
Both

of Resins
by
Use
of
...........................

Solids
Filled

Refractive
Specific
Liquid

and
and
Index

Total

Solids

Unfilled
on

Resin

Systems

47

49

for
..........

.................

Gravity
by
Hydrometers
on
Resins
.............................

II

36

51
52

53

M-R-17

M-R-18

M-R-19

M-R-20

M-R-21

M-R-22

M-R-23

Resin
Reinforcement
Phenolic
Prepregs

in Aldehyde
.........................

Degree
of Advancement
by Infra-Red
Technique
Differential
Determining
Polymerization
pH of Resins
with
pH Meter

or

54

Polymerization
55

JQelOOIOgOIOIOOQeOO0

Scanning
Calorimetry
for
the Heat
of
............................

59

and Aqueous
Solutions
.............................

61

Karl
Fisher
Water
Materials
Chemicals

Determination
in
.......................

Free
Formaldehyde
in
and Furan
Type
Resins

Aldehyde
Phenolic
.....................

Chang's
Index
- A Measure
of Degree
Cure .......................................

63

68

of
71

Cloth
M-C-I

M-C-2

Linear
Density
of Yarn
and Cord
Expressed
in Denier
.......................

74

Tensile
Fabrics

78

Properties
of Twisted

M-C-3

Twist,

M-C-4

Finish
on
Isopropanol

M-C-5

M-C-6

pH of
Water

Determination
Rayon
Yarn
Extraction

Fiber
and
and Saline

Regain

Ash Content
Temperatures

M-C-10

in

Cord,
and
..............

Yarn,

Cord

........

Using
Freon
and
....................

Fabrics
in Distilled
Solutions
.... _ ...........

Shrinkage
of Yarn
and
and Ambient
Temperature
Moisture

M-C-9

of Yarn,
Materials

Content

Cord
in Water
...................
of

Fiber

..........

of Fiber
at Increasing
..............................

Zinc
Extraction
Measurement
by
Sulfur
Content
and Elemental

by use
of HCI
and
Atomic
Absorption
..........
of Yarn,
Both
Sulfate
Sulfur
......................

III

88

93

97

i00
102

105

107

ll0

M-C-II

Rayon
Yarn
Requirements
for
Carbon
Textiles
..................................

114

Carbon

119

Visual
Rolls
M-C-14

M-C-15

M-C-16

M-C-17

M-C-18

M-C-19

Fabrics

M-C-23

Fiber
ultimate
Specification

M-C-25

M-C-26

M-C-27

M-C-28

Tensile
Limits

of

Strength
Carbon

121

Fiber

......

Fiber
Density
Specification
Limits
of
Carbon
Fiber
...........................
Fiber
Weight
Specification
Limits
Broadgoods
................................
Thread
Master

Count
Rolls

122

123
of
124

Specification
of
Broadgoods

Limits
on
................

125

Thickness
Specification
Master
Rolls
of
Broadgoods

Limits
of
................

126

Carbon
Reinforcement,
1200
ppm
Sodium,
Specifications
for
Rocket
Nozzle
Components
................................

127

Ash

129

Content

of

Filler

Strength
Rolls

Materials

...........

Specifications
for
...........................

130

Specific
Gravity
Specification
of Broadgoods
.............................
Sodium
by

M-C-24

.............

Examination
of
Broadgood
.....................................

Breaking
Broadgood
M-C-22

Specifications

Content

Flame

of

Emission

Raw
Graphite
Fabric
Physical
Inspection
pH
of
Water

Fabric
by
Extraction

Apparent
Fabric,

Volume
Prepregs,

Material

Method

..................

132

Visual
and
.......................

133

Both
Cold
and
Hot
..........................

Fabric
Thread
Count
and
Fill
Direction
Fabric
weight
Unconditioned,
Devolatilized

Filler

131

138

for
Both
Warp
........................

140

Using
Small
Specimens
of
Conditioned,
and
Methods
.....................
and
Density
and
Cured

iv

of Raw
Material

......

141

143

M-C-29

Raw
Both

M-C-30

Carbon
Minor

Broadgoods
Criteria
Major

Fabric
Inspection
and
Major
Defects
Visual
For
Both

Defects

Inspection
Minor
and

Into
..............

147

and

.............................

149

Fillers
M-F-I

M-F-2

M-F-3

M-F-4

M-F-5

M-F-6

M-F-7

Ash
Content
of
Fillers,
Pigments
and
Related
Materials
.........................

152

Particle
Size
a Sub-Siever

154

and
Sizer

Distribution
Using
........................

Percent
Inorganic
Filler
Reinforcement
in
a Resin
................................

158

Filler
Systems

161

Particle
Automatic
Carbon
Carbon
Particle

Content
in Filled
Resin
...................................
Size
by
Analyzer
Assay
Filler
Size

the
Horiba
Centrifugal
........................

163

and
Moisture
Content
of
.............................

170

Test

for

Fillers

by

SEM

.....

171

PREPREGS
P-P-I

Volatile

P-P-2

Resin
Content

Solids,
Filler,
and
of Uncured
Material

Resin

Flow

Content

Carbon
Medium
P-P-5

P-P-6

P-P-7

of

of

P-P-II

P-P-12

P-P-13

Prepregs

......

Cloth
...............

Material

Phenolic,
and
Uncured

............

Prepreg,
Content

.........

Resins
and
Prepregs
by
............................

172

173
175

177

183

Infra-Red
Spectrum
of
Resins
and
Prepregs
..............................

189

Resin
Content
of
Prepregs
by
Soxhlet
Extraction
................................

190

Volatile

195

Content

Gel
Time
for
Thermoplastic
P-P-10

Uncured

Uncured

Cloth,
Sodium

Moleweight
Chromatography

of

Volatile,
Prepregs

of

Prepregs

..............

Thermosetting
or
Resins
......................

Fiber,
and
Filler
Content
..................................

198
of
200

Extraction
of Prepregs
for
Determination
of Acetone
Soluble
Material
..................................

203

Method
Analysis

206

Percent

of

Conducting
of Resins

volatiles

Prepregs

and

Thermogravimetric
Prepregs
...........

Content

of

..................................

208

P-P-14

Flow

P-P-15

Resin
Content

Solids,
Filler,
of Prepregs

and
Cloth
.......................

211

Resin
Content

Solids,
Filler,
and
Cloth
of
prepregs
.......................

213

P-P-16

P-P-17

P-P-18

Character

Sodium
Emission

and

Compression,
Shear,
and

of

Staged

Ash
Content
for
Prepregs

Broadgoods

by Flame
.....................

Residual
volatile,
Dowel
Resin
Content
of
Prepregs

vl

.......

209

216

......

218

P-P-19

Dowel Shear of Fiber Reinforced

Laminates .................................

220

P-P-20

Compression Strength
Reinforced
Laminates

of Fiber
......................

222

P-P-21

Resin Content
Use of Factor

of Prepregs Making
"K" .........................

225

P-P-22

Specific
Prepregs

Gravity
and Density
..................................

P-P-23

Residual
Articles

volatile
Content of Molded
..................................

P-P-24

Infra-Red
Spectrum of Liquid
and
Solid Resins and Prepregs .................

229

P-P-25

Residual
Volatile
Content in
Molded Articles
...........................

230

P-P-26

Thermogravimetric
Analysis
(a),
Chemical Test Methods .....................

232

P-P-27

Thermogravimetric

Analysis

(b) ............

234

P-P-28

Thermogravimetric

Analysis

................

236

P-P-29

Resin
of

P-P-30
P-P-31
P-P-32

Tack
Lap

Content
Prepregs

of

by
Means
of
Pyrolysis
...............................

Temperature
of Prepregs
by
Shear
.................................

227
228

238

241

Wet
and
Dry
Flow
by Flash
Removal
or
Punched
Disc
...........................

243

Viscosity
Parallel

248

RDS
Disc

for

Prepregs,

,oeeeelloJo,,ooeoeeoJJeeoolee

vll

by

CUREDMATERIALS
Density

of Cured Material

Residual
Material

Volatile
Content
..................................

F-3

Compressive

F-4

Interlaminar

F-5

Thermal

F-6

Flexural

F-8

Tensile

F-9

Dry

F-10

Residual

F-II

Strength
of

Conductivity

Strength
Content

of
of

Cured

252

Material
Material

Cured

Cured
Cured

of

Volatiles
Thermal
Using

of Cured

Cured
of

250

....
......

Material

....

Thermal
Expansion
of
............................

Strength

Resin

Linear
Material

of

Shear

Coefficient
of
Cured
Material

F-7

.................

of

Cured
Cured

Material
Material
Material
Material

Expansion
of
Cured
DSC
........................

vlJl

254
257
260

261
.......
........

262
263

.......

264

......

269

272

M-R-I

Chemical
Prepregs

Analysis
of
Resins,
Fabrics,
for
Alkali
and
Alkaline
Earth

Fillers,
Metals

and

SCOPE
This
procedure
describes
a method
and
alkaline
earth
metal
impurities
calcium,
lithium,
and
magnesium)
in preimpregnates.
,

EQUIPMENT

AND

in

determining
alkali
(sodium,
potassium,
resins,
fabrics,
and

MATERIALS

2.1

Atomic

2.2

Analytical

balance,

2.3

Volumetric

flasks,

and

for

Absorption

Spectrophotometer
sensitivity
i00

ml.

0.0001

and

gm.

200

ml.

50

ml.

(one

per

sample

blank)

2.4

Graduated

2.5

Hot

2.6

Fume

2.7

Timer

2.8

Gloves;

2.9

Oven,

2.10

Muffle

2.11

Platinum

2.12

Forceps

2.13

Scissors

2.14

Matrix

standards

2.15

Nitric

Acid,

2.16

Hydrochloric

Acid

6N

2.17

Hydrofluoric

Acid

28N

2.18

Cesium

2.19

Potassium

pyro-sulfate

2.20

Deionized

Water

cylinders,

I0

ml.

and

Plate
exhaust

hood

plastic
Convection
Furnace
or

ceramic

crucibles

(30

ml.)

ppm

Na,

K,

(0.5
6N

Chloride

&

12N

for

one

Ca,

Li

per

and

sample

Mg)

NOTE:

3.

Unless
reagent

specified,
all
spectro
grade,

reagents
are
as applicable.

to

be

SAMPLING

3.1

Resins.

3.2

Fabrics.

3.3

Prepregs.

3.4

Fillers.

4.

otherwise
grade
or

Obtain

representative

Obtain
Obtain
Obtain

16

sq.

16

25

gm.

sample.

in.

sq.

in.

representative

25

gm.

sample.

PROCEDURE

4.1
4.1.1

4.2

Rea@ent

Preparation

CsC1
Stock
Solution.
Add
about
water
to a two liter
volumetric
with
agitation.
After
the CsCI
the solution
to cool
to ambient
to 2000
ml. with
deionized
water
micrograms/ml,
solution.

1200 ml.
of deionized
flask.
Add
253 gm CsCl
is in solution,
allow
temperature
and dilute
to yield
a i00,000

Ceramic
Crucible
Preparation
Ceramic
crucibles
are to be
used
for atomic
absorption
spectrophotometric
testing
of
carbonaceous
materials.
All new
crucibles
are to be
conditioned
as below.
Crucibles
that
have
been
in use
for this
procedure
may be considered
clean
(proceed
to
par.
4.2.10).

4.2.1

Label
agent

4.2.2

Place
crucibles
on
hood
and fill with
setting,
evaporate
procedure.

4.2.3

Remove
crucibles
five
minutes.

4.2.4

Rinse
times.

4.2.5

Place
the
crucibles
on the hot plate
again
and
fill
with
12N HCl.
Using
a medium
hot plate
setting,
evaporate
to near
dryness
and repeat.

4.2.6

Remove
the crucibles
for five minutes.

from

4.2.7

Rinse
plate.

deionized

the ceramic
crucibles
with
an appropriate
that
will
withstand
at least
600_C.

the

from

crucibles

copiously

a hot plate
in
6N HCI.
Using
to near
dryness

with

hot

with

plate

the

a laboratory
a medium
hot
then
repeat

and

dionized

hot

marking

allow

water

plate

water.

to

at

fume
plate

cool

least

and

Return

let

to

for

three

stand

hot

4.2.8

Fill
crucibles
with
dryness and repeat.

4.2.9

Remove the crucibles

from
cool for five minutes.
with

hot

Rinse

4.2.11

Place the crucible{

in a muffle
conditioned
to 600 T 15C., for
hours.

4.2.12

Remove the crucibles

from
desiccate
until
used.
Platinum
be used
samples
ceramic

crucibles

the

4.2.10

4.3

the

6N HCl and again

Crucible
Preparation
for samples
known
to
without
a history
of
crucibles.

evaporate

plate

deionized

to near

and allow

water

to

copiously.

furnace,
prea minimum of three

the muffle

furnace

and

Platinum
crucibles
are to
contain
silica
or for
successful
preparation
in

4.3.1

To cleanr the crucible,

fuse
about
one gram
of potassium
pyrosulfate
in the crucible.
Rotate
the crucible
to
distribute
the melt
along
the
inside
walls.

4.3.2

Pour

off

the

melt

and

allow

to

cool

to

ambient

temperature.
4.3.3

Boil
(30)
with

4.3.4

Place
with
one

the crucibles
in deionized
minutes.
Rinse
the
boiled
deionized
water.
the
6N
(I)

crucibles

HNO 3.
hour

in

Bring
Pour

4.3.5

Pour
off
deionized

4.3.6

Ignite
for at
repeat.

4.3.7

Pour
off
deionized

4.3.8

Remove
the crucibles
desiccate
until
used.

4.4
4.4.1

Sample

the acid
water.

and

fill
for

and

and

a suitable

about
thirty
several
times

acid
to a boil
and maintain
off the hot acid
and repeat.
rinse

the crucible
in
least
one hour.

the acid
water.

water
for
crucibles

container

several

times

with

a muffle
furnace
(600 + 15C)
Pour
off the hot
acid-and

rinse

from

several

the

muffle

times

with

furnace

and

Preparation

Using
clean
plastic
gloves
and clean
scissors,
cut the
sample
into
approximate
1/2 inch
squares
and transfer
into
an analytically
clean
and labled
sample
bottle.

Unused
every
4.4.2

Assure
par.

sample
seventh

4.2

will
be
crucible

that
or

the
4.3,

retained.
shall
be

crucibles
have
as
applicable.

For
multiple
samples,
blank
determination.

been

conditioned

4.4.3

Weigh
nearest

4.4.4

Add
approximately
using
forceps.
to nearest
0.i

4.4.5

Transfer
the
crucibles
to
a convection
125
+ 5C.
for
two
hours
minimum.

4.4.6

Remove

and
record
0.i
mg.

the

ambient

the

and

crucibles

from
is

record

the

Transfer
the
crucibles
600
+ 15C.
for
16 to

4.4.9

weigEt

is

Remove

the

Desiccate
Determine
Weigh

of

the

2 gm.
of
sample
Weigh
exactly
and
mg.

temperature

Weigh

weight

the

crucible

per

to

the

into
the
crucible
record
sample
weight

oven

oven

and

and

dry

desiccate

at

until

achieved.

crucibles

to

the

to
a muffle
20 hours,
or

nearest

furnace
until

0.i

mg.

and
ash
constant

at

achieved.
crucibles

from

until
ambient
ash
content,
and

record

the

the

muffle

temperature
if required
weights

to

Place
the
crucibles
on a hot
75%
of
capacity
with
deionized
12N
HCI
to each
crucible.

furnace.
is
per

the

achieved.
par.
5.2.

nearest

plate
and
water.

fill
Add

0.i

mg.

to
about
ml.
of

4.4.12

With
the
use
of moderate
heat,
effect
slow
evaporation
to near
dryness.
DO NOT
ALLOW
THE
SAMPLES
TO
REACH
DRYNESS.
Repeat
par.
4.4.11
and
4.4.12
as needed
in
order
to
effect
solution.
All
crucibles
must
be
treated
identically.

4.4.13

Quantitatively
transfer
the
crucibles
into
analytically
appropriate
size
(to measure
of
the
standard
range).

4.4.14

Add

sufficient

flask
diluted
Dilute
Agitate

to

CsCl

yield
to the

each
each

stock

a 2000
mark.

flask

to

solution

solution

ppm

the

solution
from
the
clean
volumetric
within
the
linear

CsCl

mark

prior

and
to

to

each

concentration

agitate.

analysis.

flasks
of
portion

volumetric
when

4.5

Preparation

4.5.1

4.6

of

Standard

Analysis
of USP samples
requires
the use
of a matrix
standard
below
which
the Beers
Laws
relationship
is
linear.
Empirical
data
has shown
that
for the
alkali
metals
and
alkaline
earth
metals,
the calibration
curve
appears
linear
below
0.5 ppm.
MATRIX:
The matrix
contain
each
of the
following
elements
in deionized
water
Na,
K, Ca, Li,
and Mg.
The
standard
is made
by
adding
(Volumetric
pipet)
1 ml.
of a i000 ppm
stock
solution
for each
of the elements
into
a 2000 ml.
volumetric
flask
and diluting
to volume.
Spectrophotometer

4.6.1

Start

up

Each
laboratory
shall
generate
an
procedure
for instrument
operation.
the U.S.
Polymeric
procedure.

4.6.1.1

Turn

4.6.1.2

Make
sure
air pressure
pressure
is Just
below

is
15

4.6.1.3

Turn

switch

4.6.1.4

Press
oxidant
button
left
instrument
panel
and turn
oxidant
knob
counter-clockwise
until
ball
float
goes
down
no further.
This
should
be reading
12;
if not,
adjust
knurled
knob
on nebulizer
until
a reading
of
12 is obtained.
Next
turn
oxidant
knob
clockwise
until
a reading
of 18 has been
achieved.

4.6.1.5

Press
fuel/oxidant
button
fuel ball
float
reads
7.

4.6.1.6

Remove
nebulizer
tube
from
on button
to ignite
flame.

4.6.1.7

Adjust
fuel knob
counter-clockwise
in the
flame
Just
disappears.
head
height
is 32).

4.7

Analysis

on

air

and

acetylene

appropriate
written
The
following
is

spectrophotometer

for

valves.
40 psi
psi.

and

and

acetylene

on

adjust

D.I.

H20

fuel

and

knob

press

until

flame

until
the yellow
(Make
sure
burner

Potassium

4.7.1

Adjust
monochrometer
selector
to POSITION.

to

read

4.7.2

Place
MA count
the inner
knob

4.7.3

Aspirate
the 0.5 ppm MATRIX
Standard
and adjust
the
monochrometer,
in close
vicinity
of the
originally
set wave
length,
to obtain
maximum
deflection
on the

selector
completely

to

766.5

the 1.0
clockwise.

nm;

place

position

mode

and

turn

log scale meter (right

instrument
fine tuning
of the wave length.

This

panel).

is

4.7.4

Aspirate
deionized
water or nitric
acid digestion
blank and press auto zero button
(you should at this
time select
the integration
period depending on how
stable
you want the read out to be.)

4.7.5

Start
with a slit
width of 80.
Aspirate
the 0.5 ppm
MATRIX Standard and use the photomultiplier
voltage
knob and the inner MA/count knob to obtain
a read out
of 0.50 on the digital
display.
If this cannot be
done, adjust
slit
selection
either
up or down
depending on whether you want to increase
or decrease
the read out, respectively.

4.7.6

Continuing
M/A count
out
to 50

4.7.7

Aspirate
deionized
blank
and recheck

4.7.8

Aspirate
each
sample.
ppm to be reported.
Analysis

for

to aspirate
the 0.5 ppm
standard
selector
and inner
knob
to adjust
ppm
for the
i00 to 1 dilution.
water
zero.

Sodium,

or

The

nitric

read

out

acid

will

use
the

the
read

digestion

give

direct

Calcium:

The procedure
here
is the
same
as for Potassium
except
that
the
initial
monochrometer
wave
length
for
sodium
is 589.0
nm.
and for Calcium
422.7
nm.
Calculate
the curve
for sodium
that
is linear
between
0.I and
2.5 micrograms
per ml..
4.9

Analysis

for

Magnesium:

4.9.1

Adjust

monochrometer

4.9.2

Place
MA/count
the inner
knob

4.9.3

Place

4.9.4

Turn
lamp
turret
until
Mg lamp
adjust
knurled
knob
immediately
until
lamp
current
reads
5 MA
panel)

4.9.5

DO NOT
aspirate
standard,
but
fine
tune
wavelength
achieving
maximum
deflection
on log scale
by
adjusting
monochrometer.

4.9.6

Aspirate
deionized
water
or nitric
blank
and press
auto
zero button.

mode

to

selector
completely

selector

in

read
to

A/DB

285.2

the
clock

nm.

1.0 position
wise.

and

turn

position.
locks
above
(right

into position;
lamp
on turret
instrument

acid

digestion

by

4.9.7

Aspirate
0.5 ppm MATRIX standard
and set readout
0.5 in same manner as for previous
elements.

4.9.8

Adjust
readout to 50 ppm with MA/count selector
inner knob as before with other elements.
Miscellaneous

to
and

Notes

The readout
will
be
million
(ppm)
using

in direct
sample
this
procedure.

parts

per

4.10.2

The calibration
(in terms
of sample
ppm)
cannot
be
considered
linear
over
50 ppm.
If a sample
gives
a
read
out of greater
than
50 ppm,
it must
be diluted
to give
a readout
within
the operating
range.
The
readout
value
must,
in this
case,
be multiplied
by
this
additional
dilution
to give
the
actual
sample
ppm.

4.10.3

Because
dilute
MATRIX
a new
0.5 ppm
standard
weeks
to insure
valid

5.
5.1

Moisture
sample

weight
) - (dry sample
(raw sample
weight)

Sodium,

potassium,

(analyte

weight)

I00

= % H20

Ash
X i00

(ash weight
)
(dry sample
wt)
5.3

deteriorate
rapidly,
prepared
every
two
calibration.

CALCULATIONS

(raw

5.2

standards
must
be
instrument

calcium,

_ %

ash

lithium,

g/ml.)
x (analyte
(sample
g)

or

ml.)

magnesium

= ppm

sample

REPORT

6.1

Moisture/content
shall
0.10%.(when
required)

6.2

Ash content
shall
(when
required)

6.3

Each
alkali
reported
to

and
the

be

be

reported

reported

alkaline
nearest

to

to

the

earth
metal
1.0 ppm.

the

nearest

nearest

contents

0.10%

shall

be

M-R-2
i.
I.i

2.

Percent

This
test method
resin
pickup
of

in

Manufacture

of

Broadgoods

is used
to
broadgoods.

determine

the

"in-process"

EQUIPMENT
Template

2.2

Balance,

graduated

in

(1)

gram

increments

PROCEDURE

3.1

Using
a
untreated
Designate

3.2

Treat
a four
specification.

3.3

Using
the
impregnated
Designate

4.

pickup

SCOPE

2.1

3.

Resin

template,
cut
fabric
roll
this
weight
(4)

foot

a sample
and weigh
as W I.

from
the head
of the
to the nearest
gram.

piece

fabric

of

to

template
cut
a sample
from the
fabric,
weigh
to the nearest
this
weight
as W 2.

the

desired

center
gram.

of

CALCULATIONS
%Resin

Pickup

(W 2 - Wl)/W

i00

where:
weight
fabric,
W 2 = weight
fabric,
W 1

of template
gm.
of template
gm.

- cut

piece

of

untreated

piece

of

treated

cut

the

M-R-3
,

i.i

2.
2.1

Total

Resin

This
method
describes
of
total
resin
solids
EQUIPMENT

AND

2.1.2

Desiccator

2.1.3

Hypodermic

2.1.4

Oven,

2.2.2
3.
3.1

of

Liquid

Solutions

a procedure
content
of

for
the
determination
liquid
solutions

MATERIALS

Equipment.
Balance,

2.2.1

Content

SCOPE

2.1.1

2.2

Solids

analytical,

minimum

syringe,

forced

air

2
(see

ml.

sensitivity

or

0.001

gms.

ml.

6.1)

Materials.
Aluminum
weighing
depth
5/8
inch,

dish,
weight

diameter
approximately

2-3/8
1.4

inch,
gms.

Eyedroppers
SAMPLING
Sample
size.
Unless
of
resin
solids
for

otherwise
specified,
each
determination.

use
one
gram
To
find
the

exac--_ sample
size,
the
formula
i/(total
solids)x(lfiller
content)
will
yield
the
correct
weight
to use.
The
following
table
shall
serve
as
a guide
when
the
anticipated
solids
are
known
(unfilled
only):
ANTICIPATED
20%
30%
40%
50%
60%
70%
80%
90%
100%

SOLIDS

SAMPLE
5.00
3.30
2.50
2.00
1.70
1.45
1.25
i.i0
1.00

When
the
anticipated
solids
are
not
of
solids
at
the
70%
concentration.
are
determined,
conduct
an
additional
correct
3.2

sample

Number
of
determine

known,
Once
test

+
+
+
+
+
+
+
+
+

SIZE,GMS.
0.5
0.3
0.2
0.2
0.2
0.i
0.i
0.i
0.i

run
one
set
the
solids
using
the

size.

determinations.
total
resin

solids

Unless
other
wise
in triplicate.

specified,

PROCEDURE

4.1

weighing.
gram.
The
transferring

Weigh
an aluminum
following
procedure
and weighing
the

dish
to nearest
shall
be used
resin.

0.001
for

4.1.1

Low viscosity
resins
For low viscosity
resins,
especially
resins
using
acetone
as a solvent,
use
a
syringe.
Rapidly
fill
the syringe
and wipe
off
the
outside
tip.
weigh
syringe
and
resin
to nearest
0.001
gm.
Expel
the approximate
weight
of sample
(see
3.1)
from the syringe
into
the aluminum
dish.
Retract
the syringe
piston
and
reweigh
the syringe
to
nearest
0.001
gm.

4.1.2

High
viscosity
resins
For high
viscosity
use
an eyedropper.
Quickly
discharge
the
the aluminum
dish.
Immediately
weigh
the
aluminum
dish
to nearest
0.001
gm.

resins,
sample
into
resin
and

4.2

Spreading
sample.
Tilt
and rotate
the aluminum
dish
spread
resin
over
entire
bottom
of dish.
Warm
the
resin
on a hot plate
if necessary
to accomplish
spreading
see note
6.2.
Add
approximately
6 ml.
of
toluene
to SMR dispersions

4.3

Devolatilization.
Unless
otherwise
specified,
place
samples
in an air circulating
oven
for time
and
temperature
indicated
below,
see note
6.3:
RESIN

4.4

5.1
5.1.1

TYPE

TEMPERATURE,

TIME,

oF

MINUTES

Epoxy
Polyester
Phenolic
phenyl-Silane
Silicones

320
275
275
275
275

+
T
T
T
T

5
5
5
5
5

45
20
60
60
180

SMR

275

60

Dispersions

Reweighing.
desiccator,
and residue
CALCULATIONS

+
T
T
T
T

Calculations

REPORTING
Calculate

Syringe

method

Solids,

wt.

solids

W2 - W1
x

% =
W4 -

W 3

Where:
I0

i00

as

follows:

2
1
2
2
3

_T 2

Remove
dishes
from
oven
and cool
in a
see note
6.4.
Reweigh
each
aluminum
dish
to nearest
0.001
gm.
AND

to

W1 = weight
W2 = weight
w3 = weight
W4

5.1.2

sample
= weight

Eyedropper

of aluminum dish,
gm.
of dish and residue,
gm.
of syringe,
portion
of syringe

gm.,
and

after
sample,

expelling
gm.

method.
w2 - w I

Solids,

wt%

I00

W5 - W 1
Where:
W 5 _ weight

of

dish

and

resin

sample,

gm.

5.2

Reporting.
Unless
otherwise
specified,
round-off
and
report
the average
of three
determinations
to 0.1%.
Triplicate
determinations
should
be considered
suspect
if the
range
from
the
average
exceeds
0.3%
solids.

6.

NOTES

6.1

Oven
requirements.
The oven
should
have
a wattage
range
of between
1200
and 4000 watts,
and an air
flow
rate
between
600 and 1500
feet
per minute
when
measured
at the internal
ports
with
an air flow
meter
(velometer).

6.2

Spreading
sample.
The sample
should
remain
on the hot
plate
only
as long
as is necessary
to make
the resin
liquid
enough
to spread.
A low temperature
hot plate
should
be used,
preferably
lower
than
275_F.

6.3

Placing
placed
opening
closing

6.4

Precautions
in removing
samples
samples
which
have
bubbled
from
should
be taken
to prevent
loss
spattering.

samples
in oven.
All
aluminum
dishes
should
be
in the
oven
at one time.
The
time
required
for
the door,
inserting
aluminum
dish(es)
and
the door
should
not exceed
ten
(I0) seconds.

11

from
oven.
the oven,
of sample

In removing
precautions
from

M-R-4

Specific
Semi

i.

Gravity

Determination

of

Liquids,

Solids,

and

Solids

SCOPE

i.i

Scope.
This
is a method
for the determination
of the
specific
gravity
of liquids,
semi-solids
and solids
which
are neither
water
soluble
nor
appreciably
absorb
water
at 25C.

i.i.i

Method
I.
A
flow
readily

1.1.2

Me_hod
25_C.

1.2

2.

II.

Equivalent
I and II

procedure

AND

Gay-Lussac

2.1.2

Pycnometer,

Hubbard

2.1.3

Analytical

2.1.4

Water

2.1.5

Thermometer,

2.1.6

Forceps,

2.1.7

vacuum

bath,

semi-solids

and

procedures
described
to ASTM-DI963-61.

that

solids

in

at

Methods

74C.to
6

Type

minimum

capable

of

sensitivity

maintaining

79C.in

25

0.1F.

0.0001
_

gm.

0.2%C.

intervals

inch

chamber

Materials.
Distilled

water,

2.2.2

Lint

cloth

2.2.3

Abrasive

3.1.1

materials

Type

balance,

2.2.1

3.1

for

and

Equipment.
Pycnometer,

3.

liquids

MATERIALS

2.1.1

2.2

for

Method.
The
are equivalent

EQUIPMENT

2.1

procedure
at 25C.

free

paper,

recently

boiled

fine

SAMPLING
Sample

Size.

Method
I.
The
the pycnometer
determinations.

sample
should
be
for the required

12

large
number

enough
of

to

fill

3.1.2

Method
II.
For semi-solid
materials
there
should
be
sufficient
sample
to fill
the pycnometer
one-half
full
for the required
number
of determinations.
For
solid
materials
there
should
be enough
sample
for the
required
number
of specimens
approximately
3/8 x 3/8
x 1 inch,
or an equivalent
volume.

3.2
4.

Number
conduct

of determinations.
two determinations

Unless
otherwise
on each
sample.

specified,

PROCEDURE

4.1

Calibration.
Calibrate
the

If the pycnometer
needs
pycnometer
as follows:

the pycnometer
gm.
(Wl).

to

temperature

see

and

6.1

4.1.1

Bring
0.0001

4.1.2

Fill
the pycnometer
(in such
a manner
as to prevent
the entrapment
of air bubbles)
with
cooled,
just
previously
boiled,
distilled
water
at a temperature
of
about
20C.
Insert
the stopper,
taking
care
that
no
bubbles
are trapped.

4.1.3

Immerse
constant
minutes).

in the water
temperature

room

cleaning,

weigh

bath
at 25 + 0.1C.until
is attained-(approximately

Blot
the meniscus
of water
flush
with
the surface
of

4.1.5

Remove
the pycnometer
from
the water
bath
and
wipe
dry with
a clean,
lint
free
cloth.
Cool
the
pycnometer
slightly
to prevent
loss
of water
through
capillary
and weigh
to 0.0001
gm.
(W2).
Method

4.2.1

with

a viscosity

4.2.1.1

Fill
a clean,
dry
the sample,
taking
of air bubbles.

4.2.1.2

Proceed

4.2.2

4.2.2.1

so

that

it

is

I.

Materials

the

the bore
stem.

20

4.1.4

4.2

in
the

to

as

weight

Material
flows
40 stokes.

Gay-Lussac
care
to

described
as

of

in

40

stokes

type
prevent

4.1.3

or

less.

pycnometer
with
the
entrapment

- 4.1.5,

recording

W 3.
readily

but

viscosity

is

9reater

than

Fill
a clean,
dry Hubbard
type
pycnometer
with
the
material
to be tested,
taking
care
to prevent
the
entrapment
of air bubbles.

13

4.2.2.2
4.3

Proceed as described
weight as W3.

Method
degrees

II.
C.

This

method

in
is

4.1.3
for

- 4.1.5

recording

semi-solids

at

the

25

4.3.1

Place
the
sample
in a clean,
dry Hubbard
type
pycnometer
and fill
about
one-half.
If the
sample
is
a solid,
use
a specimen
approximately
3/8 x 3/8 x 1
inch
or a sample
of approximately
this
volume.
Smooth
the
surface
on molded
or laminated
specimens.

4.3.2

Bring
the
temperature

pycnometer
and then

and
its contents
to room
weigh
with
stopper
to 0.0001

gm.

(w3).
4.3.3

5.
5.1
5.1.1

Proceed
sample
weight

as described
is porous
or
as W 4.

CALCULATIONS

AND

in 4.1.3
powdered,

- 4.1.5,
see 6.2),

(if the
recording

the

REPORTING

Calculations.
Calibration.
follows:
K

Calculate

the

pycnometer

constant

as

_ W 2 - W1

where:
K = pycnometer
W 1 = weight
W 2 = weight
W 3 = weight
W 4 = weight
water,
5.1.2

Method

I.

of
of
of
of
gm.

Calculate

constant
pycnometer,
pycnometer,
pycnometer,
pycnometer,

specific

gm.
plus
plus
plus

gravity

water,
gm.
material,
gm.
material,
plus

as

follows:

W 3 - w I
Specific

gravity

where
5.1.3

Method

symbols
II.

are

specified

Calculate

in

5.1.1

specific

gravity

as

follows:

W 3 - W 1
Specific

gravity

=
W 3 + K

where

symbols

are

specified

14

in

5.1.1

- W 4

NOTES

6.1

Cleanin 9.
viscosity

6.2

Powdered
or porous
materials
If the material
is
powdered
or porous,
add sufficient
distilled
water
to
cover
the
sample.
The pycnometer
with
water
and sample
should
then
be placed
in a vacuum
chamber
and the
pressure
reduced
almost
to the point
of boiling
the
water,
allow
to remain
at this
point
for approximately
20 minutes
then
proceed
to 4.1.2

See
the
tubes.

cleaning

procedure

15

outlined

for

M-R-5
,

Viscosity

Determination

by

the

Brookfield

SCOPE

i.i

This
is
liquids

1.2

Also
included
is the Brookfield
Thermosel
is designed
for measuring
viscosities
at
over
a range
of 100_F
to 500_F.
(Method

2.

Methods

a method
for the
using
a Brookfield

EQUIPMENT

AND

determination
Viscometer.

of viscosity
(Method
I)

of

System
which
temperatures
II)

MATERIALS

Equipment
Brookfield
Viscometer,
both methods).

Model

2.1.2

Thermometer,
(for Method

range
I).

to

2.1.3

Water
(for

capable
I).

2.1.4

Thermo-container

3.
3.1

bath,
Method

74

and

of

RVF

79

in

with

0.1F.

maintaining

controller

77 _

(for

spindles

(for

divisions

0.5F.

Method

II).

SAMPLING
Materials
having
ingredients
which
tend
to
should
be throughly
mixed
before
sampling.
representative
one-quart
sample
is required
determination.

4.

PROCEDURE

4.1

Method

4.1.1

Sample
conditioning.
Place
approximately
one quart
of sample
in a round
container
with
a sufficient
diameter
and depth
so that
the spindle
will
not
be
closer
than
one inch
at any point
to the
container.
Place
the sample
in a water
bath
and condition
to
77 + 0.5F,
unless
otherwise
specified.
Determination
Level
screws

4.1.2.2

settle
A
for each

of

viscosity.

the viscometer
by
and bubble
level.

means

of

tripod

Select
a spindle
consistent
with
expected
viscosity
and screw
it into
the viscometer
using
counter-clockwise
rotation.

16

4.1.2.3

Immerse the spindle

into the
depth where the notch on the
with the liquid
level.

4.1.2.4

Unless otherwise
specified,
rotate
the spindel
at
20 RPM, depressing
the clutch.
Release the clutch
after
one revolution
and read the outer dial
as
soon as equilibrium
is established.

4.1.2.5

If dial
reading is less than i0, repeat
a smaller
numbered spindle;
if greater
repeat using a larger
numbered spindle.
readings.

4.1.2.6

Turn viscometer
off,
spindle
thoroughly.
Method

liquid
to the
stem is even

test using
than 90,
Make two

remove sample and clean

II

Set Up viscometer
Set up
the viscometer
stand
connecting
the black
31/4 inch
coupling
post
to the
rack.
Screw
both
posts
into
the base
leaving
the cock nut
loose.
Put
the three
(3) leveling
screws
into position
on the
base.
Attach
the viscometer
to the stand
inserting
it into
the clamp,
and position
it reasonably
level
and centered
between
the stand
legs.
Lock
the
posts
tight
to the stand
base
with
the lock
nut on
the coupling
post.
Raise
the viscometer
to the
highest
position
on the stand.
Check
the power
switch
off and plug
the viscometer
power
cord
into
a
15 amp.,
115 volt,
60 cycle
A.C.
electrical
service.

4.2.2

Set Up Controller
Set controller
on a level
surface
adjacent
to thermocontainer.
Insert
the male
plug
(three-prong)
from
the thermo-container
braided
cord
into
the socket
on
the back
of the controller
(turn
and lock
connection).
Insert
the
four
inch
stainless
steel
probe
(Resistance
Thermometer)
into
the hole
in the
thermocontainer
located
directly
above
the braided
cord.
Plug
the other
end of the probe
into
the
connector
located
on the back
of the controller.
To
remove
probe,
depress
spring
clip
and carefully
slide
probe
out.
The procedure
should
not be followed
i_
the thermo-container
is at a temperature
above
100_F.
NOTE:
If the
_ainer
and
thermo-container

4.2.3

probe
is NOT
inserted
in
the contro--l-[er is turned
will
be destroyed.

Familiarization
The operator
should
alignment
procedure

become
familiar
so that
he can
17

the
on,

with
safely

thermothe

the
align

and

operate the system at elevated

temperatures.
The
system is designed to operate
in the temperature
range from ambient to a maximum of 500F. (260C.).
Precise control
of _est sample temperature
is
possible
in the i00 _ to 500_F. range with accuracy of
+ 0.5% of the controller
set point.
That is;
at
500F set point,
the test sample temperature
will
be
held to + 2.5F.
4.2.4

Determination

of

the

Viscosity

4.2.4.1

Remove

insulating

4.2.4.2

Raise
stand.

the

4.2.4.3

Remove
tool,

the sample
chamber,
and place
it in the

4.2.4.4

Using
a syringe,
graduate
cylinder
or other
suitable
measuring
device,
pour
into
the sample
chamber
the
volume
of liquid
sample
designated
on the data
sheet.
DO NOT OVERFILL!
The liquid
level
should
intersect
the spindle
shaft
at a point
approximately
1/8 inch
above
the upper
"Concical
Body"
- "Spindle
Shaft"
Interface.

4.2.4.5

Using
the
extracting
tool,
put the
loaded
chamber
back
into the thermo-container.

viscometer

cap
to

and

the

spindle.

highest

level

on

the

using
the extracting
auxiliary
holder.

Lower
the viscometer
and align
the thermocontainer.
Insert
the spindle
into
the liquid
in the chamber
and couple
it to the viscometer
(observe
left
hand
thread).
4.2.4.8

Replace

the

insulating

cap.

4.2.4.9

Set the control

knob
on the controller
to
the desired
set point
temperature
at which
viscosity
measurements
are to be made A
The Controller
scale
reads
directly
in the 0-500_F.
range
with
lF.
increments.

4.2.4.10

For temperatures
between
i00 and
250F.,
set the control
knob
initially
20F.
LOWER
than
the
desired
equilibrium
temperature
(for %-emperatures
between
250 and 500F.,
set control
knob
on
temperature
desired.)
This
will
prevent
temperature
overshoot
in the thermo-container
and reduce
the
lag
time
to reach
spindle,
chamber
and
sample
temperature
equilibrium.
As the temperature
rises
in the
thermocontainer,
the power
output
level
light
will
go from
full
ON to dimmer
and then
full
OFF.
When
the
18

temperature
in the thermo-container
has dropped to
the initial
set point
(after
about 5 minutes),
the
output level
light
will
start
to glow.
Advance the
set point knob in consecutive
steps up to the desired
setting.
About 30 minutes should be allowed
for the
system to come to
temperature
equilibrium.
EQUILIBRIUM CONDITIONS WILL BE DENOTEDBY A STEADY
GLOWOF THE OUTPUT LEVEL LIGHT ON THE CONTROLLER,
STABILIZED DEVIATION METERAND BY A STEADY DIAL
READING ON THE VISCOMETER.
4.2.4.11

Turn ON the viscometer

and leave it running
during the equilibrium
period.
The rotating
spindle
provides
agitation
which reduces
temperature
equilibrium
time and temperature
gradients
within
the test sample.

4.2.4.12

Turn on the
above prior

4.2.4.13

After
the thermo-container,
spindle,
chamber
and test sample has reached temperature
equilibrium,
viscometer
readings
are taken at different
speeds and
viscosities
are obtained
using the ranges supplied
on
the data sheet.

5.
5.1

controller
to taking

and refer
to 4.2.4
viscosity
measurements.

CALCULATIONSAND REPORTING
Calculations

for

Method

Calculate

viscosity

Viscosity

in

Where:

R
F

=
=

1
2
3
4
5
6
7

No.

follows:

centipoise
average
factor
20

Spindle

as

RPM

= RF

dial
reading
from
the following
i0

RPM

chart

4 RPM

2 RPM

Factor

Factor

Factor

Factor

5
20
50
I00
200
500
2,000

i0
40
i00
200
400
1,000
4,000

25
i00
250
500
1,000
2,500
I0,000

50
200
500
1,000
2,000
5,000
20,000

19

5.2

Calculations

Speed
(RPM)
i00
50
20
i0
5
4
2.5
2
1
0.5
5.3

for

Method

II

Spindle
21

27

5
i0
25
50
i00
125
200
250
500
IM

25
50
125
250
500
625
IM
1.25M
2.5M
5M

Number
28

50
I00
250
500
IM
1.25M
2M
2.5M
5M
10M

Reportin
9 for
Both
Methods
I and
II
Report
viscosity
in
centipoise
or
poise
(as
appplicable)
to
three
significant
figures.
results
should
be
considered
suspect
if the
duplicate
readings
exceeds
0.2%.

2O

29
i00
200
500
IM
2M
2.5M
4M
5M
10M
20M

The
test
range
for

M-R-6

Gel

Time

Determination

in

an

Oil

Bath

of

Liquid

Resins

SCOPE
Scope.
This
determination
an
oil
bath.
Method

i.i.i

I.

phenolic
Method
silicone

1.i.2

1.2

2.

method
describes
of
gel
time
by

This

method

is

two
procedures
immersing
the

in

general

for
sample

applicable

the
in

to

resins.
II.

This
resins.

Equivalent
D1472-62.

methods.
Method

gel

for

method

method

in

general

Method
I is
is equivalent

II

Dow

is

Corning

2106

applicable

equivalent
to
the

to
Dow

to

ASTMCorning

resin.

EQUIPMENT

2.1
2.1.1

Equipment.
Jar,
Pyrex,
6-inch
similar
container
Stirrer,
Test
II,

diameter,

electrical

tubes;
25 mm.

with

Method
i00
mm.

I,

8-inch

height,

or

rheostat
13mm.

120

Method

mm.;

2.1.4

Stirring
rods:
Method
I, wire,
.06
diameter
with
0.30
to
0.40
inch
loop
stem;
Method
II,
glass
rod,
i/4-inch
flattened
paddle
of
0.5
to
0.6
inch
end.

to
.08
inch
perpendicular
to
diameter
with
diameter
at
the

2.1.5

Silicone
equivalent

i00

Clamps

oil,

and

Dow

2.1.8

Thermometer,

20

2.1.9

Timer
Balance,

2.l.ll

Heater,

F-I-D173,

cs.

ringstand

Thermoregulator
sensitive
to

2.1.10

Corning

minimum
250

W.,

with
lF.
to

range

600

to

F,

lF

sensitivity
immersion

control-

intervals

0.1
type

21

480F.,

gm.

or

SAMPLING
Sample
size.
determination.
determination.
3.2

4.1

Method
I requires
2 + 0.i
Method
II requires--12
+

Number
of determinations.
run duplicate
determinations.

Unless

gm.
0.i

otherwise

for
gm.

each
for each

specified,

PROCEDURE
Preheatin9
for Method

bath.
Preheat
I or to 480 +

the oil bath

to
2 F. for Method

338 + 1.5F.
II. --If

necessary,
add oil to brYng
the oil
level
to within
1
inch
of the top.
Using
an electric
stirrer,
stir
bath
thoroughly
and continually
for
at least
5 minutes
prior
to testing
and throughout
the test
to assure
even
heat
dissipation.
Method

I.

Weighin
9 sample.
Weigh
a 2 + 0.i gm.
sample
into
a
test
tube.
Place
the wire
stirrer,
looped
end down,
into
the test
tube.
4.2.2

Immersion.

Lower

the

test

tube

into

the

holder

to

sized
to hold
the tube
loosely
suspended
by the
shall
be positioned
so that
the rim of the test
1.5 + 0.25
inches
above
the surface
of the oil.
stopwatch
is started
immediately
upon
immersion.

be

rim and
tube
is
The

4.2.3

Stirrin 9 Sample.
vertical
strokes,
for the
first
40
at the
rate
of 4

4.2.4

End
point.
The end point
is defined
as the time
when
there
is no motion
of the test
tube
in relation
to
the stirrer,
i.e.
when
the tube
moves
up and down
with
the stirrer.
CAUTION:
Be sure
the holder
is
loose
enough
to permit
this.
Method

II.

Weighin 9 sample,
test
tube.
Place
the test
tube.
4.3.2

Agitate
the
resin
with
rapid
with
not more
than
1/4 inch
strokes
seconds.
After
40 seconds,
agitate
strokes
every
5 seconds.

weigh
a 12 +
the glass
ro_

0.I gm.
, paddle

sample
down,

into
into

Immersion.
Lower
the test
tube
into
the holder
so
that
the rim of the test
tube
is 1.5 + .25 inches
above
the
surface
of the oil.
Tighten
the holder
to
prevent
slippage
of the test
tube.
The
stopwatch
is
started
immediately
upon
immersion.

22

4.3.3

Stirrin
9 sample.
Stir
the sample
by twisting
glass
rod.
Do not lift
the rod up and down.
Continue
turning
the paddle
for three
minutes.

4.3.4

End point.
The end point
is d_fined
the glass
rod can be turned
90
and
considerably
upon
releasing.

5.1

CALCULATIONS

AND

the

as the time
when
will
spring
back

REPORTING

Unless
otherwise
specified,
report
the
average
of two
tests
in minutes
and seconds
to the nearest
second.
Test
results
should
be considered
suspect
if the range
for duplicate
determinations
exceeds
i0 seconds
for gel
times
less
than
6 minutes
or 20 seconds
for gel
times
greater
than
6 minutes.

23

M-R-7

Gel

Determination

i.i

This
test
method
is
undergo
gelation
at
temperature
(Option

Liquid

Resins

at

132C

applicable
to liquid
132 v _ I_C.
(Option
B).

resins
which
A) or any other

EQUIPMENT

2.1

G.E.
gel
(Sunshine

2.2

Test

2.3

Glass

2.4

Thermometer
temperature

2.4.1

time
meter
Scientific

tubes

18

stirring

Option

to

1/4"

lC.

for

checking

bath

Monochlorobenzene,

2.4.1.3

Water

2.4.2.1

7-1/8"

accurate

2.4.1.2

Option

Co.)

mm.

rods

Voltage

2.4.2

Instrument

150

2.4.1.1

3.

of

SCOPE

2.

Time

varied

for

heating

bath

boiling

point

132C.

condenser
B

Thermostatically

controlled

oil

bath

PROCEDURE

3.1

Place
solvent
2" immersion

3.2

Turn
on cooling
monochlorobenzene.

3.3

Heat
the bath
by either
boiling
the
or circulating
oil through
a heating
wait
for an equilibrium
temperature

3.4

Place
5 to 6 cc. of
resin
in a clean
test
clean
stirring
rod with
its attached
holder
into heated
bath.
Couple
the stirring
rod
torsion
motor.
Turn

on

Gelation
timer.

the

or oil in the large

beaker
depth
of the test
tube.

test

occurs

water

to

condense

to

maintain

the

monochlorobenzene
coil
in the bath.
to be established.
tube,
add
a
and
insert
to the

meter.
when

the

buzzer

24

rings

and

turns

off

the

Notes

(Cautions):

Monochlorobenzene
ventilation.
3.7.2

Keep
1.027

3.7.3

Adjust

3.7.4

Maintain

3.7.5

Keep

torsion
inches

is

wire
free
from
kinks
between
vise
jaws.

actuating

stirring
test

a toxic
solvent,
use
with
rubber
gloves.

Handle

tube

switch
rod
in

the

to
in

25

maintain

approximately

the
bath

and

with

center
when

gap

1/4".
of

not

adequate

the
in

test

use.

tube.

of

M-R-8

RDS-ViScosity
Dynamics

of

Various

Temperatures

With

Rheomatic

Spectrophotometer

SCOPE
This
method
describes
a procedure
for
the
of
resin
viscosity
at various
temperatures
Rheometric
Dynamics
Spectrometer
(RDS).

EQUIPMENT

AND

2.1

Rheometrics
plates,
and

2.2

Oven,

2.3

Balance,

2.4

Stopwatch

2.5

Silicone

2.6

Tongue

2.7

RDS

3.

SAMPLE

MATERIALS
Dynamic
operators

forced

Spectrometer
manual

with

50

mm.

parallel

air

0.I

gm.

accuracy

Release

paper

depressors
systems

3.1

Raw

3.2

Powders

3.3

Mixed

manual

resins

4.

PROCEDURE

4.1

General

4.1.1

determination
using
the

require
require

resins

(I)

three

two

Parameter

range

200

oz.

(3)

require

Test

Temp.

one

minimum

oz.
(2)

minimum
oz.

minimum

Capabilities
o

to

395

C.

linear

stepwise

100

radians/sec.

heating

profile
4.1.2

Strain

4.1.3

Frequency

4.1.4

Physical

4.2

range

range

Power

4.2.2

Select

is

separation

Instrument

4.2.1

is

Set
up
the

Up

to

100%

0.01
of

(Method

instrument
following

to
plates

(gap)

is

0.01

to

5.0

to

45

mm

I)

and

adjust

starting

28

air

pressure

front

panel

parameters:

psi.

4.2.2.1

Starting

temperature

4.2.2.2

4.2.2.3

Frequency

4.2.2.4

Mode

cure

4.2.2.5

Test

Parallel

4.2.3

Strain

Select
follows:

50

(per

rate

BMS
I0

parameters

time

140

4.2.3.2

Sweep

rate

2.0C./min.

4.2.3.1

min./test

4.2.4.1

Gap

4.2.4.2

Radius

4.2.5

Press

0.50
-

25.00

mm.

"Plotter"
-

4.2.5.2

X-axis

max.

140

4.2.5.3

Y-axis

min.

lEO

4.2.5.4

Y-axis

max.

IE5

4.2.5.5

*-yes,

no

Press

for

all

other

quantities

"Print"

*,

',

4.2.6.2

all

4.2.6.3

4.2.7

as

ram.

min.

.6 . 1

responses

Test"

X-axis

4.2

typed

min.

4.2.5.1

4.2.6

by

point

"Geometry
-

8-256)

plate

operational

BMS

sweep

Total

Press

8-256)

(per

4.2.3.1

4.2.4

30C.

others

Time

Plotter

"

and
and
K

Torque
-

yes*

no

temperature

are

automatically

selected.

Paper

4.2.7.1

Insert

and

paper

4.2.7.2

Zero
lower
left
and
chart
by
adjustment
controls
respectively.

type

46-6210

upper
right
of the
zero

27

(5

cy.

corners
of
and
venier

in.)

each

4.2.8

Sample

Insertion

4.2.8.1

Parallel
plates
force
normal)

4.2.8.2

Sample
material
should
be
placed
on plates
preheated
to
70C.
and
allowed
to
flow
as
the
is
set.
The
_lates
are
then
allowed
to
return
to
approx.
30vC.

4.2.8.3

Using
the
is allowed
(% torque
overload).

4.2.9

single
sweep
to
equilibrate
is monitored

Material
Testing
Using
the
following
Sequence:

4.2.9.1

Temperature

4.2.9.2

Mode

Cure

4.2.9.3

Test

Parallel

4.2.9.4

4.2.9.5

Rate

4.2.9.6

START

4.2.9.7

Temperature

4.2.10

Strain
-

4.2.10.2

Reset
Plates

5.

CALCULATION

5.1

Report
by
the

5.2

Attach
(see

may
AND

(>10%
zero.

gap

mode,
the
resin
viscosit_
for
2-3
minutes
at
30_C.
to
prevent
input

"Cure

Mode"

is

initiated

by

30C.

Plate

rad./sec.

240C.

Viscosity
of
the
resin
range
will
be plotted
end
of the
test,
shut
Temperature

contact
set
to

50.00

i0.00

4.2.10.1

4.2.11

are
brought
into
and
the
micrometer

be

sample
over
the
temperature
and
printed.
At
the
desired
down
is as
follows:

30C

cleaned

by

soaking

in

acetone

REPORTING

RDS
viscosity
at various
applicable
specification.
completed
para.
4.2.9)

graph

with

28

all

temperatures

pertinent

required

information

M-R-9

i.I

Liquid
and
Mol
Weights

Gel

Determining

This
procedure
describes
methods
for
conducting
chromatogaphy
and
gel
permeation
chromatography
phenolic
resins.
It
analyzes
the
molweight
of
contituents.
EQUIPMENT

AND

2.2

M-Styragel
(USE

Syringe,

2.4

Gas

2.5

Needles

2.6

Scissors

2.7

Centrifuge

2.8

Centrifuge

2.9

Graduated

i0

tight

cc.

tubes,

50

ml.

cylinder,

2.11

Beaker

2.12

Millex-SR

2.13

Membrane

2.14

2.15

Helium

2.16

Nitrogen

gas

PREPARATION

OF

Weigh
vial

3.1.2

Add

columns,

syringe,

Balance,

3.1.1

UV

detector

and

i00

A,

cc.

2.10

Resin

with
manual.

WATER)

2.3

&

SP8000
operators

chromatography

NO

liquid
of

MATERIALS

HPLC
Spectra-Physics
autosampler,
and

3.1

Chromatography

SCOPE

2.1

3.

Permeation

i0

Analytical,

filter
TFE

ml.
Sensitivity

units,

filter

0.001

gm.

0.5

paper,

tetrahydrofuran,
(zero

disposable

0.45

UV

grade)

gas

SAMPLE

SOLUTION

grade,

THF

Samples
out
0.25
(labeled)
I0

ml.

100%

+
-

0.02

THF

gm.

into

of

the

29

resin

vial

into

glass

500

Resin

Mixes

Weigh
out
centrifuge
3.2.2

Add
tube

3.2.3

Agitate

3.2.4

Centrifuge

3.3

25.0

3.3.2

Weigh
tube

3.3.3

Add

3.3.4

Agitate

3.3.5

Centrifuge

100%

for

gm.

THF

of

sample

into

into

the

centrifuge

minutes

2-5

25

minutes

at

appropriate

speed

ml.

approximate
_

100%

0.5

gm.

THF

into

15-50
for

1/2"
of

sample

the

1/2"
into

squares
centrifuge

centrifuge

tube

minutes

2-5

minutes

at

appropriate

speed

Preparation

3.4.2

Degas

3.4.3

Decrease

solvent

with

(1-2

He
the

INSTRUMENT

D:

6.0

for

Solvent

Date

into

out

Filter
filter

1/4
flow

liters)

to

1/2

rate

by

hour
before

PROGRAMMING

Assignment
00:00:00

month
day
D - Display
4.2

of

15-50

sample

3.4.1

4.1

0.02

Prepregs
Cut

4.

ml.

for

3.3.1

3.4

3.0
+
tube

Report
R:I
REPORT
RENAME:
SAMPLE:
SAMPLE
SAMPLE
OPERATOR
DETECTOR
DETECTOR

00:00:00
hour
min.

year

File
report
FILE

sec.

Assignment
file
1

VOLUME:
CONC.:
NAME:
i: UV.
2:
;

i0 L
20 MG-ML
(your
254NM

name)
0.i

AUFS

3O

using

(high
running

0.45

flow)

um.

TFE

COLUMNTYPE; SIZE: 2xI00A,

MOBILE PHASE: Isocratic

2X500A,

A: ;
B: ;
C: THF
END OF DIALOG
4.3

Parameter
S:I

File

parameter

PARAMETER
RENAME:

file
SET:

2.
3.
4.
5.
6.
7.
8.
9.
i0.
ii.
12.
13.
14.
15.
16.
17.

LINK:
;
INITIAL
DELAY:
1
RUN
TIME:
30
NO.
OF
CYCLES:
6
FLOW
RATE:
2.00
FLOW
MODE:
QI
TEMPERATURE:
35
MOBILE
PHASE
FILE:
1
REPORT
FILE:
1
GRAPH
FILE:
1
DATA
SYSTEM
FILES:
1
CHAN
i:i
CHAN
2:
;
FULL
TIME:
1
FLUSH
TIME:
1
REPETITIONS
PER
VIAL:
TIMED
EVENTS:
XX

END

OF

4.4

Assignment

Graph
G

DIALOG
File

-- 1

Assignment
graph

file

GII
GIE5
GII5
GVO.5
XX
EXIT

4.5

GRAPH

Mobile
M

MOBILE

Phase
2

mobile
PHASE

EDIT
File

Assiqnment

phase
FILE

file

31

-STYRAGEL

WHICH SOLVENTS? C
END OF

DIALOG

MI2
M;1
MOBILE

PHASE

WHICH
END

FILE

SOLVENTS?
OF

1
C

DIALOG

MII

4.6

Data

File

Manipulation

FII

Data

system

nm

gpc-QC

CH
OD
IX
RN
NR
PW
PT
MA
FD
VE
FILE

001
002
001
001
001
015
0150
5000

RN
FS
PP
NM
CH

001
000
004
GPC-QC
001

(file

center)

001

FF
APO
FD
VE
FILE
AR
TP

file

function

NR
MS
TI

001
0
000

PW
MA
RO

015
5000
000

PT
IM

0105
00

OD

002

IX

001

SN

000

file

001
0
1

IR
NP

METHOD

0
0

DC
NT

0
0

NZ
AA

0
0

FX
XD

XX

32

0
0

EC
HD

0
0

4.7

Review

File

Values

S-I
PARAMETER

SET:

INITIAL
DELAY:
1 RUN TIME:
30 NO. OF CYCLES:
6
FLOW
RATE:
2.00
FLOW
MODE:
Q1
TEMPERATURE:
35
MOBILE
PHASE
FILE:
1 REPORT
FILE:
1 GRAPH
FILE:
1
CHAN
i:i
FILL
TIME:
1
FLUSH
TIME:
1
REPETITIONS
PER VIAL:

R-I
-VOL : I0 UL
CONC:
20 mG-ML
(your
name)
FLOW
RATE :
2.0
PRESSURE:
0000
COLUMN:
2xl00A,
2X500A,
--STYRAGEL
CHAN
i:
U.V.
254NM
0.i
A FS
MOBILE
PHASE:
ISOCRATIC
MOBILE
PHASE
FILE
1
i00.0%
C
G-I
GRAPH
FILE:
1
Channel
1:
Plot
Var. :
DET.
1
Chart
Polar:
L ATTN.:
5
Zero:
0%
Inten.:
Channel
2:
Inoperative
M-I
Mobile
Phase
File:
1
i00.0%
C
5.
5.1

Spd.:
5

0.5

PROCEDURE
HPLC:

Start-up

5.1.1

Turn

5.1.2

Adjust
the
75 psi.

5.1.3

Turn
on
position.

5.1.4

Turn
on the Spectrophotometric
is ".4 amp."
Set range
at 0.i

5.2

NO :

on

Automatic

5.2.1

Be

5.2.2

Keep

He

and
He

N2
pressure

both
switches,
Set wavelength

to

i0

psi

wavelength
at 254

and

N 2 pressure

Drive
nm.

Detector,
AUF

at

"on"

make

Operation

sure
He

both
purge,

detector
the

and
solvent

33

auto
with

sampler
low

flow

are

to

on

rate

sure

it

5.2.3

Type AT1
DID
FMI
MI1
SB1

5.2.4

Use the inner knob on the detector

range selector
to
adjust
the read out to -1200 (detector
signal)
or
type GB and adjust
the baseline
1 inch to the left
margih-_, then type GX to start
plotting.

5.2.5

Fill
one gas tight
syringe
with sample solution
and
the other one with THF; attach
each syringe
to one
Miller-SR
filler
unit.

5.2.6

Place the injector

handle in the "LOAD" position
type S_O0
to open the injector
sample solenoid.

5.2.7

Inject
1 cc. of THF to flush
the injector
inject
1 cc. of sample solution
and type
the sample solenoid.

5.2.8

Wash the syringe

next sample.

5.2.9

After
LC, inject
automatically,
handle in the "LOAD" position
injecting

5.2.10

Check

with

the

THF twice;

loop, then
S__KK
to close

fill

replace
and

it
the

repeat

with
injector

the

operation.
the

condition

by

typing:

E- elapsed
time
since
injection
T- present
oven
temperature
P- pressure
C- current
% C at ternary
valve
DIDdector
signal
F- flow
rate
5.3

Calibration
Run

5.3.2

Run molecular
weight
weight
vs. retention
Weight

blank

running

5.3.1

Mole

a THF

(before
in

sample

order

to

standards
time
on

Standards:

M.W.
Compound
93 Toluene
570 Polystyrene
955
"
3600
"

34

plot

solutions)
the

and
graph

and

baseline

plot
molecular
paper

the

5.4

Termination

5.4.1

Type

EX

to

end

5.4.2

Type

SX

to

stop

5.4.3

Shut

down

all

run
parameter
gas

set

flows

35

M-R-10
i.

Purity

of

Solvents

by

Chromatography

SCOPE

i.i

2.

This
method
describes
a procedure
for routinely
checking
purity
of solvents
through
the use
of
chromatography.
It is similar
to ASTM-D3792.
EQUIPMENT

2.1

AND

gas

MATERIALS

Equipment

2.1.1

Gas Chromatograph
with
Thermal
Conductivity
DetectorHewlett-Packard
Model
810 or any other
with
similar
capability
and performance
and operators
manual
(preferably
equipped
with
an integrator).

2.1.2

Two 6 feet
by 1/8 inch
with
packing
of Porapak
Associates)

2.1.3

Hamilton
microliter

2.1.4

Pipettes,

10.0

2.1.5

Air

sample

2.2

tight

syringe
701N
capacity)
ml,

stainless
Q. 80/100

or

1.0

equivalent

ml,

0.i

steel
mesh.

columns
(Water

(i0

ml

bottles

Materials

2.2.1

Hi@h
Purity
Solvents
Pure
samples
of each
type
of solvent
to be checked
as well
as any suspected
impurity
solvents
should
be obtained.
Nanograde
purity
is good.
For acetone,
Fisher
A-20
is recommended.

2.2.2

Distilled

3.

Water

SAMPLING

3.1

Representative
Sample
The
sample
of solvent
to be
in3ected
into
the G.C.
should
be representative.
Exercise
due care
in certain
cases
where
the
test
solvent
has
a constantly
changing
make-up.

3.2

Number
of Determinations.
impurities,
make
at least
to check
accuracy.

4.
4.1
4.1.1

When
quantifying
2 runs with
the

solvent
test
samples

PREPARATION
Column
If
to

Conditioning
columns
are new they
should
be
use
according
to manufacturer's
38

conditioned
instructions.

prior

4.1.2

Prior
to sample
injection,
the column
should
be
clear
of any contaminates
from
any previous
injections.
An isothermal
run of about
225C.
for 1/2 hour
will
clear
the column
of most
contaminates.
Care
should
be
exercised
that
the column
temperature
does
not
exceed
the maximum
rated
temperature
(250 _ C.)
since
the
column
packing
Porapak
Q will
start
to degrade.
This
purging
of the column
should
be done
either
with
the
columns
disconnected
from
the thermal
conductivity
detectors,
(Bridge
current,
off)
or with
the T.C.
temperature
well
above
the column
temperature
if the
columns
are connected.
This
will
insure
that
material
coming
out of the column
will
not condense
on a cooler
T.C.
filament.
All other
recommended
precautions
and
procedures
concerning
column
care
contained
in the G.C.
operating
manual
should
be followed.

4.2

Reference
Sample
Preparation.
Various
reference
samples
of pure
solvents
as well
as samples
containing
known
percentages
of "impurity"
solvents
should
be made
up and stored
in air tight
bottles.
These
reference
samples
will
be run later
to produce
Chromatograms
for
comparison
to test
solvents.
The analysis
at hand
will
dictate
what
"impurity"
solvents
to use
in the
reference
sample
and in what
percentages.
For example,
if the
quality
of the
recycled
acetone
obtained
from
distilling
common
pre-preg
systems
is to be checked,
the main
impurities
might
be methyl
cellosolve,
toluene,
methanol,
and maybe
some water.
Therefore,
reference
samples
of
pure
acetone
and 1%, 2%, 3%, 5%, and 10% by volume
of
these
impurities
in acetone
would
probably
be desirable.

5.1

Run Conditions
Although
run conditions
the particular
analysis,
the conditions
be close
to those
used
for common
low
analysis
(acetone,
etc.).
If no idea
nature
8r percentages
is known,
from
50 -195
C. is a good
place

5.1

.I

Helium
Flow
- Pre-set,
columns,
30-40
ml./min.

5.1.2

Main
Power,
drive,
oven
temp.
switch

5.1.3

Program

5.1.4

Oven

5.1.5

Bridge

5.1.6

Detector

a temperature
to start.

equal

on

"A"

and

"B"

oven power,
recorder
power,
chart
control,
bridge
switch,
detector
- all on.

Selector

Cover

will
vary
with
listed
below
will
boiling
solvent
of contaminate

Isothermal

- Automatic

Current
(T.C.)

200

milliamps

Temperature
37

200C.

program

5.1.7

Injector

5.1.8

Oven Temperature

5.1.9

Chart

5.1.10
5.2

Temperature

Speed

Attenuation

- 150C.

1.0
-

Sample
Injection
will
be quiet
and

- 195C.

16

inch/min.
(initially)

The
integrator
without
drift

and recorder
baselines
before
each
injection.

when
both
baselines
are stable,
10.0
injected
into
column
"A".
The
chart
marked
at the
injection
point.
From
to the maximum
point
of the air peak
(retention
time
for unabsorbed
gas).

ml.
of air is
is immediately
this
injection
in minutes
is

point
Tm

After
baseline
has
stabilized,
a reference
sample
(2.0
ml)
can then
be injected.
Again
mark
injection
point
and
observe
retention
time
for each
component
of reference
sample.
The adjusted
retention
time
for each
component
is (Tr'-Tml).
After
again
allowing
the baseline
to stabilize,
the
reference
sample
injections
are
followed
by the test
samples.
Many
different
reference
samples
may
then
be
needed
to make
an adequate
qualitative
and quantitative
analysis.
COMPOUND

IDENTIFICATION

Compound
identification
is based
upon
the adjusted
retention
time
(Tr'-Tml).
The
adjusted
retention
time
is
a function
of the carrier
gas,
column
temperature,
column
pressure
drop,
and other
factors,
thereby
indicating
the
importance
of maintaining
constant
conditions
while
comparing
reference
samples
to test
samples.

6.2

The
recommended
procedure
for qualitative
analysis
is
as follows:
With
the column
at operating
conditions,
inject
suitably
sized
samples
of liquids,
one compound
at
a time.
Adjust
the
instrument
attenuation
so that
the
peak
height
is at least
50 percent
of full
scale.
Inject
the sample
quickly
into column
"A".
Again
mark
the
injection
point,
and measure
retention
time
(Tr')
for
each
peak
in minutes
to at least
2 significant
figures.
Make
duplicate
determinations
and use
the average
value
for compounds
relative
to at least
one
injected
standard
reference
material.
All data
should
be recorded
carefully
with
each
run.
For
qualitative
analysis,
the
retention
times
of the sample
peaks
must
then
be matched
with
those
of known
standards
obtained
under
the
same
operating
conditions.
Occasionally,
it is necessary
to
38

analyze a sample in 2 different

columns under different
conditions,
measuring the retention
times of the
components and compare them with previously
determined
standards,
in order to determine
which of 2 (or more)
compounds
having
the
with
common
solvents,
is often
all that
is
QUANTITATIVE

same
retention
one type
of
necessary.

time
column

is present.
like
porapk

Q.

ANALYSIS

The
areas
under
the peaks
of the chromatogram
are
quantitative
measures
of the
amounts
of the corresponding
compounds.
The
relative
area
is usually
proportional
to
the concentration
if the
relative
responses
of the sample
concentration
components
are equal.
If this
is not the
case,
the corrected
area
of the component
is used.
It is
obtained
by dividing
the peak
area
by the relative
response
of that
component.
Therefore,
best
results
require
a calibration
curve
of peak
area,
(or height)
versus
known
amounts
of pure
components
for the given
operating
conditions.

7.2

Although
the establishment
of the true
peak
area
by
integration
is the
standard
method
for quantitative
analysis,
multiplying
the peak
by the width
of the peak
taken
at the half-height
gives
proportional
values
especially
for sharp,
symmetrical,
completely
resolved
peaks.
With
this
method,
a chart
speed
that
will
give
at
least
a 5 mm. half-width
should
be used.

7.3

When
the volumes
injected
Relationships
apply:
V1 =

(H1/H2)

x V 2 and

are

= V 1 x

the

same,

the

following

(DI/D2)

Where:
v I = vol.
percent
of sample
component
H I = Compound
peak
area
or height
in sample
H 2 = Compound
peak
area
or height
in standard
V 2 = Volume
percent
of sample
component
in
standard
W =
Weight
percent
of sample
component
D 1 = Density
of pure
sample
component
D 2 = Density
of sample

7.4

An outline
of the
recommended
procedure
used
for the
quantitative
calibration
is as follows:
With
the column
at equilibrium
operating
conditions,
inject
the
liquid
samples
of pure
components,
one compound
at a time.
More
than
one at a time
is acceptable
if you're
sure
what
peak
corresponds
to which
compound,
vary
the
sample
size
(or
concentration)
to cover
the desired
range.
Samples
of a
given
size
should
be injected
until
at least
three
peaks
39

have
the
same
area,
ideally
+ 1 percent
at the same
attenuation.
Adjust
the attenuation
in all cases
to keep
the peak
on scale
and with
a height
of at least
50
percent.
Data
should
be converted
to some
attenuation
previously
chosen
as a basis
for calculations,
for
example,
x i, x 8, x 64, etc.
Multiply
the actual
peak
height
by its corresponding
attenuation
and divide
by the
basis
attenuation.
Plot
this
peak
height
versus
quantity
of each
compound
and connect
the data
points
with
a
smooth
calibration
curve.
Label
the axis on the plot
and
for each
such
plot
show
the following
information:
Data,
column
description,
and operating
conditions.
Record
also
the purity
of the compounds
used.
The
syringe,
pipette,
or other
device
must
be flushed
at least
3 times
with
each
new compound
prior
to injecting
a sample
of
that
component

7.5

Actual
sample
then
be easily

injections
quantitated

will
generate
peaks
which
can
using
the calibration
charts.

An

a possible

analysis

example

of

All

runs

are

All

samples

Reference
Acetone
Methanol
Ethanol
From

made

injected
samples

16
16
16
8

identical
are

2.0

conditions.

ml.

-Tr'

7.5 min.
- 2.7 min.
- 5.0 min.

Calibration

Attenuation

with

follows:

Curves
Peak

Area

25
50
i00
i00

8.1

8.2

of

Ethanol

1
2
4
8

Sample
peak
of impurity
in solution
peak
area
of 75 at 16 attenuation.
calibration
work,
peak
is ethanol.

Volume

is Tr'
w 5.0
From
previous
3% by Volume.

min.

and

CALIBRATION
Before
each
calibration
and series
(or daily)
condition
the column
at
carrier
gas flow.
Determination
of Relative
2-propanol
is used
as an
factor
to water
relative

of determinations
200C.
for 1 hr.

with

Response
Factors
- Anhydrous
internal
standard.
The response
to the standard
is determined
by
4o

means
of the following
procedure.
typical
chromatogram.
It is good
the
response
factor
daily
or with
determinations.

See Fig.
1 for a
practice
to determine
each
series
of

8.2.1

Weigh
about
0.2 gm. of water
and 0.2 gm. of 2-propanol
to the nearest
0.i mg.
into
a septum
sample
vial.
If
it has been
determined
that
a correction
for the
water
content
is necessary,
weigh
2 ml.
of
dimethylformamide
into the vlal.
If the
dimethylformamide
is anhydrous,
simply
add 2 ml.of
it
as weighing
is not necessary.

8.2.2

Inject
a 1 unit
aliquot
of the
above
solution
onto
the column
and record
the chromatogram.
The
retention
order
and approximate
retention
times
after
the
air peak
are i. water,
about
0.7 min;
2. 2propanol,
about
2.8 min.;
and
3. DMF,
about
7 min.

8.2.3

The preferred
procedure
to obtain
the water
content
of the DMF is by Karl Fischer
titration.
If this
has
been
done,
calculate
the response
factor
for water
by
means
of the
following
equation:
WiAH20
R

(WH20

PWs)A

Where:
R = response
factor
W i = weight
of 2-propanol,
gm.
WH20
= weight
of water
added,
gm.
W s = weight
of Dimethyl-formamide,
AH20
= area
of water
added
A i = area of 2-propanol
peak
P = Weight
% water
in DMF
I00
8.2.4

gm.

If Karl
Fischer
titration
is not
available,
following
procedure
may be used
to obtain
a
reasonable
estimate
of the
response
factor.

8.2.4.1

Inject
the same
size
mixture,
but without
the area
of the water

8.2.4.2

The response
means
of the
Wi(AH20

the

aliquot
of DMF and 2-propanol
added
water,
as a blank.
Note
peak
in the blank.

factor
for water
is
following
equation:
- B)

WH2oAi

41

calculated

by

Where:
R

= response
factor
W i = weight
of 2-propanol,
gm.
WH20
= weight
of the water,
gm.
A i = area
of 2-propanol
peak
AH20
= area
of the water
peak
B = area
of the water
peak
in the
9.

PROCEDURE

9.1

9.

blank

weigh
to the nearest
0.1 mg.
0.6
sample
and 0.2 gm.
of 2-propanol
2 ml.
of dimethyl-formamide
into
vial.
Prepare
a blank
containing
dimethylformamide
but no sample.

gm. of water-reducible
into
a septum
vial.
the vial.
Seal
the
the
2-propanol
and

Add

Shake
the vials
on a wrist
action
shaker
or other
suitable
device
for 15 min.
To facilitate
settling
of
solids
allow
the
samples
to stand
for 5 min.
just
prior
to injection
into
the chromatograph.
A low speed
centrifuge
may
also
be used.

9.3

Inject
a 1 ml.sample
of the supernatant
from
the
prepared
solutions
onto
the chromatographic
column.
Record
the chromatograms
using
the conditions
described
in Table
i.

i0.

CALCULATIONS

i0.i

Measure
the area
of the water
peak
and the 2-propanol
internal
standard
peak
and multiply
each
area by the
appropriate
attenuation
factor
to express
the peak
areas
on a common
basis.
Use of an electronic
integrator
is
recommended
to obtain
the best
accuracy
and precision.
However,
triangulation,
planimeter,
paper
cut out,
or
ball
and disk
integrator
may
be used.

10.2

Determine
means
of

the water
concentration
the
following
equation:
AH20

H20,

the

sample

by

i00

=
Ai X

Where

W i

in

Wp

:
AH20
Ai
Wi
W
Rp

m
=
=

area
of water
peak
area
of 2-propanol
peak
weight
of 2-propanol
added,
weight
of sample,
gm.
response
factor
determined
8.2.4.2

42

gm.
in

8.2.3

or

10.3

Correction

for

Water

Content

of

Solvent

10.3.1

If the blank
indicates
the presence
of a detectable
peak
for water
in the dimethylformamide
used
as
solvent,
make
a correction
in the calculation.

10.3.2

To make
the correction,
the water
content
of the
dimethylformamide
is determined
either
by
chromatography
(8.2.4)
or, preferably,
by Karl
Fisher
titration
(8.2)
Calculate
the water
content
due to solvent
by using
the following
equation:
(Ws)(p)100
=

H20(S)%

Wp
where:
ws
W
PP

10.3.3

=
-

weight
weight
weight

of dimethylformamide,
of sample,
gm.
% water
in DMF
i00

gm.

The water
content
of the sample
in this
case
is the
difference
between
the total
percent
determined
in
10.2
and the correction
for the solvent
water
content
as determined
in 10.3.2.
For
isothermal
operation
set the column
temperature
at 140C.
After
the
2propanol
has cleared
the column
adjust
the
temperature
to 170C.
until
_MF clears
the column.
Reset
the temperature
to 140_C
for subsequent
runs.
Table

Instrument

Parameters

(Typical

Detector
thermal
conductivity
1.22m.
diameter
by 3.2mm.
outside
diameter
mesh
porous
polymer
packing
Temperatures:
Sample
inlet
Detector
Column
Initial
Final

inside
packed

200C.
240C
80C.
170C.
30C./min.

Program
rate
Carrier
Gas
Flow
rate
Detector
current
Specimen

Conditions)

helium
or
50 ml/min.
150 mA.
1 1

size

43

nitrogen

Column
with
60

to

80

.i.J

_-"1

r
INTENSITY

44

M-R-f1
i.

Infra-red

Analysis

Double
Model

1.2

Matched

beam
21 or

infra-red
equivalent,

sealed

EQUIPMENT

NaCI

spectrophotometer
and operators

Cells

0.20

mm.

Resins

Perkin
manual.
path

Elmer

length.

OPERATION

2.1

Spectrophotometer
least
i0 minutes

2.2

Before
operation,
accordance
with
manual.)

2.3

Sub-zero
and noise
week
intervals
to
instrument.

2.4

Cells
used
will
be marked
to assure
will
always
be used
in the
reference
sample
cell
will
always
be used
in

2.5

of

EQUIPMENT

i.i

2.

Spectrophotometer

must
before

be warmed
operation.

up

for

a period

spectrophotometer
must
manufacturer's
procedure.

checks
assure

must
proper

be run at
operation

be

of

at

balanced
in
(See Operators

one
of

(i)

the reference
beam and
the
the analytical

cell
beam.

A spectrum
will
be run at one
(1) week
intervals
with
acetone
in both
the sample
cell
and reference
cell
to
assure
that
the cells
are in proper
operating
condition.
The spectrum
obtained
should
not vary
more
than
+ 3% @ 100% transmission
from
a straight
line
from
9.5 to 15.0 microns.

3.

INSTRUMENT

3.1

Slit
program

SETTINGS

..............................................

3.2

Response

3.3

Speed ................................................
microns/min

3.4

Auto

4.

PROCEDURE

...............................................

suppression

4.1

Weigh
solids

4.2

Filter
filter

927

out
in

0.8

.......................................

enough
resin
spectrograde

mixture
paper.

to produce
acetone.

a 4% solution
Note
I.

through
S and S No.
(Flute
the paper
for

45

of

589 Blue Ribbon

faster
filtration).

4.3

Rinse reference
and sample cells
three time with
spectrograde
acetone.
Flush each cell with dry
nitrogen.
Load reference
cell with spectrograde
acetone.

4.4

Balance
Insert
microns

Load

sample

cell

with

extract.

spectrophotometer
and set
sample
and reference
cells.
shall
be between
0.70
and

at

8.0 microns.
Absorbance
at 8.0
0.75.
If absorbance

is greater
than
0.75
adjust
concentration
of remaining
solution
by addition
of spectrograde
acetone.
If
absorbance
is less than
0.70
evaporate
in a vacuum
oven
at room
temperature.
Scan

the

spectrum

from

2.0

to

15.0

microns.

Mark
chart
with
material
designation,
lot or batch
number,
instrument
settings,
date,
solvent,
and
operators
initials.

4.7

Compare
presence
spectrum
Note

spectrum
obtained
with
standard
spectrum
of foreign
absorption
peaks.
A standard
will
be furnished
by the Fiberite
Corp.
- Double

distilled

CP

48

Acetone

may

be

used.

for

M-R-12
i.
i.I
2.
2.1

Moisture

Content

Aquatest

IV

Glass
is 24

equivalent

vials

Photo

with

Syringe

- Tuberculin

Syringe
reagent.

needles

vacuum

4.1

or

sample
ml.

2.5

by

Use

of

a Photo

volt

Unit

Volt

EQUIPMENT

Mechanical
if care
is

3.1

Resins

APPARATUS

2.4

3.

of

type

- Need

shaker
taken

caps

to

suitable

1 ml.

size

be

to

5"

reach

- An ultrasonic
bath
not
to heat
samples.

vial

into

can

volume

the

also

be

used

oven

REAGENT
Methanol.025%).
SAMPLE

Reagent
Dry with

grade,
low in H20
molecular
sieves.

(must

be

less

than

PREPARATION

Dry the sample

vials
and caps
oven
at II0_C.
long
enough
to
(about
15 minutes).
Remove

and

place

immediately

by heating
drive
off

into

in
any

a vacuum
moisture

a desiccator

to

cool.

When
cooled
to room
temperature,
weigh
approximately
35 grams
of sample
into
each
vial
to the nearest
0.i mg.
(The desirable
sample
size
contains
100-3000
micrograms
of H20 so adjust
the sample
size
accordingly).
Add

20

ml.

of

Methanol

Prepare
a solvent
blank
into dried
vial
and cap
4.6

5.1

Shake
vials
samples
are

using

a volumetric

by plpeting
immediately.

on a mechanical
now
ready
for

shaker
analysis.

20

for

pipet.
ml.

30

of

Methanol

minutes.

The

ANALYSIS
Determine
the moisture
content
of the blank
solvent
first.
Draw
a 1 ml.
sample
into
the syringe,
being
careful
to remove
all air bubbles.
Inject
sample
into
the Aquatest
IV titration
vessel.
The
sample
must
be
discharged
below
the surface
of the vessel
solution.
47

5.2

6.

Perform
average
Perform
average

this
step
in triplicate
and calculate
the
micrograms
of H20
in the solvent
blank.
triplicate
runs on each
of the sample
vials
the values.

CALCULATIONS

[(mcgs

H_O

= moisture

sample)-(mcgs
Sample
content,

H20
in Blank)]x
wt.
in g. x 106

% water

48

20ml.

Meth

i00

and

M-R-13
i.

pH

of

Liquid

Resins

by

Use

of

a pH

Meter

SCOPE

i.i

This
method
covers
a procedure
value
of liquid
resins.

for

determining

the

pH

EQUIPMENT
pH meter.
combination
Operators
2.2

pH

2.3

150

Distilled

3.

Accumet
model
825 MP with
electrode
and temperature
Manual
would
be of use.

buffers,
ml.

4,

7,

glass
body
compensator.

10.

beakers
water.

PROCEDURE

3.1

Calibration

3.1.1

Perform
nearest

3.1.2

Remove
the electrode
from
the
with
distilled
water
and place
solution
of the necessary
pH.

3.1.3

Press

"stby/meas".

Press

"i

Enter
point
press

electrode
efficiency
from
the most
calibration,
e.g.
91.4%
is entered
"enter"

Enter

pH

a 1 point
calibration
using
the
to the expected
pH measurement.

pt

3.2
3.2.1

3.2.2

Press
pH

buffer

storage
solution,
in fresh
buffer

rinse

cal".

buffer

value

Wait
for millivolt
"ente r" .
3.1.8

pH

used

reading

e.g.
to

"7.00"
stabilize

recent
2
as ".9140"

press
and

"enter".
press

"stby/meas".

Measurement
Remove
the electrode
with
distilled
water
measured.
Press

from
the buffer
solution,
and immerse
in sample
to

"stby/meas".

49

rinse
be

3.2.3

Press
corner

3.2.4

Wait
the

3.2.5

Press
rinse

"stby/meas",
with
acetone

3.2.6

Place

the

"mode"
(skip

until
this

for
reading
nearest
0.I

electrode

pH
step

appears
if pH
1

to
stabilize
pH unit.

in the
lower
right
is already
displayed).
and

remove
electrode
then
distilled
back

into

5O

the

read

from
water.
storage

pH

value

sample

to

and

solution.

M-R-14

1.
i.i

2.

Resin
Solids
and
Unfilled
Systems

Total

Both

Aluminum

2.3

Oven-gravity
convection
at 135 + lC.

2.4

Desiccator

balance
dry

dish

(0.001

gm.

sensitivity)

- Cenco

No.

12720

type-thermostatically

Preheat
three
drying
dishes
in the oven
at 135 + lC
for
30 + 2 minutes.
Cool
the dishes
in the desiccator
to
room
temperature
and weigh
to the nearest
milligram

gm.).

3.2

Weigh
2.8
milligram,

3.3

Place
the
samples
in the drying
oven.
Heat
at 135 + lC.
and then
transfer
the samples
desiccator
and cool
to room temperature.

3.4

Reweigh

to 3.2 gm.
into
each

the

samples

of
of

to

resin
solution
to the nearest
the tared,
dried
dishes.

the

nearest

for 3 hours
to the

milligram.

CALCULATIONS
For

unfilled

% Resin

4.2

controlled

PROCEDURE

(0.001

4.1

and

EQUIPMENT

2.2

4.

Filled

This method
is used
to determine
the percent
of non
volatile
material
in solutions
of formaldehyde-phenol
resins
or other
resin
solids.

Analytical

3.1

for

SCOPE

2.1

3.

Solids

For

Solids

filled

% Total

resin

resin

Solids

systems:

= Final
total
wgt.
- wgt.
of dish
x
Original
total
wgt.
- wgt.
of dish

I00

systems:
= Final
total
wgt.
- wgt.
of dish
x
Original
total
wgt.
- wgt.
of dish

61

I00

M-R-15
i.
1.1
2.

Refractive

Index

SCOPE
The refractive

index

is

determined

on all

resins.

EQUIPMENT

2.1

Abbe refractometer,

2.2

Constant

2.3

Pumping system

3.

on Resins

Bausch and Lomb Model 519A

temperature
for

bath

(25.0 + 0.5C.)

water

PROCEDURE

3.1

Set the constant

Assemble
pumping
refractometer.
standard
sample.

3.2

Place
a drop
of resin
on the glass
prism
and close.
Turn
on light
and adjust
instrument
so that
the line
at the
intersection
of the cross
hairs.

4.
4.1
NOTE:

temperature
bath
at 25.0C
system
to circulate
water
Calibrate
the
refractometer

+ 0.5C.
t_rough
the
with
the

is

CALCULATIONS
Report

reading

on

the

scale.

Refractometer
must
be calibrated
before
each
series
of determinations.
Calibration
is accomplished
using
sample
of known
refractive
index
supplied
with
the
instrument.
Proceed
with
the calibration
as directed
by the instrument
manufacturer.

52

M-R-16
i.

Specific

Gravity

by

Hydrometers

on

Liquid

Resins

SCOPE

i.i

This
method
gravity
of
,

is applicable
liquid
resins.

Series

of

hydrometers

2.2

Ungraduated

cylinder

2.3

Thermometer

3.1

determining

the

specific

EQUIPMENT

2.1

3.

for

PROCEDURE
Pour
liquid
resin
into ungraduated
cylinder
and adjust
temperature
to 25 + 0.5C.
Place
into the liquid
a
hydrometer
covering-the
range
of specific
gravity
of
the
liquids
being
tested.
Read
the hydrometer
at the
level
of the liquid
and record.

53

M-R-17
i.
I.i

Resin

Reinforcement

This
method
is used
volatile
reinforcement

Phenolic

Prepregs

to

determine
the
in an aldehyde

percent
phenolic

of

nonresin

EQUIPMENT
Analytical

2.2

Crucibles

23

Oven
- gravity
controlled
at

2.4

Muffle

Balance;

accurate

convection
135 + lC.

furnace

set

at

to

type

788

0.i

mg.

thermostatically

5C.

PROCEDURE

3.1

Determinations

3.2

Weigh
tared
788

3.3

Place
crucibles
transfer
to a

are

approximately
crucibles
+ 5C.
for

Weigh

to

Place
+ 5.0

crucibles
min.

Transfer
Reweigh
as W 2 .

Aldehyde

SCOPE

2.1

3.

in

the

in

duplicate

three
which
have
1 hour.

in 135
desiccator-to
nearest
in

crucibles
samples

run

to

grams
been

lC.
oven
cool.

milligram

and

788

to

desiccator

the

of
resin
previously

5C.

nearest

for

solution
fired

hours

designate

muffle

to
milligram

and

as

furnace

into
at

W I.

for

hours

cool.
and

designate

CALCULATIONS
%

Resin

Reinforcement

W2
W1

54

weight
weight

of
of

crucible
crucible

i00

M-R-18

Degree
of
Technique

Advancement

or

Polymerization

by

Infra-Red

SCOPE
This
method
describes
a procedure
for the determination
of the degree
of advancement
or polymerization
of
aldehyde-phenolic
resins.
An infrared
analytical
technique
is employed
which
differentiates
molecular
structural
changes
resulting
from
polymerization.
This
method
applies
to raw resin
as well
as preimpregnated
fabric,
to unmodified
as well
as modified
resins,
and to
filled
as well
as unfilled
prepregs.

I.i

2.

EQUIPMENT

2.1

AND

MATERIALS

Equipment

2.1.1

Infrared
spectrophotometer,
equivalent,
and operators

2.1.2

Sodium

chloride

variable

2.1.3

Sodium

chloride

liquid

2.1.4

Funnel,

2.1.5

Beakers,

100

2.1.6

Stirring

rod,

2.1.7

Scissors

2.1.8

Graduated

2.1.9

Syringe,

path
cell,

IR-8,

or

cell
0.20

mm.

1/2"

height

60
ml.
glass

cylinder,

50

ml.

2 ml.

2.1.10

Centrifuge

2.1.11

Vacuum

2.1.12

Aluminum

2.2

Beckman
manual

oven
pans,

2 1/2"

diam.

Materials

2.2.1

Acetone,

water

2.2.2

Filter
paper,
equivalent

2.2.3

Infrared
absorbance

chart

free,
S & S

paper,

saturated
No.

589

2.5

55

to

with
Blue

16

silica

Ribbon,

microns,

gel
or

SAMPLING

3.1

Sufficient
approximately

sample
shall
be taken
to provide
2 grams
of resin
solids.

PROCEDURE
Operation
and Calibration
For
operation
and calibration
of the
see SCM-7-01
for the
IR-8
instrument
procedures.
4.2

spectrophotometer,
or other
equivalent

Adjustment
of variable
cell
The variable
path
cell
shall
be adjusted
to the
exact
thickness
of the 0.20 mm.
sodium
chloride
cell.
In order
to determine
that
the thicknesses
are closely
matched,
fill
both
cells
with
acetone
using
a syringe.
When
properly
matched,
the
resulting
spectrum
will
not vary
by
more
than
+ 3.0% from
100.0%
transmission
when
measured
between
9.5 and
15.0 microns.
Adjust
the variable
path
cell
as necessary
in order
to attain
the above
tolerance.
Solution

Preparation

Raw Resins
Raw
resins
known
or suspected
of having
solvents
other
than
acetone
shall
be devolatilized
under
vacuum
without
heat
for a minimum
of four
hours
or until
disappearance
of the absorption
bands
indicating
their
presence.
This may
require
as long
as
24 hours
for some
solvents
such
as isopropanol.
(As an
alternate,
isopropanol
can be removed
by adding
30 ml.
acetone
to 2 gm. aldehyde-phenolic
resin
and
periodically
stirring
at RT without
vacuum
over
0.5 hr.
during
which
both
acetone
and isopropanol
are largely
volatilized).
Add
sufficient
acetone
to the resin
to
effect
a 4 to 6 % solids
solution.
Stir with
a glass
stirring
rod and allow
to stand
for ten minutes.
If
the
solution
is not clear,
centrifuge,
or filter
using
S & S No. 589.
Seal
filtrate
in a vial
if there
is to
be any time
delay.
Continue
per
instruction
in Para.
4.4.
4.3.2

Preimpregnated
Resins
Cut the sample
into
approximately
1/2 inch
squares
or lengths.
If the dry
resin
content
of the prepreg
is known,
use
the
following
formula
to determine
amount
of prepreg
and
acetone
to use:
191
DRC

grams
of
Dry Resin

prepreg
in 36 ml.
Content,
gm.

of

acetone

If the dry
resin
content
of the prepreg
is not known,
arbitrarily
use
6 grams
of prepreg
in 36 ml.
of
acetone.
Place
the prepreg
and acetone
in a i00 ml.
58

beaker.
Stir with
a glass
rod and allow
to stand
for a
minimum
of 20 minutes,
with
occasional
stirring.
Filter
using
S & S No.
589.
Seal
filtrate
in a vial
if
there
is to be any time
delay.
Extraction
efficiency
should
be determined.
Extraction
efficiency
must
be at
least
90%
(see Para.
6.1)
in order
to achieve
an
accurate
result.

4.4

Adjustment
of Concentration
Fill
the 0.20 mm.
cell
with
the
resin-extract
from Para.
4.2, using
a syringe.
Fill
the variable
path
cell
with
water
free of acetone.
Position
both
cells
in their
respective
holders
in the
spectrophotometer,
without
placing
the pen upon
the
chart
paper,
start
machine
operation
at ii microns
by
setting
to "Scan"
position.
Determine
absorbance
at
approximately
12.15
microns
(12.1
to 12.2 microns).
The
concentration
of the extract
must
be further
adjusted
(if
necessary)
to produce
linear
absorbance
between
40%
and
45% at this
wavelength.
This
may
be accomplished
by
removing
the
sample
and adding
acetone
(if the absorbance
is too great)
or by partially
volatilzing
the acetone
at
room
temperature
(if the absorbance
is too small).

4.5

Scan
Place
the pen to 5.0 microns
and place
on chart
paper.
Start
machine
operation
by setting
to scan
position.
Scan
the spectrum
from
5.0 to 16.0 microns
at
0.54 microns
per minute.
The pen will
automatically
raise
off the chart
when
the scan
is complete.
Remove
the
chart
and label
it in accordance
with
Para.
5.2.
Turn
function
control
to "STOP"
and return
pen
carriage
to 2.5 microns.
Tilt
pen backwards
to prevent
accidental
contact
with
metallic
chart
bed.

4.6

5.1

Clean
Up
Remove
thoroughly
with
air.
Place
the
CALCULATIONS

cells
acetone
cleaned

AND

Calculations
follows:

from
the instrument.
Clean
followed
by dry nitrogen
or dry
and dried
cells
in a desicator.

REPORTING

Calculate

the

Advancement

Index

as

5.1.1

Construction
of tangential
base
line.
Construct
tangential
base
line
over
the absorbance
occurring
at
approximately
9.8 microns,
extending
from
approximately
9.45
to 10.2 microns.
Also
construct
a tangential
base
line
over
the absorbance
occurring
at approximately
12.15
microns
extending
from
approximately
11.5
to 12.5
microns.

5.1.2

Construction
perpendicular
occurring
at

of perpendiculars.
to the wavelength
approximately
9.8

57

Construct
a line
at the absorptions
to 12.15
microns
which

passes
through
tangential
base
5.1.3

5.1.4

Advancement

Index.
Index

Advance.

(IRPI)=

Index

Line

Reportin@.
informatlon:

5.2.2

Sample

5.2.3

Lot

5.2.4

Date

5.2.5

Gain,

5.2.6

Advancement
to

(IRZB)

and

Advancement

(IRPI)

Record

Spectrum

the

Base
Base
Lo 9
Log

and

Base
Base

report

and
Line
Line

Index,
IRZB

Absorb.
Absorb.

Line
Line
the

are

@
@

between
line
at
This
is

Infrared
as
@
@

follows:
12.15
Micr.
9.8
Microns

12.15
Microns
9.8
Microns

following

number
identification

or

batch

of

number

test

balance

the

5.2.7

Identity

5.2.8

Extraction

6.1

The

Polymerization

5.2.1

6.

absorbance

Determination
of
absorbance.
Determine
the
absorbance
units
(to
three
significant
figures)
the
maximum
absorbance
and
the
tangetial
base
approximate
9.8
and
12.15
microns
absorptions.
the
base
line
absorbance.

Base

5.2

the
maximum
line.

and
Index

nearest
of

settings

(IRPI)

0.01
the

speed

or

Baseline

Index

(IRZB)

unit

operator

efficiency

if

calculated

NOTES
Extraction
extraction
of normal

Efficiency.
efficiency.
laboratory

It
is desirable
This
can
be
done
techniques.

58

to determine
by
a variety

M-R-19

Differential
Scanning
Heat
of Polymerization

Calorimetry

for

Determining

the

SCOPE
This
procedure
differential

EQUIPMENT

AND

describes
a method
scanning
calorimetry

Perkin-Elmer
manual

DSC-IB

2.2

Sample

crimped

2.3

Nitrogen

3.1

conducting

MATERIALS

2.1

3.

for

pans,
gas

or

equivalent

analyzer

and

operators

supply

SAMPLING
Obtain

small

(i

oz.)

representative

sample.

PROCEDURE
Perform
analyzer

test

with
Sample

a Perkin-Elmer
DSC-IB
pan must
be crimped

Atmosphere:
The peak
area
is determined
baseline
under
the peak.
planimeter
or equivalent.
onset,
pea k (s), maximum,
The heat
of polymerization
follows:

Hs

by extrapolating
the
Measure
the peak
area
with
Record
the temperature
of
and completion
of reaction.
shall
be calculated
as

= H r x Wr x As x Rs x Sr
Ws x Ar x Rr x Sr

where

:
of

equivalent

Room
temp.
to 325C.
(598K)
20 c./minute
I0 mcal./sec.
(20 mvfs)
Empty
gold
pan plus
lid on
reference
side
Nitrogen
(40 ml./min.)

Temperature
range:
Rate
of heating:
Sensitivity
range:
Reference:

4.2

or

= heat

W
A
S
R

= weight,
mg.
2
= peak
area,
in.
= chart
speed,
in./sec.
= range
setting,
mcal./sec.,

polymerization,

59

cal/g.

in.

Subscripts:
r = reference
s = sample
Meltin

4.3.2

9 Point

(calibration

standard)

Determinations

Polymeric
materials
may be determined
endotherm.

by

and organic
solids
melting
points
the apex
of the peak
of melting

Pure
metal
melting
onset
of the melt

points
may
endotherm.

8O

be

determined

as

the

M-R-20
i

pH

of

Resins

and

Aqueous

Solutions

with

pH

Meter

SCOPE

This

i.i

of

method
pH

This

1.2

of

describes
aqueous

method

is

equivalent
AND

solutions
similar

pH

2.1.2

Beakers,

to

liquid

the

determination

resins.

ASTM-E70-52T

and

will

yield

MATERIALS

meter

with
200

glass

electrodes

ml.,

tall

form

Materials

2.2.1

Buffer

2.2.2

Distilled

water

2.2.3

Denatured

ethyl

and

for

Equipment

2.1.i

2.2

procedure

results.

EQUIPMENT
2.1

standards

of

pH

4,

7,

i0

alcohol

SAMPLING

3.1

Sample
immerse

Size.
the

3.2

Number

of

A minimum
electrodes.

sample

determinations.

duplicate

of

i00

Unless

determinations

will

ml.

is

otherwise

be

run

on

required

to

specified,

each

sample.

PROCEDURE
Standardization
standardized
4.1.1

Allow

of
daily

sufficient

pH meter.
prior
to

use

The

time

complete

for

as

pH meter
follows

must
(see

warm-up

be
6.1):

of

pH

meter

amplifier.
Immerse

clean

If necessary,
temperature
Read

pH

electrodes

of

set
temperature
buffer.

Place

pH

standard
control

buffer
knob

solution.
to

meter.

Using
the
calibrating
indicate
pH
value
of
4.1.6

in

meter

in

control
buffer.

"Stand-by"

81

knob,

condition.

set

pH

meter

to

4.1.7

4.2

Remove
water.

buffer

Determination
will
be found

of
as

4.2.1

Immerse

4.2.2

If necessary,
temperature

4.2.3

Read

4.2.4

Remove
proper

5.
5.1

6.
6.1

and

pH

electrodes

pH.
The
follows:

electrodes

of

rinse

in

pH

of

the

with

distilled

solution

to

be

tested

sample.

set temperature
samples.

control

knob

to

meter.
sample
and
solvent.

CALCULATIONS
Reporting.
units,
the
the
average
significant

AND

rinse

electrodes

thoroughly

with

REPORTING

If the range
results
should
of duplicate
figures.

of determinations
be considered
determinations

exceeds
suspect.
to two

0.i pH
Report

NOTES
Standardization.
The pH meter
should
be calibrated
weekly
in accordance
with
SCM-7-02.
If for any
reason
the pH meter
cannot
be calibrated
properly,
consult
SCM7-02
for possible
electrode
failure
and electrode
servicing.

82

M-R-21
i.

Karl

Fisher

To determine
and chemicals,
reagent.

2.

EQUIPMENT

2.1

AND

in

Materials

Chemicals

the percentage
titrate
with

of water
stabilized

in

various
materials
Karl
Fisher

MATERIALS

Equipment

2.1.1

Aquatrator
Cortland
manual.

2.1.2

Analytical
Scientific,

2.1.3

Desiccator

2.1.4

Dropping

2.2

(Junior)
St.,
Chicago

Precision
Illinois

Scientific
60647,
and

Balance
- Mettler,
Model
Cat.
#2742
(et al).

B5;

Co.,
3737
operators

W.

will

Bottle

Materials

2.2.1

Karl
K-3.

2.2.2

Methanol

3.1

Determination

SCOPE

i.i

3.

Water

Fisher

Reagent

- Fisher

Scientific

Co.,

Cat.

#SO-

(Borden)

ASSEMBLY
Follow
"Operating
Instruction"
booklet
supplied
instrument.
If assistance
is required,
contact
Bainbridge
Quality
Control
Office,
of Precision
Scientific,
Co.
Arrangements
will
be made
for
assistance
and operating
know-how.
Note

Note

I:

II:

with

assembly

In assembly,
do not
set up the Water-Methanol
burette
and drying
tubes
for same.
This
is
modification
by the laboratory
in which
we
eliminate
the Back
Titration
Method;
using
Methanol
in the Reaction
Vessel
and Distilled
Water
for standardizing,
etc.

a
dry

In place
of Drierite,
use
Silica
Jel which
we
feel
is a more
effective
desiccant
and which
also can
be oven
dried
and reused,
a property
lacking
with
the Drierite.

63

DETERMINATION

OF

4.1

After
assembly
Mode
Selector
ADJUST".

4.2

With
full

DIRECT
scale

Note:

4.3

Turn

and plug-in,
energize
switch
from the
"OFF"

ADJUST
knob,
position
indicating
"20" for normal
operations.

MODE

SELECTOR

switch

to

DIRECT

In a direct
titration
the
will
start
at a low meter
the endpoint
is approached.

Add
the dry Methanol
covers
the electrodes.
Note:

Set

unit
by
position

turning
the
to "DIRECT

needle

to

Always
turn
the DIRECT
ADJUST
knob
counterclockwise
before
switching
to the ADJUST
position.
This
will
prevent
accidental
damage
to the meter
needle
if the DIRECT
ADJUST
knob
is set too far
clockwise.

Note:

4.4

ENDPOINT

The Methanol
the electrodes
by the Teflon
the

stirring

at

into

the

TITRATE.

Micro-Ammeter
reading
and

reaction

needle
increase

vessel

so

must
cover
the electrodes,
must
not be so low as to
stirring
bar.
the

desired

slow

that

as

it

however,
be damaged

rate.

Fill
the Karl
Fisher
burettes
by pumping
the appropriate
plunger.
Be sure
to place
your
finger
over
the hole
below
the plunger.
When
the reagent
has
filled
the
burette,
release
your
finger
and the plunger.
The
reagent
will
then
syphon
to the
"0" ml. mark.
Caution:

Do not allow
titrant
which
is inserted
in
burette.

to enter
the drying
the stopper
on the

tube

4.7

Dispense
Karl
holds
steadly

4.8

Remove
Sample
Filling
Port
Stopper
and place
2 drops
of
distilled
water
so the current
drops.
Replace
stopper
and vacuum
purge
the vessel
by depressing
and holding
the
pump
switch.
(Amount
of purging
depends
on the humidity
present
in the
room.
Normally,
15 seconds
is adequate
for humid
ambient
conditions.)
Note:

Fisher
between

solution
17/19.

until

See
"Operating
Instructions",
A, "Vacuum
Pump
System".

84

the

black

Section

needle

IV,

Subtitle

4.9

Check
burette
to insure
that
reagent
is at the
"0" line,
titrate
until
an endpoint
is reached.
Initial
addition
of titrant
will
cause
current
needle
to swing
upscale
and
then
drop
as titrant
reacts
with
the water.
Further
addition
swings
the current
needle
in increasing
upscale
increments.
As endpoint
is approached,
the
increments
become
smaller.
If a single
drop
maintains
this
endpoint
for a specified
time
(will
not
fade),
stop
the
titration
and
record
the meter
value
so noted.
This
is the
Endpoint.
Note:

It is extremely
important
that
whatever
meter
value
is chosen
for the endpoint,
that
this
value
be used
for both
calibration
and actual
sample
titrations.
It is also
extremely
important
that
the
full-scale
adjustment
be left
at the
same
value
for calibrating
and actual
sample
titrations,
i.e.,
"20"
for normal
operations.

DETERMINATION

OF

KARL

5.1

After

5.2

To determine
water
to the

"Factor",
Methanol

5.3

vacuum
rate.

the

5.4

Fill
until

determining

purge

FISHER

FACTOR

Endpoint

the

Set

mls.

of

K.

F.

Solution

The milligrams
of Water
per
called
"Factor",
which
must

DIRECT

TITRATION

6.1

Energize
the OFF

6.2

With
Full

DIRECT
Scale

6.3

Turn

MODE

6.4

Determine

6.5

Add

6.6

vacuum
rate.

F.
is

a few
Record

the

the K. F. burette.
Titrate
the Endpoint
is reached.

Record

system

again
add
solution.

system.

(K.

Solution
operable.

drops
of distilled
sample
weight.

stirring

with

at

K.

F.

used.
milliter
of
be determined

turning
the MODE
to DIRECT
ADJUST.

SELECTOR

switch

"Factor"

if

purge

desired

Solution

Solution
is
at least
once

SELECTOR

switch

ADJUST
knob,
position
indicating
"20" for normal
operations.

to

the

METHOD

unit
by
position

sample

only)

Methanol
system.

to

DIRECT

necessary
Solution.
Set

the

65

from

needle

to

TITRATE.

(at

least

Record
stirring

once
sample

at

the

a day).
weight.
desired

6.7

Fill
the

the

K.F.

Endpoint

Record

ml.

Burette.
is

of

Titrate

with

K.F.

Solution

until

reached.

K.E.

Solution

used.

CALCULATION
Milliters
Milligrams

K.F.
Soln.
of Sample

x "Factor"
used

i00

- % water

NOTES
ACCURACY:
Several
factors
will
influence
accuracy;
mainly
moisture
pick-up,
dirty
burettes,
spent
drying
chemicals,
insufficient
volumes
of titrant,
chemical
reaction
with
other
chemical
(Ref:
"AQUAMETRY"
by
Mitchell
and Smith,
vol.
5)

8.2

8.3
8.4

8.5

8.6

The moisture
problem
is greatly
reduced
by use
of the
vacuum
pump
whenever
the sample
stopper
is removed.
Drying
tubes
are clearly
exposed
and should
be changed
whenever
the contents
have
absorbed
moisture
as indicated
by the color
change.
All connections
are positive
and
easily
checked.
Droplets
that
the

of reagent
in
burette
should

the
be

burette
cleaned.

bore

clearly

indicate

An endpoint
setting
(in direct
titration)
which
is too
high
will
be toward
the
insensitive
portion
of the meter
scale.
If the current
needle
never
approaches
this
setting,
obviously
the endpoint
setting
is too high
or
the span
is too low
(high
resistance
solution
with
corresponding
low current
reading).
The platinum
electrode
tips
can become
coated
and
insensitive.
They
should
be cleaned
in warm
sulphuric
acid-dichromate
solution
Rinse
with
distilled
water
and
acetone,
and dry
thoroughly.
When
removing
the vessel,
wipe
any liquid
droplets
from
the underside
of the
gasket.
When
adding
a powdered
sample
with
a dry powder
funnel,
be sure
the sample
does
not
adhere
to the vessel
walls.
DRAINING
REACTION
VESSEL:
Several
sample
determinations
can be run before
the liquid
level
in the vessel
reaches
the burette
tips.
It is suggested
that
a portion
of this
liquid
be transferred
to the new
reaction
vessel.
However,
rather
than
remove
the vessel,
an alternate
choice
is to stop
the stirring,
remove
the sample
inlet
stopper,
and syphon
the liquid
to a level
Just
above
the
electrode
tips.
Replace
the stopper,
vacuum
purge
with
dry air,
and readjust
the stirring.
Syphoning
is
88

accomplished
by squeezing the air out of a plastic
wash
bottle
(provided),
inserting
its tube into the reaction
vessel and withdrawing
the unwanted solution.
9.

TROUBLE SHOOTINGGUIDE

9.1

10.

Follow
"Operating
Instruction"
booklet
supplied
with
instrument.
Please read.
THIS IS IMPORTANT for maximum
efficiency.
PARTS LIST

10.1

It is suggested the following

parts
stocked.
Note parts list
operating

10.1.1

Electrode,

10.1.2

Reagent,

10.1.3

Desiccant,

10.1.4

Burette

be purchased
instruction.

and

platinum
Karl

Fisher

Silica

(Refrigerate

unused

bottles)

Jel*

*Tel-Tale
Silica
Gel from Davison Chemical Co.,
Baltimore,
MD. 21203.
This is Grade 42, Mesh Size
6/16, comes in 1 lb. cans.
NOTE: Save reagent bottle
caps,
replacements
for cap with stopper.

87

drill

for

M-R-22

Free
Resins

Formaldehyde

in

Aldehyde

Phenolic

and

Furan

Type

SCOPE

i.i

When
Hydroxylamine
Hydrochloride
reacts
with
dissociated
Free
Formaldehyde,
Formaldoxime
is formed
with
a
quantitative
liberation
of Hydrochloric
Acid.

1.2

The
liberated
acid
is titrated
with
base.
This
method
used
since
it
is accurate
in the
presence
of
alkali
sensitive
materials
as well
as
in the
presence
of
aldehyde

2.1

phenolic

EQUIPMENT

AND

groups

MATERIALS

Equipment

2.1.1

pH

2.1.2

Ground

2.1.3

Beakers,

2.1.4

Burettes,

2.1.5

Graduate

2.1.6

Analytical

2.2

is

Meter

(Beckman
glass
150
25

or

equivalent)

dropping

bottle

ml.,

ml.

ml.

250

with

rubber

bulb,

15

ml.

(2)

Cylinders,

25

balance,

and

accurate

50

ml.
to

0.0001

gm.

Materials

2.2.1

Sodium

Hydroxide,

2.2.2

Sulfuric

2.2.3

Hydroxylamine
gm.
of
amine
solution
is

Acid,

0.5N,

before

2.2.4

Methanol,

CP

2.2.5

Distilled

water

PROCEDURE

3.1

METHOD
than

3.1.1
3.1.1.1

A
5%

Follow
Fill

0.1N

0.1N

Hydrochloride
- prepared
by
dissolving
salt
in 1 liter
distilled
water.
This
adjusted
to pH
4.0
with
0.5N
Sodium

Hydroxide

3.

0.5N,

use.

(formaldehyde

free)

- For
aldehyde-phenolic
free
formaldehyde:
in

duplicate:

the

medicine

dropping

88

resins

bottle

containing

with

the

less

resin.

70

3.1.1.2

By difference,
into
a 250 ml.

3.1.1.3

Add
20 ml. of
from
graduate
Note:

weigh
accurately
beaker.
methanol
cylinders.

and

3.00

20

ml.

of

gm.

of

sample

distilled

water

More
methanol
may
be added;
enough
to
completely
disperse
the sample.
In such
a
case
record
ml.
of methanol
used
and carry
out
a blank
with
the same
amount
of methanol
plus
20 ml. water.
For novolacs,
use methanol
only.

3 .i.i.4

Adjust
pH to 4.00 using
0.1N
sulfuric
acid
or 0.1N
sodium
hydroxide.
Employ
the electrodes
and stir
vigorously
with
a glass
stirring
rod after
each
addition
of titrant.
Do not touch
the electrodes
with
the stirring
rod.

3.1.1.5

Add
has

3.1 .i .6

Stir

3.1 .i .7

Titrate
the sample
with
0.5N
sodium
hydroxide,
using
the electrodes
and stirring
as above,
to pH 4.00.
Record
ml. sodium
hydroxide
used.

3.1.i.8

Run

3.2

3.2.1

3.3
3.3.1

3.4

3.4.1

50 ml. of the hydroxylamine

a pH of 4.00
from
a graduate
and

let

blank

on

stand

all

METHOD

above,
except
minutes.
C

- For

which

5 minutes.

reagents

at

METHOD
B - For aldehyde-phenolic
more
free
formaldehyde
As
40

hydrochloride
cylinder.

under

phenolic

(3.1.1.6)

resins

least

once

resin

containing

- Stir

containing

a day.

and

let

5%

or

stand

urea:

As in Method
A, except
under
(3.1.i.7)
- Add cracked
ice,
adjust
pH meter
to 10_C
temperature
setting
and
titrate
the sample
with
0.5N
sodium
hydroxide
using
the
electrodes
and stirring
as above
to pH 4.00.
Record
ml.
sodium
hydroxide
used.
METHOD
phenol

D - For furan
and less
than

resins
containing
both
5% free
formaldehyde:

urea

and

As in Method
A, except
under
(3.1.1.3)
- Add
20 ml.
methanol;
under
(3.1.1.5)
- Add
15.0 ml.
of
hydroxylamine
hydrochloride
reagent
which
has
a pH of
4.O0.

89

CALCULATION
mls.

4.2

If
mls.

0.5N

IN

NaOH

sodium
IN

_ Free
CH20
(using
3 gm. sample).

hydroxide

NaOH

is

x N
Wt.

= Free CH20
(using
gm. sample)

x 3.002
Sample

= % Free

NaOH

& exactly

used:

-ORmls.

N/2

CH20

7O

IN

NaOH

and

exactly

M-R-23
i.
i.i

2.
2.1

Chang's

Index

Measure

Degree

of

Cure

SCOPE
This
method
describes
a procedure
for
an arbitrary
measure
of
the
relative
degree
of
cure,
advancement,
polymerization
of liquid
aldehyde-phenolic
resins
aldehyde-phenolic
prepregs.
EQUIPMENT

AND

or
or

MATERIALS

Equipment

2.1.1

Buret,

2.1.2

Balance,

2.1.3

Triple

beam

2.1.4

Pipet,

25

2.1.5

Aluminum
5/8
inch

cups,

1.5

gm.,

2.1.6

Hypodermic
delivery

syringes,
needles

2.1.7

Oven,

2.1.8

Desiccator

2.1.9

Filtering

2.2

of

50

ml.
analytical,

sensitivity

of

0.0001

gm.

balance
ml.

forced

diameter

ml.,

i0

ml.,

3/8

30

inches,

ml.

height

with

air

crucibles,

fritted

glass,

medium

or

fine

Materials

2.2.1

Distilled

2.2.2

Acetone

2.2.3

Filter

3.

SAMPLING

3.1

LiqUid

water

paper,

Whatman

#41,

#42,

or

equivalent

resins.

3.1.1

i0

grams

for

resins

between

50%

and

100%

3.1.2

20

grams

for

resins

between

30%

and

50%

3.1.3

For
resins
proceed
to

solids,

measure

near
4.3.

20%

71

solids

solids
solids
per

4.2

and

3.2

Prepreg

materials

3.2.1

15 grams
content

for

materials

of

between

40%

and

50%

dry

resin

3.2.2

20 grams
content

for

materials

of

between

30%

and

40%

dry

resin

4.
4.1

4.1.1

4.1.2

4.2

PROCEDURE
Preparation
solutions

as

of intermediate
follows:

Prepare

solutions:

duplicate

Liquid
resin.
Mix
in a flask
the appropriate
sample
size
weighed
on the triple
beam
balance,
with
about
ml.
of acetone.
Determine
the resin
solids
of the
mixture
according
to the method
of 4.2.
Prepre@
materials
Soak
the appropriate
sample
chopped
to about
i/2" x 1/2"
and weighed
in a
a triple
beam
balance,
with
50 ml. of acetone
minutes
minimum.
Swirl
occasionally.
Filter
extracted
material
through
Whatman
#41 or #42
paper.
If the material
contains
fine
filler,
filtration
may
require
the use
of a medium
or
fritted
glass
filtration
crucible.
Determine
solids
of the solution
per
4.2.
Determination
of resin
Determine
resin
solids
follows:

50

size,
flask
on
for
15
the
filter
thorough
fine
the resin

solids
of intermediate
solutions.
of intermediate
solutions
as

4.2.1

Weighin 9 and devolatilization

Weigh
on the
analytical
balance
by difference
from
2 ml. syringe,
2 ml of
intermediate
solution
or liquid
resin
of 3.1.3.
Discharge
the solution
into a tared
aluminum
solids
dish.
Volatilize
in a forced
air oven
at 275 + 5F.
for 30 minutes.
Cool
in a desiccator
and
reweYgh.

4.2.2

Calculation
follows:
Resin

4.3

4.3.1

of

resin

solids,wt.%=

Preparation
of
final
solution

solids.

wt.
Wt.

of
of

4.0%
resin
as follows:

sample
sample
solids

Calculate

after
before

resin

160
solids

72

from

volatil,
volatil.

solution.

Calculations
for dilution.
Calculate
grams
of intermediate
solution
to be
W1 =

resin

4.2.2

w l,
used

solids

Prepare

as

i00

the

the weight
as follows:

in

Calculate
follows:

W 2,

the

weight

of

W 2 = 40

acetone

to

be

used,

as

- W1

4.3.2

Dilution.
On the analytical
balance,
introduce
W 1 into
a 125 ml.
flask
from
a large
syringe
as quickly
as
possible
to the nearest
0.001
gm.
Immediately
introduce
W 2 to the nearest
0.001
gm.
into the
flask
from
a large
syringe
as quickly
as possible.
Long,
steel
delivery
needles
simplify
these
operations.
Stopper
the
flask
and swirl
lightly
to mix.

4.3.3

verification
of 4.0%
resin
solids.
For adequate
precision,
solids
must
be between
3.95%
and 4.0%.
Occasionally
verify
resin
solids
by the procedure
4.2.2
except
use
an 8 ml.
sample
size.
This
change
sample
size keeps
the
total
weight
of resin
used
roughly
equal
for both
determinations.

4.4

5.1

of
in

Titration.
Pipet
25 ml.
of the final
solution
of 4.3
into
a 125 ml.
erlenmeryer
flask.
Titrate
with
distilled
water
to the first
perceptible,
persistent
end point.
Recognition
of the end point
is made
easier
if a strong
compact
light
beam
is shined
through
the flask
during
titration.
Colloidal
particles
scatter
the beam
at the
end point.
CALCULATIONS

AND

REPORTING

Reporting.
Report
the average
number
of ml.
of water
used
as Chang's
Index.
Duplicate
determinations
should
be considered
suspect
if they
differ
by more
than
0.3 ml.

73

M-C-I
l

Linear

Density

of

Yarn

and

Cord

Expressed

in

Denier

SCOPE

i.i

ThiS
method
covers
the determination
of linear
density
tire
or industrial
yarn
or cord
from
a high
traverse
package;
such
as, a pin,
tube,
or bobbin.
Linear
density
is corrected
to commercial
moisture
regain
and
expressed
in denier
units.

1.2

This
method
Section
II

2.
2.1

APPLICABLE
ASTM

is
and

with
ASTM
Option
3.

Methods

885-75,

DOCUMENTS

Standards

D 123-75
Materials

Definitions

D 885-75
Industrial
Fibers.

Testing
Tire
Cords,
Tire
Cord
Fabrics,
and
Filament
Yarns
made
from Man-made
Organic-Base

1907-75

Test

D 1909-68
Table
Textile
Fibers.
3.

consistent
D 1907-75,

of

of

for
for

Yarn

Terms

Relating

Number

by

Commercial

the

to

Textile

Skein

Moisture

Method

Regains

for

DEFINITIONS

3.1

Density,

3.2

Denier,

3.3

Commercial
moisture
regain,
- an arbitrary
value
formally
adopted
asthe
regain
to be used
with
weight
of the
moisture-free
material
when
calculating
(i) the yarn
number,
(2) the commercial
or legal
weight
of a shipment
of delivery
or any specific
textile
material,
or (3) the
weight
of a specific
component
in the analysis
of fiber
blends.

4.
4.1

5.

SUMMARY

linear,
-

OF

- mass

a measure

of

per
linear

unit

length

density

in

gm.

per

METHOD

A skein
of yarn
is wound
on a reel,
oven-dried,
weighed.
The
linear
density
is calculated
from
weight
and length
of the skein.
USES

AND

9000

SIGNIFICANCE

74

and
the

m.

5.1

The determination
of linear
density
consists
of measuring
a length
of yarn
or cord,
drying
and weighing
it.
Since
yarns
and cords
are extensible
to varying
degrees,
it is
essential
to measure
length
by reeling
under
controlled
tension.

5.2

Predried
air is used
in drying.
If predried
air is not
used,
then
small
amounts
of moisture
will
be retained
by
the fiber
in the oven,
the actual
amount
varying
with
the
type
of fiber,
the temperature,
and the
relative
humidity
of the
air entering
the oven.

APPARATUS

6.1

Reel.,
1 m. + 0.4%,
equipped
with
tensioning
device
and a revolution

6 2

Brabender
Moisture
Tester,
Semi-automatic,
Type
FD or
FDA,
or equivalent,
supplied
with
a current
of air at
rate
sufficient
to change
the air
in the oven
at least
once
every
4 min.
the current
of air shall
be predried
(less
than
0.01
grams
of water
per
i000
L.) by
circulating
through
dehydrating
units.

6.3

7.1
8.

Rack
for
or cone,
SAMPLING
One

holding
supply
side unwinding
AND

skein

a yarn
or
counter.

cord

package,
over-end
for
for bobbins
of cord.

yarn

tube

SPECIMENS

specimen

is

taken

from

each

sample

PROCEDURE

8.1

Adjust

8.2

Position
sample
package
on holder
and lace
through
guides
and tension
device
and attach
to an arm of the reel.
Let-off
is over-end
for yarn
tube
or cone
and
from
side
for bobbin
or cord.
Set

yarn

counter

or

to

cord

tension

device

on

reel

to

zero

Wind
to exact
revolutions
skeins:
Nominal
Yarn
or
Cord
Denier
ii00/i

the

following

length

Revolutions
81

1650/1

55

2200/1

41

75

oz.

Nominal Yarn
or
Cord Denier

Revolutions

1100/2

37

1650/2

24

1650/3

15

2200/3

ii

8.5

Turn reel so that arm to which the end was attached

is in
the same position
as at the start,
with scissors
cut and
remove the skein from the reel.
Fold the skein to fit
into the Brabender drying
cup.

8.6

Dry to constant
weight in the Brabender Moisture
Tester
at 105 + 2_ C.
In practice
it has been found that the
equipment described
and starting
with a preheated
Brabender,
constant
weight is reached in 1 hr.

8.7

with the test specimen cup in position

over the built-ln
balance,
lift
the cup with the control
lever and turn
"On" the illuminated
dial.
Add gram weights
to the
weight cup to bring the scale reading in the illuminated
dial between "7.6" and "8.6".
Record the weight added to
the weight cup to the nearest 1 mg and the dial
reading
to the nearest 0.i percent.
CALCULATIONS
Calculate
using the

the linear
density
equation below.

Linear

Density,

denier

(21.0

- W

- 0.I
L

B)

to the nearest

9000

(i

whole

denier

+ R)

where:
W
B
R
L

= weight
added
to the Brabender
weight
cup,
gm.
= reading
on the Brabender
illuminated
dial,
%.
= commercial
moisture
regain,
for
rayon
ii.0
percent,
expressed
as a decimal.
= length
of yarn
or cord
in skein
specimen,
m.

Note:
The expression
(21.0
- W
weight
in grams
of the specimen
built-in
balance
in the Brabender

76

- 0.I B) is the
as determined
by the
Moisture
Tester.

i0.

REPORT

i0 .i

State
that
STM
003-75.

the

10.2

Report

following

the

10.2.1

Linear

10.2.2

Identity

density
of

specimen

to

was

tested

as

information:
nearest

analyst.

77

whole

denier

directed

in

AVTEX

M-C-2

i.

Tensile
Twisted

Properties
Materials

of

Yarn,

Cord,

and

Fabrics

of

SCOPE

i.i

This
method
covers
the determination
of tensile
properties
of tire
or industrial
yarns
made
of rayon,
cords
twisted
from such yarn
and fabrics
woven
from
such
cord,
products
that
are made
specifically
for use
in the
manufacture
of pneumatic
tires
or reinforcing
other
rubber
goods
and for other
industrial
applications.

1.2

Options
and
(2)

1.3

This
method
applicable

2.
2.1

are included
for the
oven-dried
specimens.

APPLICABLE
ASTM

testing

is consistent
with
except
as noted.

ASTM

of

(1)conditioned

885-72

for

sections

DOCUMENTS

Standards

D 76-67,
Textile

Specifications
Materials

for

of

Tensile

Terms

Testing

Relating

to

Machine

for

D 123-75,
Materials

Definitions

Textile

D 885-75,
Industrial
Fibers

Testing
Tire
Cords,
Tire
Cord
Fabrics
and
Filament
Yarns
Made
From
Man-Made
Organic

Base

3.

DEFINITIONS

3.1

Atmosphere
for testing
tire
cords
and
industrial
yarns,
air maintained
at a relative
humidity
of 5_ + 2 percent
and at a temperature
of 24 + 10 C. (75 + 2OFT.

3.2

LASE,
load
at specified
elongation
the load-elongation
curve.

as

interpreted

from

3.3

EASL,
elongation
the load-elongation

as

interpreted

from

3.4

For
definitions
of tensile
used
in this method
refer
and Method
D 885-74.

at

specified
curve.

load

test
and other
textile
terms
to ASTM
Definitions
D 123-75

78

SUMMARY

OF

METHOD

4.1

A specimen
of yarn
or cord
is clamped
in a tensile
testing
machine
and then
stretched
until
broken
Breaking
load,
breaking
elongation,
load
at a specified
elongation
(LASE)
and elongation
at a specified
load
(EASL)
are obtained
directly

4.2

This
method
content
of

4.2.1

options
with
respect
to moisture
at the time
of testing:

Option
testing

i, conditioned
(in
with
the
standard

Option

2,

This method
bobbins
and
4.4

covers
two
the specimens

moisture
atmosphere

equilibrium
for
for testing)

oven-dried.
covers
taking
cord
specimens

specimens
from
tubes,
cones
from woven
fabric
tabbies

or

Testing
of yarn
or cords
other
than
rayon
usually
require
different
conditioning
prior
to testing
and different
values
of reading
LASE,
Refer
to ASTM
D 885-75.
USES

AND

SIGNIFICANCE

5.1

The levels
of tensile
properties
obtained
when
testing
yarns
and cords
are dependent
on the history
of the
specimen
and on the specific
conditions
used
during
the
tests.
Among
these
conditions
are rate
of loading,
type
of clamps,
gage
length
of the specimen,
temperature
and
humidity
of the atmosphere,
rate of airflow
across
the
specimen
and temperature
and moisture
content
of the
specimen.
The
relative
importance
of these
factors
varies
with
each
type
of fiber.
Testing
conditions
accordingly
must
be specified
precisely
in order
that
test
results
on a specific
sample
will
be reproducible

5.2

For further
statement
885-75,
Section
13.

on

uses

and

significance

see

ASTM

APPARATUS

6.2

Tensile
Testin 9 Machine
- Instron
with
C or CT
The instron
is a single-strand
testing
machine
constant-rate-of-extension
type
(CRE).
The
specifications
and methods
of calibration
and
verification
shall
conform
to ASTM
D 76-67

Load
cell.
of the

Clamps

operated

- Pneumatic

capstan

type,

automatically

For

yarn

-Instron

4C,

Cat.

2714-004

For

cord

-Instron

4D,

Cat.

2714-006

79

6.3

Pretensioning
A2-93.

6.4

Oven
- A ventilated
drying
oven
controlled
in a
e%-emperature
range
of 105 + 3C.
The oven
shall
be
supplied
with
a current
o7 air sufficient
to change
the
air once
every
4 min.
Exit
port
for air must
be open.
The
specimens
shall
be protected
from direct
radiation
of
the
heating
units.
The oven
shall
be supplied
with
air
from
the testing
room,
see
3.1.
Ovens
meeting
these
requirements
are Precision
Scientific
Cat.
1236
or Freas
Model
835A.

6.5

Drying
Rack
- A
See Figure
I.

6.6

Cl_!_s - 1
each
group
Denier

Device

in.
of

Reel

6.9
7.
7.1

Pressure

removable

Bulldog
or
specimens.

- hand

Twist
Counting
operated.

- Instron

rack

Hunt

to

No.

- Alfred

8.1

4D

fit

O,

(Cat.

into

two

A58-29

the

or

oven,

required

6.3

for

Suter,

20

in.,

hand

Tape.

CONDITIONING
Option
i, Conditioned.
Samples
shall
be at equilibrium
with
the standard
atmosphere
for testing,
3.1.
Equilibrium
shall
be reached
by adsorption.
Exposure
overnight
has been
found
to be sufficient.
Note
i.
Note
1 - When
inter-laboratory
percent
moisture
regain
in the
testing
shall
be reported.
A 1
corresponds
to about
2 percent
strength,
inverse
relationship.

7.2

or

operated.

Instrument

Sensitive

4C

comparisons
were
made,
yarn
cord
at the time
of
percent
change
in regain
change
in tensile

option
2, Oven-dried.
Cord
samples
overnight
in the standard
atmosphere
setting
and equalizing
of twist.
PREPARATION

AND

HANDLING

OF

shall
for

be conditioned
testing
to allow

SPECIMENS

All yarn
specimens
shall
be tested
for twist.
Box
process
yarns
and pre-twisted
continuous
process
yarns
specimens
shall
have
3 tpi,
Z twist,
inserted
with
the
twist
counting
instrument
prior
to mounting
in the
tensile
testing
machine
for conditioned
specimens
and
prior
to mounting
in the dryer
racks
for oven-dried
specimens.
See ASTM
D 885-75.

8O

8.2.1

Yarns
with
twist
and cords.
Specimens
are taken
directly
from the tube,
cone,
bobbin
or tabby
for
mounting
in the tensile
testing
instrument.

8.2.1.1

For samples
on tubes,
cones
or bobbins,
specimens
shall
be taken
from
the center
portion
of the
traverse
since
yarn
or cord
in the transverse
reversal
at either
end of the package
can contain
abnormal
twist
that
may not equalize
along
the length
of the yarn
or cord
in handling
the specimen.

8.2.1.2

Strip
at least
two yards
of yarn
or cord
to eliminate
yarn
or cord
at the end
of the transverse
and to
eliminate
yarn
or cord
that
may have
lost
twist
by
running
out to a free
end.

8.2.1.3

Hold
the end of the yarn
or cord
firmly
in one hand.
Unwind
approximately
20 in. and with
the other
hand
grasp
the yarn
or cord
firmly
and then
cut with
scissors.

8.2.1.4

The specimen
shall
into
a radius
less
twist.
If it does
specimen.

8.2.1.5

not be allowed
to kink
or bend
than
1 in. to prevent
migration
discard
it and take
another

of

The
specimen
shall
be
mounting
in the clamps
prevent
loss of twist.

held
firmly
until
after
of the Instron
instrument

8.2.1.2

Yarns

Select

8.2.2.1

Attach
end in right-hand
clamp
of the twist
counting
instrument.
With
left-hand
clamp
set at 20 in. lace
yarn
through
left-hand
clamp
and the pre-tensioning
device.
Pull
to pre-tension
the yarn
specimen
and
close
the left-hand
clamp.
Insert
60 turns
z twist
(3 tpi_.

without

NOTE
8.2.2.2

8.3

tpi

Remove
the
instrument

Option

8.3.1

Yarns

2.
with

is

twist.

threads

per

specimen
from
and handle
as

specimens

as

in

to

8.2.1.1

inch.
the twist
counting
in 8.2.1.4.

Oven-dried.
twist

and

cord

on

cones

or

bobbins.

8.3.1.1

Strip
sample
8.2.1.2.

8.3.1.2

Attach
the end of the yarn
or cord
to an arm of the
denier
reel and unwind
onto
the reel
sufficient
revolutions
of yarn
or cord
to provide
the number
of

and

hold

specimens

81

as

in

8.2.1.i

&

specimens required
from a package.
Bobbins shall
unwound from the side.
Tubes or cones shall be
unwound

8.3.1.3

over-end.

Prior
to cutting
package,
wrap
a
around
the band
press
firmly
to
around
the reel
sensitive
tape.
Mark

be

on

the

the yarn
or cord
from
the supply
piece
of pressure
sensitive
tape
of yarns
or cords
from
a package
hold
the band.
Approximately
20
apply
a second
piece
of pressure

tape

identification

of

the

and
in.

sample.

Cut the band

at the ends
on the outside
of the 20 in.
section,
apply
a clip
to either
end and hang
in the
dryer
rack.
As in 8.2.1.4
the band
of specimens
shall
not
be allowed
to kink
or be slack
when
hung
between
hooks
across
from
each
other
in the
rack.
If
band
is not slack
or if it sags
excessively
to allow
twisting
or kinking,
discard
the band
and wind
another
adjusting
the distance
between
the two pieces
of pressure
sensitive
tape.
Yarns

without

Insert
twist
8.2.2.2.

twist.
and

Select
handle

specimens

specimens

as

as

in

8.2.1.i.

in

8.2.2.1

&

8.3.2.2

Transfer
twisted
specimen
to two pieces
of pressure
sensitive
tape,
mounted
adhesive
side up 20 in. apart
on table.
When
sufficient
specimens
have
been
so
prepared
from the tube
or cone,
apply
a second
strip
of pressure
sensitive
tape
on top of the specimens
and the tapes
on the table.

8.3.2.3

Mark
on
sample.

8.3.2.4

Remove
clips.

the

tape

on

one

the tapes
from
Hang
clips
in

end

the
the

the

table
dryer

identification

of

and mount
each
end
rack as in 8.3.1.5.

the

in

Note
2 - Special
dryer
racks
may
be used
where
the
twisted
specimens
are mounted
in spring
clips
of the
racks
when
the specimen
is removed
from
the twist
counting
instrument.
Cords

in

fabric

tabbies.

Test
tabbies
of tire
cord
fabric
shall
be mounted
on
a stiff
medium;
i.e.,
paperboard,
to prevent
kinking
of the cords.
If not so mounted
or if cords
show
evidence
of kinking,
and replacement
tabby
is not
available,
it shall
be noted
on the test
report.
82

8.3.3.2

With scissors
an area about
specimens for

cut the filling

yarns and remove from
3/4 in. wide to provide
sufficient
cord
testing.
Cut
into
the heavy
tabby
area

about
1 in. parallel
and
then
cut across
across
the cords
to
in a clip.
like
manner

Cut
and

cord
specimens
kinking
of the

8.3.3.3
8.3.3.4

8.3.4

9.
9.1

to the band
of cords
selected
the cords
selected
and then
cut
remove
the band
of cords.
Mount

into
mount

the band
rack
as

tabby
area
in
of the band
of

in a clip.
Hold
clips
to prevent
cords
at any time
as in 8.2.1.4.

Identify
the band
of
small
piece
of paper
Hang
dryer

the other
heavy
the second
end

of
in

Place
rack
in the
for yarn
and three
hours.

cord
under

specimens
with
marking
one of the clips.

cord
specimens
8.3.1.5.

by

the

clips

in

on

the

oven
and dry for a minimum
of an hour
hours
for cord
or a maximum
of seven

PROCEDURE
Adjustments

to

Instron

testing

instrument.

9.1.i

Select
a load
scale
such
that
the estimated
breaking
load
of the specimen
is below
90 percent
of the fullscale
load
of the Instron
and the area
of interest
of
the
initial
part
of the load-elongation
curve;
i.e.,
LASE
or EASL,
is above
10 percent
of the
full-scale
load
of the Instron.

9.1.2

Rate
of operation
of the Instron
cross-head
i00 percent/min
of the nominal
gage
length
specimen;
i.e.,
I0 in./min.

9.1.3

Rate
of Operation
of the Instron
chart
paper
shall
200 percent/min
of the nominal
gage
length
of the
specimen;
i.e.,
20 in./min.
Note
3.

shall
of the

be

be

Note
3 - This
combination
of rates
of cross-head
and
chart
paper
is readily
obtainable
with
standard
gearing
supplied
by Instron.
One
inch of chart
paper
on the
abscissa
(time)
axis
is equal
to 5 percent
extension
of
the
specimen
which
facilitates
interpreting
initial
areas
of the load
elongation
curve,
LASE
and EASL,
for
a high
modulus
material
as oven-dried
rayon.
This
rate
of cross-head
movememnt
is at variance
with
that
specified
in ASTM
D 885-75,
Section
15.2
and Table
2
i.e.,
120 percent/min.
This
difference
is insequential
as to its effect
on tensile
properties
of yarn
or cord
either
from
the rate
of extension
or the cooling
effects
on oven-dried
specimens.
83

9.1.4

Adjust the Instron

so that,
in the starting
the distance
from nip to nip of the clamps
axis
of the specimen
(including
with
the snubbing
surfaces)
is i0 + 0.I in.

9.1.5

the

position,

portion

Adjust
the pre-tension
device
to 4 oz
on the specimen
with
the clamps
closed
of cross-head
movement.

along
the
in contact

(113 g) tension
prior
to start

Note
4 - the amount
of tension
developed
in the
specimen
varies
significantly
with
the
rate
of pull
on
the specimen
to actuate
the pneumatic
clamp.
A very
slow
pull
produces
a low tension;
a hard
jerk
a high
tension.

91.6
9.2
9.3

Adjust
air pressure
yarn
and 2 ply cord

for
and

pneumatic
clamps
40 psi for
3 ply

Option
1 - Test
the conditioned
atmosphere
for testing.

specimens

Option
2 - If more
than
25 seconds
elapse
the oven-dried
specimen
from
the oven
and
the testing
machine,
discard
the specimen
another.

to 30
cord.
in

the

psi

for

standard

between
taking
breaking
it in
and take

Note
5 - This method
covers
testing
oven
dried
specimens
directly
from
the oven;
as such the time
from
the oven
to the
instant
of break
of the specimen
is important
since
it affects
the temperature
of the specimen,
5.1.
This
is at variance
with
ASTM
D 885-75,
Section
22.2.3,
where
provisions
are made
for cooling
the dried
specimen
to room temperture
before
testing.
The latter
is a more
precise
and sophisticated
provision
of the method.

9.4

9.5

Remove
thespecimen
of yarn
or cord
from
the
sample
package
or tabby
for conditioned
testing
Option
i, or
from
the oven
for oven-dried
testing,
Option
2, and
handle
in such
a manner
that
no change
in twist
can occur
prior
to closing
the jaws
of the clamps
on the specimen.
Do not
touch
with
the bare
hand
that
portion
of the
specimen
which
will
be between
the nips
of the clamps.
Lace
the specimen
over
the horn
and down
between
the jaws
of the upper
clamp
and close
the clamp
by pressing
the
cord
in the left
hand
against
the pneumatic
switch
on the
upper
clamp.
Lace
the specimen
around
the horn
and up
through
the Jaws
of the lower
clamp
and over
the pulley
of the pre-tension
device.
Close
the lower
of the specimen

clamp
with
a sharp
in the
right
hand.

84

steady
Note

pull
on
4 above.

the

end

9.6

With the Instron

clamp set on "Auto",
the cross-head
automatically
starts
moving to separate the clamps when
the lower clamp is closed.

9.7

Discard
the test on a specimen
of the nip of a jaw.

that

9.8

Repeat 9.2
specimens.

required

9.9

Read from the chart the individual

specimen breaking
load
in pounds and elongation
in percent,
and the elongation
at specified
load (EASL) or load at specified
elongation
(LASE) as required
by the specification.

through

9.6

for

the

breaks

within

1/8

in.

number of

9.10 To facilitate
reading the chart do not superimpose more
than five breaks on the same starting
point on the chart.
i0.

CALCULATIONS

I0.I

Calculate
ibs.

the

average

breaking

load

i0.2

Calculate
the
0.i percent.

average

breaking

elongation

10.3

Calculate
the average
by the specification.

10.4

For yarns calculate

the average
grams per denier to the nearest
Breaking

Tenacity,

where:

1
ii.
ii.I

S
D

to the

to the

gf/d

breaking
tenacity
0.01 gf/d.

following

used.

information.

ll.l.l

Option

(Conditioned

11.i.2

Average

breaking

load.

11.1.3

Average

breaking

elongation.

11.1.4

Average

LASE

ii.1.5

Average

breaking

or

nearest

EASL,

where

tenacity,
85

in

S(453.6)
D

REPORT
the

0.1

EASL or LASE where and as required

= average
breaking
load
in pounds
= linear
density
in denier
as determined
ASTM
Method
D 885-72,
section
ii, or
= grams
force
per denier
= 453.6
grams

gf/d
oz.

Report

nearest

or

oven-dried).

specified.
for

yarn

only.

by
M-C-I

11.1.6

Full

11.1.7

Number

ii .1.8

Identification
tests.

of

technician

Identification

of

sample.

Any

scale
of

load

setting

specimens

abnormal

of

for

condition

each

of

Instron

in

pounds.

test.
who

specimen,

carried

out

Ref.

the

8.3.3.1.

Note
6.
Designation
is
a sequential
number
for
ASTM
Standard
Test
Methods
and
Practices
followed
by
a two
digit
number
indicating
the
year
of
issue
or
revision.
A small
case
letter
indicates
subsequent
revision
in one
year,
as
I02-75A.
Note

7.

Revision

Note
test.

8.

tpi

is

editorial
turns

(or

86

except
twists)

for
per

8.3.4.
inch

in

this

"O

o_
I,=.

O
o_

O9

Eo
_"O4
U-,--

--

-,-I

d
o--

oO

o--

T"-

LO
T--

- (_.

87

M-C-3
1.

Twist,

Determination

in

This
method
covers
direction
of twist

1.2

For cords,
this method
twist
of the cords
and
before
cording.

1.3

This
method
Section
32

2.1

APPLICABLE
ASTM

is
and

the determination
in single
filament

of amount
yarn
or

covers
the determination
the twist
in the single

consistent
D 1423-71,

with
ASTM
Methods
D
Section
9.3 through

and
cord.
of the
yarn

8859.5.

75,

DOCUMENTS

Standards

D 123 - 75
Materials.

Definitions

D 885 - 75
Industrial
Fibers.

Testing
Filament

D
3.

Cord

SCOPE

1.1

2.

Yarn,

1423

71

Twist

of

Terms

Tire
Cords,
Yarns
made

in

Yarns

by

Relating

Tire
from

the

to

Textile

Cord
Fabrics
and
Man-Made
Organic

Direct-Counting

Base

Method.

DEFINITIONS

3.1

Twist,
the number
of turns
about
its axis
l-_h
observed
in a yarn
or other
textile
expressed
in turns
per inch.

3.2

Direction
of twist,
the direction
of twist
in yarns
and
other
textile
strands
is indicated
by the capital
letters
"S" and
"Z"
Yarn
has S twist
if, when
the yarn
is held
in a vertical
position,
the visible
spirals
or helices
around
its central
axis
conform
in direction
of slope
to
the middle
portion
of the letter
"S" and Z twist
if the
visible
spirals
or helices
conform
in direction
of slope
to the central
portion
of the letter
"Z."
When
two or
more
yarns,
either
single
or plied,
are twisted
together,
the letters
"S" and
"Z" are used
in a similar
manner
to
indicate
the direction
of the last
twist
inserted.

3.3

Tire
Cord,
a twisted
or formed
structure
composed
of two
or more
single
or plied
industrial
yarns.
Each
individual
single
or plied
yarn
element
in a cord
has the
same
nominal
twist,
direction
of twist,
length,
and
tension.
The direction
of twist
is used
to combine
the
single
or plied
yarn
elements
into
a cord
structure
in a
direction
opposite
to that used
in the yarns.

88

per unit
strand

of

3.4

Cord
twist,
the amount
of twist
in a cord
made
from
or more
single
or plied
yarns.
Cord
twist
is based
the
initial
length
of a cord
specimen.

3.5

Sin@le
twist,
the
element
in a tire
the element
after

3.6

Ori@inal
twist,
the twist
yarn
as the component
was
more
complex
structure.

3.7

Twist
take-up,
extile
strand
of the original

3.8

For definitions
of
to ASTM
Definitions
SUMMARY

OF

amount
of twist
cord
structure
twist
has been

the change
caused
by
untwisted

two
on

in each
single
yarn
based
on the length
of
removed
from
the cord.

in a single
or plied
before
incorporation

or cabled
into the

in length
of a yarn
or other
twisting
expressed
as a percent
length.

other
terms
D 123-75.

used

in

this

method

refer

METHOD

The turns
of twist
in a known
length
of yarn
are counted
as they
are being
removed
by rotating
one end of the
specimen
while
the other
end remains
fixed
until
the
elements
of the yarn
being
tested
are parallel
and free
from twist.
The number
of turns
required
to remove
the
twist
is reported
per unit
length.
4.2

The
amount
of twist
in the component
elements
of a plied
or cabled
yarn
is determined
as follows:
one end of the
yarn
is fixed
while
the other
end is rotated
until
the
structural
components
are parallel.
Any one or all of
these
components
may
then
be used
as test
specimens.
USES

AND

SIGNIFICANCE

The determination
of twist
in a straight
section
of a
yarn
is notthe
simple
straight-forward
operation
it
appears
to be,
for the test
results
may
be greatly
influenced
by variations
in test
procedures
and
techniques.
In all manipulations,
extreme
care
is
necessary
to prevent
rotation
of either
end
of the
specimen,
which
would
alter
the twist.
5.2

The twist
in a yarn
before
it is packaged
may
be
different
from that
of the yarn
after
it has been
withdrawn
from the package
because
of changes
in tension
and the effect
of the method
of withdrawal.
If the yarn
is withdrawn
over-end,
a slight
increase
or decrease
in
twist
will
take place,
depending
upon
the direction
of
the twist
in the yarn,
the direction
of winding
on the
package,
and the length
of the turn
(or wrap)
on the
package.

8S

5.3

5.3.1

5.4

The optimum amount of twist

depends upon the use for
which the yarn is intended.
The amount of twist
affects
both the strength
and elongation
properties
of the yarn
with increased
twist
being associated
with increased
elongation.
The relationship
between twist
and strength
is more complex.
In filament
yarns,
some twist
(up to 7 tpi)
(280 tpm)
or a suitable
sizing
is desirable
to facilitate
textile
operations.
A small increase
results
in a loss in
strength.
However, higher twist
in such yarns may be
used to subdue luster
or increase
elongation,
or to
secure other special
effects,
as in crepe fabrics.
For

further

twist,

6
6.1

refer

information
to

6.3

Pick

7.2

Uses
and Significance
D 1423-71,
Section

of
5.

Twist
tester,
Alfred
Suter,
Precision
Scientific
Co.,
or
equivalent
consisting
of a pair
of clamps,
one of which
is rotatable
in either
direction
and positively
connected
to a revolution
connector.
The
tester
may
be handor
power-driven.
The position
of one clamp
(or both
clamps)
shall
be adjustable
to accommodate
specimens
of the
lengths
of i0 and 20 in. and to permit
measuring
the
change
in length
during
untwisting.
Means
shall
be
provided
for applying
the specified
tension
of the
specimen
and
for determining
the specimen
length
with
an
accuracy
of + 0.002
in.
(0.5 mm).
The movable
but
nonrotatable-clamp
shall
be capable
of being
traversed
with
substantially
no friction
to permit
determining
the
untwisted
length
of the specimen
under
the
specified
tension.
The counting
device
shall
be re-setable
to zero
count
and shall
indicate
the
total
number
of turns
to the
nearest
whole
turn.
TensioningWeights,

7.1

on
Method

APPARATUS

6.2

7.

ASTM

for

Twist

Tester,

1 oz

and

4 oz.

needle

SAMPLING
Select

yarn

or

cord

samples

to

represent

the

test

lot.

When
sampling
tubes,
cones,
or bobbins,
take
specimens
from
the side,
not over
end,
of the package,
and from
the
center
of the traverse,
not at the ends
of the package.
This
is extremely
important
in taking
specimens
for twist
and tensile
tests
since
the yarn
or cord
structure
is
disturbed
and twist
migrates
at a traverse
reversal
and
when
taking
a specimen
for test purposes
the twist
is not
as likely
to return
to its original
location
as when
the
yarn
or cord
is removed
from
the package
in production.
9O

7.3

When
sampling
fabric
tabbies,
its mounting
board.
Cut the
them
from
areas
of the fabric

leave
filling
to be

the tabby
mounted
yarns
and
remove
sampled.

on

PROCEDURE

8.1

Set the clamps

to secure
a nominal
gage
length
of
20 + 0.02
in. for yarn
and cord
from
bobbin
of i0 + 0.02
in.-for
cord
from
fabric
tabby.
For
the Alfred
Su_er
Precision
instrument
this
is accomplished
by setting
the
assembly
holding
the left
side
clamp
fixture
to a setting
of 17 + 0.02
in. for bobbin
specimens
and 7 + 0.02
in.
for taSby
specimens.
Set the counter
to zero.
Set the
tension
in the left
side clamp
for 4 oz.
Lock
the left
side
floating
clamp
with
the floating
pointer
at 3 in.

82

with
the yarn
or cord
package
to be tested
located
near
and behind
the twister
testing
instrument,
strip
yarn
or
cord
from
the package
by unwinding
from
the side
for
about
3 yd. to a side yarn
or cord
that
may
have
lost
twist
due
to an unrestrained
end.
Continue
stripping
until
yarn
or cord
has passed
a traverse
reversal
so that
the specimen
to be tested
will
have
come
from
the center
portion
of the package,
7.2.

8.3

Without
releasing
the yarn
or cord
lace
it through
the
clamp
on the right
side
of the
instrument.
Tighten
the
clamp.
Guide
the specimen
through
the clamp
at the left
and around
the hook
of the tensioning
device.
Pull
on
the end
of the specimen
until
the pointer
on the floating
left
side
clamp
reads
exactly
3 in.
Tighten
the left
clamp
on the specimen.
Release
the left
side
clamp
device.

8.3.1

8.4

when
mounting
specimens
of cord
from
a fabric
tabby,
grasp
one cord
near
the heavy
end of the tabby,
cut the
cord
between
the point
grasped
and the heavy
end of the
tabby.
Without
releasing
the cord
lace
it through
the
right
clamp
and tighten.
Release
the cord.
Grasp
the
other
end of this
cord near
the other
heavy
end of the
tabby.
Cut the cord
between
this
point
grasped
and the
heavy
end of the tabby.
Hold
taut
to prevent
the cord
specimen
from going
slack
and kinking.
Proceed
as in
8.3 to lace
the left
side clamp.
Set
the gearing
to the right
side
clamp
to untwist
the
specimen
with
the counter
moving
in an increasing
direction.
Remove
the twist
completely
by turning
the
right
side
rotation
clamp
until
the cord
elements
are
parallel
as determined
by passing
a pick
needle
between
the untwisted
elements
from one clamp
to the other.
For
a yarn
the
right
side side
clamp
is rotated
until
the
filaments
are essentially
parallel
as determined
by
91

passing
to the
number
number.

8.5

9.1

a pick
needle
within
the
filaments
from
one clamp
other.
Record
the direction
of twist
and the
of turns
in the specimen,
to the nearest
whole

For a cord
specimen
the twist
in the single
element
is
determined
by removing
by cutting
all but one of the
single
elements
(yarns)
between
the clamps.
The yarns
removed
are cut near,
within
0.25
in, of both
clamps.
Without
changing
the original
tensioning
weight
record
the length
of the one single
yarn
remaining
by reading
the scale
on the floating
left
clamp.
This
value
is
added
to the setting
for the left
assembly,
8.1.
CALCULATIONS
Calculate
to
each
specimen
Twist,

tpi

the
in

nearest
0.i tpi
turns
per
inch.

the

amount

of

twist

in

= N/L

where:
N

= number
of turns
to the nearest
whole
number
observed
in the specimen
of cord
or single
element.
= length
of the specimen
to the nearest
0.05
in.
before
untwisting,
8.1 for an original
yarn
or
cord,
8.5 for an element
of a cord.

9.2

Calculate
the
the
specimens

i0.

REPORT

i0.i

State
AVTEX

10.2

Report

10.3

Average
cord.

10.4

Direction

10.5

Identity

average
tested.

twist

that
the specimens
STM 006-76.
the

following

turns

of
of

per

to

were

the

nearest

tested

as

0.i

tpi

directed

for

in

information:
inch

twist

for

for

yarn;

analyst.

92

yarn;

single

single

and

and

ply

for

ply

for

cord.

M-C-4
i.

Finish
on
Extraction

Rayon

Yarn

Using

Freon

and

Isopropanol

SCOPE

i.i

This
method
yarn
using
extraction

1.2

This
is a general
method
for finish
and follows
closely
ASTM
Method
D 2257-75,
except
the alcohol
specified
is
isopropanol
instead
of methanol.

2.
2.1

3.
3.1

3.2

4.
4.1

5.

APPLICABLE
ASTM

covers
the determination
of finish
Freon
and isopropanol
solvents
with
apparatus.

on rayon
Soxhlet

DOCUMENTS

Standards

123-75,

Definitions

2257-75,

of

Extractable

Terms

Matter

Relating
in

to

Textiles

Yarn

DEFINITIONS
Finish
- a lubricant
manufacturing
process
processing.

added
that

to
is

a fiber
necessary

For
definitions
of other
textile
terms
method,
see ASTM
Definitions
D 123-75.
SUMMARY

OF

or

yarn
in the
for handling

used

in

and

this

METHOD

A specimen
is extracted
in a Soxhlet
apparatus,
first
with
Freon
113 and then
with
isopropanol.
The solvents
are evaporated,
combined,
and the
residue
dried
and
weighed.
The amount
of extracted
matter
is reported
as
percentage
of the original
weight
of the specimen.
USES

AND

SIGNIFICANCE

5.1

This
method
of finishing
manufacture.

is used
for the determination
material
applied
to the yarn

5.2

Finishing
be wound

5.3

Besides
the quantitative
result,
examination
of the
extracted
residue
for odor,
physical
state
etc,
for
deviations
from
normal
frequently
may be revealing
as
the yarn
manufacturing
procedure
including
finishing
application.

materials
are
and processed.

added

93

to

a yarn

of the
during

to

enable

amount

it

to

to

5.4

The
residues
of the two may be separated
and weighed
to
determine
their
ratios
for deviations
from normal
and
also
for analysis
for identification
of components.
APPARATUS

AND

REAGENTS

Soxhlet
Extracion
Apparatus,
Pyrex
glass,
equipped
ground
glass
Joints.
Extractor
body
50 mm.
internal
diameter,
250 mm. length,
capacity
to top of siphon
ml.,
flask
size
250 or 300 ml.
capacity.

6.2

Stainless
or monel
discs
with
four
1/4 in. holes,
body
to prevent
specimen

6.3

Electric
heaters,
for heating
flasks,
equipped
controllers
for continuous
variation
of heater
temperature;
such
as, Precision
Type
H heaters
Superior
Electric
Co. Type
116 Powerstats.

6.4

6.7
6.8

6.9

bath,

of

0.01

Analytical
weighing

balance,
residue.

sensitivity

of

0.0001

Freon
113,
available
from
a halogenated
hydrocarbon
trifluoroethane.
alcohol,

6.11

Evaporation

8.1

SAFETY

gm.

for

gm.

weighing

for,

grade

aluminum,

50

ml.

usable

capacity.

PRECAUTION

Normal
safety
precautions
flammable
solvents.
SAMPLING
From
25 +

E. I. Dupont
DeNemours
and Co.
solvent
- 1,1,2
trichloro-l,3,3

industrial

dish,

with

residue.

sensitivity

Isopropyl

with

maintaining

balance,

Tongs.

7.1

predrying

of

Analytical
specimen.

6.10

7.

for

AND

SPECIMEN

each
package
0.i gm.

to

must

be

exercised

with

SIZE
be

tested,

take

specimen

weighing

CONDITIONING
Neither

200

1 3/4 in. diameter

perforated
for insertion
in the Soxhlet
plugging
siphon
outlet.

Drying
oven,
ventilated
capable
temperature
of 105 + 3C.
Steam

with

preconditioning

nor
94

conditioning

is

necessary.

i0.

PROCEDURE

i0.i

Place the disc level

in the bottom of the Soxhlet
extractor
apparatus.
Place each specimen in a separate
Soxhlet
body such that the top of the specimen is below
the top of the siphon.
Insert
the extractor
body into a
flask.

i0.2

Pour sufficient
Freon 113 over the specimen to fill
the
extractor
body to the siphoning
level
and furnish
sufficient
excess to prevent the flask
from going dry
during the extraction.
A total
of about 225 ml. is
required.

10.3

Attach
boiling
minutes.

10.4

i0.5

10.6

10.7

the

condenser
and adjust
the heater
such
that
rate
produces
a siphoning
about
every
20
Carry
out the extraction
for 1 1/2 hours.

At the
end of a siphoning
disassemble
the condenser,
squeeze
the specimen
against
the inside
of the Soxhlet
body,
with
a stirring
rod.
Transfer
specimen
to an
oven
for minimal
drying.
Reassemble
the Soxhlet
and
boil
to fill
the body with
the Freon
113 solvent
from
the
flask.
Disassemble
and set aside
the Freon
113 in
the
body.
Solvent
remaining
in the flask
should
be 2030 ml.
Pour
the contents
evaporating
dish.
ml.
each
of Freon
dish.
Place
the
evaporate
to prevent

of the boiling
flask
into a tared
Rinse
the flask
twice
with
about
113 and pour
into
the evaporating

evaporating
the solvent
losses.

dish
with

on
as

the steam
bath
little
boiling

Remove
the specimen
from
the oven
into
the Soxhlet
body.
Reassemble
to a second
flask.

10.8

Repeat

10.2

I0.9

Repeat

10.3.

10.10

the

using

and
as possible

and place
it
the Soxhlet

again
apparatus

isopropanol.

At the
end of a siphoning
disassemble
the condenser,
squeeze
the specimen
against
the inside
of the Soxhlet
body
and discard
the specimen.
Reassemble
the Soxhlet
and boil
to fill
the body
with
the isopropanol
solvent
from
the flask.
Disassemble
and set aside
the
isopropanol
flask
should

in the body.
be 20-30mi.

Solvent

95

remaining

in

the

10.11

Pour the contents

from this second boiling
flask
into
the evaporating
dish on the steam bath.
Rinse the
second flask
twice with 5 to i0 ml. of isopropanol
into
the evaporating
dish.

10.12

Evaporate

i0.13

Transfer
oven and
constant
dryings,
change in

10.14

Record

ii.
ii.i

to dryness

on the

steam bath,

see 10.6.

the aluminum dish with the tongs to the drying

dry at i05C + 3C oven temperature
to
weight;
that-is,
until
consecutive
15-minute
cooling
in a desiccator
and weighing
show a
weight of less than 0.0001 gm.

the

weight

to the nearest

0.0001

gm.

CALCULATIONS
Calculate
specimen
F, percent

the percent of combined extracts

to the nearest 0.01 percent.
=

100

for

each

(i)

L/W

where:
F
L
W

combined
extract
percent,
as is
constant
basis
= weight
of combined
extract,
gm.
= weight
of specimen,
origin,
gm.

or

Footnote:
This

method

is

similar

to

FMC

96

Method

FP

1 of

1 June

1966.

M-C-5
I.

pH of Fiber
Solutions

and Fabrics

in Distilled

Water

and Saline

SCOPE

i.i

This method covers the determination

in distilled
water.

1.2

Other AVTEX Methods for pH are STM 127, pH of fiber

by
Indicator
and STM 129, pH of fiber
in saline
solution
by
pH meter.

2.
2.1

pH of

ASTM Standards
Definitions

of Terms Relating

to Textile

DEFINITIONS

3.1

pH - a measure of acidity
or alkalinity
represented
the logarithm
of the reciprocal
(negative
logarithm)
the concentration
of hydrogen ions.

3.2

For other
Definitions

4.
4.1
5.
5.1

5.2

6.

fiber

APPLICABLE DOCUMENTS

D 123-75
Materials.
3.

of the

textile
terms
D 123-75.

in this

method,

refer

by
of

to ASTM

SUMMARYOF METHOD
A specimen of fiber
is soaked in distilled
water.The
solution
is measured for pH using a pH meter.
USES AND SIGNIFICANCE
The acidity

or alkalinity

certain
end
human
skin.

uses;

This
is
specific

such

of
as,

an empirical
method
sample
weight
and

fiber

is

important

nonsensitivity

of

since
it is the
solution
volume.

for
product

pH

of

or

probes.

APPARATUS

6.1

pH

meter

6.2

Beakers,

6.3

Graduated

6.4

Analytical

6.5

Glass

with
100

electrodes,
ml,

250

Cylinder,
Balance,

stirring

combination

probe

ml.
i00

ml.

sensitivity

rod.

97

of

0.01

gm.

to

6.6

Magnetic

6.7

pH buffer

solutions,

6.8

Distilled

water.

6.8.1

7.
7.1

stirrer.
5 pH, i0 pH.

Neutralize
stock solution
of distilled
water to 7.0 +
0.2 pH with meter using 0.i N HCL or 0.i N NaOH, using
Magnetic stirrer.
SAMPLES AND SPECIMENS
Take representative
samples
manufacturing
operation.
From each sample weigh

of fiber

one specimen

or yarn
of i0

of the

+ 0.i

gm.

PROCEDURE
8.1

Calibrate

the

pH meter

using

the

buffer

solutions.

8.1.1

Wash probe with distilled

water from a wash bottle.
Immerse usable part of probe into distilled
water in a
beaker.
Lift
probe from water and rinse with distilled
water from a wash bottle.
Drain.
Do no wipe.

8.1.2

Pour about 50 ml. of one of the two buffer

solutions
into a I00 ml. beaker.
Immerse the probe into the
buffer
solution.
Allow meter indicating
needle to
the

meter

to

8.1.3

Remove

wash

as

directed

8.1.4

Pour
about
50 ml.
of the second
buffer
solution
into
a
second
i00 ml.
beaker.
Immerse
the probe
into
the
buffer
solution.
Allow
meter
indicating
element
to
come
to rest.
Meter
should
check
pH of second
buffer
within
+ 0.05 pH.
If meter
reading
is outside
this
tolerance
a problem
exists
with
either
the meter
or the
buffer
solutions
which
must
be resolved.

probe

and

8.2

Measure
beaker.

8.3

Using
meter
adjust
pH
with
magnetic
stirrer,

8.4

Place
a l0 +
Immerse
witE
for 1 min.
+

indicate

in

the

0.i gm.
stirring
5 sec.

specimen
rod and

98

pH

7.0 +
HCl o_

of fiber
agitate

of

8.1.1.

100 ml. of distilled

water,
pH 6.8,
Place
beaker
on magnetic
stirrer.
of water
to
using
0.01N

pH

come
the

to rest.
Adjust
buffer
solution.

into
fiber

into

0.05,
0.01

250

ml.

mixing
N NaOH.

the beaker.
in solution

8.5

At end of 1 min. pour out water into a i00 ml. beaker,

squeezing
the fiber
with the glass rod.
Place pH probe
(or probes)
into i00 ml. beaker and measure pH of
solution.
Swirl or otherwise
agitate
solution.
REPORT
State that
057-76b.

specimen

Report

pH of solution.

Report

identity

was tested

of analyst.

99

as directed

in AVTEX STM

M-C-6

Shrinkage

of Yarn and

Cord

in

Water

and

Ambient

Temperature
i.
i.i

2.
2.1

SCOPE
This method
covers
meter
lengths
when
APPLICABLE
ASTM
D

3.

the shrinkage
of
exposed
to water

Standards
123-75

Definitions

of

Terms

Relating

3.2

For definitions
method,
refer

5.

SUMMARY

OF

Textiles

to

of other
textile
ASTM
Definitions

a meter
of the

terms
used
D 123-75.

length
length

in

of
prior

this

METHOD

A meter
of conditioned
yarn
or cord
is measured
under
tensioning
weight
sufficient
to straighten
but not to
stretch
the yarn
or cord
before
and after
exposure
to
water
at room
temperature
followed
by drying
and
conditioning.
The
change
in length
is expressed
as a
percentage
of the length
before
exposure.
USES

AND

SIGNIFICANCE

5.1

Shrinkage
strain
in

5.2

The amount
processing

6.

to

DEFINITIONS
Shrinkage
- the change
in length
of
yarn
or cord
expressed
as a percent
to exposure
to the shrinkage
medium.

4.1

in

DOCUMENTS

3.1

4.

rayon
yarn
or cord
at room
temperature.

in yarn
or cord
is
the yarn
following
of shrinkage
in
characteristics;

a measure
of
manufacture.

the

yarn
or cord
affects
e.g.
wet
treatment.

residual

wet

APPARATUS

6.1

Measuring
scale
for at least
20
end and a pulley

- a table
with marks
1 m apart,
mm scale
mm.
interior
to the
1 meter
marks
at one
at the end
of the table.

6.2

Weight

with

6.3

Marking

6.4

Tray

4 oz.,

cllp.

pen.

100

6.5

Water

6.6

Oven,

7.
7.1
8.
8.1
9.

drying,

capable

of

maintaining

105

5C.

SAMPLING
Test

samples

per

package.

CONDITIONING
Condition

sample

prior

to

testing.

PROCEDURE

9.1

Measure
a specimen
by extending
measuring
scale.
Hang
a 4 oz.
sample
over
the pulley,
holding

9.2

Mark
a specimen
by placing
marks
on the yarn
or cord
exactly
in line
with
the one meter
marks
on the table.
Disconnect
the weight,
cut the sample
from
the package
approximately
2 m. long with
the marked
specimen
in the
center.

9.3

Coil
without
tangling
on
water
at room
temperature.
float.

the yarn
weight
on
onto the

tray.
Sample

or cord
over
the
the end of the
other
end,

Immerse
the tray
in
must
not be allowed

to

9.4

At the end of 1/2 min.

remove
the tray
from the water,
drain
to remove
excess
oven
at i05 _ 5C.
for 1 hr. to dry.

9.5

Remove
tray
from
the
laboratory.

9.6

Place
the sample
on the measuring
scale
as at the time
of
marking
with
one
end held
and the other
end extended
over
the pulley
With
the 4 oz. weight
attached.
Align
one
mark
on sample
with
a mark
on the scale.
Measure
and
record
the length
between
the two marks
on the sample
to
the nearest
mm.

I0.

CALCULATION

i0.i

oven

and

condition

Calculate
the shrinkage
in
0.i percent
using
Equation
S,

percent

= i00

(M-L)/M

the
I.

with
the sample
water,
place
in

sample

specimen

for

to

the

specimen,
1 m.
after
exposure,

m.

(I)

where:
S
M
L

= Shrinkage,
percent
= Original
length
of
= Length
of specimen
101

2 hours

nearest

in

M-C-7

Moisture

i.

Regain

This
method
content
of

1.2

This
method
is
Procedure
2.
APPLICABLE

2.1

3.

of

Fiber

SCOPE

i.i

2.

Content

ASTM

covers
yarn.

the

determination

consistent

with

of

ASTM

the

Method

moisture

2654,

DOCUMENTS

Standards

D 123-75
Materials

Definitions

of

Terms

D 2654-71
Material.

Moisture

Content

Related

and

to

Moisture

Textile

Regain

of

Textile

DEFINITIONS

3.1

Moisture
content
- the amount
of moisture
in a material
determined
under
prescribed
conditions
and expressed
as a
percentage
of the weight
of the moist
material,
that
is,
the original
weight
comprising
the dry substance
plus
any
moisture
present.

3.1.1

Moisture
"as is",

3.1.2

Moisture
content
differs
from moisture
the basis
used
for calculations.

3.1.3

Moisture
calculations
are commonly
based
on the weight
of a specimen
which
has been
dried
by heating
in an
oven.
If the air in the oven
contains
moisture,
the
oven-dried
specimen
will
contain
some
moisture
even
when
it no longer
shows
a significant
change
in weight.
In order
to ensure
that
the specimen
is molsture-free,
it must
be exposed
to desiccated
air until
it shows
no
further
significant
change
in weight.

3.2

4.

content
is also
referred
"as received",
or "wet"

For definitions
refer
to ASTM
SUMMARY

OF

4.1

A I0 gm.
constant
desiccated

4.2

Since
the
Brabender

of other
Definitions

to as
basis.

textile
terms
D 123-75

moisture

regain

in

on

only

this

an

on

method

METHOD
specimen
reweight
air.
original
in-oven

of
in
The

yarn
is weighed
and dried
a Brabender
oven
supplied
moisture
content
is read.

weight
balance

is
is
102

i0
in

gm.,
the
moisture

to
with

read-out
content.

of

the

5.1

USES

AND

SIGNIFICANCE

This
method
utilizes
test
to measure
the
specimens
of yarn.
not
recommended
for

a i0 gm. sample.
It is an excellent
variations
in moisture
content
of
Because
of the specimen
size
it is
commercial
weight
determination.

APPARATUS

6.1

Brabender
oven,
operated
at 105 + 3C.,
supplied
with
a
current
of air at a rate sufficient
to change
the air in
the oven
at least
once
every
4 min.,
the air to the oven
shall
be predrled
by circulating
through
Electro
Dryer
units.

6.2

Brabender

6.3

Reel,

1 m.

SAMPLES

AND

7.

predrying

balance

SPECIMENS

7.1

Take
care
to
either
before

7.2

Strip
sufficient
yarn
from the package
to remove
the
outside
layer
of yarn.
In practice
this
is accomplished
by taking
samples
for other
test
less
sensitive
to
moisture;
such
as, finish,
linear
density,
etc.
from the
outer
layers.
Unwind
a skein
of about
11-12
gm.
Cut
from
reel.
Weigh
to exactly
i0 grams
using
the Brabender
preweight
balance.

7.3

Take

8.
8.1

not
or

1 specimen

allow
after

per

the yarn
drying.

to

change

moisture,

sample.

PROCEDURE
Daily

check

the

calibration

of

the

Brabender

balances.

8.1.1

Check
the predrying
in the
specimen
pan
i0 gm.

8.1.2

Check
the
in-oven
balance
by placing
a i0 gm. weight
the
balance
pan.
Read-out
scale
should
read
zero.
Place
a 9 gm. weight
on the balance
pan.
Read-out
scale
should
read
i0.0.

balance
by placing
a
and adjusting
balance

103

i0 gm. weight
to indicate

on

8.2

_lace
the
l0 gm. specimen
in a cup in the oven
at 105 + 3
C.
Dry
to constant
weight
as follows:
Dry
for 1 hr.Stop
the
fan and weigh
specimen
in the oven.
Record
percent
moisture
content
to the nearest
0.i percent.
Start
the fan and dry
for an additional
1/2 hr.
Stop
the
fan and
reweigh
the specimen.
If the change
in reading
is greater
than
0.i percent
moisture
content,
continue
drying
and checking
the weight
every
15 min.
until
the
specimen
has reached
constant
weight.
REPORT

9.1

Report

9.2

Average

9.3

Report

the

following:

moisture
identity

regain
of

for

analyst.

104

specimens

tested.

M-C-8
i.
i.i

Ash

Content

of

2.1

This

method

APPLICABLE

Increasing

covers

ASTM

by

the

determination

exposure

at

75

Definitions

of

Terms

SUMMARY

OF

to

in

Textile

and textile
D 123-75.

terms

combustion
for 3
200C,
1 hour
at 400C

in

this

method

USES
The
the

AND

refer

to

METHOD

A specimen
of rayon
fiber
or yarn
_s ignited
furnace
for 3 hours,
1 hour
at 200 C + 25vC,
400C
+ 25C
and 1 hour
at 800C
+25C.
The
remainYng
weight
of

6.

content

DEFINITIONS

For definitions
ASTM
definitions

5.1

ash

temperature

Related

3.2

5.

the

Standards

Ash,
dry method
- the
residue
after
hours
in muffle
furnace,
1 hour
at
and 1 hour
at 800C.

4.1

of

increasing

3 1

4.

Temperatures

DOCUMENT

D 123 Material.
3.

at

SCOPE

of rayon
fiber
muffle
furnace.
2.

Fiber

is expressed
the original

as a percentage
specimen.

in a muffle
1 hour
at
residue

of

the

"as

is

indicative

is"

SIGNIFICANCE

ash content
of rayon
method
of manufacture.

fiber

or

yarn

of

APPARATUS

6.1

Porcelain
crucible,
Coors
for staple
fiber
and Coors
capacity
for yarn.

6.2

Muffle
furnace,
electric,
HEVI
Duty
Electric
Company,
with
controller,
Thermolyne
Temcometer,
Sybron
Corporation,
or equivalent,
capable
of maintaining
200
25 c., 400 + 25 c. and 800 + 25 _ C.

6.3

Crucible

6.4

Analytical

balance,

6.5

Desiccator

with

12, approx.
250 ml.
capacity
09, approximately
50 ml.

tongs.
sensitivity

desiccant.

105

of

0.0001

gm.

7.

USES

7.1

8.

AND

SIGNIFICANCE

The test
unit.

specimen

shall

be

selected

to

represent

the

PROCEDURE

8.1

Determine
the crucible
tare
weight
muffle
furnace
at 800_C
+ 25_C
for
slightly
and place
in th_ desiccator
temperature.
Weigh
to the nearest

8.2

Weigh
in
of about

8.3

Place
the crucible
with
the specimen
in the muffle
furnace
at 200 _ 25C.
_or 1 hour.
Increase
the
temperature
to 400 + 25_C.
for one hour.
Increase
temperature
to 800 T 25C.
for 1 hour.

8.4

9.

test

by
i0

heating
in the
minutes,
cool
to cool
to room
0.0001
gm.

the tared
crucible
a specimen
of
5 gm. to the nearest
0.0001
gm.

Cool
the crucible
and
desiccator
to cool to
0.0001
gm.

residue
slightly
room
temperature.

fiber

or

yarn

the

and place
in a
Weigh
to nearest

CALCULATIONS

9.1

Calculate
percent.
Ash,

the

percent

percentage

= R
W

- T
- T

of

ash

to

the

nearest

0.01

(100)

where:
R
W
T
i0.

= weight
of crucible
and
gm.
= weight
of crucible
and
= tare weight
of crucible,

residue

after

original
gm.

combustion,

specimen,

gm.

REPORT

i0.i

State
AVTEX

10.2

Report

that
the specimens
STM 092-76.
the

10.2.1

Ash

10.2.2

Identity

were

tested

0.01

percent.

following.

content
of

to

nearest

analyst.

106

as

directed

in

M-C-9

i.
i.I

2.
2.1

Zinc Extraction
Absorption

3.1

4.
4.1

5.

Use

of

HCI

and

Measurement

by

This
method
covers
the determination
of extractable
in rayon
fiber
or yarn
by atomic
absorption
method.
zinc
is extracted
by bringing
a specific
weight
of
specimen
to a boil
in a specific
volume
of HCl.
APPLICABLE
ASTM

zinc
The

DOCUMENTS

Standards
Definitions

of

Terms

Relating

to

Textile

DEFINITIONS
For
definitions
refer
to ASTM
SUMMARY

OF

of textile
Definitions

terms
123-75.

used

AND

this

in 1 N HCl.
The
Atomic
Absorption
standard.

SIGNIFICANCE

The amount
of zinc
of the manufacture

in
of

rayon
fiber
the product.

or

yarn

is

5.2

The
use

in

rayon

or

yarn

may

amount
of zinc
performance.

APPARATUS

AND

Analytical
Beaker,

method

METHOD

A specimen
of fiber
or yarn
is boiled
solution
is diluted
and evaluated
by
Spectrophotometer
against
a reference
USES

in

5.1

6.

Atomic

SCOPE

D 123-75
Materials
3.

by

REAGENTS

balance,
250

plate

sensitivity

of

ml.

6.3

Hot

6.4

Pipettes,

6.5

Volumetric

6.6

Graduated

cylinder,

6.7

Distilled

water.

6.8

HC1,

reagent

1 N,

fiber

in

indicative

hood,

2 ml.,
flasks,

electric.
5 ml.,
i00
i00

20

ml.

ml.,
ml.

grade.

107

1000

ml.

0.001

gm.

affect

end

6.9

Zinc,

standard

solution,

6.9.1

Zinc,

6.9.2

Pipette
20 ml.
of the i000 ppm
standard
zinc
solution
into
a i000 ml. volumetric
flask
and make
to volume
with
distilled
water.
Mix.
Identify
as Solution
A.
Pipette
5 ml.
of solution
A into
a I00 ml. volumetric
flask
and make
to volume
with
distilled
water.
Mix.
This
solution
contains
1 ppm
zinc.
Identify
as Sol.

6.10

Standard

1 ppm.

Atomic
Model

Solution

Light

source-zinc

6.10.2

Flame

type

6.10.3

Wave

length

6.10.4

Slit

setting

7.
7.1

8.
8.1
9.

ppm,

Harleco,

Absorption
Spectrophotometer,
360 and operators
manual.

6.10.1

6.11

i000

Hengar

hollow

setting
- 0.7

granules

lamp.

oxidizing,

214

B.

Perkins-Elmer

cathode

- air-acetylene,

Phila.

lean,

blue.

nm.

nm.

(boiling

chips)

SAMPLING
Representative
gm.

sample

to

provide

duplicate

specimens

3-4

CONDITIONING
Neither

preconditioning

or

conditioning

is

necessary.

PROCEDURE
Weigh

3.5

0.i

gm.

specimen

to

the

nearest

0.001

gm.

Place
specimen
in 250 ml.
beaker
containing
a few Hengar
chips.
Add
i00 ml. of 1 N HCI.
Mark
level
of solvent
with
fiber
completely
immersed
by placing
on the outside
of the beaker
the bottom
edge
of a gum paper
label
even
with
the
top of the solvent
level.
Bring
to boil
on hot
plate
under
a hood.
Remove
and cool
to room temperature.
Add 1 N HCl to bring
solvent
volume
back
to bottom
edge
of the label.
Mix
thoroughly
with
glass
rod.
9.3

Pipette
Dilute

9.4

Calibrate

5 ml.
aliquot
to volume
with

9.4.1

Set

zero

9.4.2

Set

i00

the

Atomic

transmission
percent

into a i00 ml.

volumetric
distilled
water.
Mix.
Absorption
with

transmission
108

flask.

Spectrophotometer.
distilled
with

water
1 ppm

blank.

zinc

standard.

9.5

Read
specimen
solution,
Spectrophotometer.

9.6

Repeat
falls

i0.

CALCULATION

i0 .i

for duplicate
specimen
out of specifications.

Calculate
zinc,

9.3,

amount

percent

of
(R

zinc
x D)

on

Atomic

Absorption

whenever

to

nearest

/ S

(104 )

first

0.005

specimen

percent.

where:
R

D =
S =
ii.

reading
of AA,
direct
in ppm
scale
calibration.
Dilution
factor,
(i00)
(I00)
specimen
weight,
gm.

for

1 ppm

full

/ 5

REPORT

ii.i

State
Method

ll.2

Report

the specimens
STM 118-76.
the

were

following

i1.2.1

Average

amount

of

11.2.2

Range
of duplicate
if two were
run.

i1.2.3

Identification

of

tested

as

directed

in

AVTEX

0.005

percent

information:
zinc

to

specimens

analyst.

109

nearest
to

nearest

0.005

percent

M-C-10

I.
i.I

2.
2.1

Sulfur
Sulfur

Content

3.1

4.
4.1

Yarn,

Both

Sulfate

and

Elemental

SCOPE
This
method
sulfate
and
APPLICABLE
ASTM

covers
the
free sulfur

determination
of sulfur,
form,
in rayon
fiber.

in

DOCUMENTS

Standards

D 123-75
Materials.
3.

of

Definitions

of

Terms

Related

to

Textile

DEFINITIONS
For
definition
ASTM
Definition
SUMMARY

OF

of textile
D 123-75.

terms

in

this

method

refer

to

METHOD

A specimen
of yarn
is dissolved
Conc.
hydrochloric
acid
is added
and the solution
boiled
down
to

in conc.
nitric
acid.
with
potassium
chlorate
release
the nitric
acid

and nitrates.
The
alkalinity
is adjusted
with
ammonium
hydroxide
and the sulfate
and sulfur
converted
to barium
sulfate
with
the addition
of barium
chloride.
The barium
sulfate
precipitate
is filtered,
washed,
dried
and
weighed.
The weight
is converted
to free sulfur
and
reported
as a percentage
of the original
specimen.
5.

USES

AND

SIGNIFICANCE

5.1

The
amount
indicative

5.2

Sulfur
fiber

6.
6.1

of
of

sulfur
method

present
in a
of manufacture

content
is of
and is covered

importance
in grading

rayon
fiber
is
of the
fiber.

to some
uses
standards.

of

APPARATUS
Beaker,

250

Analytical
Muffle

ml.,

Phillips

balance,

furnace,
crucible,

sensitivity

capable

6.4

Gooch

6.5

Filtering

Coors

6.6

Asbestos,
purified
Baker
Chem.
Co.

flask,

conical

with

of

0.0001

gm.

800C.

7 M.
adapter

acid

washed

110

for

Gooch

long

crucible.

fiber,

J.

T.

rayon

6.7

Graduated

6.8

Hot

6.9

Oven,

cylinders,

capable

Pipette

6.11

Desiccator

200

ml.

of

105

with

3 C.

desiccant

REAGENTS

7.1

Nitric

7.2

Hydrochloric

7 2.1

acid,

i:i

Potassium

7.4

Methyl

7.5

Ammonium

7.6

Barium

7.6.1

SAMPLES

grade
reagent

on

volume

reagent

grade
basis

grade

indicator

hydroxide,

conc.,
reagent

reagent

grade

grade

chloride,
5 percent
solution,
prepared
with
distilled
water

nitrate,
prepared
AND

HCI

chlorate,

Nitrate,

Silver
basis

conc.,

of

chloride,

Silver

reagent

acid,

orange

Barium
basis

Weigh

conc.,

solution

7.3

8.

ml.,

plate

6.10

7.

25

reagent

weight-volume

grade

i0 percent
solution,
with
distilled
water

weight-volume

SPECIMENS

specimen

of

0.001

gm.

fiber.

PROCEDURES
9.1

Place
the
1 gm. specimen
of fiber
in a 250 ml. Phillips
beaker.
Add
15 ml.
of concentrated
nitric
acid
and warm
slightly.
Agitate
the mixture
until
the fiber
is
dissolved.
When
the yarn
is practically
free
from
sulfate
and
free
sulfur,
the solution
will
be clear.

9.2

Place
the
beaker
containing
the solution
on a hot plate
in a hood
and boil
down
to about
i0 ml.
Cool
to room
temperature.
Add
20 ml. of conc.
hydrochloric
acid
and
few crystals
of potassium
chlorate.
Continue
boiling
until
the volume
is reduced
to about
i0 ml.
Cool
slightly,
add another
20 ml.
of hydrochloric
acid
and

111

boil until
point
the
9.3

brown
fumes
solution
is

Remove
the
beaker
orange.
Neutralize
ammonium
hydroxide
distilled
water.

are
free

no
of

longer
nitric

visible.
acid
or

At this
nitrates.

from the hood.

Add
3-5 drops
of methyl
the solution
with
concentrated
to yellow
color.
Dilute
with
20 ml.
Make
solution
acidic
with
i:I

hydrochloric
acid
(pink),
add 1 ml.
excess.
Bring
to a
boil
and
add 15 ml. of 5 percent
barium
chloride
solution
with
stirring,
adding
the first
4 ml.
very
slowly
dropwise.
Again
bring
to boil
and boil
for 2 min.
Allow
to stand
at least
2 hrs.
or overnight.
Preparation
Prepare
beaker.
9.4.2

of
a

Gooch

slurry

crucible.
of

asbestos

in

distilled

water

in

Place
the Gooch
crucible
in the adapter
on the
filtering
flask.
Pour
the slurry
of asbestos
slowly
into
Gooch
crucible
with
suction
applied
to the
flask
until
a matt
develops
that completely
covers
the bottom
of the
crucible
about
2 mm.
thick.
Wash
with
200 ml.
of distilled
water
to remove
any fine
fibers:
Dry
in
an oven
at _05 + 3C. for 30 min.
Transfer
to muffle
furnace
800_C.
and ignite
to constant
weight.
Thirty
min.
is generally
adequate
followed
by cooling
to room
temperature
in a desiccator,
and weighing
to 0.0001
gm.
for tare
weight
of prepared
Gooch
crucible.

9.5

Filter
solution
from
9.3 through
tared
prepared
Gooch
crucible
in adapter
on filtering
flask
with
suction
applied.
Scrub
Phillips
beaker
with
a rubber
policeman
to completely
transfer
all the contents
to the crucible.

9.6

Wash
precipitate
with
hot distilled
water
until
free
of
chlorides
as determined
by absence
of turbidity
in the
filtrate
wfth
the addition
of a few drops
of i0 percent
silver
nitrate
solution.
200 ml.
of hot distilled
water
has been
found
to be adequate
generally.

9.7

Dry prepared
Gooch
at 105 + 3_C.
for

9.8

Transfer
constant
0.1%
of
followed

9.9

The

crucible
30 min.

with

precipitate

to the muffle
furnace
at 800C.
weight,
that
is, until
it loses
its weight
at 30 min.
intervals
by cooling
in the desiccator.

precipitate

is

barium

sulfate.

112

in

an

oven

and ignite
to
no more
than
of drying

i0.
10.1

CALCULATIONS
Calculate
elemental
percent.

the amount
sulfur
in

Sulfur,

percent

of
the

100

sulfate
specimen

(K

x P)

and
to

free
sulfur
the nearest

as
0.001

/ W

where:
K
P
W

ratio
weight
= weight
s weight

of atomic
weight
of sulfur
to
barium
sulfate,
0.1373
of barium
sulfate
precipitate,
of fiber
specimen,
gm.

113

molecular
gm.

M-C-If
i.

Rayon

Requirements

for

Carbon

Textiles

SCOPE

1.1

This
specification
to be used
in the

2.

APPLICABLE

2.1

covers
the
manufacture

FMC

FMC
FMC
FMC
FMC
FMC
FMC
FMC
FMC
FMC
FMC

Fiber

STM
STM
STM
STM
STM
STM
STM
STM
STM
STM

requirements
for rayon
of carbon
textiles.

yarn

DOCUMENTS

Publications
- The
following
this
specification.
Unless
issue
specified
below
shall

2.1.1

3.

Yarn

documents
otherwise
apply:

form
a part
of
indicated,
the

Division

003:
005:
006:
010:
057:
069:
092:
114:
140:
118:

Similar
Methods
Measurement
of:
in this manual
Yarn
Denier
...............
M-C-I
Yarn
Strength
.............
M-C-14,
2
Yarn
Twist
................
M-C-3
Yarn
Finish
Content
.......
M-C-4
Yarn
pH ...................
M-C-5
Yarn
Shrinkage
............
M-C-6
Ash Content
...............
M-C-8
Moisture
Content
..........
M-C-43
Sulfur
Content
............
M-C-10
Zinc Content
..............
M-C-9

REQUIREMENTS

3.1

Qualification
specification
and has passed

3.2

Material
- Unless
otherwise
specified,
the material
purchased
to this
specification
shall
be rayon
code
2175,
made
by the FMC Fiber
Division.
The yarn
shall
not
be
treated
with
a finish
of any kind
other
than
the standard
water-dispersable
finish
originally
applied.

3.3

Chemical
Requirements
- The
yarn
shall
be as follows:

- The material
finished
under
this
shall
be a product
which
has been
tested
the qualification
tests
specified
herein.

Ash
Content,
Wt. %
Sulfur
Content,
Wt.%
Zinc
Content,
Wt.%
pH
Finish
Extractables,

chemical

requirements

0.7 Maximum
0.25
Maximum
0.07
Maximum
5.0 - 8.0
0.2 - 1.0

Wt.%

114

of

the

3.4

Physical
Requirements
- The
yarn
shall
be as follows:

physical

Twist,
turns,
per
inch,
(tpi)
Conditioned,
Strength,
Lbs.
Conditioned
Elongation,
%
Moisture
Content,
wt.%
Denier,
gms./9000
meters
Shrinkage,
%
QUALITY

ASSURANCE

requirements

Min.
1.6
10.3
5.5
1590.0
2.9

of

the

Max.
2.4
13.5
9.5
13.0
1710.0
4.7

PROVISIONS

4.1

Quality
Control
System
specifcations
apply
in
material
supplied.

Lot.
Unless
otherwise
specified,
all Rayon
yarn
shipped
1_-h--one truckload
shall
be considered
a lot
for purposes
of inspection
and tests.
The invoice
number
for a
particular
truckload
is the lot number
identification.

Requirements
allparticulars

- FMC Fiber
relevant

Division
to

4.3

HITC0
Inspection
- The HITCO
inspector
shall
make
such
inspections
as are necessary
to determine
that
the
material
is in accordance
with
the requirements
of this
specification
with
regards
to purchase
order,
packaging,
marking,
packing,
and acceptance
or qualification
tests.

4.4

Supplier
Inspection
- Unless
otherwise
specified,
the
supplier
is responsible
for the performance
of
inspections
necessary
to determine
that
the material
is
in accordance
with
the requirements
of this
specification
with
regards
to purchase
order,
packaging,
marking,
packing,
and acceptance
or qualification
tests.
These
inspections
shall
be made
prior
to submission
for
customer
inspection
and acceptance.
Except
as otherwise
specified,
the supplier
may utilize
his own facilites
or
any commerdial
facility
acceptable
to the customer.
Inspection
records
of the examinations
and tests
shall
be
kept
complete
and available
to the customer.

4.5

Customer
rejected
failure

4.6

Classification
of Tests
- The
inspection
and testing
of
the material
shall
be classified
as follows:
Qualification
Tests
Acceptance
Tests
Qualification
Tests
- The qualification
tests
for this
material
shall
consist
of all tests
listed
in Table
I.
At the discretion
of HITCO
these
tests
may
be repeated
subsequent
to the
intial
qualification.

4.7

Rejection
- Any
in its entirety
to meet
purchase

lot inspected
at one time
may
and be subject
to return
for
order
requirements.

115

be

4.7.1

4.7.2

Sampling
specified,
sufficient
shall
be
inspection.

for
Qualification
Tests
- Unless
ten
(i0)
representative
samples
size
to
perform
the
qualification
selected
at
random
from
the
lot

Qualification
Test
Report
furnish
to
customer
three
verifying
that
the
material
qualification
requirements

- The
material
supplier
copies
of
a report
of
conforms
to
the
of
this
specification.

TABLE

FMC
FMC
FMC
FMC
FMC
FMC
FMC
FMC
FMC
FMC
FMC

Content
Strength
Elongation
Content

Shrinkage
4.8

Acceptance
Tests
shall
consist
of

- The
acceptance
all
listed
in
TABLE

STM
STM
STM
STM
STM
STM
STM
STM
STM
STM
STM

092
140
118
057
010
006
005
005
037
003
069

material

II

FMC
FMC
FMC
FMC
FHC
FMC
FMC
FMC
FMC

Content

Conditioned
Conditioned
Moisture

this

2
2

Test
Method
in this
manual

Content

pH
Finish
Twist
Denier

H-C-8
M-C-10
M-C-9
M-C-5
M-C-4
M-C-3
M-C-14,
M-C-14,
H-C-7
M-C-I
M-C-6

tests
for
Table
II.

Characteristic
Ash

shall
tests

Test
Method
in this
manual

Ash
Content
Sulfur
Content
Zinc
Content

Conditioned
Conditioned
Moisture
Denier

for

Characteristic

pH
Finish
Twist

otherwise
of
a
tests
presented

Strength
Elongation
Content

Shrinkage
4.8.1

Sampling
specified,
conformance
randomly
produced

4.8.2

Rejection
for
Acceptance
Tests
any
one
or more
of
the
acceptance
Table
II,
another
package
shall
from
the
same
3300
pound
batch.

STM
STM
STM
STM
STM
STM
STM
STM
STH

092
057
010
006
003
005
005
657
069

M-C-8
H-C-5
H-C-4
M-C-3
M-C-1
M-C-14,
M-C-14,
M-C-7
M-C-6

2
2

Plan
for
Acceptance
Tests
Unless
otherwise
all
shipments
shall
be
acceptance
tested
for
to
this
specification.
One
sample
shall
be
selected
from
each
3300
pounds
of
yarn
and
tested
to the
requirements
of
Table
II.

118

If any
sample
fails
tests
described
in
be
randomly
sampled
The
retest
data
shall

be averaged
with
the original
data
obtained
on the
first
sample.
If the average
test data
passes
the
minimum
requirements,
the
3300 pound
batch
is accepted.
If the average
test
data
is below
the minimum
requirements,
the
3300 pound
batch
being
tested
shall
not be shipped
to the weaver
or to HITCO.
In the event
that
subsequent
failures
are repetitive
to a
significant
degree
as determined
by the
supplier,
the
supplier
may
request
a specification
amendment
subject
to the
review
and approval
of HITCO.
4.8.3

4,9

Acceptance
Test Report
- The material
supplier
shall
furnish
to customer,
with
each
shipment,
three
copies
of a report
of tests
verifying
that
the lot of material
conforms
to the acceptance
requirements
of this
specification.
Test
Procedure
- The test
procedure
shall
accordance
with
the applicable
procedures
Tables
I and II.

be in
listed

Test
This
Ash Content
Sulfur
Content
Zinc Content
pH
Finish
Content
Twist
Conditioned
Conditioned
Denier
Shrinkage

5.1

5.2

PREPARATION

FMC
FMC
FMC
FMC
FMC
FMC
FMC
FMC
FMC
FMC

Strength
Elongation

FOR

STM
STM
STM
STM
STM
STM
STM
STM
STM
STM

092
140
118
057
010
006
005
005
003
069

in

Methods
Manual

M-C-8
M-C-10
M-C-9
M-C-5
M-C-4
M-C-3
M-C-14,
M-C- 14,
M-C-I
M-C-6

2
2

DELIVERY

Packaqing
= The yarn
shall
be packaged
on tubes.
Each
layer
of tubes
in the case
shall
be separated
by a
divider.
There
shall
be 8-10 pounds
of yarn
per tube,
to i0 pound
tubes
may be supplied
as ordered
by the
customer.

Packing
- Unless
otherwise
specified,
the rayon
yarn
shall
be packed
in a clean,
dry case of the standard
size
and type normally
used
by FMC Fiber
Division.
The case
shall
be so constructed
as to insure
acceptance
by common
or other
carrier
for safe transportation
at the lowest
rate,
to the point
of delivery
specified
by the purchase
order.

117

5.3

Marking
- Cases
shall
be marked
in
Fiber
Division
standard
practices.
include,
but not be limited
to the
1650/720/2.0-z,
2175.
Manufacturer's
Manufacturer's

6.1

Rayon
names.
invoice

Yarn,

MDS

accordance
Marking
following

2015,

with
FMC
shall
information:

Code

number.

NOTES
Ordering
Data
not
be limited

- Procurement
documents
should
to the
following
information:

1650/720/2.O-Z,
Rayon
2175.
Place
of inspection.
Place
of Delivery.
Weight
of Material.
AVTEX

FIBER

Yarn,

MDS

SPECIFICATIONS

2015,

FOR

Product
Date
of Issue
Code
Description

Test

specify,

Code

BURLINGTON

Carbonizing
Yarn
11/30/76
2175
1650/720
Filament

Method

Cond.
Strength,
Cond.
Elongation,
Finish,
%
Shrinkage,
%
Twist,
T.P.I.
Denier
pH
Moisture,
%
Ash
Content,
%
Sulfur
Content,
Zinc
Content,
%

lbs.
%

Min.

Max.

10.3
5.5
0.2
2.9
1.6
1590
5.0

13.5
9.5
1.0
4.7
2.4
1710.0
8.0
13.0
0.7
0.25
0.07

but

Test
Method
STM
STM
STM
STM
STM
STM
STM
STM
STM
STM
STM

Yarn

Test
Methods
This
Manual

005
005
010
069
006
003
057
087
092
140
118

M-C-2,14
M-C-2,14
M-C-4
M-C-6
M-C-3
M-C-I
M-C-5
M-C-7
M-C-8
M-C-10
M-C-9

E. J. Epp,
Manager
Technical
Services
This
specification
is to be reissued,
advised
in writing

is effective
through
December,
1977.
If
Avtex
Manager
of Technical
Services
must
during
October,
1977.

These
Other

relate
may
get

specifications
laboratories

to Avtex
different
118

analytical
levels.

results.

it
be

M-C-12
i.

Carbon

Fabric

Specifications

SCOPE

i.i

This
specification
covers
one type
of carbon
in solid
rocket
motor
nozzle
components.

1.2

The
carbon
fabric
intended
for use
nozzle
components.

2.

Material.
specification
woven
into
properties

2.2

Yarn.
weave

2.3

Tracer
fabric

3.1

specification
is
of solid
rocket

The

material
furnished
under
shall
be a pan base
carbon
a satin
harness
8 fabric
and
as defined
in 3.1.

motor

Three
thousand
the
fabric.
Yarns
and Fabric
finishes
within

CLASSIFICATION
Inspection
as quality

OF

filament

yarn

Finishes.
the fabric

shall

this
fiber
(T-300)
supplied
with

be

used

INSPECTIONS

requirements
conformance

specified
tests.

herein

are

classified

Visual
examination
............................
Fiber
ultimate
tensile
strength
...............
Fiber
density
.................................
Weight
........................................
Thread
Cou_t
..................................
Thickness
.....................................
QUALITY

ASSURANCE

to

Tracer
yarns
and
shall
be acceptable.

Test
This

4.

used

REQUIREMENTS

2.1

3.

covered
by this
in the manufacture

fabric

Methods
Manual
M-C-31
M-C-14
M-C-15
M-C-16
M-C-17
M-C-18

PROVISIONS

4.1

Sampling.
inspection

Each
lot of
as follows:

material

4.2

Lot.
A lot shall
consist
of that
quantity
of material
w-h-i-6h is manufactured
at one time,
using
the same
process,
and under
the same
conditions
of manufacture.
Any change
in materials,
formulation,
processes,
tools
conditions
from
lot to lot shall
require
approval
by
Thiokol.
A lot shall
not
consist
of more
than
250
pounds.

119

shall

be

sampled

for

or

4.3

Samples.
A material
sample
of sufficient
perform
all tests
specified
herein
shall
the outside
end of each master
roll.

4.4

Test
Specimens.
A minimum
of three
specimens
shall
be
tested
from
each
sample
for each
of the properties
requiring
test
specimens.
All
test
results
shall
be
reported
to the procuring
organization.
The
average
test
results
of three
test
specimens
shall
be reported
in
addition
to the
reporting
of the individual
test
specimen
value.
The average
results
of each
test
shall
meet
the
requirements.

5.

quantity
to
be selected
from

DEFINITIONS

5.1

Master
Roll.
roll
shipped

5.2

Sample.
roll.

5.3

Specimen.
used
for

A specimen
testing.

5.4

Typical
of the

A master
roll
to the procuring
sample

is

cut-out

is

Materials.
The
material
covered

5.4.1

Fabric

Style

ES-1252

5.4.2

Fabric

Style

W-133

is

the wide
activity.
section

a cut-out

broadgoods

of

section

following
materials
by this
specification:
manufactured

manufactured

120

by
by

Woven

Fiberite

cloth

of

are

fabric

master

sample

typical

Structures

M-C-13
i.
1.1
2.

Visual

Examination

of

Broadgood

Roils

SCOPE
Each

roll

of

raw

material

shall

be

visually

examined.

MATERIAL

2.1

Broadgoods.
The material
shall
have
no holes,
non-uniform
weave,
resin
build-up,
contaminants,
defects
which
would
render
more
than
5 percent
roll unsuitable
for the
intended
use.

2.2

To--_," Tape
material
shall
be free
from
dirt,
grease,
or any other
contaminates.
Tape
shall
be uniform
in appearance
and
free
from holes,
tears,
nonuniform
weave
and any other
defects
which
may
be detrimental
to
the use
of the material
for the purpose
intended.

121

tears,
or other
of any

M-C-14

1.
i.i

1.2

Fiber
Ultimate
Tensile
of Carbon
Fiber

Strength

Specification

Limits

SCOPE
A certificate
of compliance
supplier
shall
be submitted
verification
of requirement.
Limits
Minimum
Maximum

(psi)
312,000
--

122

from
the
and will

carbon
fiber
be acceptable

for

M-C-15
i.
1.1

1.2

Fiber

Density

Specification

Limits

of

Carbon

Fiber

SCOPE
A certificate
of compliance
supplier
shall
be submitted
verification
of
requirement.
Limits

(g/cc)

Minimum
Maximum

1.7
--

from
and

123

the
will

carbon
fiber
be
acceptable

for

M-C-16
i.

Fiber

Weight

Specification

Limits

of

Broadgoods

SCOPE

i.i

The
weight
determined

of
in

1.2

Limits

(ounces

Minimum
Maximum

10.0
12.0

the
material
accordance
/

on
with

sq.yd.)

124

all
ASTM

master
rolls
D 1910-64.

shall

be

M-C-17

Thread
Count
Broadgoods

Specification

Limits

on

Master

Roils

SCOPE
The
thread
count
shall
be
determined
1.2

Limits

(Yarns

per

of

on
all
master
with
ASTM
D

rolls
1910-64.

inch)
Warp

Minimum
Maximum

the
material
in accordance

Direction
22.0
26.0

125

Fill

Direction
21.0
25.0

of

M-C-18

i.

Thickness
Broadgoods

Specification

Limits

of

Master

Roils

of

SCOPE

i.i

The
thickness
at
5
shall
be determined-in

1.2

Limits
Minimum
Maximum

psi
tensioning
accordance
with

(inch)
0.016
0.021

126

on all
master
rolls
ASTM
D 1777-64.

M-C-19

Carbon
Reinforcement,
1200
for Rocket
Nozzle
Components

ppm

sodium,

Specifications

SCOPE
This
specification
reinforcement
for
components
1.2

one
solid

type
of
rocket

carbon
motor

nozzle

is

The carbon
reinforcement
covered
by this
specification
intended
for use
in the manufacture
of carbon
cloth
aldehyde-phenolic
for reinforced
plastic
nozzle
components
REQUIREMENTS

covers
use
in

Qualification
specification
qualification

2.2

Material

The material
furnished
shall
be a product
which
requirements.
The

specification
satin
fabric
2000
to 2850
CLASSIFICATION

material

shall
finally
degrees
OF

furnished

Qualification

under

this

be a rayon-based
carbon
eight
harness
processed
at a temperature
range
of
Fahrenheit
(F).

INSPECTIONS

Inspection
and testing
of
be classified
as follows:
3 .i .i

under
this
has met
the

and

the

Conformance

carbon

reinforcement

shall

Inspections
Methods
in
This
Manual

Visual
Examination
........................
Carbon
Assay
and Moisture
Content
.........
Ash
Content
...............................
Weight
....................................
Breaking
Strength
.........................
Specific
Gravity
..........................
Thread
Count
..............................
Thickness
.................................
Sodium
Content
............................

M-C-13
M-C-20
M-C-8,
M-C-16
M-C-22,
M-C-23
M-C-17
M-C-18
M-C-24

21
2

SAMPLING
Qualification.
Two
rolls
of material
shall
be processed
and tested.
Sodium,
ash and carbon
specimens
shall
be
removed
from
the beginning
end
and at 5 other
equally
spaced
axial
locations
along
the length
of each
roll.
One
of each
specimen
shall
be removed
at left,
center,
127

and right
locations
at each
axial
station;
21 total
test
sites.
Three
each
specimens
for all other
properties
shall
be removed
from the exposed
end of each
roll.
Samples
of material
(approximately
2 x 2 inches)
shall
be
removed
from
each
test
site
and sent
to Morton
Thiokol.
These
samples
shall
be tested
for weight
loss
in air and
for alkali
and alkaline
earth
metals
by spectrographic
emission,
for information
only.
One
additional
roll
of
material
shall
be randomly
selected
from
the first
production
lot and subjected
to the
same
tests
as
specified
for the two initial
rolls.
4.2

Quality
conformance.
Each
roll
in the lot shall
be
tested
for carbon,
sodium
and ash content.
Six
specimens,
three
from each end of the rolls,
shall
be
tested.
Three
specimens
shall
be removed
from
the
exposed
end of sampled
rolls
and tested
for moisture,
weight,
breaking
strength,
specific
gravity,
thickness,
and thread
count.
The number
of rolls
to be selected
for
test
shall
be in accordance
with
Table
I.
In addition,
one roll
shall
be selected
at random
from each
of the
first
I0 production
lots
and tested
for sodium
and ash
content
as specified.
Table
Number

1 to
4 to
Ii to
4.3

4.4

I:
of

Sampling
rolls

in

lot

Number
of sample
be selected
for

3
i0
45

rolls
to
testing

All
3
5

Lot.
A lot shall
consist
of that
quantity
of material
w-h-fch is manufactured
at one time,
using
the
same
process,
and under
the same
conditions
of manufacture.
lot shall
not
consist
of more
than
2500
pounds.
Individual
rolls
shall
not exceed
125 pounds.

Accept-reject
criteria.
The lot of material
(qualification
or quality
conformance)
shall
be
acceptable
provided
all individual
values
for sodium,
ash
and carbon
content,
and the average
values
for all other
properties
for each
roll
selected
meet
the requirements.
In the event
that
a single
specimen
fails
to meet
sodium
or ash content,
two repeat
tests
may
be conducted.
The
roll
shall
be acceptable
with
respect
to sodium
and ash
content
if both
repeat
tests
meet
the
applicable
requirements.
Failure
to meet
sodium,
ash,
or carbon
content
requirements
within
one roll
shall
reject
that
roll.
Report
all individual
and average
values
and test
data.

128

M-C-20
i.
I.i

Ash

Content

of

Filler

Material

SCOPE
The ash
follows:

content

determination

shall

be

performed

as

NOTE:
The
ashed
samples
shall
be used
to measure
sodium
content.
Care
should
be exercised
not
to contaminate
the
sample
with
sodium.
Samples
should
not be touched
with
the hands.
2.

PROCEDURE

2.1

Take
test
oven

2.2

Remove
the
desiccator.

2.3

Weigh
approximately
2 grams
of the
nearest
0.i mg.
into
separate
tared
crucibles.

2.4

Heat
the
16 to 18

2.6

Remove
the crucible
in a desiccator
to

2.7

Obtain
the
as follows:

an approximate
4 gram
representative
sample.
Place
specimen
in a beaker
and dry in an air circulating
at 225 + 5 OF. for a minimum
of one hour.

Percent

specimen

crucible
hours
or

from

oven

and

cool

in

cooled
specimen
to the
ceramic
or platinum

in a muffle
furnace
at 600 + 15C
until
constant
weight
is acEieved.
containing
the ashed
cool
and weigh
to the

post-heat

ash

the

(A-B)

weight

x
W

and

calculate

specimen,
nearest
the

Where:
A
B
w

=weight
= weight
= weight

2.8

Report

ash

2.9

Retain

specimen

2.10

of crucible
of crucible,
of original

content

Limits

(percent

Minimum
Maximum

0.0
0.5

to

for

the

plus
ash,
gm.
specimen,
nearest

measurement

ash)

129

gm.
gm.

0.i0
of

percent.

sodium

place
0.i mg.

percent

i00

content.

for

ash

M-C-21
i.

Breaking

Strength

Specifications

for

Broadgood

SCOPE

i.I

The
breaking
specified
in

1.2

Limits

strength
test
ASTM
D 1682.

(ib/inch

of

be

conducted

as

width)
Warp

Minimum
Maximum

shall

direction
20
__

130

Fill

direction
15

Rolls

M-C-22
i.
i.i

1.2

Specific

Gravity

Specification

of

Broadgoods

SCOPE
The
test
accordance
alternate
Limits
Minimum
Maximum

for specific
with ASTM
method.

(at

gravity
135 or

25C)

1.8
1.9

131

shall
C 604

be conducted
may
be used

in
as an

M-C-23

i.

Sodium
Method

Content

of

Filler

Material

by

Flame

Emission

SCOPE

i.i

2.

The sodium
content
with
the following:

determination

shall

be

in

accordance

PROCEDURE

2.1

Obtain

2.2

Wash
down
laboratory
milliliters

Bring
the acid mixture
to a boil,
cool
the crucibles
transfer
the contents
of each
to a one
liter
volumetric
flask
and dilute
to volume
with
distilled
water
or
deionized
water.

ash

sample

as

in

M-C-20.

the walls
of each
crucible
with
distilled
or
grade
deionized
water
and add approximately
5
(ml.)
concentrated
hydrochloric
acid
to each.

2.4

Determine
the sodium
content
of each
flask
by flame
emission
at 589 nanometers
(nm) using
the instrument
manufacturers
operating
instructions
and a calibration
curve
for sodium
which
is linear
between
0.i and 2.5
micrograms
per milliliter.

2.5

Report
(ppm).

sodium

content

to

the

132

nearest

i0

parts

per

million

M-C-24
i.

Raw

Graphite

Fabric

Visual

and

Physical

Inspection

SCOPE

i.i

Scope.
for the

1.2

Classification.
Raw
graphite
fabric
shall
be classified
into
the three
following
groups.
The classification
depends
on visual
and physical
characteristics.
Group
Group
Group

2.
2 1

2.1.1

3.1

describes
grouping
of

a detailed
procedure
raw graphite
fabric.

A
B
C

APPLICABLE

DOCUMENTS

The
following
form
a part

of

documents,
the
issue
this
instruction:

U. S. Polymeric,
Inc.:
(a)
QCi-9-1,
Material
Control
(b)

3.

This
instruction
inspection
and

QCi-10-1,

in

effect

Identification,

Indication

of

Set

inspection

at

the

Storage

Inspection

by

time,

and

Stamps

PROCEDURE
Machine
follows:

set-up.

up

the

machine

as

3.1.1

Vacuum.
Turn
for leaks
and
necessary.

3.1.2

Threadin@
the
leader.
Starting
from
the unwind
side
of
the inspection
machine,
thread
a leader
under
the
first
roller,
uP over
the top
roller,
down
through
the vacuum
head,
under
the next
roller
and then
to the
rewind
roller.
See Figure
i.

3.1.3

Unpacking.
Carefully
polyethylene
wrapping
not touch
with
hands,
of product.

on the
dirt.

vacuum
Change

and
the

check
vacuum

unpack
the fabric
for repackaging.
because
of sodium

the vacuum
bag
if

bag

saving
the
Use gloves,
contamination

3.1.4

Mounting
the
fabric.
Place
the roll
of fabric
unwind
shaft
and secure
the roll with
chucks.
two-sided
tape,
attach
the leader
to the
fabric
close
to the leading
edge
as possible.

3.1.5

Alignment
of fabric.
Run the fabric
through
the
machine
at low speed
to the windup
end with
the brake
off.
Center
the
fabric
on the rollers
if necessary.
Remove
the leader
and tape
the fabric
to a 3-inch
ID
133

do

on the
Using
as

core
on
uniform
and the

the wind-up
shaft
providing
good
alignment
tension
on the
fabric
between
the windup
first
roller.

3.1.6

Maintaining
alignment.
Maintain
good
windup
shaft
by adjusting
the position
shaft.

3.1.7

Inspection
maintain
brake
to

3.2

and
shaft

alignment
on the
of the unwind

speed
and tension.
Start
the machine
and
slow
speed
with
the brake
on.
Adjust
the
provide
optimum
tension.

Inspection
and classification.
General
inspection
shall
be conducted
from
the back
of the machine,
viewing
the
fabric
in the vertical
position
and over
the top
roller;
see areas
A and B of Figure
i.
Inspect
for bagginess
in
area
C.
Sampling
shall
be as designated.

3.2.1

3.2.1.1

Group
A.
following:

Group

Color

Pieces.
There
the
roll.

3.2.2

rolls

shall

conform

to

the

Defects.
The
roll
shall
be free
from
visual
defects
including
bags,
puckers,
brittleness
or stiffness,
weave
defects,
holes
and tears.
All workmanship
must
be of the highest
quality.
Color.

3.2.1.4

Length.
shall
be
Group
B.
following:
Color.

shall

be

shall

be

The minimum
20 yards.
Group

Color

uniform
no

shall

more

length

rolls

of

shall

be

throughout

any

conform

uniform

Brittleness
and stiffness.
or stiff
areas
in the roll.

than

the

three

pieces

piece

in

to

the

throughout

There

shall

roll.

the
be

no

in

roll

roll.
brittle

3.2.2.3

Creases.
There
shall
be no more
than
two
(2) creases
per width
of fabric.
Creases
shall
be a minimum
of
two
(2) yards
apart.
No crease
shall
fold
over
or be
deeper
than
three
eights
(3/8)
inch nor
longer
than
six inches.

3.2.2.4

Weak
material.
The
permitting
stretching
inspection.

3.2.2.5

Weave
defects.
distortion
or

There
pulled

material
shall
or distortion

shall
be
threads.
134

no

not
be
during

excessive

weak,

weave

3.2.2.6

Holes
and tears.
Holes
and tears
greater
than
three
eights
(3/8)
inch in any one dimension
shall
be a
minimum
of three
(3) yards
apart
in the warp
direction.
There
shall
not be more
than
two
(2) per
sixty
(60) yards.
Holes
shall
not be greater
than
one
(i) inch.

3.2.2.7

Width.
The width
of the
fabric
than
two
(2) inches
throughout
not
be ragged
uneven
edges.

shall
not
the roll.

3.2.2.8

Length.
shall
be

any

3.2.2.9

Bag.
Bag shall
not exceed
the
measured
in a 30 inch
horizontal

The minimum
length
nine
(9) yards.

of

piece

following
span:

vary
There

in

more
shall

roll

limits

when

3.2.2.9.1

The
bag shall
be no greater
(1-1/2)
inches
in depth
by
width
of the fabric
or

than
one and
three-fourths

3.2.2.9.2

The
bag shall
(2-1/2)
inches
of the
fabric

than
two and one-half
one-half
(1/2)
the width

3.2.2.9.3

The
bag shall
be no greater
than
four
depth
by one-third
(1/3)
the width
of

3.2.2.9.4

In no
depth.

case

3.2.3

Group
C.
Group
more
defects
in

3.2.4

Borderline
placed
in

3.2.5

be no greater
in depth
by
or

shall

the

bag

exceed

four

(4)
the
(4)

one-half
(3/4)
the

inches
fabric.
inches

in

C shall
be rolls
that
contain
one
excess
of those
for groups
A or B.

material.
the lower

of

Borderline
the two

material
groups
in

in

or

shall
be
question.

Unlisted
defects.
Any
defects
which
are not
listed
above
found
within
a roll of material
shall
be brought
to the
attention
of the shift
supervisor
or leadman,
when
found,
in order
that
an immediate
evaluation
and
grading
can be made
on the material.

3.3

Packaging.
Each
roll
of fabric
shall
be repackaged
the origznal
shipping
container
with
the polyethylene
wrapping
as originally
received.
Rolls
originally
supported
shall
be repackaged
in the same manner.

3.4

Marking.
QCi-9-1

3.5

Segregation.
accordance

Each
roll
and QCi-10-1.

with

shall

be

Non-conforming
QCi-9-1.
135

marked

in

items

shall

accordance

be

in

with

segregated

in

4.
4.1

5.
5.1

REPORTING
Duplicate
inspection
reports
shall
be kept
for each
roll
inspected.
The
inspection
reports
for Group
A and B
shall
be stamped
"visually
accepted"
and reports
for
Group
C shall
be stamped
"Hold
for material
review"
in
accordance
with
QCi-10-1.
One copy
of the report
shall
be forwarded
to Incoming
Quality
Control
and the other
shall
be retained
in inspection.
NOTES
Definitions.

5.1.1
the
5.1.2

5.2

The deviation
of the
fabric
from
the
e established
by two
(2) parallel
bars
fabric
is spanned.

Creases.
Creases
in the
fabric.

are

Handling
of high
purity
purity
fabrics,
gloves
contamination.

small

bags

or

fabrics.
When
must
be Worn
to

136

wrinkles

handling
avoid

horizontal
over
which

appearing

high

VISUAL

INSPECTION

OF

RAW

GRAPHITE

FABRIC

F
R
O
N
T

O
_

_'1<
SIDE

VIEW

Fig.

137

-!"

r !

M-C-25
i.
i.I

2.
2.1

pH

of

EQUIPMENT

AND

Beakers,

2.1.3

pH

2.1.4

Watch

2.1.5

Hot

minimum

150

meter,

Hot

Water

Extraction

ml.

Corning

glass,

65

sensitivity

tall

gm.

form

model
mm.

0.i

7 or

equivalent

(2-1/2")

plate

Materials
Distilled

water,

freshly

boiled,

pH

7.00

0.05

SAMPLING
Sample
of at

3.2

Number
conduct

4.1

and

MATERIALS

balance,

3.1

4.

Cold

Equipment

2.1.2

3.

Both

This
procedure
describes
two methods
for the
determination
of pH of raw fabrics.
Method
I describes
procedure
for the determination
of pH using
cold
water
extraction.
Method
II describes
a procedure
for the
determination
of pH using
hot water
extraction.

Pan

2.2.1

by

SCOPE

2.1.1

2.2

Fabric

size.
least

The
test
8 gms.

requires

of determinations.
Unless
duplicate
determinations

a representative

sample

otherwise
specified,
on each
sample.

PROCEDURE
Method
I.
Cold water
determinations
of pH.

extraction

of

fabrics

for

4.1.1

Extraction.
weigh
4.0 + 0.2 gms.
of fabric,
cut to
approximately
1/2"
x 1/5" pieces,
into
a 150 ml.
beaker.
Add
i00 + 2ml.
of room temperature
freshly
boiled
distilled
water
with
a pH of 7.0 + 0.05.
Stir
the
fabric-water
mixture
and ascertin
that
the fabric
has
been
thoroughly
wetted.
Cover
with
a watch
glass
and allow
to stand
at room temperature
for 60 + 5
minutes.

4.1.2

Determination
of pH.
If necessary,
calibrate
the pH
meter
in accoraance
with
SCM-7-02.
Rinse
the
electordes
with
distilled
water
and immerse
the
electrodes
about
one inch
in the solution
to be tested.
138

Turn
the instrument
to
seconds
to pass
before
reading
to the nearest
4.2

4.2.1

5.1

Method
II.
determination

Hot water
of pH.

the
"read"
position
taking
a reading.
0.02
pH unit.

extraction

of

fabrics

and allow
Record
the

for

15

the

Extraction.
Weigh
4.0 +
0.2 grams,
of fabric,
cut to
approximately
1/2" x 1/5" pieces,
and transfer
to a 200
ml.
beaker.
Add
i00 + 2 ml.
of freshly
boiled,
distilled
water
with _ pH of 7.0 + 0.05.
Cover
with
a
watch
glass
and boil
on a hot plate
for 20 to 30
minutes.
Remove
from the hot plate
and allow
the
solution
to reach
room
temperature.
Add
freshly
boiled,
distilled
water
with
a pH of 7.0 + 0.05
to
bring
the volume
to i00 + 2 ml.
and determine
the pH as
in 4.1.2.
CALCULATIONS

AND

REPORTING

Report
the average
of
Duplicate
determinations
the
range
exceeds
0.5

two
pH

tests
should
unit.

139

to
be

0.01
pH unit.
considered
suspect

if

M-C-26
i.
i.i

1.2
2.
2.1
3.

Fabric

Thread

Count

for

Both

Warp

and

Fill

Direction

SCOPE
Scope.
This
determination
inch
of woven

method
describes
of the number
cloth.

Equivalent
191 b, Meth6dmethod,
5050.. iThis
EQUIPMENT

AND

Equipment.

of

method

a procedure
warp
and

for the
fill yarns

is

similar

apparatus

with

to

per

CCC-T-

MATERIALS
Thread

counter

magnifier

SAMPLING

3.1

Sample
size.
Sufficient
sample
shall
be obtained
so as
to permit
specified
number
of determinations
to be made
in each
the warp
and fill directions.

3.2

Determinations.
determinations
directions.

4.

Unless
will
be

otherwise
specified,
made
in each
the warp

PROCEDURE

4.1

Preparation
of sample.
The
smoothly
and without
tension

4.2

Determination

4.2.1

4.2.2

5.
5.1

five
and fill

of

thread

cloth
shall
be
on a horizontal

laid
out
surface.

count.

Area
of determination.
The
actual
count
shall
be
determined
from
representative
sections
of the cloth
along
the warp
and fill directions.
No count
shall
made
nearer
than
3 inches
to the selvage
edge,
or
either
end,
and no two determinations
should
include
the samethreads.
Inches
for each
count.
threads
per inch,
count
determination;
if there
inch,
count
three
inches
CALCULATIONS

AND

be

If there
are more
than
25
one
inch
for each
are fewer
than
25 threads
per
per
each
determination
made.

REPORTING

Average
the specified
number
of determinations
for each
warp
and
fill direction
and report
these
values,
rounded
off
to the nearest
whole
number.

140

M-C-27
i.

Fabric

Weight
Conditioned,

Using
Small
Specimens
of
and Devolatilized
Methods

Unconditioned,

SCOPE

i.i

This
method
describes
a procedure
for determination
fabric
weight
using
small
specimens.
Unconditioned,
conditioned,
and devolatilized
methods
are included.

1.2

The

2.

procedure

is

equivalent

to

CCC-T-191,

Method

of

5041.

EQUIPMENT

2.1

Scissors

2.2

Analytical

Steel

balance,

template,

2.4

Stanley

2.5

Desiccator

Oven

Timer

2.9

Oven,

3.

humidity

capable

3.1
4.

forced

SAMPLE
One

or

with

Desiccator
2.8

6.76

knife

relative

sensitivity

of
with

inches

0.0001

gm.

square

equivalent
conditioning
of

65

chemicals

2%

maintaining
silica

giving

70 +

gel

or

3F.

equivalent

air

SIZE
linear

yard

shall

be

taken

for

test.

PROCEDURE

4.1

From
the sample,
cut at random
five
(5) specimens
each
6.76
inches
square.
No specimen
shall
be closer
than
three
inches
to the selvage.
Weigh
individual
specimens
to 0.01
gm.

4.2

If the
for 24
3 F.

4.3

If devolatilized
method
is used,
omit
paragraph
4.2 and
suspend
specimens
in a forced
air oven
at 320 _ + 5F.
for
15 Z 0.25 minutes.
Weigh
individual
specimens
Eo 0.01
gm.

conditioned
method
is used,
precondition
+ 2 hours
at 65 + 2% relative
humidity
Weigh
individual-specimens
to 0.01
gm.

141

specimens
and 70

CALCULATIONS

AND

REPORTING

5.1

The
its

5.2

To calculate
unconditioned
obtain
the average
of the
Designate
as Unconditioned
of the
five
fabric
weights

5.3

To calculate
conditioned
fabric
weight,
average
of the five
values
of paragraph
as Conditioned
Fabric
weight,
W2.
The
fabric
weights
should
not exceed
2.0%.

5.4

To calculate
devolatilized
fabric
weight,
obtain
the
average
of the five values
of paragraph
4.3.
Designate
as Devolatilized
Fabric
Weight,
W 3.
The
range
of the
five
fabric
weights
should
not
exceed
2.0%.

5.5

To

individual
weight
in

calculate

specimen
weight
ounces
per square

volatile

in grams
yard.

equivalent

to

fabric
weight
(as received),
five values
of paragraph
4.1.
Fabric
Weight,
W I.
The
range
should
not exceed
3.0%.

content,

use
W1

% Volatile

is

Content

the

following

- W 3 x

=
W 1

142

obtain
the
4.2.
Designate
range
of the five

i00

formula:

M-C-28

i.
i.i

Apparent
Volume
and
and Cured
Material

Density

of

Raw

Fabric,

Prepregs,

SCOPE
This
procedure
describes
a method
for determinations
of
apparent
volume
of raw fabrics,
prepregs,
cured
parts
and
other
related
materials
by use
of an air comparison
pycnometer.
After
apparent
volume
has been measured,
apparent
density
can be calculated.
This method
is
suitable
for the analysis
of non-surface
active,
noncompressible
materials.
NOTE:
Instrument
limitations.
Materials
such
as carbon
fabric
will
not yield
reproducible
values,
however
graphite
fabric
will
yield
reasonably
accurate
results
even
though
it is surface
active.

2.
2.1

EQUIPMENT

AND

MATERIALS

Equipment.

2.1.1

Pycnometer,
operators

2.1.2

Oven,

930,

Beckman,

analytical,

bottle

with

minimum

equivalent

and

sensitivity

0.001

gm.

regulator

NOTE:
Unless

Usable
gases.
Any
otherwise
specified

2.1.5

Vacuum

source

2.1.6

Laboratory

3.

or

vacuum

Balance,
Gas

Model
manual.

inert
gas may
use helium.

be

used.

knife

SAMPLING

3.1

Sample
Size.
Obtain
a representative
size
sample
of
approximately
five
(5) grams
for bulky
materials
(raw
fabrics
should
be about
i" by 36").
For
solid
materials
(cured
parts),
a sample
size
up to 50 c.c.
can be
measured.
A greater
degree
of accuracy
can be achieved
by using
larger
sample
sizes,
but the sample
size will
be
dependent
upon
the ability
of the sample
to fit into
the
sample
cup
(maximum
volume
50 c.c.).

3.2

Number
of determinations.
Unless
otherwise
one determination
will
suffice
but, multiple
must
be made,
see paragraph
4.3.1.

143

specified,
measurements

4.

PROCEDURE

4.1

Sample
conditionin
9.
Unless
otherwise
specified,
condition
sample
by inserting
in a vacuum
oven
heated
to
275 + 5F.
After
exposure
under
full
vacuum
for 20 to
30 minutes,
remove
sample
from
oven
and
immediately
weigh
to nearest
0.001
gm.

4.2

Instrument

calibration.

4.2.1

Initial
warm-up.
At the start
of a series
of
measurements
the instrument
should
be loosened
and
warmed-up.
This
is done
by turning
both
the measuring
and
reference
handwheels
in and out
several
times
with
the purge
and coupling
valves
open.

4.2.2

Volume
check.
Accuracy
of the unit
should
be checked
for volume
by inserting
either
the
I" or 1-1/2"
steel
test
ball
in the sample
cup,
and measuring
volume
of
the ball
per paragraph
4.3.
The volume
readings
obtained
from the test balls
should
be a consistent
8.58 ml.
for the i" steel
ball
and 28.96
ml.
for the
1/2"
steel
ball.
If the ball measurement
exceeds
a
volume
tolerance
of + 0.15
ml.
for either
ball,
refer
to the
Instruction
Manual
for adjustment
instructions.

i-

NOTE:
Ball
checks,
when
checking
several
samples
during
one series
of tests,
periodic
checks
of the ball
should
be made
to make
sure
the
instrument
is still
reading
accurately.
This
is best
done
by checking
the
ball
in between
every
third
or fourth
sample
that
is
being
tested.
4.2.3

4.3

Zero
check.
The
zero check
procedure
is identical
to
paragraph
4.3,
but is made
with
the sample
cup clean
and empty.
If the final
counter
reading
is other
than
zero,
refer
to the Instruction
Manual
for adjustment
instructfons.
Specimen
volume
designated,
the
in determination

measurements.
Unless
otherwise
following
procedure
shall
be utilized
of apparent
volume:

4.3.1

Adjust
gas pressure
pressure
no greater

regulator
on
than
2 psi.

4.3.2

With
purge
and coupling
valves
open,
rotate
both
handwheels
in a counter-clockwlse
direction
to the
extreme
position.
Turn
the measuring
wheel
until
starting
number
is reached
(located
on a plate
affixed
to the
side
of the case above
the measuring
handwheel).

144

the helium
Turn
vacuum

tank
to
supply

a
on.

4.3.3

Insert
previously
conditioned
into
the sample
cup
and insert
and secure
it firmly.
Open

purge

and

coupling

and weighed
sample
cup

specimen
into position

valves.

Open
vacuum
valve
and allow
evacuate,
then
close
valve.

i0

seconds

for

system

to

4.3.6

Open
gas
pressure

4.3.7

Open
vent
valve
for 5 seconds
equilibrium,
then
close
vent

4.3.8

Wait
for
l0
valve
(this

4.3.9

Wait
for
i0 seconds
then,
turn
both
handwheels
clockwise
simultaneously
until
the
reference
wheel
stops.
Apply
minimum
amount
of pressure
after
the
wheel
initially
stops.
Keep
the pointer
on the scale
during
this
process.

(helium)
valve
to equilibrate,

seconds
should

and allow
then
close

5 seconds
for
gas valve.

for pressure
and purge
valves.

then
loosen
the coupling
be rotated
a couple
of times)

4.3.10

Wait
for
alignment
handwheel

i0 seconds
and adjust
pointer
by image
to the zero mark
with
the measuring
(See Instruction
Manual).

4.3.11

Open
coupling
valve.
counter
directly
in

4.3.12

Open
purge
valve
and
consistent

Read
ml.

specimen

volume

on

valve
and vent
valve,
then
close
vent
repeat
steps
4.3.2
through
4.3.11
until
readings
are obtained
on each
specimen.

NOTE:
When
opening
coupling
valve,
(differential
pressure)
indicator.
position,
true null
was not obtained
should
be repeated.

145

observe
null
If it shifts
and the run

5.1

CALCULATIONS

AND

Calculations.
apparent
volume

REPORTING
To calculate
apparent
density
use
the following
formula:

from

NOTE:
Specific
gravity.
Density
and specific
gravity
may
be considered
identical
for all practical
purposes
in
the measurements
of materials
whose
density
does
not vary
appreciably
with
temperature.
Density

5.2

Weight
Volume

of dried
reading

specimen,
obtained,

Reportin
9.
Report
specific
gravity
figures.
In addition
to reporting
report
specimen
weight
and apparent
Specific

Gravity

= Density
Density

146

gms..
c.c.

to four
specific
volume.
=

of

H20

gm./cc.

significant
gravity,

Density
0.9975

Sp.G.

M-C-29

Raw
Carbon
Fabric
Defect
Categories

I.

SCOPE

i.i

Raw

2.

Carbon

Fabric

Into

Both

Minor

and

Major

Inspection

MATERIAL

2.1

Run material
Control
and

2.2

CSA(II05,1183)
side up

3.

Inspection

as follows
Production
Fill

or as instructed
management.
side

up

by

Quality

VCK-VCL(1073,1113)

Warp

DEFECTS
Defects
are classified
as
minor
defects,
i.e. those
be considered
major.

3.1

Table

of

Minor

Minor
3 .i .i

3.1.2

Defects

either
minor
or major.
exceeding
the allowables

and

Allowables

Defects

Allowables

Oil
free
finger
prints
causing
localized
weave
distortion

3 per

Frayed
fill
bands
across
the width,
e.g.
rack bands

6"
of

Puckers

3.1.5.1

3.1.5.2

3.1.6

linear

long
roll

by

yard

width

< 9 square

Mispicks,
floats,
skips,
outs,
missing
picks
3.1.5

Large
shall

in.area

end
4 per

linear

yd.

Kinks
Clusteredless
per

24 or
6" x 6"

clusterslinear

yd.

area

Continuous
- not
closer
than
3 inches

42 or less/linear
(2% of end count)

yd.

Bagginess

3.1.6.1

One
(20

only
maximum)

Loss
from

of tension
the edge

<

6"

in.

3.1.6.2

Both
edges
(20 yds.
maximum)

Loss
from

of tension
the edge

< 4"

in.

edge
yds.

147

3.2

Table

of

M@Jor

Major

Defects

and

Defect

minor
in
allowables

Min.

3.2.1

Any
the

3.2.2

Spot
- any noticeable
caused
by oil,
dirt
foreign
material

excess

wrinkles
greater
or less
apart

0.i

0.i
or

Folds
or
occurance
6 inches
2 inches

3.2.4

Holesgreater

any occurance
than
1/4 inch

3.2.5

Splice

3.2.6

Cut or tearwhich
cannot
a hole

3.2.7

Change
in
at splice

- any
than
than

0.5

0.i
dia.

bad splice(not
good
splice

0.5
0.2

flat)

any occurance
be considered

warp

and

fill

0.5

side

Reject

Roll

INSPECTION

4.1

Inspect
and
fill out
those
defects
greater

4.2

Defective
but not

4.3

Material

with

approved.
shall
be

Material
rejected.

5.

Defect/yd.

of

3.2.3

4.

Allowables

yardage
less
than

an inspection
sheet
than the
allowables.

equals
minimum

3.0%

or

the
of

less

with

amount
0.i or

defective
3.0%

or

recording

only

of affected
yardage
0.5 as above.
material

more

shall

defective

CALCULATIONS
Percent

Defective

= Total

number
Total

148

of def.
ydg.

yds

be

material

(100%)

M-C-30

Broadgoods
Minor
and

WRAPPING

Visual
Inspection
Major
Defects

and

3"

1.2

Fabric

1.3

Use
a minimum
of 1 unit
desiccant
6 mil
*poly
bags
and tape
excess
core
to create
a good
seal.

1.4

Wrap
material
below.

such

1.5

Width

inches

1.6

Roll

2.1

diameter

core

shall

be

36-48

size

- No

2-6"
taped

defects

(do

Oil
free
finger
causing
localized
distortion

2.1.2

Frayed

2.1.3

Puckers

2.1.4

Mispicks,
end outs,

2.1.5

Kinks

fill

than

material

to

full

width

that

Defects
are classified
minor
defects,
in those
considered
major.
Minor

longer

minimum,

2.1.1

not

bands

Both

floats,
missing

2.1.5.2

Continuous
- Not
closer
than
3"

14"

diameter

maximum

minor
the

6"

skips,
picks

unwrap

or major.
allowable

linear

long

by

9 square

4 per

linear

Large
shall
be

yard

width

of

inch

area

roll

yard

2 clusters
per linear
yard
(2% of end count)

42 or less
per linear
yard
(2% of end
count)

2.1.7

Contamination
brushed
away

can

but

2 per

linear

be

do
149

not

remove)

yard

and

per

Allowable

3 per

across

core.

bags
per MiI-D-3464
at material
edges
to

remove)

Abnormal
slot
or spring
marks
less
than
2" wide

(record

the

will

as either
exceeding

2.1.6

defects

of

material

24
6"

that

width.

the

Clustered
or per
6"
area

Major

the

prints
wave

2.1.5.1

2.2

For

REQUIREMENTS

i.i

2.

Criteria

Min.

2.2.1

Holes

less

2.2.2

Tears

or

2.2.3

Wrinkle
4" long

2.2.4

Heavy
resin
diameter

2.3

Major

than
cracks

less

2.3.2

Treater

2.3.3

Contamination,

2.3.4

Holes

2.3.5

Weak

2.3.6

Heavy

resin

2.3.7

Tears

or

2.3.8

Selvage

caused
by
caused
by
occurances
folds

long

than

to

i"

0.I

splice

wrinkle

brittle

roll)
or foreign
contamination.
are
acceptable,
however,
to your
supervisor.

foldovers

which
i"

0.i
0.i

oil,
grease,
treater
fuzz
and report

that

can

not

can
be

not

be

removed.

removed.

diameter.

areas.

spots

cracks
(trim

4"

than

and

and

larger
or

up

(remove

0.i

than

less

spots

defects

Spots
Spots
record

in

excess

greater
and

of

than

I"

4"

diameter.

long.

remove)

Splicing

2.4.1

Open

2.4.2

Splice

2.4.3

Splices
can be no
than
5 yards
from

2.4.4

Flag

3.

diameter

foldovers

2.3.1

2.4

i"

Allowances
Per Yard

splice

(do

must

all

not

allow

splices

bond

the

together

material

to

with

tape).

roll

up

less
than
5 yards
apart
the end of the
roll.
and

record

on

inspection

smoothly.
nor

closer

sheet.

INSPECTION

3.1

Inspect
and
those
major

3.2

Defective
but not

fill out an inspection

defects
greater
that

yardage
less
than

equals
minimum

the
of

150

sheet
recording
the
allowable.

amount
of
0.i linear

affected
yard.

only

yardage

3.3

Material
approved.
shall
be

with
5.0%
Material
rejected.

or less defective
with
5.0%
or more

material
defective

shall
be
material

CALCULATIONS
% Defective

= Total

No. of
Total

151

defective
yardage

yards

i00

M-F-I
i.

Ash

Content

of

Fillers,

Scope.
This
determination
pigments
and
1750VF.

1.2

Equivalent
procedures.
ASTM-D1506-59.

2.1

EQUIPMENT

AND

method
describes
of ash content
related
materials

2.1.2

Oven,

2.1.3

Analytical

balance,

2.1.4

Crucibles,

porcelain,

This

a
of

procedure
ignitable
which
will

procedure

for the
fillers,
ash
at

is

equivalent

to

furnace
forced

air
minimum
wide

sensitivity,
form

with

0.1

mg.

covers

SAMPLING

3.1

Sample
least

3.2

Number
of determinations.
run duplicate
determinations.

4.1

Materials

Equipment.
Muffle

4.

Related

MATERIALS

2.1.1

3.

and

SCOPE

i.i

2.

Pigments

size.
5 gm.

Obtain

representative

Unless

sample

otherwise

of

at

specified,

PROCEDURE
Drying
sample.
Condition
about
porcelain
crucible
in a forced
minutes
at 225 +
5_F.

5 gm. of sample
air oven
for 60

in a
5

4.2

Weighin
9.
gram
into

4.3

Ignition.
Place
sample
into muffle
furnace
at 1750
+ 50
F.
Ignite
for about
4 hours.
A longer
time
period
may
be necessary.
Keep
the furnace
door
open
about
1/4 inch
to admit
air.
Check
for completeness
of ashing
by
cooling
the sample
in a desiccator,
weighing,
reigniting
for 1 hour,
then
cooling
in a desiccator
and re-weighing,
as often
as necessary,
to contant
weight.

4.4

Final
weight.
When
ashing
is determined
complete,
cool
the sample
in a desiccator,
crucible
and residue
to 0.0001
gm.

Weigh
about
2 gm. to
a prefired
and weighed

152

the nearest
porcelain

to

0.0001
crucible.

be
then

reweigh

CALCULATIONS

AND

Calculations.

REPORTING
Calculate

ash

content

as

follows:

W3-W 1
Ash

Content,

Wt.

i00

W2-W 1
where:
W 1 = weight
W 2 = weight
W 3 = weight
5.2

of
of
of

prefired
crucible
crucible

Reporting.
Unless
otherwise
report
ash content
to 0.01%.
should
be considered
suspect
than
0.1%
ash content.

153

crucible,
gms.
plus
sample,
gms.
plus
residue,
gms.
specified,
round
off
and
Duplicate
determinations
if they
differ
by more

M-F-2
i.
i.i

2.

Particle

Size

and

This
procedure
describes
the method
particle
size
of a powdered
material
Sub-Siever
Sizer.
EQUIPMENT

AND

a Sub-Siever

Sizer

Sub-Siever

2.2

Brass

Sample

Tube

2.3

Brass

Porous

Plugs

2.4

BX

2.5

Small

2.6

Sample

Filter

Paper

Powder

for determining
the
using
the Fisher

MATERIALS

Fisher

Sizer,

and

operators

manual

14-313-5

Discs

3/4"

Dia.

Funnel

Thief

SAMPLING

3.1

A representative
required.

3.2

when
drums
or other
large
the use
of a sample
thief
representative
sampling.

3.3

An average
required.

4.

Using

SCOPE

2.1

3.

Distribution

OPERATING

of

sample

at

PROCEDURE

least

(See

(approximately

containers
is required

three

(3)

Operators

1.0

are
to

ounce)

to be
insure

determinations

is

sampled,
a

are

Manual)

4.1

Before
using
the Sub-Sieve
Sizer,
make
certain
that
the
drying
tube
is filled
with
the
indicating
drying
agent,
10-20
mesh
Drierite.
The Drierite
has been
treated
with
a substance
that
indicates
the state
of dryness
of
the agent,
the condition
of which
can be determined
by
observing
the drying
tube
through
the small
window
in
the left
side
of the cabinet.
A blue
color
indicates
that
the
agent
is satisfactory.
A pink
color
indicates
that
the
agent
must
be replaced
with
fresh
stock.

4.2

The
Sample
Packing
Assembly,
consisting
of the
rack
and
pinion,
(i) compact
the powder
sample
after
the sample
has been
weighed
into
the sample
tube,
and
(2) also
measure
the
actual
height
of the packed
powder
sample.
Before
these
can be done,
however,
the assembly
must
be
adjusted
to compensate
for the thickness
of the two
porous
plugs
and filter
papers
which
serve
to confine
the sample
in the sample
tube.
154

4.3

The
sample
following:

packing

assembly

can

be

adjusted

by

the

4.3.1

Set
two porous
plugs
between
them
on the
that
the lower
plug

4.3.2

using
the Rack
and Pinion
Control
(E), guide
the
rack
down
onto
the top porous
plug.
The
tip of
the pointer
should
now coincide
exactly
with
the
baseline
on the Calculator
Chart.
If not,
loosen
the
locknut
that
holds
the lower
brass
post
in its mount
and adjust
the height
of the post
by screwing
it up or
down.

4.3.3

When
the tip of the pointer
coincides
exactly
with
the baseline
on the Calculator
Chart,
the
initial
level
of
the liquid
meniscus
in the manometer
must
be
made
to exactly
coincide
with
the upper
edge
of the
curved
portion
of the metal
cross
bar
attached
to the
rack.
Use the Manometer
Level
Control
but only
when
the sample
tube
is not
attached
to the instrument.
Once
the adjustment
has been made
for a particular
determination,
the Manometer
Level
Control,
must
not
be turned
until
that
determination
has
been
completed.
Check
the manometer
level
before
each
successive
determination
and correct
as necessary.
All water
level
measurements
are taken
with
reference
to the
upper
edge
of the curved
portion
of the cross
bar,
and
all chart
readings
with
reference
to the
extreme
tip
of the pointer
mounted
on this
same
cross
bar.

4.4
4.4.1

4.5
4.5.1

Porosity

with
two filter
papers
brass
post
(J), making
certain
touches
the upper
end of the post.

Scale

The
porosity
of a packed
sample,
or the
ratio
of the
air space
in the sample
bed to the
total
volume
occupiedby
the packed
sample,
is read directly
from
the Porosity
Scale
located
along
the bottom
edge
of the
Calculator
Chart.
A given
sample
may
be packed
to
many
different
porosities.
Therefore,
an Optimum
Porosity
Point,
or the porosity
setting
at which
a
particular
powder
can be measured
on the
Sub-Sieve
Sizer
with
the minimum
possibility
of error,
must
be
found.
For micropulverized
dicyandiamide
(dicy)
this
Optimum
Porosity
Point
has
been
determined
to be 0.625.
Measurin@

Particle

Size

Plug
the line
cord
into an applicable
receptacle,
flip
the power
switch
(L) to
the
instrument
to warm-up
for 20 minutes
chance
to stabilize.
While
the unit
is
perform
steps
4.5.2
through
4.5.8.
155

ON,
and
to give
warming

allow
it a
up,

4.5.2

Lay
a paper
disc
over
one end of the sample
tube.
Then,
with
the perforated
surface
of the plug
against
the surface
of the paper
disc,
push
one of the
two porous
plugs
about
one-half
inch
into
the tube,
forcing
the paper
to crimp
around
the edges.

4.5.3

Place
the tube
with
the paper

4.5.4

weight
(to within
0.01
gm.)
a sample
of dry
powder
equal
in grams
to the true
density
of the
sample.
(For each
new
lot of dicy,
its density
must
be calculated
with
the use
of the Helium
Pycnometer.)

4.5.5

Using
a powder
funnel,
completely
transfer
weighed
sample
into
the sample
tube.
Tap
the tube
to settle
the powder.

4.5.6

vertically
in the
rubber
side
of the plug
up.

Lay
a second
paper
disc
over
the
sample
tube,
and
force
the other
disc
down
into
the tube.

support

top of
porous

the
the side

the
plug

and

of

paper

4.5.7

Place
lower
post.

4.5.8

Using
the Rack
rack
until
the
plug.

4.5.9

Move
the Calculator
Chart
so that
the pointer
set at the Optimum
Porosity
Point
* for the
sample
to be tested.
(For Dicy
this
is 0.625).

4.5.10

Using
the Rack
and Pinion
Control,
rack
until
the tip of the pointer
is set on the Sample
Height
Curve

4.5.11

without
remove
disturb

4.5.12

Mount
the sample
tube
between
the
rubber
cushioned
supports
Just
to the right
of the brass
post
(J) and
twist
the Clamp
Assembly
Control
(H) to the right
until
the tube
is locked
into place,
making
an airtight
seal
at both
ends
of the tube.

4.5.13

Adjust
the Pressure
Control
(G) until
bubbles
rise
in the
Pressure
Regualtor
Standpipe
at the
rate
of
to three
per second.
The liquid
level
in the
manometer
tube
will
rise
slowly
and
reach
a maximum

the sample
tube
on the
plug
touching
the upper

and Pinion
flat bottom

brass
end

post
(J)
of the

Control
(E),
end touches

with

the

lower
the
the upper

lower
on the
on the

is

the
rack
chart.

moving
the chart,
raise
the rack
and
the
sample
tube,
being
careful
not
to
the
sample.

158

two

height
within
upon
particle

30 seconds
size.

to

several

minutes,

depending

4.5.14

Once
the
liquid
in the manometer
reaches
its maximum
level,
and without
disturbing
the position
of the
Calculator
Chart,
turn
up the rack until
the upper
edge
of the cross
bar coincides
with
the liquid
meniscus
in
the manometer.

4.5.15

Read
the
reading.

4.5.16

Repeat
three
report

4.5.17

In order
to determine
the Optimum
Porosity
Point
for
a given
sample,
perform
steps
4.5.9
- 4.5.15
and
repeat,
each
time
moving
the Calculator
Chart
to the
left
0.05
Porosity
Units,
beginning
with
0.80.
Discontinue
the analysis
when
the chart
runs
off
scale
at 0.40
or when
the sample
is packed
as tight
as
possible.

4.5.18

Plot
all readings
on a sheet
of graph
paper
and
connect
the points.
The mid-point
of the plateau
the curve
is the optimum
porosity
point.

particle

size

off

the

chart

and

record

steps
4.5.2
- 4.5.15
two or more
times
(3) reproducible
readings
are obtained,
the average
particle
size value.

157

the

until
and

of

M-F-3
i.
i.i

2.

Percent

Inorganic

Reinforcement

This
method
is used
to determine
the
inorganic
filler
used
as reinforcement

a Resin

percentage
of
in a resin.

EQUIPMENT
apparatus

Analytical
milligram
Centrifuge
suitable
centrifuge

2.4

Drying
oven
maintaining

consist

of
of

the

following:

weighing

to

the

(International
Model
V-2)
equipped
head,
trunions
and shields
to handle
tubes.
Capable
of 3,000
RPM.

Centrifuge
Aluminum
high.

shall

balance
capable
(0.001
gm.).

2.3

the_mostat!cally
135 _ + 1.0_C.
tubes

50

weighing

ml.

dish

controlled

and

nearest

with
50 ml.

capable

of

capacity.
approximately

57

mm

dia.

Ii

mm.

SAMPLES

3.1

Resin
solid
samples.

3.2

Filler
samples
of resin
taken
solids
sample.

3.3

It is important
that
samples
be thoroughly
stirred
before
and filler
samples
to prevent
material.

4.

In

SCOPE

The

3.

Filler

samples

shall
from

shall

consist

consist
the same

of

of three
container

three

2.8-3.2

gm.

7-10
gm. samples
as the resin

be at room
temperature
and
weighing
out
resin
solids
settling
of the
filler

PROCEDURE

4.1

Determine
the resin
solids
of the
sample
by weighing
three
2.8-3.2
gm. samples
of thoroughly
stirred
resin
into
three
separate
tared
aluminum
dishes.
Weigh
each
sample
to the nearest
milligram
and designate
this
weight
as W I.

4.2

Place
the
samples
the_mostat_cally
135v ! I'0_C
for

in the aluminum
dishes
in the
controlled
drying
oven
which
is
a period
of 3 hours
+ 5 min.

158

at

4.3

After
the
samples
have
been
in the oven
for three
hours,
remove
them
from
the oven
and place
them
in a
desiccator
to cool
before
weighing.
After
the samples
have
cooled,
weigh
the samples
and designate
the weight
as w 3 .
FILLER

CONTENT

5.1

Determine
the filler
content
of the
resin
by weighing
three
7-10
gm. samples
of thoroughly
stirred
resin
into
three
separately
tared
50 ml.
centrifuge
tubes.
Weigh
the samples
to the nearest
milligram.
Designate
this
weight
as W 3.

5.2

Dilute
the
resin
in the centrifuge
tubes
with
35 ml.
of
acetone.
Stir
the contents
of the centrifuge
tube
with
a glass
stirring
rod and wash
the
rod clean
of all
resin
with
a minimum
of acetone
from
a wash
bottle.
Place
the samples
in the centrifuge
and counterbalance
with
identical
centrifuge
tubes
filled
with
acetone
to
the same
level
as the
resin
samples.
(It is important
to
use
the same
solvent
as in the samples
due
to weight
loss
of the
acetone
by evaporation
in the centrifuge.)

5.3

6.1

Centrifuge
the samples
at 3,000
RPH
for 20 minutes.
Remove
the samples.
Pour
off the supernatant
liquid
making
certain
no filler
is removed.
Fill
the
sample
tubes
with
35 ml.
of acetone
and stir
with
a glass
stirring
rod.
Wash
the
stirring
rod clean
with
a minimum
amount
of acetone
from
a wash
bottle
Return
the
samples
to the centrifuge
and spin
at 3,000
RPM
for 20
min.
a second
time.
Pour
off
the supernatant
liquid
and
repeat
the procedure
a third
time.
After
the third
spinning,
pour
off the supernatant
liquid
and wash
down
the outside
of the centrifuge
tubes
to remove
any resin
which
may
have
spilled
over
the side
of th_ tubes.
Place
the tubes
in the drying
oven
at 135 + 1.0_C.
for three
hours.
Remove
the tubes
at the end oT this
period
and
place
them
in a desiccator
to cool.
When
the specimens
have
cooled,
re'weigh
to the nearest
milligram.
Designate
the weight
as W 4.
CALCULATIONS
Calculate

the

W2/W 1
Average

resin

= Resin
=

solids
Solids

as

follows:

= A

(Al+A2+A3)/3

= A Avg.

159

6.2

Calculate

the

W4/A

avg.

percent

i00

filler

% filler

as
in

follows:

dry

resin

where:
w I _ Original
weight
of resin,
filler
and
solvent,
gms.
W 2 = dry weight
of resin
and filler,
gms.
W 3 = original
weight
of resin
filler
and
solvent
in centrifuge
tube,
gms.
W 4 = weight
of filler
remaining
in centrifuge
tube,
gms.

160

M-F-4

i.i

Filler

Content

This

method

is

in

2.2

50

2.3

Disposable

2.4

Membrane

2.5

Whatman

4.25

2.6

Whatman

4.7

2.7

Aluminum

2.8

vacuum

2.9

Air

for
resin

ml.

balance,
tri-pour

the

Systems

determination

of

filler

systems.

sensitivity

0.0001

gm.

beakers

syringes

(3cc.)

filtration

funnel

cm.
cm.

GF/F

filters

EPM

weighing

2000

filters

pans

system
circulating

2.10

Desiccator

2.11

Stirring

2.12

Teflon

Resin

EQUIPMENT
Analytical

3.1

used

filled

2.1

3.

Filled

SCOPE

content

in

oven

rod

with

gasket

47

163

rubber

3C.

policeman

mm.

SAMPLING
It
is
important
that
samples
obtained
from
resin
mixes
are
thoroughly
mixed
Lab
sub-samples
also
must
be
thoroughly
mixed
and
at
room
temperature
prior
to use.
These
precautions
must
be
taken
to prevent
settling
of
the
filler
material.
This
analysis
is to
be
performed
in
triplicate
Mix
samples
with
air
driven
stirrer
for
15 minutes
minimum.
PROCEDURE

4.1

Determine

4.2

Precondition
several
pairs
2000
on
the
bottom
and
one
filtering
approximately
25
pair
of
filters
Place
the
pan
and
dry
at
{63 + 3C.
Preconditioned
filters
are

the

total

solids

content

of

the

material.

of
filters
(one
Whatman
EPM
whatman
GF/F
on
the
top)
by
ml.
of
acetone
through
the
filters
in an
aluminum
weigh
for
20 minutes
or until
dry.
to be
stored
in a desiccator

161

4.3

Weigh
a preconditioned
pair
of filters
and pan
(from
4.2)
to the nearest
0.0001
gram
and place
the pair
of filters,
with
the smaller
filter
on top,
in the membrane
filtration
apparatus
(W2).
A teflon
gasket
is to be
placed
on top of the stainless
steel
screen
prior
to
placing
the filters
in the
apparatus.

4.4

Transfer
using
a
nearest

4.5

Add
35-45
thoroughly.
filtering
rinses
to

46

Filter
the contents
of the filtering
funnel
through
the
pair
of filters.
Stir
the solution
frequently
to avoid
settling
of the
filler
onto
the shoulder
of the
filtering
funnel.
Rinse
the
sides
of the filtering
funnel
with
acetone
to insure
that
all the filler
is
entrapped
in the filters.

4.7

Remove
the
filters
from the
filtering
funnel
and place
back
into
the original
weighing
pan
(the top filter
should
be placed
into
the pan
first
and covered
by the
larger,
bottom
filter).
Transfer
any filler
remaining
on the
bottom
rim of the
filtering
funnel
to the
weighing
pan with
a small
metal
spatula.
Close
loosely
around
the edges
and dry.
Cool
to room
temperature
in desiccator
and reweigh
to the nearest
0.0001
gm.
(w3).

2-3 grams
of resin
to a 50 ml.
tri-pour
disposable
syringe.
Record
this
weight
0.0001
gram
and designate
as W I.

beaker
to the

ml. of acetone
to the 50 ml. beaker
and
Transfer
the contents
to the assembled
funnel
(4.3).
Repeat
twice,
adding
all
the filtering
funnel.

stir

CALCULATIONS
W 1 x Avg.

_4 x
W5

I00

% Total
i00
= %

Solids

= W5

Filler

where:
W 1 = Original
weight
of resin,
filler,
solvent,
gm.
W 4 = Dry
filler
weight
(W 3 - W2),
gm.
W 5 = Total
solids
weight
of initial
sample,

162

gm.

M-F-5

i.i

Particle
Analyzer

Size

Horiba

This
particle
alternative

EQUIPMENT

to

should

AND

Horiba
and

size
the

Automatic

be

used

is
in
method.

in

no

way
The

conjunction

an
manual

with

this

MATERIALS

CAPA-500

Centrifugal

Operators

Automatic

Particle

Analyzer

Manual.

Cuvettes,
(H)
mm.

2.3

Glass

2.4

Pipettes,

2.5

Pasteur

Pipettes

2.6

Pipette

Bulb

2.7

Ultrasound

2.8

Beakers,

2.9

Spatula

2.10

Analytical

2.11

Kimwipes

2.12

Ethylene

2.13

Glass

Microspheres,

2.14

Glass

Microspheres,

34.8

2.15

Glass

Microspheres,

110.6

2.16

Acetone,

2.17

Vacuum
PREPARATION

method
for
determining
liquids
using
the
Horiba
Partical
Analyzer.

method
manual

2.2

3.

Centrifugal

This
procedure
describes
the
particle
size
of powders
and
CAPA-500
Centrifugal
Automatic

method
method.

2.1

the

SCOPE

Note:

by

pyrex

Vials,

with

25

ml.

teflon

with

disposable,

lids,

14

(W)

caps

i0

ml.

Bath
500

ml.

Balance,

Glycol,

99%+

0.0001

gms.

purity
-

um.
um.
um.

industrial

OF

STANDARDS

AND

163

SOLUTIONS

sensitivity

14

(D)

45

3.1

Standards

3.1.1

Depending
on the particle
three
glass
microspheres

3.1.i.i

1 -

5 um.

3.1.1.2

34.8

um.

3.1.1.3

110.6

3.1.2

3.2

size
range
desired,
standards
available:

there

are

um.

Weigh
i0.0
mg. of standard
into
a 25 ml.
glass
vial.
Add
20 ml.
of ethylene
glycol.
Mix well
by shaking,
and place
vial
in ultrasound
bath
for thirty
minutes.
Samples

3.2.1

Depending
on the samples
to be run,
each
method
for
sample
preparation
will
be different,
namely
the
solvent
used
and the concentration
of the sample
desired;
therefore,
various
addendums
have
been
added
at the end of the method
to take
care
of this
situation.

3.2.2

For carbon
black
Addendum
i.

3.2.3

For

4.
4.1

E-03

and

E-24

powders

and

finishes,

resins,

please

please

refer

refer

to

to

Addendum

PROCEDURE
Blank

4.1.1

The blank
standards

must
be run
or samples.

4.1.2

Use the
blank;

4.1.3

Fill
both
cuvettes
with
solvent.
The
liquid
level
in
the cuvette
should
be between
the two
engraved
lines.
Cap the cuvette,
and make
sure
there
are no air
bubbles.

4.1.4

Program
analyzer:

same
e.g.

the

solvent
ethylene

following

4.1.4.1

Solvent

viscosity

4.1.4.2

Solvent

density

4.1.4.3

Sample

4.1.4.4

Diameter

first,

before

used
for
glycol.

parameters

density
(max.)
164

the

running

samples

into

the

any

to

run

Horiba

the

2.

4.1.4.5

Diameter

(min.)

4.1.4.6

Diameter

(div.)

4.1.4.7

Centrifugal/Sedimentation

4.1.4.8

Speed

if

Mode

centrifugal

mode

is

selected

4.1.5

Depending
on the samples
to
particle
size
analysis
will
the parameters
described
in

4.1.6

For carbon
black
Addendum
i.

4.1.7

For

4.1.8

Place
one cuvette
the
cell
holding

4.1.9

Place
the other
the cell
holding

4.1.10

Close
the sample
chamber
and press
on the
control
panel.
Measurement
two
seconds,
and the mean
value
is

4.1.11

Samples

4.2

E-02

and

are

powders

E-24

now

be run,
each
method
for
have
different
values
for
Section
4.1.3.

and

finishes,
in
bar

resin,

please

reference
until
the

cuvette
in
bar until

ready

to

please

refer

to

to

Addendum

cell
holder,
and
cuvette
is fixed.

sample
cell
the cuvette

be

refer

turn

holder,
and
is fixed.

the
"BLANK"
is made
for
stored.

2.

turn

button
thirty-

run.

Standards

4.2.1

Fill
cuvette
with
standard,
as prepared
in section
The liquid
level
in the cell
should
be between
the
engraved
lines.
Cap the cuvette
carefully,
making
no air
bubbles
are introduced.

4.2.2

Place
cuvette
in
holding
bar until

4.2.3

The cuvette
in the
reference
only
ethylene
glycol.
Secure
the cell
holding
bar.

4.2.4

The Horiba
following

sample
cell
the cuvette

Analyzer
manner:

should

is

4.2.4.1

Solvent

viscosity

4.2.4.2

Solvent

density

4.2.4.3

Sample

4.2.4.4

Diameter

density
(max.)

is
is
is

cell
the

be

19.90

i.ii
2.30

holder,
and
is fixed.

gm./cc
gm./cc

i0.0
165

microns

the

cell

holder
should
contain
reference
cell
with

programmed

cps

turn

3.1.
two
sure

in

the

4.2.4.5

Diameter

(min.)

is

0.01

4.2.4.6

Diameter

(div.)

is

1.0

4.2.4.7

Speed

4.2.4.8

Sample

4.2.4.9

Running

is

2,000

The
above
standard,
4.2.5

Close
running
second.

the

4.2.6

Press
After

the
run

4.2.7

Make
sure
standard,

4.2.8

Each

4.3

is

"START"
stops,
that
see

must

be

run

1
for

second
glass

microspheres

Press
the
"SET"
in this
case,

Sample
start

the
blank
is
Section
4.1.

standard

mg/ml

minutes,

button.
data
will

is now
printing

run

before

button.
12 minutes,

The
1

running.
out.
running

the

twice.

Samples

4.3.2

Place
cell

4.3.3

The

cuvette
by
turning
cuvette

only
Secure

4.3.4.2

12

0.5

sample
chamber.
time
should
appear,

Fill
cuvette
with
should
be
between
cuvette
carefully
introduced.

4.3.4.1

is

parameters
are
1 - 5 minutes.

4.3.1

4.3.4

microns

rpm

concentration
time

microns

The

in

in

sample.
The
liquid
in
the
cell
the
two
engraved
lines.
Cap
the
making
sure
no
air
bubbles
are

sample
the
cell

the

cell
holder,
holder
bar.

reference

cell

solvent,
the
same
solvent
the
cell
by
turning
the
Horiba

Analyzer

should

black

powders

For
carbon
Addendum

i.

For

and

E-02

4.3.5

Close
running

the

4.3.6

Press
After

the
run

E-24

finishes,

sample
chamber.
time
should
appear.
"START"
stops,

button.
data
will

166

be

and

holder

used
cell

should

contain

as

resins,

refer

the

for
the
holding

programmed

and

secure

sample.
bar.
follows:

refer

to

to

Addendum

Press

the

"SET"

Sample
start

is now
printing

button.

running.
out.

2.
The

4.3.7

Make

sure

that

samples.
4.3.8

Each

See

sample

the

blank

Section

must

be

is

run

before

running

any

4.1.
run

twice.

RESULTS

5.1

It is crucial
that
the absorbance,
shown
in the
absorbance
vs.
time
graph,
does
not exceed
1.0.

5.1

The average
cumulative

5.1

The
average
diameter
sample
to sample.

5.1

The
average
diameter
for the glass
microspheres
standard,
1-5 microns,
should
be about
4.3 + 0.i microns.
The
value
should
be entered
in the particle
size
calibration
log
for future
reference.

diameter,
distribution.

D(avg.),

must

not

167

is

based

vary

by

on

more

50%

than

of

the

10%

from

PARTICLE

SIZE

ADDENDUM

CARBON

SAMPLE

BLACK

POWDERS

AND

RESINS

Take
2
ethylene
mg./ml.
HORIBA

PREPARATION

PREPARATION

Weigh
2 mg.
of
sample
in a 25
ethylene
glycol;
concentration
in ultrasound
bath
for
thirty
1.2

SAMPLE

ml.

ml.

vial.
is 0.i
minutes.

20

ml.
Mix

of
well

of
0.i
mg./ml,
solution
and
add
20 ml.
of
glycol
in a 25 ml.
vial;
concentration
is
0.01
Mix
well
in ultrasound
bath
for
thirty
minutes.

ANALYZER

DATA

2.1

Solvent

is

2.2

Solvent

viscosity

2.3

Solvent

density

2.4

Sample

ethylene

glycol

2.5

Diameter

(max.)

is

5.0

2.6

Diameter

(min.)

is

0.01

microns

2.7

Diameter

(div.)

is

0.50

microns

2.8

Speed

2.9

Sample

2.10

Running

is
is

density

is

Add
mg./ml.

is

4,000

i.Ii
1.90

cps.

gm./cc.
gm./cc.
microns

rpm

concentration
time

19.90

is

is
ii

0.01

minutes,

mg./ml.
31

168

seconds

PARTICLE

SIZE

ADDENDUM
E-03
1.

SAMPLE

AND

E-24

FINISHES

PREPARATION

i.i

Weigh
120 mg. of sample
in a 25 ml.
vial
if the percent
solids
is 20%.
Add
20 ml.
of deionized
water;
concentration
is 6.0 mg./ml.
Mix well
in ultrasound
bath
for thirty
minutes.

1.2

Weigh
60 mg. of sample
in a 25 ml.
vial
if the percent
solids
is 40%.
Add
20 ml.
of deionized
water;
concentration
is 3.0 mg./ml.
Mix well
in ultrasound
batch
for thirty
minutes

2.

HORIBA

ANALYZER

DATA

2.1

Solvent

is

deionized

2.2

Solvent

viscosity

2.3

Solvent

density

2.4

Sample

2.5

Diameter

(max.)

2.6

Diameter

2.7

Diameter

2.8

Speed

2.9

Sample
mg./ml.

2.10

Running

density

is

water
is

is
is

0.94

0.99

cps.
gm./cc.

1.25

gm./cc.

is

2.0

microns

(min.)

is

0.01

microns

(div.)

is

0.25

microns

5,000

rpm

concentration
(40% solids)
time

is

is

6 minutes,

6.0

mg./ml.

34

169

seconds

(20%

solids),

or

3.0

M-F-6
i

Carbon

and

Moisture

Content

of

Carbon

Filler

SCOPE

i.i

Assay

Carbon
assay
and moisture
content.
moisture
content
determination
shall
with
the
following:

The
be

carbon
assay
in accordance

and

PROCEDURE

2.1

Dry
a 30_ milligram
specimen
225 + 5 _F.
before
combustion
(to The
nearest
0.i percent)
sample.

2.2

Conduct
the carbon
assay
in
or by the
alternative
method

2.3

Calculate
following:
Percent

the

moisture

moisture

to a constant
and base
the
on the weight

accordance
specified.

content

= W

- W]
W

in

weight
percent
of the

with

ASTM

accordance

at
carbon
dried

with

3176

the

(100)

where:
W =
wI =
Report

specimen
specimen

the

results

weight
weight

prior
after

to

nearest

the

to drying
, gram
drying,
gm.
0.i0

(gm.)

percent.

Alternative
carbon
assay
determination.
The
alternative
carbon
assay
determination
shall
be accomplished
using
LECO
CHN-600
Carbon,
Hydrogen,
Nitrogen
Analyzer,
or
equivalent,
have
an operators
manual
available,
as
follows:
2.5.1

Insert
the
capsule.

2.5.2

Crimp
escape

2.5.3

Place
the capsule,
balance
to determine
weight
stabilizes,

2.5.4

Place

2.5.5

Push

2.5.6

when
the
displayed

2.5.7

Report
percent

the
of

dried

top
the

capsule
the

sample

of the
sample

in

analyzer

into

the

capsule
material.

with

of

the
key

analyzer
to

sample

begin

carbon

test

170

a tared

forceps

with
sample
back
on
net
sample
weight.
push
the ENTER
key.

analysis
is complete,
and a print-out
will

percent

top

to

tin

prevent

the LB-20
When
the

chamber.

analysis.
the results
occur.

results

to

the

will

nearest

be

0.10

M-F-7
i.
i.i

2.
2.1

Particle

Size

Test

for

Fillers

by

SEM

SAMPLING
Representative
samples
are to be obtained
by selecting
a
number
of containers
and sampling
each
container
with
a
thief.
Mixing
and selecting
the appropriate
size
sample
and storing
in air tight
containers
until
ready
for
analysis.
TEST

METHODS
Scanning
Electron
Microscope
(SEM)
Method
was
applied
to a visual
sampling
and 20,000x
magnification.
The
minimum
and maximum
particle
size
is determined,
and
a
representative
group
of particles
spanning
the
full
range
is selected.
From
this
selected
group
each
particle
is measured
and an arithmetic
average
size
is
calculated.
NOTE:

The two methods,

SEM and the
not give
equivalent
results,
used
in conjunction
with
the

171

HORIBA
method
do
and hence
should
manual
method.

be

P-P-I
i.
i.i

2.

Volatile

Content

of

Uncured

Prepregs

SCOPE
The volatile
content
of each
material
shall
be determined
following:

sample
of the
in accordance

uncured
with
the

PROCEDURE

2.1

Cut a 16 + 2 square
of 1.5
inches
across

2.2

Weigh

2.3

Place
specimen
in a recirculating
oven
preheated
stabilized
to 325 + i0 F. for i0 + 1 minutes.
should
be placed
to get
adequate
aTr circulation.

2.4

Remove
specimen
room
temperature.

2.5

Remove
nearest

2.6

Calculate

the

specimen

inch
the
to

and

specimen
width
of

the

nearest

place

in

from
the desiccator
0.01
gram
(W2).
percent

0.01

gram

a desiccator

and

volatiles

with
a minimum
width
the prepreg
fabric.

as

weigh

(Wl).

and

the

and
Specimens

cool

specimen

to

to

the

follows:

W1 - W 2
Percent

Volatiles

x i00
W1

where:
W 1 = uncured
weight
of specimen,
W 2 = final
weight
of specimen,
2.7

Report
volatile
percent.

2.8

Limits

Minimum
Maximum

(wt

content

of

specimen

gm.
gm.
to

percent)

Normal
3.5
6.00

Retest

172

Properties
3.5
6.5

the

nearest

0.i

P-P-2

i.i

Resin
Solids,
Material

Filler

and

Cloth

Content

of

Uncured

SCOPE
These
properties
determined
for
following.

of
each

the uncured
material
sample
in accordance

shall
with

be
the

PROCEDURE
Place
0.01
2.2

a 1.5 + 0.2 gram

specimen
gram
(specimen
weight)
in

Calculate
W

specimen

Where:

2.3

devolatilized
wt

Percent
volatiles

specimen

(% volatiles)

volatiles
content.

is

weighed
to the nearest
250 ml. beaker.
weight

(W)

x (specimen
i00

the

value

as

follows:

wt.)

determined

from

the

Add
50 ml.
of N, N dimethylformamide
(DMF)
and bring
to a
boil.
Gently
stir
the boiling
DMF and prepreg
cloth
for
a minimum
of 5 minutes.
Remove
beaker
from
heat
source
and cool
for a minimum
of 5 minutes
while
stirring
gently.

2.4

Decant
and
ml.
beaker.

2.5

Rinse
ensure
fabric

2.6

Finally
traces

2.7

Add

all

2.8

Dry
350
and

a filter
+ i0 OF.
crucible

gm.

(W2).

2.9

transfer

the

liquid

the remaining
fabric
complete
extraction
and add the rinses

Dry
the
i0 OF.,
reweigh

rinse
the
of DMF.
rinses

to

fabric

the

solution

to

a second

with
DMF several
times
to
of resin
and filler
from
to a second
250 ml.
beaker.
with

second

acetone

250

ml.

to

remove

beaker.

fabric
in an oven
for 15 + 1 minutes
at
cool
in a desiccator
to room
temperature
to the nearest
0.01
gm.
(Wl).

Using
an aspirator
or
of the second
250 ml.
crucible
or filtering

2.11

Rinse

the

all

and a crucible
or filtering
crucible
for a minimum
of 30 minutes.
Weigh
or filtering
crucible
to the nearest

2.10

crucible

and

250

at
filter
0.01

325 +
and-

vacuum
pump,
filter
the contents
beaker
through
a filter
and
crucible
into
a vacuum
flask.
filter
173

or

filtering

crucible

several

times

with

acetone

to

remove

all

resin.

2.12

Dry
the crucible
and contents,
at 350 + i0 OF.
for 20
+ 1 minutes,
cool
in a desiccator
to room
temperature
and
reweigh
to the nearest
0.01
gm.
(W3).

2.13

Calculate
the
cloth
content
Resin

solids

Filler

resin
solids
as follows:
content

content

Cloth

content

% = W4/W
%

= WI/W

content,

= W

filler

(W I + W4)
W

content,

(i00)

(i00)
(i00)

Where:
W

= calculated
devolatilized
weight
of prepreg
specimen,
gm.
W 1 = weight
of fabric
after
resin
and
filler
removal,
gm.
W 2 = crucible
and filter
or filtering
crucible
weight,
gm.
w 3 = filler
+ crucible
or filler
+ filtering
crucible
weight,
gm.
W 4 = W3-W2
- filler
weight,
gm.
2.14

Report
content

the
to

resin
solids,
filler
content,
the nearest
0.i0
percent.

2.15

Limits

(wt

percent)

Minimum
Maximum

Dry Resin
Solids
32.0
37.0

174

Carbon
Filler
8.0
16.0

and

cloth

Cloth
47.0
60.0

and

P-P-3
I.
1.2

2.

Resin

Flow

of

Uncured

Material

SCOPE
Resin
flow
for each
sample
be determined
in accordance

of the uncured
material
with
the following.

shall

PROCEDURE

2.1

Using
a 4-inch
by 4-inch
+ 1/8-inch
template,
cut four
squares
across
the width
of the fabric.
All
squares
shall
be bias
cut to eliminate
fiber
loss
in testing.
Stack
the squares
uniformly
on each
other
to make
a
specimen,
where
the width
of the tape
is less
than
4
inches
wide,
cut the tape
in 4-inch
lengths
and place
side
by side
to fabricate
a 4-inch
by 4-inch
specimen
ply.
Stack
four
plies
alternately
placed
90 degrees
to
the previous
ply direction.
Place
each
ply uniformly
on
each
other.

2.2

Weigh
the
and
record

2.3

Place
the specimen
between
release
film.
Preheat
the
press
to 325 + i0 OF.,
position
the specimen
in the
middle
of the-press
plate
and apply
the press
load
of 150
+ i0 psig.
immediately.
Press
loa_
the specimen
for a
minimum
of i0 minutes
at 325 + i0 _F.

2.4

Remove
the
temperature.

2.5

Using
a knife,
original
size
reinforcement

2.6

Reweigh
record

2.7

Calculate
Percent

specimen
as W I.

of

specimen

from

the

to

the

press

nearest

and

cool

scrape
off the
resin
flash
to
of the specimen.
Do not
remove
from the original
dimensions.

the
specimen
as W 2.
the
flow

4 plies

to

percent

the

resin

= W I - Wax
W1

nearest

0.01

flow

follows:

as

gram

100

Where:
w I m uncured
W2 =
2.8

Report

final

resin

weight
weight

flow

to

of
of

the

specimen,

specimen,
nearest

175

gm.
gm.

0.I

percent.

0.01

to

gram

ambient

the
any

and

2.9

Limits

Minimum
Maximum

(wt.

percent)
Normal
i0.0
20.0

Retest
8.0
23.0

176

P-P-4

1.
i.i

2.

Carbon
Cloth,
Phenolic,
and Uncured
Content

Preimpregnated,

Medium

Sodium

SCOPE
This
specification
covers
medium
sodium
carbon
cloth
reinforcement
preimpregnated
with
aldehyde-phenolic
for rocket
motor
nozzle
components.

resin

MATERIAL
The material
shall
be a carbon
fabric
reinforcement
impregnated
with
a carbon
filled
phenolic
resin
and either
slit
into
straight
or bias
tape
for wrapping
or supplied
as broadgoods.
The
cut tape
ends
shall
be joined
by
splicing
and stitching
with
nylon
thread.
Bias
tape
and
straight
tape
cut ends
shall
be Joined
by butt
splicing.
Broadgoods
roll widths
shall
be 36-48
inches
and shall
be
rolled
onto
the paper
core
with
the warp
side
of the
impregnated
fabric
on the outside
face
of the
rolls
selvage
shall
be removed
to provide
two parallel
roll
edges.

2.1

Resin.
The
requ--frements

2.2

Reinforcement.
fabric
conforming

2.3

Resin
with

2.4

Splicing
stitching
STW4-2919.

2.5

Age
of material.
The material
shall
be shipped
months
of manufacturing
data
and shall
be tested
certified
within
60 days
of shipment.

2.6

Process
of manufacture.
material
after
initial
by this
specification
requalification.

3.

STORAGE

resin
system
shall
conform
of MIL-R-9299,
Grade
A.

filler.
a minimum

The
to

reinforcement
STW4-3184.

The
resin
filler
carbon
assay
of

thread.
specified

shall

to

the

be

carbon

shall
be carbon
90 percent.

powder

The splicing
thread
used
for the
in 3.2 shall
be in accordance
with

Any
change
qualification
shall
be cause

within
and

in process
or
testing
as required
to require

LIFE

The material
shall
have
a shelf
life
of 6 months
after
the
date
of manufacture
when
stored
at 50 degrees
Fahrenheit
(F), maximum,
in sealed
plastic
bags
with
a 1-unit
(minimum)
desiccant
bag conforming
to MIL-D-3464.
After
date
of receipt
of the broadgoods,
the maximum
cumulative
out-of-storage
time
shall
be 30 days.
Storage
life
requirements
shall
apply
until
the material
has been
177

completely
component
3.1

tape
shape.

wrapped

onto

a mandrel

to

form

rough

Shelf
life
extension.
The
shelf
life
of broadgoods
and
tape
rolls
may
be extended
for three
additional
6 month
periods
provided
the material,
upon
retest,
conforms
to
the
retest
requirement
for resin
flow,
volatile
content,
and
residual
volatile
content.
The maximum
allowable
cumulative
shelf
life
of broadgoods
and tape
rolls
slit
from
broadgoods
shall
not exceed
24 months
from
the date
of manufacture
of the original
broadgoods
lot.
The
number
of broadgoods
and tape
rolls
to be tested
for
shelf
life
extension
shall
be as follows:
No.
of broadgoods
tape
rolls
in lot

or

No. of broadgoods
tape
rolls
to be

1-3
4-40
41-65
66-100

or
tested

ALL
4
5
6

A lot
of material
shall
be acceptable
if the
average
of
the three
tests
for each
selected
roll meets
the
shelf
life
extension
requirements.
Failure
of any of the
selected
rolls
to meet
these
requirements
shall
require
all
rolls
within
the lot to be tested
for only
those
material
properties
which
failed
to meet
specification
requirements.
3.2

Conditioning
for shelf
life
extension
retest.
Material
which
fails
to meet
the maximum
allowable
Volatile
and
resin
flow
requirements
may
be conditioned
to extend
the
shelf
life
by subjecting
all the
rolls
in the
lot which
failed
to meet
the requirements
of 3.1 to the
following:

3.2.1

Place
material,
chamber
supported
damage.

3.2.2

Expose
material
to vacuum
of
Mercury
(Hg) and a temperature
for a period
of 7 to 9 days.

3.2.3

broadgoods
through

and/or
core(s)

less
of

slit
tape,
to prevent

in vacuum
material

than
1 inch
of
60 to 90 degrees

After
completion
of drying
process,
randomly
select
rolls
to be tested
using
the
following
sampling
plan.
Obtain
samples
from
outside
and inside
each
sampled
roll
and
retest
for volatile
content
and resin
flow.

178

No. of broadgoods
rolls
or tape
rolls
to be
selected
for retest
sampling

No. of broadgoods
rolls
or tape
rolls
remaining
in the original
lot

1 - 2
3 - 40
41 - 65
66 - i00
Failure
of
requirements
tested.

3.2.4

All
3
4
5

any of
shall

the selected
require
all

rolls
to meet
the
conditioned
rolls

to

be

3.3

Out-of-Storage
time
extension.
The
30-day
out-of-storage
time
may
be extended
for one
additional
30-day
period
provided
that
each
roll has met the
shelf
life
extension
requirements
and the average
of three
tests
has met the
retest
requirements.

3.4

Preparation
and storage
of samples
selected
for retest.
Each
lot of broadgoods
or tape
roll
samples
shall
be
promptly
put
into an individual
plastic
bag,
sealed,
properly
labeled,
and stored
at 50 degrees
F., maximum.
Prior
to testing
and removal
from
the plastic
bag,
the
samples
shall
be conditioned
at 60 to 80 degrees
F. for
hours,
minimum.
The samples
shall
be tested
within
72
hours
after
removal
from the broadgoods
or tape
rolls

4.

CLASSIFICATION

OF

INSPECTIONS

The
inspection
requirements
classified
as qualification
conformance
tests
4.1

Uncured

4.1.i
4

examination

Volatile
Dry

content

resin

Carbon

solids

filler

4.1.5

Cloth

Content

4.1.6

Resin

flow

4.1.7

Sodium

4.2
4.2.1

Cured

herein
and

are
quality

Material

Visual
2

specified
inspections

......................
ooiIoeeoleiieowoDueo.."

P-P-26

........................

F-14

Content

4eguoouloeloeo,eeJ,

...........................

..............................

Content

M-C-31

..........................

M-F-55
P-P-2
P-P-3
M-C-24

Material

Density

.................................
179

F-I

4.2.2

Residual

4.2.3

Resin

4.2.4

Compressive

4.2.5

Interlaminar

4.2.6

Thermal

4.2.7

Coefficient

4.2.8

Flexural

4.2.9

Tensile

5.

volatiles
Content

......................

...........................
Strength
Shear

.l.,,,..o.

strength
strength

expansion

F-4

F-6

....lieem.JeIee.o.,.

thermal

F-14

F-5

....o..........o.-..."

Conductivity
of

DSl..Qe...

F-16

........

F-7

.......................

F-8

........................

F-9

SAMPLING
Each
lot of
sampled
for

5.1

5.2

carbon
cloth
aldehyde-phenolic
inspection
as follows:

shall

be

Lot.
A manufacturing
lot of preimpregnated
material
s--_all consist
of material
which
is impregnated
in one
continuous
production
run, using
one batch
of the
impregnator's
resin
and additives
mixed
in one vessel
one time.
Lot
not

size.
consist

Lot

acceptance

lot
of
of more
test

carbon
cloth
aldehyde-phenolic
than
8000
pounds.

at

shall

samples.

Sampling
for uncured
material
properties.
Each
sample
shall
be of sufficient
size
to perform
all of the
uncured
material
inspections
and tests.
Each
sample
shall
be marked
with
the roll
number,
lot number,
and
the
location
in the
roll
from which
the
sample
was
taken.
Each
broadgoods
roll
in the lot shall
be
sampled
at the beginning
of the
roll,
and
at the end of
the roll.
5.3.2

Sampling
for cured
material
properties.
A sample
of
sufficient
Size
to perform
all the
cured
material
inspections
and test
specified
herein
shall
be taken
from
the outside
end of each
broadgoods
roll
selected
at random
from
each
lot.
The number
of rolls
to be
selected
shall
be determined
as follows:

180

Number

1
3
41
66

of

rolls

to
to
to
to

2
40
65
ii0

in

lot

Number
of rolls
to be
selected
for sampling
All
3
4
5

Failure
of a roll
sample
to conform
to the
requirements
of this
specification
shall
be cause
to withdraw
that
roll
and shall
require
that
all other
rolls
in that
lot
be tested
for only
those
material
properties
which
failed
to meet
specification
requirements.
5.3.3

Sampling
for sodium
content.
Samples
of sufficient
size
to perform
sodium
test
shall
be removed
from
the
exposed
end of each
broadgoods
roll
selected
at random
from
each
lot.
Failure
of a roll
to conform
to the
requirements
of this
specification
shall
be cause
to
withdraw
that
roll
and shall
require
all other
rolls
in
that
lot to be tested
for sodium.
The number
of rolls
to be selected
shall
be as follows:
Number

of

1
3
41
66
5.4

rolls

to
to
to
to

in

lot

No. of rolls
selected
for

2
40
65
ii0

to be
sampling

all
3
4
5

Test
requirements.
Three
tests
shall
be performed
for
each
of the material
properties
specified
herein
on the
samples
taken
from
each
broadgoods
roll
sampled.
All
individual
test
results
shall
be reported.
The average
values
of the test
results
and at least
two of the three
individual
test
values
shall
be used
to determine
conformance
to the
requirements
of this
specification.
Where
applicable,
testing
of individual
specimens
for
more
than
one property
shall
be permissible.

5.4.1

Test
conditions.
Unless
otherwise
specified,
all tests
shall
be performed
under
ambient
conditions.
Where
the
temperature
or time
is critical
to the results
of the
test,
these
controls
shall
be specified
in the
applicable
test
procedure.

5.4.2

Supplier
retest.
When
the average
lot
fails
to conform
and the cause

test
value
of
of the
failure

be attributed
to improper
preparation
of the
or testing
machine
anomaly,
a new test
shall
conducted
on a sample
from
the same
broadgoods
from
which
the failed
specimens
were
removed.
181

any
can

specimen
be
roll

6.1

DEFINITIONS
.
A method
of stabilizing
yde-phenolic
polymer
in a
cloth
by temperature
cycling.

and
solid

6.2

Coefficient
of thermal
expansion.
thermal
expansion
is the slope
of
the
75 degrees
F. and 400 degrees
the linear
expansion
curve.

6.3

Tape
cloth

6.4

Sample.
broadgoods

6.5

Specimen.
used
for

A specimen
testing.

6.6

Broadgoods.
cloth
fabric

roll.
tape

A tape
roll
is
from
a broadgoods

Broadgoods
impregnated

is

width

section

a cut-out

material
is
with
resin.

182

the
the

carbon

The coefficient
of
the secant
llne
between
F. line
intersection
of

a narrow
roll.

sample
is a cut-out
roll
or tape
roll.

retaining
state
on

of

of

the

section

of

a wide

impregnated

roll

impregnated

the

of

sample

carbon

P-P-5
i.

Moleweight

of

Resins

and

prepregs

by

Chromatography

SCOPE

1.1

This
procedure
describes
methods
for
conducting
Chromatography
and
gel
permeation
chromatography
aldehyde-phenolic
resins.
It determines
the
of
the
constituents.
EQUIPMENT

AND

MATERIALS

2.1

HPLC
Spectra-Physics
autosampler,
with

2.2

Styragel
(USE
NO

2.3

Syringe,

2.4

Gas

2.5

Needles

2.6

Scissors

2.7

Centrifuge

2.8

Centrifuge

2.9

Graduated

I0

syringe,

cc.

tubes,

50

ml.

Balance

2.11

Beaker

2.12

Millex-SR

2.13

Membrane

2.14

2.15

Helium

2.16

Nitrogen

gas

PREPARATION

OF

3.
3.1

Resin

columns,

cylinder,

with
UV
detector
and
operators
manuals.
2

i00

A,

500

cc.

2.10

&

SP8000
appropriate

chromatography
WATER)

tight

liquid
of
moleweight

i0

filter
TFE

disposable

ml.

units,

0.5

(Tetrafluroethane)

tetrahydrofuran,
(zero

UV

filter
grade,

grade)

gas

SAMPLE

SOLUTION

paper,

0.45

THF

Samples

3.1.1

Weigh
out
(labeled)

3.1.2

Add

I0

ml.

0.25

100%

0.02

THF

gm.

into

of

the

183

resin

vial

into

glass

vial

3.2

Resin

Mixes

3.2.1

Weigh
tube

3.2.2

Add

3.2.3

Agitate

3.2.4

Centrifuge

3.3

out

25.0

3.3.2

Weigh
tube

3.3.3

Add

3.3.4

Agitate

3.3.5

Centrifuge

gm.

100%

15-50
for

THF

of

sample

into

into

the

centrifuge

centrifuge

tube

minutes

2-5

25

minutes

at

appropriate

speed

ml.

approximate
!

100%

0.5

gm.

THF

into

15-50
for

1/2"
of

sample

the

1/2"
into

squares
a

centrifuge

centrifuge

tube

minutes

2-5

minutes

(Speed-7)

Preparation

3.4.2

Degas

3.4.3

Decrease

solvent
(1-2
liters)
(Tetrafluoroethene)
with

INSTRUMENT

D:

6.0

for

Solvent

Date

into

out

Filter
filter

He
the

1/4
flow

to

1/2

rate

by

hour

before

using

(high

0.45

flow)

running

PROGRAMMING

Assignment
00:00:0_

month
day
D - Display
4.2

0.02

of

sample

3.4.1

4.1

Prepregs
Cut

4.

ml.
for

3.3.1

3.4

3.0

Report

File

R:I
REPORT
RENAME:
SAMPLE:
SAMPLE
SAMPLE

report
FILE

OPERATOR
DETECTOR
DETECTOR
COLUMN
MOBILE

00:00:00
year

VOLUME:
CONC.:

hour

min.

sec.

Assignment
file
1

i0
L
20 MG-ML

NAME:
(your
name)
i: UV.
254NM
0.i
2:
;
TYPE;
SIZE:
2xl00A,
PHASE:
Isocratic

AUFS
2X500A,

184

-STYRAGEL

um.

TFE

A:
;
B:
;
C: THF
END
OF
4.3

DIALOG

Parameter
S:I

File

parameter

PARAMETER
RENAME:

file
SET:

2.
3.
4.
5.
6.
7.
8.
9.
i0.
Ii.
12.
13.
14.
15.
16.
17.

LINK:
;
INITIAL
DELAY:
1
RUN
TIME:
30
NO.
OF
CYCLES:
6
FLOW
RATE:
2.00
FLOW
MODE:
QI
TEMPERATURE:
35
MOBILE
PHASE
FILE:
1
REPORT
FILE:
1
GRAPH
FILE:
1
DATA
SYSTEM
FILES:
1
CHAN
i:i
CHAN
2:
;
FULL
TIME:
1
FLUSH
TIME:
1
REPETITIONS
PER
VIAL:
TIMED
EVENTS:
XX

END

OF

4.4

Assignment

Graph
G

DIALOG
File

Assignment

graph

file

GII
GIE5
GII5
GVO.5
XX
EXIT
4.5

GRAPH

Mobile
M

MOBILE
WHICH

EDIT

Phase
2

mobile
PHASE
SOLVENTS?

File

Assignment

phase
FILE

file

2
2

185

END

OF

DIALOG

MI2
M;I
MOBILE

PHASE

WHICH
END

FILE

SOLVENTS?
OF

1
C

DIALOG

MII
4.6

Data

File

Manipulation

FII

Data

system

nm

gpc-QC

CH
OD
IX
RN
NR
PW
PT
MA
FD
VE
FILE

001
002
001
001
001
015
0150
5000

RN
FS
PP
NM
CH

001
000
004
GPC-QC
001

(file

function

NR
MS
TI

001
0
000

PW
MA
RO

015
5000
000

PT
IM

0105
00

OD

002

IX

001

SN

0OO

file

001
0
1

IR
NP

0
0

DC
NT

0
0

NZ
AA

0
0

FX
XD

XX
METHOD
4.7

center)

001

FF
APO
FD
VE
FILE
AR
TP

file

Review

File

Values

S-I

186

0
0

EC
HD

0
0

PARAMETER

SET:

INITIAL
DELAY:
1 RUN TIME:
30 NO.
OF CYCLES:
6
FLOW
RATE:
2.00
FLOW
MODE:
Q1
TEMPERATURE:
35
MOBILE
PHASE
FILE:
1 REPORT
FILE:
1 GRAPH
FILE:
1
CHAN
i:i
FILL
TIME:
1
FLUSH
TIME:
1
REPETITIONS
PER VIAL:

R-I
-VOL:
i0 UL
CONC:
20 mG-ML
(your
name)
FLOW
RATE :
2.0
PRESSURE:
0000
COLUMN:
2xl00A,
2X500A,
--STYRAGEL
CHAN
i:
U.V.
254NM
0.1
A-FS
MOBILE
PHASE
FILE
1
i00.0%
C
G-I
GRAPH
FILE:
1
Channel
1:
Plot Var. :
DET.
1
Chart
Polar:
L ATTN.:
5
Zero:
0%
Inten.:
Channel
2:
Inoperative
M-I
Mobile
Phase
File:
1
i00.0%
C
5.
5.1

Spd.:
5

0.5

PROCEDURE
HPLC:

Start-up:

5.1.1

Turn

5.1.2

Adjust
psi.

5.1.3

Turn
on
position_

5.1.4

Turn
on the Spectrophotometric
is ".4 m amp"
Set range
at

5.2

NO:

on

He
the

Automatic

and
He

N2
pressure

both
switches,
Set wavelength

to

i0

psi.

Wavelength
at 254

0.i

and

N 2 pressure

Drive
nm.

at

Detector,
AUFf

"on"

make

Operation

5.2.1

Be

sure

5.2.2

Keep

He

5.2.3

Type

AT1
DID
FMI
MII
SBI

both
purge,

detector
the

and
solvent

187

auto
with

sampler
low

are

flow

to

on

rate

sure

it

75

5.2.4

Use the
inner
knob
on the detector
range
selector
to
adjust
the
read
out to -1200
(detector
signal)
or type
GB and
adjust
the baseline
1 inch
to the
left margin,
then
type
GX to stop
plotting.

5.2.5

Fill
one gas
tight
syringe
other
one with
THF;
attach
SR filler
unit.

5.2.6

Place
the
injector
handle
in
type
SO to open
the
injector

5.2.7

Inject
1 cc.
of THF to
inject
1 cc.
of sample
the sample
solenoid.

5.2.8

Wash
the
sample.

5.2.9

After
LC,
handle
in
operation.

5.2.10

Check

syringe

the

with

with
each

solution
to one

flush
the
injector
solution
and type

THF

by

and the
Miller-

the
"LOAD"
position
sample
solenoid.

twice;

inject
automatically,
the
"LOAD"
position

condition

sample
syringe

fill

loop,
SK to

it

replace
and
repeat

with

then
close

the

Calibration

(before

typing:

running

5.3.1

Run

5.3.2

Run molecular
weight
weight
vs.
retention
Mole

THF

Weight

blank

in

order

sample
to

plot

standards
time
on

Standards:

M.W.
Compound
93 Toluene
570 Polystyrene
955 "
3600
"
5.4

Termination

5.4.1

Type

EX

to

end

5.4.2

Type

SX

to

stop

5.4.3

Shut

down

all

run
parameter

gas

set

flows
188

solutions)
the

and
graph

baseline

plot
paper

next

the injector
the
injecting

E- elapsed
time
since
injection
T- present
oven
temperature
P- pressure
C- current
% C at ternary
valve
DIDdetector
signal
F- flow
rate
5.3

and

molecular

P-P-6
i.
1.1

2.

Infra-red

of

Resins

and

Prepregs

SCOPE
This
method
spectrum
of

is used
for determination
liquid
and solid
resins

or

of infrared
prepreg.

APPARATUS

2.1

Beckman
operators

2.2

Sodium

2.3

Solvent:
chloride.

Spectrum

4250,
Beckman
manual.
chloride

Acculab

8 or

equivalent,

and

disk.

Spectrograde

acetone,

THF

or

methylene

PROCEDURE

3.1

Place
a small
amount
of material
to be tested
in a 50-ml.
beaker.
Add
about
15 ml. of spectroquality
acetone
and
stir
with
a glass
stirring
rod to dissolve.
If the
material
doesn't
dissolve
in acetone,
spectroquality
THF
or methylene
chloride
may
be used.

3.2

Place
several
drops
of the
chloride
crystal
and allow

3.3

Zero

3.4

the

I.R>

beam

as

the

solution
on the sodium
to dry
at room
temperature.
instrument

manual

describes.

Makela
quick
scan
of the region
from
2000
cm -i to i000
cm
.
When
the transmittance
is between
15 and 25
percent
at most
intense
peak
the right
concentration
is
on the crystal.
Twenty
percent
is the ideal
transmittance.

3.5

Start
the scan
at
the
infrared
from

3.6

Do

any

necessary

90%
2.5

transmittance.
to 16 microns.

calculations.

189

Scan

the

sample

in

Resin

P-P-7
i.

Content

of

Prepregs

by

Soxhlet

Extraction

SCOPE
This
method
describes
a procedure
for the determination
of the resin
content
on carbon,
graphite,
fortisan
and
nylon
prepregs
by soxhlet
extraction.
Special
provisions
are
included
to determine
the
resin
content
of filled

I.i

systems.
,

EQUIPMENT

2.1

AND

Equipment.

2.1.1

Balance,

2.1.2

Bottle,

2.1.3

Crucible,
30

analytical,

filtering,

2.1.5

Desiccator

2.1.6

Extraction
x

Flask,

2.1.8

Furnace,

2.1.9

Oven,

glass,

medium

grade,

pyrex,

extra

coarse,

mm.
filtering,
muffle,

forced

ml.

least

1000

(325 _

5F.)

extraction

hot

Vacuum

500
at

air

assembly,

25F

125

ml.

capacity

plate

system

Materials

2.2.1

Extraction

2.2.2

Solvent,

2.2.3

Filter,
glass
or equivalent.

3.

fritted

thimbles,

Soxhlet
with

2.1.11

gm.

holder

85

2.1.7

2.1.10

0.0001

ml.

Crucible

25

sensitivity

wash

2.1.4

2.2

MATERIALS

thimbles,
technical
fiber,

paper,
grade
5.5

fat-extracted,

(see

4.5)

cm.,

Reeve

SAMPLING

190

Angel

25

grade

x 85

mm

934AH

3.1 .i

Broad@oods.
The sample
shall
include
the entire
width
of the unit
being
tested,
less
the
first
two
inches
in
from
each
selvage
edge.
A sufficient
number
of strips,
1 x 2 inch
from the usable
width,
shall
be cut into
1/2
inch
by 1/2
inch squares,
to provide
enough
samples
for
the
required
number
of soxhlet
extractions
per
sample.
These
squares
shall
then
be well
mixed,
using
extreme
care
not
to knock
off any
resin,
before
the actual
samples
are taken.

3.1.2

Chopped
Stock.
Obtain
a representative
10-15
grams
and mix thoroughly,
using
to knock
off
any resin.

3.2

Number
of determinations.
run duplicate
determinations

bulk
extreme

Unless
otherwise
on each
sample.

sample
care

of
not

specified,

PROCEDURE

4.2

Volatile
prepreg

content.
per PTM-17,

Thimble
thimble

type.
types

CARRIER

Carbon
and
Fortisan
Nylon

4.3.1

Thimble
condition

sets
Store
4.3.2

at

Identify
325 _ +

of 3 and Weigh
in a desiccator

Glass.
furnace.

Dry

for

Cool

the

THIMBLE

TYPE

30
in

the

following

Paper
Glass
Glass

Unless

with
5_F.in

of

specified,

graphite

conditioning.
as follows

Paper.
hours

volatile
content
or as specified.

Unless
otherwise
shall
be used:

MATERIAL

4.3

Determine
PTM-32,

otherwise

specified,

a soft
lead
pencil
a forced
air oven.

immediately
together
minutes

at

a desiccator

and dry
Remove

to 0.001
gm.
with
recorded
950 +
and

25F.in

_eigh

to

for
in

(Wl).
weight.
a muffle
0.001

gm.

(Wi).
4.4

Sample
Weighing.
Unless
otherwise
specified,
transfer
a
2.5 + 0.5 gm. sample
to the weighed
thimble
and weigh
to
0.00[
gm.
(W3).
When
paper
thimbles
are used,
they
must
be reweighed
to 0.001
gm.
(W2) before
addition
of the
sample.
See note
6.1 for precautions
regarding
paper
thimbles.

4.5

Extraction.
extraction
portion
of

Position
assembly.
the
90 ml.

the

thimble

Add
90
to the
191

within

the

ml.
of solvent,
extraction
tube

Soxhlet
adding
a
so that

about
2/3 of the thimble
is covered,
the
remainder
is
added
to the boiling
flask.
The
following
solvents
are
suggested
for the listed
resins.
However,
experience
shall
dictate
solvent
to be used
(see note
6.2).
RESIN

SUGGESTED

Phenolic
Epoxy
Silicone
Polyester

SOLVENT

Ethyl
alcohol
or dimethylformamide
Acetone
or methyl
ethyl
ketone
Piperidine
or toluene
Acetone
or MEK

(DMF)
(MEK)

Turn
on the cooling
water
for the condenser.
Turn
on the
hot plate
to effect
heating
of the
solvent.
When
condensation
of the solvent
occurs,
adjust
hot
plate
temperature
to effect
3 to I0 reflux
changes
per hour.
For high
boiling
solvents,
such
as DMF,
it may
be
necessary
to wrap
the extraction
tube with
aluminum
foil.
Ensure
that
the solvent
is condensing
and dropping
into
the extraction
tube.
Continue
to reflux
for a minimum
of
four
hours.
4.6

Determination
of filler
appeared
in the extract,
determined
as follows:

when
the

present.
If
filler
weight

filler
must

has
be

4.6.1

Conditionin
9 of crucibles.
Place
a glass
fiber
filter
in a fritted
glass
crucible
(see note
6.3).
Condition
in a forced
air oven
for 15 to 20 minutes
at 325_
+
5F.
Allow
the crucibles
to cool
in a desiccator
and
weigh
to 0.001
gm.

4.6.2

Filtering.
Set up the vacuum
system
and
filter
the
resin
extract.
Using
a wash
bottle
of acetone
or
appropriate
solvent
wash
out the extraction
tube
and
flask,
putting
all washings
in the
filtering
crucible.
Wash
the
residue
clean
of resin.
About
50 ml.
of
acetone
or appropriate
solvent
will
usually
suffice.
Do not
stir
the solution
on the
filter.

4.6.3

Unremovable
filler.
If after
washing
the
extraction
flask_with
solvent
there
is some
filler
which
is caked
on the
flask
and cannot
be removed,
the
following
procedure
can be used
for carbonaceous
filled
aldehydephenolic
resins:
Place
the
flask
in a muffle
furnace
at 750 _ + 25_F.
for a minimum
of one hour.
Cool
in a
desicattor
and weigh
to 0.001
gm.
If the
flask
has
been
prepared,
subtract
the tared
weight
and
add this
filler
weight
to that
of 4.6.4
If the
flask
has not
been
prepared,
place
in a muffle
furnace
and burn
off
the carboneceous
filler
at i000
+ 50F.
for a minimum
of

one

hour.

Cool

in

a desiccator

gm.

192

and

weigh

to

0.001

4.6.4

4.7

5.
5.1
51.1

Dryina
filter
crucible.
Dry the filter
crucible
in a
fsrce_
air oven
for a minimum
of one hour
at 325 +
5 F.
Cool
in a desiccator
and weigh
to 0.001
gm. -Add
this
filler
weight
to the carrier
weight
of 4.7.
Drying
thimbles.
Remove
thimbles
from
the extraction
assembly.
Drain
off the solvent
and dry to essentially
constant
weight
at 325 + 5F.in
a forced
air oven
(see
note
6.4).
If paper
thimbles
are used,
remove
from the
oven
in sets
of three
or less
and weigh
immediately
to
0.001
gm.
(W4).
Glass
thimbles
may
be cooled
in a
desiccator
before
weighing.
CALCULATIONS

AND

Calculations

REPORTING

where

paper

Dry
resin
content
(resin
solids)
as
DRC,

wt.

i00

thimbles

(DRC).
follows:
[ 1

are

used.

Calculate

dry

resin

[(W4-WI)/(W3-W2)

content

(I-V/100)]]

where:
w I = weight
of dried
thimble,
gms.
w 2 = weight
of thimble
after
storage
desicator,gms
W 3 = weight
of thimble
plus
sample,
w 4 = weight
of thimble
plus
extracted
gms.
v
= volatile
content,
wt.%
5.1.2

Wet
resin
content
(WRC).
Calculate
(total
pick-up)
as follows:
WRC,

5.1.3

5.2.1

= i00

Wet
resin
solids
as follows:
WRS,

5.2

Wt.

where

glass

Dry resin
content
(resin
solids)
as

where

resin

[(W 4 - WI)/(W3-W2)
Calculate

(WRS).

gms.
sample,

wet

resin

wt.%=I00[I-[(W4-WI/W3_W2)]_(V/100)]=WRC_

Calculations

DRC,

[ 1 -

wet

in

wt.%

symbols

i00

thimbles

(DRC).
follows:

are

Calculate

specified

193

in

5.1.1

]
solids

v
used.
dry

resin

[ I-[(W4-WI)/(W3-WI)(I-(V/100))]]

are

content

content

5.2.2

Wet
resin
content
as follows:
WRC,

5.2.3

WRS,
5.3

wt.%

= i00

i00

wet

resin

solids

[l-(W4-Wl)/(W3-Wl)]
Calculate

(WRS).

[I-[(W4-WI)/(W3-WI)]

Reportin
9.
Unless
otherwise
content
to the nearest
0.1%.
should
be considered
suspect
1.5%.

wet

resin

solids

(V/100)]=WRC-V

designated,
report
resin
Duplicate
determinations
if they differ
by more
than

NOTES

wt.%

Wet
resin
solids
as follows:

Calculate

(WRC).

Paper
thimbles,
when
paper
thimbles
are used,
it is good
laboratory
practice
to periodically
determine
a blank
on
the procedure.
This
is especially
true
when
conducting
the extraction
on a new
product
for the first
time.
Under
normal
conditions,
single
thimbles
shall
be used.
However,
particle
size
of a filler
may make
it necessary
to use
double
thimbles.

6.2

Selection
of solvent.
phenolics
with
carbon
following
rule
shall
content
is less
than
than
3.8%.

6.3

Use of 91ass
fiber
filter
to prevent
the fritted
glass
with
the
filler.

6.4

Thimble
normally

6.5

Calculation
of resin
content.
This
method
has used
carrier
weight
for the calculation
of resin
content.
There
are occasions
where
it may be desirable
to
calculate
resin
content
by using
the resin
extract
which
has
been
dried
down
by the appropriate
means
and weighed.
Calculating
resin
content
using
resin
extract
typically
gives
higher
results
and more
variability
than
when
thimble
weight
is used.

For
carbonaceous
filled
aldehydeor graphite
reinforcement,
the
apply:
DMF must
be used
when
resin
31% and/or
volatile
content
is less

glass
filter

drying
time.
The drying
two hours
minimum.

194

time

fiber
from

for

filter
becoming

the

is used
clogged

thimble

is

P-P-8
i.

volatile

of

Prepregs

SCOPE

1.1

Content

The
purpose
of
the determination
materials.
EQUIPMENT

2.1

AND

this method
is
of volatile

2.1.2

Hooks,

2.1.3

Oven,

forced

2.1.4

Oven,

dead

2.1.5

Mettler
balance,
0.001
gram

or

2.1.6

Stanley

equivalent

2.1.7

Wide

2.1.8

Desiccator

3.1.1

3.1.2

4.
4.1
4.1.1

for

Equipment
Steel
inches

3.1

a procedure
preimpregnated

MATERIALS

2.1.1

3.

to describe
content
of

templates,

"S"

inches

by

inches

and

inches

by

shaped
air
air

knife

mouth

or

ceramic

equivalent,

crucibles,

capable

Coors

No.

of

weighing

or

to

equivalent

SAMPLING
Sample

Size

Prepregs
other
than
unidirectional
tapes.
Three
specimens
4 inches
by 4 inches
are cut randomly
from
representative
sample
one
foot
from
edge
of prepreg.
Unidirectional
tapes.
inches
(or equivalent
shall
be randomly
cut
the material.

Three
specimens
2 inches
by 2
of 4 square
inches
per specimen)
from
a sample
representative
of

PROCEDURE
Prepregs

other

than

unidirectional

Preparing
samples.
Cut three
specimens
using
steel
template
to the nearest
0.001
gm.

195

tapes.
4

inch
by
and weigh

inch
collectively

4.1.2

4.2

Testing
samples.
Attach
"S" shaped
hook
to one corner
of each
specimen
and place
the
specimens
in the
designated
type
of oven
for required
time
and
temperature
as per
the chart
in 4.2.2.
Suspend
the
specimens
individually,
allowing
room
for free
air
circulation
between
each.
Do not
allow
the door
to
remain
open
longer
than
I0 seconds
while
loading
the
specimens.
If dripping
of resin
occurs
repeat,
hanging
each
specimen
by diagonal
corners.
Remove
the
specimens
from
the oven,
desiccate
for 5 minutes
and
reweigh
collectively
to the nearest
0.001
gm.
Desiccation
may
be waived
unless
specifically
required
by customer
specification
or test
method,
provided
the
weighing
is done
immediately
upon
removal
of the
specimens
from
the oven.
Unidirectional

tapes.

4.2.1

Preparing
samples.
Cut
three
2 inch
by 2 inch
(or
equivalent)
specimens
and weigh
each
into
a previously
tared
crucible,
to the nearest
0.001
gm.

4.2.2

Testing
samples.
Place
the crucibles
in the designated
type
of oven
for the required
time
and temperature
as
per the chart.
Do not allow
the oven
door
to remain
open
longer
than
i0 seconds
while
loading
oven.
PREPREG

TYPE

* TEM.,
320
220
320
275
320
320
220
450

Phenolics
or Phenylsilanes
Polyesters
Standard
Epoxies
Special
Epoxies
Silicones
Paper,
Melamines
Paper,
Polyesters
Polyimides
Miscellaneous
*
All
temperature
tolerances
tolerances
are + 0.25 minutes.
air except
as noted.

are
+
5F;
AI[
ovens

**
For miscellaneous
prepreg
types,
time
are as per customer
specification.
Remove
minutes
5.
5.1

CALCULATIONS
Prepregs

the crucibles
and reweigh
AND
other

*TIME,

8,

Dead

8,
i0,

Dead
Dead

unidirectional

196

tape.

MIN.
9
Air
9
15
5
Air
Air
i0

all time
are forced

temperatures

from
the oven,
desiccate
each
to the nearest
0.001

REPORTING
than

OF.

and

for
gm.

5.1.i

Calculate
%

volatile

Volatile

= W]

content

- w2 X
W1

as

follows:

i00

where:
w I = Original
weight,
gms.
w 2 = Final
weight,
gms.
5.2
5.2.1

Unidirectional
Calculate
%

tapes.
volatile

Volatile

(W]

content
- Wc)

as

follows:

(W 2 - We)

I00

W 1 - Wc
where:
W1 =
Wc
W2 =

5.3

Repeated

tests

Weight
Weight
Weight
gms.
should

of
of
of

crucible
crucible,
crucible

agree

197

and original
sample,
gms.
and sample
from
oven,

within

0.2%.

gms.

P-P-9
I.
i.i

2.
2.1

Gel

Time

for

Thermosetting

or

Thermoplastic

Resins

SCOPE
This
time
using

procedure
describes
of thermosetting
or
a cure
plate.

EQUIPMENT

AND

a method
catalyzed

for determining
thermoplastic

gel
resins

MATERIALS

Equipment

2.1.1

Stop

watch,

2.1.2

Cure

plate

2.1.3

Thermometer,

2.1.4

Tongue

2.1.5

Bent
medicine
1 ml.

2.1.6

Cleaning

2.1.7

Oven,

0.i

20

depressor

sec.

to

divisions

600F.

, accurate

slivers,
droppers,

about
with

1/8

to
inch

2F.
wide

useful

capacity

of

approx.

sample

of

I0

gms.

Blade
to

at

least

500

2F

3.

SAMPLING
A

representative

3.1

Sample
size.
required.

3.2

Number
of determinations.
make
three
determinations.

4.
4.1

Unless

specified,

PROCEDURE
Preconditi6ning
precondition
temperatures,
RESIN

cure
plate.
Unless
the cure
plate
to one
consistent
with
resin

TYPE

otherwise
specified,
of the following
type:

TEMPERATURE
480
350
275
325
325
400
350

Silicones
(uncatalyzed)
Silicones
(catalyzed)
Polyesters
phenolics,
phenyl
Silanes
Epoxies,
(General)
Polimides
Epoxies
(Special)
4.2

otherwise

about

+ 3F.
T 2F
T 2F.
2F.
T 2F
(unless
otherwise
3F
specified)
T 3F.

Preparation
of cure
plate
and
resin.
Clean
the cure
plate
thoroughly.
The
sample
must
have
a solids
content
specific
to that
resin
system.
Adjust
if necessary.
198

is

4.3

4.4

Starting
gel.
Using
an eye dropper,
draw
in as much
sample
as it will
hold.
This
will
be 1.0 _ 0.2
grams.
Transfer
completely
to the
spot
on the cure
plate
directly
above
the thermometer.
Commence
timing
with
stop
watch.

Detection
of end point.
Do not disturb
the
resin
blob
until
a few seconds
prior
to minimum
gel time
expected.
At this
time,
the gel time
is close,
with
the
clean
tip
of the
sliver,
poke
at the resin
with
an up and down
movement
(see Note
6.1).
As gel time
approaches,
the
sliver
will
carry
strings
of resin,
when
the
resin
is
gelled,
the sliver
will
not
carry
any resin
and the
resin
will
have
rubbery
appearance.
Note
the time
in seconds
required
for gelation.
Repeat
the test
for a total
of
three
results.
CALCULATIONS

AND

REPORTING

Average
the three
results
and
report
the value
in seconds
or minutes
and seconds.
The
results
should
be considered
suspect
if the range
of the three
results
exceeds
10% of
the average
gel time.
,

6.1

6.2

NOTES
when
poking
at the resin,
do not attract
resin
to a
certain
point,
but merely
poke
and move
lightly
across
order
to pick
up a small
drop
which
will
string
when
lifted
upward.
If the
resin
is gelled
when
it is
disturbed,
repeat
the operation
but probe
earlier.
For E-715
and
until
gelation

E-735,
use
occurs.

constant

199

stroking

of

the

resin

in

P-P-10

Volatile,

Fiber,

and

Filler

Content

of

Prepregs

SCOPE

i.i

This
procedure
describes
methods
volatile
content,
fiber
content
EPDM
prepregs
such as R2066P.
EQUIPMENT

AND

2.1

Aluminum

2.2

Oven,

2.3

Timer

2.4

Desiccator

2.5

Porcelain

2.6

Muffle

determining
the
filler
content
of

MATERIALS

weighing
air

of
and

dishes,

circulating,

with

approx.

at

least

1.5
300

gm.

5F

desiccant

crucible,
furnace,

25

at

ml.

least

capacity,

1500

with

cover

25F

SAMPLING

3.1

A representative
sample
of 4
material
(normally
40 inches)

inches
by the
is required.

3.2

The
number
of
each
individual

shall

4.
4.1

determinations
test below

be

as

width

of

specified

the

in

PROCEDURE
Volatile

4.1.1

Volatile
the

4.1.1.i

Content
content

shall

be

determined

each

2"

in

accordance

with

following:

Cut
3 specimens
tested

2"

from

each

nearest
dish

mg.

sample

to

be

41.1.2
) Weigh
place

each
2" x 2" to
into
an aluminum

4.1.1.3

Condition
sample
and aluminum
dish
oven
@ 285 + 10F
for 55 + 2 min.

4.1.1.4

Remove,
cool
only)
to the

in desicattor,
and
nearest
mg.
(W2)

200

in

weigh

individually
circulating

(2

2 sample

air

4.1.2

Calculation

Volatile

Content,

lW]

- W_[
W1

i00

where:
W 1 = Original
sample
weight,
grams
W 2 = Sample
weight
after
55 minutes
285_F.,
gm.
Report
individual
and average
values.
4.2

Total

4.2.1

Filler

Determine

Content
the

filler

content

as

follows:

4.2.1.i

Cut
the 2" x 2" (W2) sample
into
1/2"
place
into
a previously
fired
(1450
_
tared
crucible.

4.2.1.2

(W3) weigh
to the nearest
mg.
sample
and crucible,
then
cover
crucible,
and _lace
an a muffle
furnace
for
1 hr. + 5 min.
at 800 _ + i0 F.

4.2.1.3

Remove
crucible
and place
into
a desiccator
to cool
to touch
(do not
remove
cover
from
the crucible).

4.2.1.4

(W4)

4.2.2.

Weigh

crucible

and

Content,
Content,

=i00

sample

without

- W3

- W 4 x
W2

x 1/2"
10F.)

and
and

cover,

gm.

Calculation
Total
Total

Filler
Filler

100

where:
W2"=

Sample
weight
after
55 + 5 min.
@
280
+ 5F,
gm.
W 3 - Crucible
and sample
(without
cover)
burn
off,
gm.,
to nearest
mg.
w 4 = Crucible
and sample
(without
cover)
burn
off,
gm.,
to nearest
mg.
Report
the
results.
4.3
4.3.1

Fiber

individual

and

average

values

for

before
after

these

Content

Determine

fiber

content

by

201

calculation

as

follows:

4.3.2

Calculation
Total

Filler
29.8

26.7

(these
R2066P)

202

constants

apply

only

to

P-P-f1

Extraction
of Prepregs
Soluble
Material

for

Determination

of

Acetone

SCOPE

i.I
or
1.2

2.

This method
describes
ount
of acetone-soluble
laminated
phenolic
products

Equivalent
Test
Method
46.
EQUIPMENT

2.1

methods.
Standard

AND

a procedure
material
in

This
method
is
No.
406,
Method

for determining
prepreg,
molded

equivalent
7021
and

to Federal
ASTM-D494-

MATERIALS

Equipment.

2.1.i

Specimen
fragmentator
- a suitable
drill
press,
bench
lathe,
planer,
milling
machine,
grinder,
or file
will
be needed
to breakup
specimen
into
fragments.

2.1.2

Sieves,

U.S.

Standard,

Weighing

bottle,

Soxhlet

extraction

40

oz.

and

glass

140

mesh

stoppered

assemble,

125

ml.

capacity

with

hot

plate
Balance,
Drying
2.2

analytical,
chamber

capable

of

0.001

maintaining

gm.
122

80

mm.

4F

Materials.
Extraction

2.2.3

sensitivity

thimble,

paper,

Aluminum
inches

dishes,

diameter

Acetone,

reagent

grade

25
2-1/2

mm.

D X

inches,

height

L.
1-1/16

SAMPLING

3.1

Sample
size.
Each
sample
shall
weigh
a minimum
of 15
grams.
The sample
shall
be a composite,
representative
of the prepreg,
molded
or laminated
part
from
which
it
was taken

3.2

Number
of determinations.
make
three
determinations

Unless
on each

203

otherwise
sample.

specified,

4.
4.1

PROCEDURE
Prepreg.
Prepreg
materials
larger
than
1/2 inch.

4.1.2

Molded
shall

4.1.2.1

or laminated
be prepared

as

shall

be

parts.
Molded
follows:

cut

or

in

squares

laminated

no

parts

Grinding.
The method
of grinding
up the material
for
sieving
should
be such
that
no undue
heating
of the
particles
will
occur
which
might
tend
to further
cure
the material.
Drilling
is the preferred
method
where
the size
and shape
of the part
permits.
In any case,
the particles
should
be of the
smallest
size
practicable,
so that
they
will
pass
through
a 40-mesh
screen
with
a minimum
of reworking
or grinding.

4.1.3

Screening.
Screen
the material
through
a 40-mesh
sieve.
Regrind
the part
which
does
not pass
through
the 40-mesh
sieve
until
it does,
resieve,
and blend
with
the
original
part which
passed.
Place
the sample
on a !40-mesh
sieve
and screen
by using
either
a
standard
screen
shaker
(such
as the Rotap)
or by hand
screening.
In the latter
case,
the screen
should
be
rotated
with
a slight
tapping
for a period
of one
minute
or more
until
there
are virtually
no further
screenings.

4.1.4

Bottling
sample.
The
sample
for analysis
should
be
removed
from
the 140-mesh
screen
and placed
in the
two-ounce
bottle.
Care
should
be taken
that
the sample
is immediately
placed
in this
bottle
and closed
up so
as to prevent
absorption
of moisture
by undue
exposure.

4.2

Extraction.
From
the material
in the bottle,
accurately
weigh
out
1.0 + 0.05 gm.
into
a tared,
open
texture,
quantitative
fTlter
paper
12 to 15 cm.
in diameter.
Place
the
filter
paper
containing
the
test
specimen
in a
standard,
single
thickness,
paper
extraction
thimble,
80
mm. by 25 mm.
Close
the thimble
so that
none
of the
sample
can
float
out.
Place
the thimble
in an extraction
tube
and add 50 ml.
of acetone.
Start
the water
in the
condenser
and adjust
the heat
so there
are between
15 and
20 dumps
per
hour.
Carefully
maintain
this
rate
for
four
hours
minimum.
After
the siphon
empties,
remove
the
flask
and empty
the contents
into
a weighed
aluminum
dish.
Rinse
the flask
with
acetone
three
times
and
add
the washings
to the extract
in the dish.

4.3

Drying.
chamber
constant
dryings

Place
the dish
in a well
ventilated
drying
maintained
at 122 + 4F.
and dry the sample
to
weight.
Keep
the-dish
in a desiccator
between
to prevent
moisture
pickup.

204

5.1
5.1.1

CALCULATIONS

AND

REPORTING

Calculations.
Acetone
extractables.
extractable
materials
E

= _3

- W2
W1

Calculate
as follows:

the

percent

of

acetone

i00

where:
E = acetone
extractables,
wt.
%
W 1 = sample
weight,
gm.
W 2 = tare weight
of aluminum
pan,
gm.
W 3 = final
weight
of pan
and extract,
5.1.2

Percent
uncured
as follows:
U

resin.

Calculate

percent

gm.
uncured

resin

E/T

where:
U
T
5.1.3

= uncured
resin,
= resin
solids,

Degree
of polymerization.
polymerization
as follows:
Degree

5.2

Reporting.
following

5.2.1

Percent

5.2.2

Degree

5.2.3

Cure

6.
6.1

wt.%
wt. %

of

acetone
of

cycle

Note

Calculate

polymerization

Unless
otherwise
information:

(see

degree

i00

specified,

extractable

6.1)
of

- U
report

the

material

polymerization
used

in

preparation

of

sample.

NOTES
The resin
solids
resin
solids
of

figure
must
be representative
the sample
extracted.

205

of

the

P-P-12

Method
Resins

of
Conducting
and
prepregs.

Thermogravimetric

1.0

SCOPE

i.i

This
procedure
thermogravimetric

2.0

EQUIPMENT

2.1

Perkin-Elmer

Model

TGS-2

2.2

Perkin-Elmer

DSC-2

Programer,

2.3

Appropriate

3.0

SAMPLING

3.1

Obtain

4.0

PROCEDURE

4.1

Balance

describes
analysis

AND

small

(i

oz.)

sample

Controls

Filter

4.1.3

Recorder

Mode

4.1.4

Recorder

Range

4.1.5

Weight

Suppression

switch

4.1.6

Weight

Suppression

thumb

on
-

DSC-2

io
-

short
-

a;s the

Sample

4.2.2

Temperature

RANGE

4.2.3

Temperature

ZERO

4.2.4

Lower

4.2.5

Cooling
Heater

holders

LIMIT

(See

recorder

direction

manual)

mg.
-

I00

sheen

mg.
dial

00.000

Programmer

empty

RATE
Control

ZERO
and
procedure
9235)

I0

TG

4.2.1

4.3.1

equivalent

equivalent

representative

4.1.2

4.3

or

or

manual

Power

Use

for
conducting
and
prepregs.

Thermoanalyzer

4.1.1

4.2

of

MATERIALS

operators

the
method
of
resins

Analysis

RANGE
(or

Calibration
Calibration

350oK
-

(or

as

as
as

calibrated
calibrated

required)

160o/min.

Unit
Setting
as
indicated

206

as

determined
on
calibration

from

calibration
card
993-

4.3.2

Power

4.3.3

oC

4.4

oK

HEAT
switch

(on

back

panel)

oK

Recorder

4.4.1

CHART
chart

4.4.2

Weight

4.4.3

Second
zero;

SPEED
speed
Pen:
Pen:
or
FDC:

-slow
when
RANGE

(e.g.,
5
temperature
-

20

Thermocouple:
RANGE
-

mm/min.)
change
is started

my.;

i0

207

my,

right-hand
RANGE
- 1
left-hand

to

faster

zero
volt,
zero

right-hand

P-P-13
1.

Percent

Volatiles

Content

of

Prepregs

SCOPE

1.1

2.

This
procedure
is
volatiles
content

Cutting

2.2

Analytical

2.3

Air-Circulating

3.1

determining
material.

the

percent

EQUIPMENT

2.1

3.

applicable
for
for impregnated

Board

or

Template

Balance,

sensitivity

Oven,

325 +

0.001

gm.

10F.

PROCEDURE
This
test
is to be run in triplicate.
+ 1/8"
straight
cut from
left,
center,
width
of broadgoods.

3.1.1

Weigh

the

specimen

to

3.1.2

Place
specimen
in a circulating
stabilize
to 325 + i0 degrees
Specimens
should
_e placed
to
circulation.

3.1.3

Remove
specimen
room
temperature.

3.1.4

Remove
from
the nearsest

3.1.5

Calculate

and

the

place

nearest

in

Percent
-

volatiles

Volatiles

= w]

0.01

gram

4"
the

(Wl).

oven,
preheat
and
F. for i0 + 1 minutes.
get
adequate
air

a desiccator

the desiccator
and
0.01 gram
(W2).

percent

Cut
three
4"
right,
across

as

weigh

and

the

cool

specimen

to

to

follows:

- W 2 x
W1

i00

Where:
W 1 = uncured
weight
of specimen,
W 2 = final
weight
of specimen,
3.1.6

Report
volatile
percent.

content

of

2O8

specimen

gm.
gm.
to

the

nearest

0.1

P-P-14
i.

Character

of

"B"

Staged

Broadgoods

SCOPE

i.i

2.

Flow

This
test
is
characteristics

applicable
of "B"

for the determination

of
staged
broadgoods
material.

flow

EQUIPMENT

2.1

Cutting

Board

Analytical

or

Template

Balance,

sensitivity

0.001

gm.

Laminar
press
capable
of meeting
temperature
requirments
of this
method,
325 _ _ 10F,
150
3.

the

and pressure
Z i0 psig.

PROCEDURE

3.1

This
test
from left,
broadgoods.

is run in triplicate.
Cut
one specimen
center,
and right
across
a piece
of

each

3.1.1

Cut
four
4-inch
by 4-inch
+ 1/8 inch
squares
sample
location.
All
squares
shall
be bias
eliminate
fiber
loss
in testing.
Stack
the
uniformaly
on each
other
to make
a specimen.

3.1.2

Weigh
the
specimen
and record.

3.1.3

Place
the specimen
between
release
film.
Preheat
the
press
to 325 + i0 F.,
position
the specimen
in the
middle
of the press
plate
and apply
the press
load of
150 + i0 psig.
immediatly.
Press
load
the specimen
for
a minimum
of l0 minutes
at 325 + i0 degrees
F.

3.1.4

Remove
the
temperature.

3.1.5

Using
a knife,
original
size
reinforcement

3.1.6

Reweigh
as W 2 .

the

specimen

of

four

from

plies

the

to

press

the

and

nearest

cool

scrape
off the
resin
flash
to
of the specimen.
Do not
remove
from
the original
dimensions.

specimen

to

the

209

nearest

0.01

from
each
cut to
squares

gm.

0.i

to

gm.

ambient

the
any

and

record

3.1.7

Calculate

the

Percent

percent

Flow

resin

W]

- W2
W1

flow
x

as

follows:

100

where:
W 1
w 2
3.1.8

Report

resin

=
=

uncured
final

weight
of specimen,
weight
of
specimen,

flow

to

the

210

nearest

0.1

gm.
gm.
percent.

P-P-15
i.

Solids,

Filler,

and

Cloth

Content

of

Prepregs

SCOPE

i.i

2.

Resin

This
method
is applicable
solids,
filler,
and cloth
epoxy
or aldehyde-phenolic

for determining
the
content
of prepregs
resin
matrix.

resin
having

an

PROCEDURE

2.1

Resin
solids,
filler
content
and cloth
content.
These
components
of the uncured
material
shall
be determined
for each
sample
in accordance
with
the
following:

2.1.1

Place
a 2 1/4 + 1/4"
nearest
0.01 gm.
(R)
beaker.

2.1.2

Calculate
W

devolatilized

= specimen

where:

square
specimen
weighed
(specimen
weight)
in a

wt.

specimen

(percent

weight

(W)

to
250

as

volatiles)(specimen
100

percent
volatiles
is
the volatile
content.

the

value

the
ml.

follows:
wt[

determined

from

2.1.3

Add 50 ml. of N, N dimethylformamide

(DMF)
and bring
to
a boil.
Occasionally
gently
stir
the boiling
DMF
and
prepreg
cloth
for a minimum
of 5 minutes.

2.1.4

Decant
and transfer
250 ml. beaker.

2.1.5

Rinse
ensure
fabric

2.1.6

Finally
traces

2.1.7

Add

all

2.1.8

Dry
350
and
gm.

a filter
and a crucible
or filtering
crucible
at
+ 5_F.
for a minimum
of 30 minutes.
Weigh
filter
crucible
or filtering
crucible
to the nearest
0.01
(w2).

2.1.9

Dry the
+ 10F.

liquid

the remaining
fabric
complete
extraction
and add the rinses
rinse
the
of DMF.
rinses

to

fabric
in
minimum.

temperature
2.1.10

the

and

fabric

the

Using
an aspirator
or
of the second
250 ml.
crucible
or filtering

to

the

second

with
DMF several
times
to
of resin
and
filler
from
to a second
250 ml.
beaker.
with

second

an oven
Cool
in

reweigh

solution

to

acetone

250

ml.

to

remove

beaker.

for 20 minutes
minimum
a desiccator
to room
the

nearest

all

0.01

gm.

at

325

(Wl).

vacuum
pump,
filter
the
contents
beaker
through
a filter
and
crucible
into
a vacuum
flask.
211

2.1.11

Rinse
the crucible
several
times
with

2.1.12

Dry
the crucible
and contents
at 350 + i0 degrees
F.
for
20 minutes
minimum.
Cool
in a desiccator
to room
temperature
and
reweigh
to the nearest
0.01
gm.
(W3).

2.1.13

Report
content

3.

the
to

and
filter
acetone
to

or filtering
crucible
remove
all resin.

resin
solids,
filler
content,
the nearest
0.i0
percent.

and

cloth

CALCULATIONS

3.1

Calculate
the
cloth
content

3.1.i

Resin

3.1.2

Filler

Cloth

resin
solids
as follows:

Solids

content

content

content

(percent)

(percent)

(percent)

content,

= W4/W

= Wl/W

filler

= w-(wl+w4_
w

content

and

(i00)

(I00)

(i00)

Where:
W
wI
W2
W 3
W4

= calculated
devolatilized
weight
of prepreg
specimen,
gm.
= weight
of fabric
after
resin
and filler
removal,
gm.
= crucible
and filter
or filtering
crucible
weight,gm.
= filler
+ crucible
and filter
or filtering
crucible
weight,
gm.
= W 3 - W 2 = filler
weight,
gm.

212

P-P-16
i.
i.i

2.

Resin

Solids,

Filler

of

prepregs

an

EQUIPMENT
board

2.2

250

beakers

2.3

Membrane

2.4

Whatman

4.25

2.5

Whatman

4.7

2.6

Analytical

2.7

Aluminum

2.8

Vacuum

2.9

Circulating

ml.

filtration
cm.
cm.

funnel
GF/F

EPM

balance,
weighing

pump

or

200-230

mesh

2.11

Acetone

or

2.12

Desiccator

2.13

Ultrasonic

2.14

Teflon

filters
2000

sensitivity

0.0001

gm.

pans

oven,

163 +

filtering
DMF

47

or
mm.

3C

sieve

technical

cleaner

gasket

filters

aspirator

air

2.10

3.2

Content

This
method
is applicable
for determining
the
resin
solids,
filler
and cloth
content
of prepregs
having
epoxy
or aldehyde
phenolic
resin
matrix.

Cutting

3.1

Cloth

SCOPE

2.1

3.

and

grade

hot

plate

(optional)

PROCEDURE
Precondition
several
pairs
of filters
(one Whatman
EPM
2000
on the bottom,
one Whatman
GF/F
on the
top)
by
filtering
approximately
25 ml.
of acetone
through
the
pair
of filters.
Place
the filters
in an aluminum
weighing
pan
and dry @ 163 + 3 C.for
20 minutes
or
until
dry.
Preconditioned
fTlters
are
to be stored
in
desiccator.
Weigh
a 2 1/4 + i/4" square
specimen
to the nearest
0.0001
gm.
and-place
in a clean
250 ml.
beaker.
Alternative
sample
sizes
(Specimen
Weight)
may
be
specified.

213

3.3

Ultrasonically
extract
the sample
twice,
for three
minutes
each
time,
in 50-75
ml.
of acetone.
Fresh
solvent
is to be used
for each
three
minute
extraction.
Ultrasonic
extraction
must
be performed
under
a fume
hood.
Stir
the samples
several
times
during
extraction.
Alternatively,
the samples
may
be extracted
for five
minutes
with
50-75
ml.
of boiling
DMF.
(For prepreg
weights
over
6 gm. use
150 ml.
of solvent.)

3.4

Weigh
a preconditioned
pair
of filters
and pan
(from
3.1)
to the nearest
0.0001
gm.
and place
the pair
of filters,
with
the smaller
filter
on top,
in the membrane
filtration
apparatus
(W2).
Note:
If the
filter
sticks
gasket
may be placed
between
stainless
steel
screen,
and

to the funnel
the bottom
repeat.

base,
filter

a teflon
and the

3.5

Hold
the specimen
in the beaker
with
a glass
stirring
while
decanting
the
liquid
solution
through
a 200-230
mesh
filtering
sieve
placed
on top of the
filtering
funnel.

3.6

Rinse
the
remaining
complete
extraction
rinsing
is indicated
Add

all

rinses

to

fabric
twice
of the resin
by a clear
the

filtering

rod

with
acetone
to ensure
and filler.
Complete
acetone
solution.
funnel

per

Step

3.5.

Remove
the fabric
and place
into
a preweighed
aluminum
drying
dish.
Any
fiber
remaining
on the
filtering
sieve
is to be transferred
to the aluminium
weighing
pan using
a rubber
policeman.
Dry
the
fabric
in an air circulating
oven
@ 163 + 3C.
for 20 minutes
or until
dry.
Cool
in
a desiccator-to
room
temperature
and weigh
to the nearest
0.0001
gm.
(Wl).
3.9

3.10

Filter
theocontents
of
pair
of filters.
Rinse
with
acetone
to insure
in the filters.

the
filteing
funnel
through
the
the sides
of the
filtering
funnel
that
all the
filler
is entrapped

Remove
the filters
from
the
filtering
funnel
and place
back
into the original
weighing
pan
(the top
filter
should
be placed
into
the pan first
and covered
by the
larger,
bottom
filter).
Transfer
any
filler
remaining
on the bottom
rim of the
filtering
funnel
to the
weighing
pan with
a small
metal
spatula.
Close
loosely
around
the edges
and dry
in an air circulating
oven
@
163 + 3C. for 20 minutes
or until
dry.
Cool
to room
temperature
in a desciccator
and
reweigh
to the nearest
0.0001
gm.
(w3).

214

4.

CALCULATIONS
Devolatilized
W

= Specimen

Resin

Solids

Filer

Content

Cloth

Content

specimen
wt.

wt.

(% Volatiles)(Specimen
i00

I W

(W]
W

+ W4)

W4/W

i00

= WI/W

i00

Wt.)

i00

Where:
W - Calculated
devolatilized
specimen
wt.,
gm.
W 1 = Weight
of fabric
after
resin
and
filler
removal,
gm.
w 2 = Preconditioned
filter
weight,
gm.
W 3 = Filter
and filler
weight,
gm.
W 4 = W 3 - W 2 I filler
weight,
gm.

215

P-P-17
I.
1.1

Sodium

Ash

Content

by

Flame

Emission

for

Prepregs

SCOPE
The procedure
materials
as
NOTE:

Care

samples

and

determines
applicable.
should

with

be

sodium

sodium

taken

by

and

not

to

touching

ash

content

contaminate

with

of

the

hands.

EQUIPMENT

2.1

Beakers

2.2

Analytical

2.3

Muffle

2.4

Desiccator

2.5

Circulating

2.6

Cermamic

2.7

250

2.8

ASTM

2.9

Concentrated

balance,

furnace,

ml.

above

air
or

platinum

600

16.6

Hot

2.11

Perkins-Elmer
and operators

gm.

15C

crucibles
flasks

ohm

resistivity

hydrochloric

2.10

0.0001

oven

volumetric

Type

sensitivity

acid

plate
atomic
manual

absorption

instrument

or

equivalent

PROCEDURE
Take
specimens
which
weigh
test
specimens
in individual
circulating
oven
at 225 _ _
one
hour.

approximately
3 grams.
Place
beakers
and dry
in an air
5 degrees
F. for a minimum
of

3.2

Remove
the
desiccator

3.3

weigh
approximately
2 grams
of each
cooled
specimen
the nearest
0.i mg. into
separate
tared
ceramic
or
platinum
crucibles
(Wl).

3.4

Heat
the crucibles
degrees
C. for 16
achieved.

specimens

from

the

in a muffle
to 18 hours

216

oven

and

furnace
or until

cool

in

to

at 600 + 15
constant
weight

is

3.5

Remove
place

the

ashed

specimens,

3.6

Wash
down
the walls
of each
crucible
and add
approximately
5 milliliters
hydrochloric
acid
to each.

with
(ml.)

distilled
water
concentrated

3.7

Bring
the acid
mixture
to a boil.
Cool
the crucibles.
Transfer
the contents
of each
to a 250 ml.
volumetric
flask
and dilute
to volume
with
distilled
water.

3.8

Determine
the
sodium
of each
flask
by flame
emission
at
589 nanometers
(nm.)
using
the
instrument
manufactures
operating
instructions
and a calibration
curve
for sodium
which
is linear
between
0.i
and 2.5 micrograms
per
milliliter.

3.9

The calibration
curve
is made
by measuring
the
absorbance
on a minimum
of 3 standard
solutions,
generally
in the 1
ppm to I0 ppm
liquid
range.
Either
plot
the absorbance
vs. ppm liquid
on graph
paper
or run a linear
regression
analysis.
The correlation
coefficient
should
be >.99 to
assure
linearity.
Using
the graph
or linear
fraction
obtain
the ppm of the liquid
sample
(part
3.8) by
inputting
the absorbance
of the sample.
(Note:
The
absorbance
of the sample
should
be bracketed
by the
standards).

4.

containing
and cool.

CALCULATIONS
ppm

4.1

the crucibles
in a desiccator

of

Sol.

Sample

% Ash

= W2/W

1 x

Report

the

results

= ppm

of

liq.

sample
Wl

dilution

100%
to

3 significant

217

figures.

ratio

P-P-18

i.

Compression,
Content
of
MOLDING

Volatile,

Dowel

Shear,

Material

1.2

Specification

1.3

I.

P.

Designation

REQUIREMENTS

2.2

Pre-cut

2'3

Staging:

2.4

Cure

temperature:

2.5

Cure

Pressure:

2.6

Cure

time:

120

2.7

Cool

under

pressure

one

laminate
i0"

3.

INSPECTION

3.1

Absence
surface

25

10"

warp

warp

marked

direction

minutes

and

250F

325F
1,000
+

15

x
i0"

I0"

fill

0.125"

direction.

5F.

10F.

50

psi

minutes.
before

removing

from

press.

REQUIREMENTS
of
blisters,
delamination,

voids,
cracks,
or contamination.

REQUIREMENTS

SPECIMEN

4.1

Mold
thick.

4.2

Mark

warp

4.3

Cure

temperature

4.4

Apply
contact
pressure
for
30 + 5
pressure
for
two
cycles
before-slowly
pressure.
Do not
prestage.

4.5

Maximum

4.6

Cure

laminate

RESIDUAL

1/4"

porosity,

1/4"

0.250

Mold

time:

120

under

325F

1,000
+

pressure

REQUIREMENTS
one

0.050"

direction

pressure,

SPECIMEN

uneven

VOLATILE

15

10F.

+__50

seconds,
and
applying

psi.

minutes

5.1

.025".

COMPRESSION

4.

5.

-4926

Number

Mold

Cool

Resin

STW5-3140

Card

SPECIMEN

Mx

2.1

4.7

and

PROCEDURE

1.1

Residual
prepregs

2"

diameter

before
by

removing.

DOWEL
2

1/2"

218

SHEAR
thick

billet.

dump
maximum

5.2

Use

5.3

Have

5.4

Staging:

5.5

Cure

temperature:

5.6

Hold

at

5.7

Cure

pressure:

5.8

Cure

time:

120

5,9

Cool

under

pressure

6.

approximately
all

180

plies
25

in

same

minutes

at

Cut
32
bars).

6.2

Staging:

15

6.3

Cure

50

10F.)

minutes.

1/2"

removing

RESIN
x

for

temperature:

(325F

psi.

before

5F.

5F.

10F.

1000
+

temperature

rectangles

255

250F

cure

REQUIREMENTS

6.1

direction.

325F

325F.,

SPECIMEN

plies.

5"

from

CONTENT
per

specimen

approximately

325F.

press.

(Pyrolysis

2-6

minutes.

10F.

6.4

Cure

pressure:

6.5

Cure

time:

6.6

Pull

Hot.

6.7

There
repeat

1,000
i0

should
with

be
a

50

psi.

minute

no

longer

resin

flash.

staging

219

If
time.

there

is

resin

flash,

P-P-19
i.
i.i

2.

Dowel

Shear

Strength

Fiber

This
method
reinforced
406, Method

Laminates

measures
the shear
strength
of
plastic
laminates
based
on Fed.
1041a.

fiber
Test

test

2.2

Shear

per

jig

machine
Fed.

Test

i0,000
Method

capacity.

ibs.
406,

Method

1041

PROCEDURE

3.1

Machine
diameter

the
by

specimen
to 0.375
1.125
inch minimum

3.2

Measure

the

diameter,

3.3

Place
double

3.4

Load

3.5

Record

the specimen
shear
jig,
the

machine

the

d.,

in
per
at

maximum

of

+ 0.000/
length.
the

test

the 0.375
inch
above
reference.

0.015
load

to

0.025

carried

-0.002

specimen,
diameter
Fig.

inch

by

inch

the

per

strength

= 2L
_--d 2
4

or

minute.

specimen,

L
= psi
2--A

Where:
L= maximum
load
carried,
d = diameter,
in.
A = cross
sectional
area,

ibs.
Pi

d2
4

Report

to

3 significant

digits.

220

in.
three
i.

CALCULATIONS
Shear

4.1

Method

EQUIPMENT
Universal

4.

Reinforced

SCOPE

2.1

3.

of

inches

L.

plate

l.U
_uJ

Z
CO
0
m
_J
I.,LJ
F-,CO
-I q"

f.D

,,,o t
...Jit I
nrr
rr-Uj_.I .---_
(.)l.lJ

C_
_ 4-1 1

co g/')

m._

,..1
0
n

|
I

ILlz
r- w

I
I

,_u.i
I.IJ1_..
Lue,7o

,--t

I1)

-,'-t

i
I

-T- -G'|
|

5_
""

_ mb
WZ
"rW

221

P-P-20
i.

Strength

of

Fiber

Reinforced

This method
measures
of fiber
reinforced

the compression
strength
plastic
laminations.

and

modulus

EQUIPMENT

2.1

Universal
operators

2.2

Double
machine
access

2.3

Strain
gages,
such
as Micro-Measures
equivalent,
with
amplification
to

3.

Laminates

SCOPE

1.1

Compression

test
machine
manual

of

I0,000

lb.

capacity,

cross
specimen
holders
per ASTM
D
L-shaped
ASTM
D 695. The holder(s)
to strain
gage(s)
when
modulus
is

the

and

695 mounted
will
allow
taken

on

CEA-00-062UW-120
load
chart

or

PROCEDURE
t

= 0.125

0.025

inches

w I = 0.75

0.020

inches

w 2 = 0.50

0.015

inches

3.13

0.030

s =

1.5

+ 0.030

r =

1.5

inches

3.1

t and w 2 are
micrometer.

3.2

The loading
all parallel
direction.

3.3

The sample
These
are
the inside
above

3.4

Environmen_ally
within
+ 5_F
minute
prior

inches
inches

measured

with

0.157

inches

radius

nose,
platen
and specimen
ends
to better
than
0.0010
in. per

is held
supported
through

ball-flat

(4 Planes)
1.0 in. in

are
any

between
two I shaped
pieces,
Figure
i.
with
finger
tight
nuts
and bolts
on
the sample
consistent
with
number
2

conditioned
for
i0 + 1 min
to wet tests.

222

specimens
prior
to

are held
dry
tests

and

2 _

3.5

The
precision
strength
is

of the
calculated

test
as

is better
pounds/in.

_han

1%.

The

P
= C = A

Strength

C
i0---00= ksi
and
is
digits.

usually
reported
The modulus
E

in

ksi

to

three

significant

A
E
1,000,000

and is usually
figures.

= Maximum

= Load
40%

load

taken
of

= Original

reported

(Ib)
from

in

= Msi

Msl

carried

the

to

by

three

the

stress-strain

typical

minimum

cross

significant

specimen.
curve

from

value.
sectional

223

area,

in 2.

20

to

U9
C4
0

0
o

0i

=
_- -I-I

O0
eqCD
(DO
(DO
4-I

d
cO +I

-+I

C_J

I
d_

.,-I

o
oi
..c:
r'|

E
o_

o
Q.
CO
.4.=='

c_

d_

d+i

224

P-P-21
1.
I.i

Resin

Content

of

Prepregs

Making

Use

of

Factor

"K"

SCOPE
This
method
is applicable
for
all carbon-reinforced
aldehyde-phenolic
compounds.
The
Fixed
Carbon
Content
Factor,
K, is determined
for each
individual
compound
and
is a function
of the amount
of carbonaceous
char
formed
under
these
controlled
conditions.
K is calculated
from
data
compiled
from
the pyrolysis
of samples
of the
molding
material
in which
the resin
solids
have
been
determined
gravimeterically
through
pyrolysis
then
they
can be correlated
with
the known
resin
solids
of the
specimens.
Example:

2.

Gravimetric
Wt.
Loss
by

Determination
Pyrolysis

34.0
6i-_?E.
504

Balance,

2.2

Lindberg
Model
_50035A
least
1500
+ 25UF.

2.3

Vacuum

2.4

Clamps

2.5

Vacuum

2.6

Manometer

2.7

Vacuum

2.8

Type

2.9

Vycor

3.

2.060

APPARATUS

2.1

2.10

34.0%
16.504

analytical,

precision
(or

not

more

equivalent)

than
Tube

0.0001
Furnace

gm.
at

Pump

Tubing,

Trap,
Drain

Rubber,

Dewar

Water

Type

Lines

Tube

Heavy

wall

Vacuum

Flasks

PROCEDURE

3.1

Wipe
air

specimens
30 minutes

3.2

Record

3.3

Place
tube

each

clean
using
acetone
and
minimum
before
testing.

specimen

weight

to

nearest

test
specimen
in vycor
tube,
place
furnace
and tightly
attach
tube
to

225

allow

0.0001

to

dry

gm.

in

(Wl).

tube
into
the
test
apparatus.

3.4

Start
vacuum
pump
and evacuate
system
to 3 inches
of
mercury
absolute
maximum.
Check
for
air leaks
by
clamping
off hose
to vacuum
pump
and noting
manometer,
leak
rate must
be less
than 0.20
inches
of mercury
per
minute.
Recheck
Joints
until
this
level
is achieved.

3.5

With
vacuum
on and pressure
stabilized
mercury
maximum,
place
the vycor
Tube
tube
furnace
at 1500 + 25F.

3.6

Continue
pyrolysis
for approximately
30 minutes
or until
manometer
or gauge
reading
is same
reading
as it was
before
pyrolysis,
whichever
is longer.

3.7

when
from
room

3.8

when
specimen
is cool,
turn
off vacuum
and carefully
let
air into
system.
When
pressure
equilibrium
is reached,
remove
specimen
from test
tube
and weigh
to nearest
0.0001
gm.
(W2).

4.

pyrolysis
is
furnace,
and
temperature.

complete,
cool under

at 3 inches
of
in the preheated

turn
off furnace,
remove
tube
vacuum
until
specimen
is at

CALCULATE
Calculate
Resin

resin

content,

content
percent

as

follows:

= W]

- W2 x
Wl

100

x K

Where:
W 2 = Weight
of specimen
after
pyrolysis,
W 1 = Weight
of specimen
before
pyrolysis,
K
= Fixed
carbon
content
factor,
to be
prepreg
manufacturer.

226

gm.
gm.
supplied

by

P-P-22

Specific

Gravity

and

Density

of

Prepregs

SCOPE
This method
covers
the determination
of the
specific
gravity
and density
of solid
plastics
by displacement
of
liquid
and determination
of the change
in weight
Based
on ASTM
D 792, Method
A.
2.

EQUIPMENT

2.1

Analytical

2.2

Sample

2.3

Alcohol,

wetting

2.4

Distilled

water

2.5

Copper

3.

balance

suspension

of

0.1

mg.

accuracy

device
agent,

or

equivalent

wire

PROCEDURE

3.1

Each
sample
of 1/2 to i 1/2
W I.
The precision
here
and
is 0.i mg.
The temperature

3.2

A piece
of thin,
approximately
0.01
in.,
copper
wire
is
weighed
with
as much
of it immersed
in the water
as will
be in 3.4.
If the specific
gravity
of the sample
is less
than
1 and,
if it floats,
a sinker
is weighed
with
the
wire.
This
weight
is W 3.

3.3

Pre-wet
the
and then
in

3.4

W 2 is
third

4.

sample
suspended
an intermediate

the weight
of the
bath
of distilled

by the
distilled

sample
water.

It is called
measurement

wire
in
water

completely

lab.
bath.

alcohol

immersed

in

CALCULATIONS
Specific
Density

4.1

gm.
is weighed.
in the
following
is 23 _ 2C.

gravity
m

0.9975

_ Wl/
x

(W 1

specific

The density
is the specific
times
the density
of water

(W 2

- W3))

gravity

above

gravity
at this

as measured
temperature.

227

(gm./cm3.)
above

P-P-23
1.
i.i

2.
2.1

Residual

volatile

Content

of

Molded

Articles

SCOPE
This
method
is used
to determine
the volatile
content
remaining
trapped
in a molded
article.
This
volatile
content
may consist
of entrapped
water
of condensation,
unreacted
phenol,
residual
solvent,
plasticizers,
or
volatile
mold
release
agents.
EQUIPMENT
Balance

accurate

to

0.001

gm.

Desiccator
Air
3.

circulating

oven,

Cut
a specimen
center
2" x 2"
specimen
clean

3.2

Place

the

specimen

3.3

Weigh

the

specimen,

3.4

Place
163 +

t e
5_C.

specimen

3.5

Remove
the
desiccator
temperature

4.

5C

at

least

PROCEDURE

3.1

3.6

163

Reweigh

the

1.000
+ 0.050"
by 1.000
+ 0.050"
from
the
section
of the test
panel.
Wipe
the
with MEK
and
air dry
20 minutes
minimum.
in

a desiccator

for

18

24

hours

hours

minimum.

(Wl).
in

the

oven

specimen
from
the
for approximately
is reached.
specimen,

for

oven
and cool
30 minutes
or

minimum,

in a
until

at

room

(W2).

CALCULATIONS"
percent

volatile

_ Wl

- W_
W1

100%

Where:
W 1 = initial
weight,
gm.
W 2 = final
weight,
gm.
5.
5.1

REPORT
Report
0.1%,

the
individual
and
as percent
residual

average
volatile.

228

results

to

the

nearest

P-P-24

i.
1.1

2.

Infra-Red
prepregs

of

Liquid

and

Solid

Resins

and

SCOPE
This
method
spectrum
of

is used
for determination
liquid
and solid
resins

or

of infrared
prepreg.

APPARATUS

2.1

Beckman
operators

2.2

Sodium

2.3

Solvent:
methylene

3.

Spectrum

4250,
Beckman
manual.
chloride

Acculab

or

equivalent

and

disk.

Spectrograde
chloride.

acetone,

THE

(Tetrahydrofuran)

or

PROCEDURE

3.1

Place
a small
amount
of material
to be tested
in a 50-ml.
beaker.
Add
about
15 ml. of spectroquality
acetone
and
stir
with
a glass
stirring
rod to dissolve.
If the
material
doesn't
dissolve
in acetone,
spectroquality
THF
or methylene
chloride
may be used.

3.2

Place
several
drops
of the
chloride
crystal
and allow
Zero

the

I.R.

beam

as

per

solution
on the
sodium
to dry
at room
temperature.
the

instrument

manual.

Mak?
a quick
scan of the region
from
2000
cm -1. to
cm -.
When
the transmittance
is between
15 and
25
percent
at most
intense
peak
the
right
concentration
on the crystal.
Twenty
percent
is the ideal
transmittance.
3.5

Start
the scan
at
the
infrared
from

3.6

Do

any

necessary

90%
2.5

transmittance.
to 16 microns.

calculations.

229

Scan

the

i000

sample

is

in

P-P-25

Residual

Volatile

Content

in

Molded

Articles

SCOPE
This
method
is used
to determine
the
volatile
content
remaining
trapped
in a molded
article.
This
volatile
consist
of entrapped
water
of condensation,
unreacted
phenol,
residual
solvent,
plasticizers,
volatile
mold
release
agents
or a combination
thereof.
2.
2.1

3.

TEST

SPECIMENS

The test
specimen
shall
consist
of a 1.000
+ 0.050"
x
1.000
+ .050"
x 0.125
+ 0.025".
Three
specTmens
shall
be
tested-for
each
determTnation.
Direct
comparison
of
values
between
samples
shall
not be made
unless
all
samples
so compared
do not
vary
by more
than
_ 10% from
a
nominal
given
thickness.
APPARATUS

3.1

Balance.
weighing

3.2

Oven.
A thermostatically
capable
of maintaining
C. shall
be used.

4.

may

An accurate
analytical
to the nearest
milligram

the

balance
shall

capable
be used.

of

controlled
air
circulating
test
temperature
within

oven
2

PROCEDURE

4.1

Conditioning
specimens.
Specimens
shall
be
in a desiccator
over
Silica
gel for
a period
prior
to weighing.

4.2

Initial
Weight.
After
the specimens
have
been
conditioned
they
shall
be individually
weighed
on an
analytical
balance
to the nearest
milligram.
This
weight
is to be designated
as W I.

4.3

Devolatillzation.
After
the specimens
have
been
weighed
they shall
be placed
in an air circulating
oven
maintained
at 163 + 2 C. for a period
of 4 hours
+ 5
min.
After
this
Time
the
specimens
shall
be removed
and
placed
in a desiccator
over
silica
gel
and allowed
to
cool to ambient
temperature.
After
reaching
ambient
temperature
the
specimens
shall
be re-weighed
to the
nearest
milligram
and this
weight
designated
as W 2.

230

conditioned
of 18 hours

CALCULATIONS
Percent

Weight

Loss

The
volatile
shall
be expressed
loss
as compared
to the original

as a percentage
specimen
weight

Percent

weight

loss

W]

- W_
wI

weight
(Wl).

i00

where:
w I = the
w 2 = the
5.2

The
and

initial
weight
of the test
specimen,
final
weight
of the test
specimen,

gm.
gm.

values
obtained
for three
specimens
shall
be averaged
reported
as weight
loss
for the sample
tested.

231

P-P-26
i.

Thermogravimetric

Analysis

2.

MATERIAL

3.

EQUIPMENT

Test

Methods

Method
by:
Analysis

CCA-3

Fabric

(512C.

Test)

Setting

3.1

Heater
Control:
Zero
- + 20
Range
- + i0
TGS
- 2

3.2

Auto
Balance:
Power
- on
Filter
- Lo
Tare
- Pointer
at the
Recorder
Range
- I00
Recorder
Mode
- Short

Load

middle

of

green

line

Recorder:
Pen 2 - (Zero
pen by holding
zero
switch
down;
adjusting
knob until
pen is "0" on the right
hand
of the chart)
Range
- 1 volt
Power
- Servo
Pen
i (Zero
by following
instruction
of pen
2)
Range
- 1 my.
Polarity
- (-)
Chart
Speed
- 5 mm./min.

3.4

Differential
Scanning
Calorimeter:
Power
- On
Lower
- Unit
- 100C
Upper
Limi
- 512 + 10C
Cooling
Range
- 16_C/min.
Heating
Rate
- 160VC/min.

3.5

Air

3.6

Operators

4.

Chemical

SCOPE
Chemical
Test
Thermogravimetric

3.3

(a)

TEST

flow

rate

- 80

ml./min.

(Zero

gas

side

air)

manuals.

METHOD

4.1

Cut

three

4.2

Disengage
pressure

4.3

Loosen

samples
spring

screw,

then

1/4"
latch

lower

x
of

1/4"

of

fabric

balance

cover

down

232

furnace

to

release

gas

4.4

Swing

loading

platform

4.5

Place

samples

on

4.6

Raise
latch
that
until
Turn

underneath

platinum

pan

furnace
carefully,
tighten
screw,
(Note:
Bubbles
should
appear
on
is
immersed
in water;
if
not,
turn
bubbles
heater

come

out)

control

to

heat

and

Make
mark
on
chart
by lowering
manually
and
raising
pen
again
small
division,
this
will
give

and
engage
spring
the
outlet-tubing
balance
cover

recorder

mode

Turn

4.10

Adjust
chart

Pen-1
until
it reads
I00
on
the
by
turning
the
"% adjust
knob"

4.11

Lower
on DSC

both

4.12

Pen-2

should

adjust
upper
is attained
4.13

When

Pen-2

4.14

Push

"cool"

power
,

5.1

mode

pens,

to

power

level

off

reaches

at

after
and

chart,

heat

20

mark,
until

start
minutes,

recorder

left

push

512-514C.

push

512-514C,

button

knob-servo,

Mg

sample

knob

limit
and
on chart

to

Pen-I
and
advancing
chart
(reading
will
be
1 mg
per
the
weight
of
sample).

4.9

recorder

pan

hand

of

"heat"

button

otherwise

512-514C.

timer
raise

for
both

mark

20

minutes
pens,

mode-short

CALCULATIONS
Read
% loss
directly
on chart)
using
Pen-i
Note:

Lower
150C.

from

furnace
only
or
less.

chart

when

233

(1%

loss/small

temperature

division

drops

to

P-P-27
i.

Thermogravimetric

(b)

SCOPE
Chemical
Test
Thermogravimetric

2.

MATERIAL

3.

EQUIPMENT-Setting

Method
By:
Analysis

CCA-3

3.1

Heater
Control:
Zero
- + 20
Range
- + i0
TGS - 2

3.2

Auto
Balance:
Power
- On
Filter
- Lo
Tare
- Pointer
Recorder
Range
Recorder
Mode

3.3

Analysis

Fabric

(1000C.

Test)

Load

at the
- i00
- Short

middle

of

green

line

Recorder:
Pen 2 (Zero
pen by holding
zero switch
down;
knob until
pen is "0" on right
hand
side
of
Range
i volt
Polarity
(-)
Pen 1 (Zero
by following
Range
No mv.
Polarity
(-)
Chart
Speed
5mm./min.

instruction

3.4

Differential
Scanning
Calorimeter:
Power
On
Lower
Unit
i000_.
Upper
Limit
1000_C.
Cooling
Range
40C
/min.
Heating
Range
20C
/min.

3.5

Air

3.6

Operators

4.

TEST

flow

rate

80

ml./min.

(zero

of

gas

Pen

adjusting
chart)

2)

air)

manuals.

METHOD

4.1

Cut

three

4.2

Disengage
pressure.

4.3

Loosen

samples
spring

screw,

then

of

fabric

latch

of

lower

1/4"
balance

down

234

1/4".
cover

furnace.

to

release

gas

4.4

Swing

loading

platform

underneath

Place

samples

on

Raise
spring

furnace
latch.

carefully,

control

tighten

Turn

to

4.8

Make mark
on chart
by lowering
manually
and raising
pen
again
small
division,
this
will
give

4,9

Turn

mode

to

heat

Adjust
chart

4.11

Lower
both
on
DSC.

4.12

Pen-2
should
upper
limit
on chart.

level
off at
and push
heat

4.13

Push
pens,

button
after
knob
servo,

5.1

and

recorder

"cool"
power

engage

power

mode

to

that

is

Mg.

Pen-1
and
advancing
chart
(reading
will
be 1 mg per
the weight
of sample).

Pen-i
until
it reads
i00 on the
by turning
the
"% adjust
knob".
pens,

and

sample.

4.10

screw,

appear
on the outlet-tubing
not,
turn
balance
cover
until

4.7

recorder

pan.

pan.

NOTE:
Bubbles
should
immersed
in water
if
bubbles
come
out.
heater

platinum

knob-

chart,

push

1000C.
mark,
until
1000C.

1000C.
is
and recorder

left

hand

"heat"

of

the

button

otherwise
mark
is

adjust
attained

reached,
raise
mode-short.

both

CALCULATIONS
Read % loss directly
on chart
using
Pen-i

from

chart

NOT_:
150_C.

only

when

Lower
furnace
or less.

235

(1%

loss/small

temperature

drops

division

to

P-P-28
i.
I.i

Thermogravimetric

Analysis

SCOPE
This
procedure
thermogravlmetric
EQUIPMENT

describes
analysis

AND

the
of

Perkin-Elmer

Model

TGS-2

2.2

Perkln-Elmer

DSC-2

Programer,

2.3

Appropriate

operators

Thermoanalyzer

Obtain

4.

PROCEDURE

4.1

Balance

small

(i

oz.)

equivalent

representative

4.1.2

Filter

4.1.3

Recorder
operators

Mode
manual)

4.1.4

Recorder

Range

4.1.5

Weight

Suppression

switch

4.1.6

Weight

Suppression

thumb

Use

on
-

DSC-2

io

as

short

the

TG

4.2.1

Sample

4.2.2

Temperature

RANGE

4.2.3

Temperature

ZERO

4.2.4

Lower

4.2.5

Cooling
Heater

sample

Controls

Power

4.3.1

equivalent

manuals.

4.1.1

4.3

or

or

SAMPLING

3.1

4.2

for
conducting
and
prepregs.

MATERIALS

2.1

3.

method
resins

holders

LIMIT

sec.

7DI,6

and

7D2,1

in

mg.
-

i00

steel

mg.
dial

00.000

Programmer

empty

RATE
Control

ZERO
and
procedure
9235)

i0

(see

RANGE
(or

Calibration
Calibration

350K.
-

(or

as

as
as

calibrated
calibrated

required)

160/min.

Unit
Setting
as indicated

as

236

determined
on
calibration

from

calibration
card
993-

4.3.2

Power

4.3.3

C.

4.4

HEAT

OK.

switch

(on

back

panel)

K.

Recorder

4.4.1

CHART
chart

4.4.2

Weight

4.4.3

Second
zero;

SPEED
speed
Pen:
Pen:
or FDC:

slow
when
RANGE

(e.g.,
5
temperature
-

20

Thermocouple:
RANGE
-

mm/min.)
change
is started

mv.;

i0

237

right-hand

RANGE
- 1
my.,
left-hand

to

faster

zero
volt,
right-hand
zero

P-P-29

Resin

Content

by

Means

of

Pyrolysis

of

Prepregs

SCOPE
Resin

1.1

content

shall

be

determined

in

accordance

with

the

following.
2.

PROCEDURE
Prepare

test

Cut
32
prepreg
2.1.2

Stage

specimens

rectangles
sample.
the

32

as
(1/2

follows:
inch

rectangles

at

by

inches

255

5F.

Note:
Staging
time
is dependent
and flow
and must
be determined

nominal)

from

reduce

flow.

to

on the
resin
system
from
experience.

2.1.3

Using
the
32 rectangles,
inch by 5 inches.

2.1.4

Cure
the specimen
at 325 + 10F.and
i0 + 1 minutes.
If any resin
flashes,
longer
staging
time.

I000
+
repeat

2.1.5

Cut the bar

into
approximately
form
three
test
specimens.

equal

mold

bar

1/2

three

1/2

i0 psi.
for
and use

lengths

2.3

Record

2.4

Place
the test
tightly
attach

2.5

Start
the vacuum
pump
and evacuate
the
system
to i0 + 5
mm.
of mercury
(Hg) absolute.
Check
for
air leaks
by
clamping
off the hose
to the vacuum
pump
and noting
the
manometer
The
leak
rate must
be less
than
five
millimeters
(mm.)
(0.02
in.)
per minute.
Recheck
joints
until
this
level
is achieved.

2.6

with
the vacuum
on and the pressure
stabilized
at i0
mm. Hg, place
the Fisher
burner
under
the
specimen.
Adjust
the
flame
area
to cover
the sample
completely,
in Fig.
i.
NOTE:
A tube
used
in place

to

specimen
the tube

furnace
of the

the

in
to

the
the

nearest
vycor
test

maintained
at
Fisher
burners.

238

ketone
before

to

wipe
the specimen
and allow
to air
testing.

weight

ethyl
minimum

by

2.2

specimen

clean
using
methyl
dry
for 20 minutes

inch

0.001

gram

test
tube
apparatus.

1500

(MEK)

(W).
and

25F.may

5
as

be

2.7

Continue
pyrolysis
for
the manometer
or gauge
was
prior
to pyrolysis,
NOTE:
If
the Fisher
complete.

residue
burners

approximately
30 minutes
or
reading
is the same
reading
whichever
is longer.

collects
in
under
those

until
as it

the vycor
test
tube,
place
areas
until
the
burnout
is

2.8

when
under
vycor

2.9

when
the Specimen
is cool,
turn
off vacuum
and
carefully
let
air into the
system.
When
pressure
equilibrium
is
reached,
remove
specimen
from
test
tube
and weigh
to the
nearest
0.001
gram
(WI).

2.10

pyrolysis
is complete,
vacuum
until
specimen
test
tube
Just
under

Calculate

dry

Dry

content,

resin

resin

turn
off burners
and cool
is at room
temperature
(touch
test
specimen
very
carefully).

content
%

as

(i.00

follows:

- WI/W)100(K

Where:
W 1 = weight
of specimen
after
pyrolysis,
W
= weight
of the specimen
prior
to
pyrolysls,gm.
K
= a constant
as shown
below

gm.

K Factors
U.

S.

Polymeric

FM

Fiberite

5055

2.008
Note:

These

2.11

Report

the

2.12

Limits

(percent

Minimum
Maximum

30.0
38.5

4926

2.060

constants
dry

MX

resin
dry

are

unique

content
resin

to

content

239

for
the
by

each

nearest
weight)

material.
0.I

percent.

W
(D
D

0
CO

O2
W
O9
Z
W

240

P-P-30
i.

Tack

Temperature

of

Prepregs

by

Lap

Shear

SCOPE

i.i

Scope.
This
method
describes
a procedure
establishing
the minimum
tack
temperature
materials
by lap shear
where
the specimen
under
a specified
pressure
while
heating.
does
not
give
a shear
strength.

1.2

Purpose.
blocking

2.

The
purpose
temperature

EQUIPMENT

2.1

AND

Asbestos

2.1.2

Hot

MATERIALS

block,

Press

device,
watch

2.1.6

Weight,

15

3"

variable

Metal

Stop

2.2

laminates,

plate,

2.1.5

2"

lbs.

3"

temperature
2"

capable

and/or

1/4",
of

weight

applying

electric
(or

control

other

125
50

5 grams.

2 ibs.

of

force

timer
specified

weight)

Materials.

2.2.1

Cellophane
SAMPLING

3.1

4.

is to confirm
material.

Equipment.

2.1.1

3.

of this
method
of pattern
grade

for
of prepreg
overlap
is
This
method

The
sample
should
be large
enough
to provide
a sufficient
number
of i" x 3" specimens
to determine
minimum
tack
temperatur_
.
Unless
otherwise
specified,
specimens
shall
be cut
so as to optimize
sample
size
and shall
be
in either
the warp
or fill
direction.
PROCEDURE

4.1

Preparation

of

test

specimen.

4.1 .i

Preconditioning
hot plate.
Unless
otherwise
specified,
preheat
the hot plate
to the
specified
temperature
(+3F.).
Place
the
2" x 2" x 1/4"
block
and the
15pound
(or other
specified)
weight
on the hot plate
during
this
preheat
time.

4.1.2

Heating
form
a
side.

test
specimen.
Take
two
i" x 3" specimens
and
one-inch
overlap,
placing
warp
side
to fill
Place
between
a fold
of cellophane.
Place
the
241

cellophane-wrapped
specimen
on the hot
plate,
place
the
2" x 2" x 1/4" metal
block
on the overlap,
and place
the
15 pound
(or other
specified)
weight
on the
2" x 2"
x 1/4"
metal
block.
Allow
the specimen
to heat
for
30
+ 2 seconds.
Remove
the weight
and metal
block
and
take
specimen
from the hot plate.
4.1.3

Specimen
bonded,
specimen

4.1.4

Specimen
is bonded.
As quickly
and
delicately
as
possible,
(5 seconds
maximum),
place
the
overlapped
area
between
the platens
of a room
temperature
press.
The platens
of the press
shall
be covered
with
asbestos
laminates
which
are covered
with
cellophane.
Unless
otherwise
specified,
apply
50 + 2 ibs.
until
the
specimen
is cool
(about
1 to 2-minutes).

4.2

does
not bond.
If the specimen
has not
confirm
this condition
with
an additional
before
changing
temperature.

Testing
specimen.
Clamp
one end of the specimen
in jaws
of spring
load
dial
scale.
Load
other
end
of the
specimen
at a
constant
rate
thus
forming
a lap
shear
test.
Continue
loading
until
shear
or break
occurs.
Minimum

tack

temperature.

Specimen
supports
weight.
measurable
load
(see 6.1),
(usually
at 10F.
intervals)
support
a measurable
load.
4.3.2

5.1

If the specimen
supports
a
decrease
temperature
until
specimen
will
not

Specimen
does
not
support
weight.
If the specimen
does
not
support
a measurable
load,
continue
testing,
increasing
the hot plate
temperature
(usually
at 10F.
intervals)
until
the specimen
will
support
a measurable
load.
Report
load
in pounds.
Test
two
additional
specimens
at this
temperature.
CALCULATIONS

AND

REPORTING

Reporting.

5.1.1

Report
minimum

5.1.2

Report
the
measurable
temperature
specimens.

the
average
load
tack
temperature.

in

pounds

minimum
tack
temperature
load
is supported.
The
must
be established
by

NOTES:
A measurable
load
for
shall
not
be less
than three
load
shall
be three
pounds.

242

of

three

specimens

at which
a
minimum
tack
a minimum
of

three

the purpose
of this
test
pounds.
The measurable

at

P-P-31
i.

Wet

and

Dry

Flow

by

or

This
is a method
for the determination
flash
removal
or punched
disc.
Both
as is) and dry
(devolatilized)
flows

2.

EQUIPMENT

2.1

AND

Punched

Disc

of flow
by either
wet
(prepreg
tested
are
incorporated.

MATERIALS

Equipment.

2.1.1

Laboratory

press,

2.1.2

Analytical

balance,

2.1.3

Caul
plates,
(optional)

2.1.4

Steel

2.1.5

Laboratory

2.1.6

Punch

2.1.7

Calipers,

2.2

hydraulic,
0.0001

stainless

templates,

2"

500
gm.

and

5 psi,

350

5F

sensitivity

steel,

2"

1/16"

4"

thick,

6"

x 6"

4"

knife

press

with

cutting

graduated

in

die,
0.01

2.500"

diameter

inch

Materials.

2.2.1

Release
teflon,

2.2.2

TX - 1040
equivalent

2.2.3

Mochburg
Seattle,

3.1

Removal

SCOPE

i.i

3.

Flash

films,
coated
light

Fabric,
Wash.)

cellophane,
fabric.
weight

mylar,

teflon

Grade
CW-1850
or equivalent.

aluminum

coated

(West

foil,

glass

fabric,

Coast

Paper

or

Co.,

SAMPLING
Sample
size.
The
sample
shall
be large
enough
so that
the required
number
of 4" x 4" plies
may
be cut.
Unless
otherwise
specified,
cut
specimens
on the bias.
The
total
specimen
weight
should
be 25 to 30 grams,
except
in
the case
of the high modulus
graphite
tape.
The
following
table
will
serve
as a guide
in determining
the
number
of plies
per
specimen:

243

MATERIAL
GLASS

NUMBER

OF

108
120
128
143
341
181
182
183
184

16
10
8
6
6
6
4
3
3
NUMBER

MATERIAL

OF

Asbestos
Carbon

Number
each

PLIES

i0
4

Graphite
High
Modulus
(tape)
3.2

PLIES

(TYPE)

4
3

Graphite

of

determinations.

sample,

unless

Conduct

ot_'erwise

one

determination,

on

specified.

PROCEDURE
Temperature
and
pressure
has
unique
flow
properties
temperatures
and
pressures
otherwise
specified,
use
and
temperatures:
RESIN

for
resin
types
Each
resin
type
which
must
be tested
at
peculiar
to
that
type.
Unless
the
following
standard
pressures

TYPE

PRESSURE,

Phenolics
Press
Grade
Vacuum
Grade
All
Other
Epoxies

Unidirectional
Vacuum
Grade
All
Other

Tape

Polyesters
Press
Grade
Vacuum
Grade
Silicones
Other
Resins

325
325
325

15
15
50

325
275
275

50
15
50

275
275
350

200

244

TEMP,F.

500
15
150

Must
be
designated

All
resin
system
being
utilized
with
the
high
modulus
graphite
tapes

psi

specifically

300

NOTE:
Pressure
for epoxy
systems.
Use caution
in
selecting
pressure
and temperature
for epoxy
systems
as
wide
variety
of applications
require
varied
conditions.
4.1.1

Tolerances:

4.1.1

Pressure
maximum

4.1.2

Temperature

4.2

shall
have
of + 5 psi.
shall

Lay-up
for tapes.
be used
for tapes:

4.2.1
4.2.1.1

4.2.2

4.2.2.1

Lay-up

for

have
The

of

a tolerance
following

5%

of

lay-up

but

with

5F.

procedure

shall

tapes.

Using
strips
about
4" long,
lay up four
(4) plies
at
least
4" square.
Lay up the plies
so that
the strips
of each
successive
ply are orientated
90 _ to the
strips
in the preceding
ply.
Cut
flow
specimens
using
4" x 4" template.
Do not
cut specimens
on the
bias
unless
so designated.
Unidirectional
graphite.
Cut

enough

i0".
Lay
successive
ply.

tapes

strips

Using
Weigh

4.2.2.3

Sandwich
the 4-ply
of 181 glass
fabric
cellophane
release
High

a 4"
each

modulus

other

to

make

than

up

the

four

high

(4)

modulus

plies

up the plies
so that
tee fibers
ply are orientated
90
to the

4.2.2.2

4.2.3

a tolerance

i0"

of each
preceding

x 4" template,
cut specimen
on the
specimen
to the nearest
0.01
gm.

graphite

specimen
with
on each
side
film.
Proceed
unidirectional

two
and
to

bias.

(2) 6" x 6"plies

place
between
4.3.2.

tapes.

4.2.3.1

Cut
three
plies,
4" x 4" evenly
spaced
across
the
width
of the material
and orient
them
0o, 90o,
0o.
Weigh
the layup
to the nearest
0.01
gm.

4.2.3.2

Sandwich
the specimen
with
one 6" x 6" ply of TX-1040
release
fabric,
followed
by two
(2) 6" x 6" plies
of
Mochburg
bleeder
fabric
(each
side).
Place
the
entire
layup
between
cellophane
or teflon
release
film.
Proceed
to 4.3.2.

4.3

Pressing

Specimens

245

4.3.1

If wet
flow
is to be determined,
weigh
the proper
number
of specimens
to 0.01 gm. or as specified.
This
weight
is not necessary
if dry flow
is all that
is
desired.
NOTE:
Weighing.
to 0.001
gm.
In
weigh
to nearest

4.3.2

Properly
Position
specified
pressure

If greater
general,
if
0.0001
gm.

accuracy
the flow

is
is

desired,
weigh
5% or less,

align
the specimens
between
release
film.
in the center
of a press,
reconditioned
to
temperature,
and close
to the specified
as rapidly
as possible.

NOTE:
Caul
used
unless

plates.
Caul
plates
will
specifically
designated.

not

normally

the

be

4.3.3

The time
otherwise

4.3.4

Release
pressure
at end of time
interval
and
immediately
remove
the release
films
if used.
If dry
flow
is to be determined,
use care
in removing
the
release
films
so that
none
of the flash
is lost.

4.4

Weighing

in the press
3_i minutes

the

flash

shall
be i0 minutes
minimum
greater
than
the gel time.

removal.

4.4.1

If dry
flow
is to be determined,
weigh
with
flash
to 0.01
gm. or as specified.

4.4.2

Scrape
off
dull
knife,
reinforcement

4.4.3

Reweigh

4.5

Punched
proceed

laminate

to

disc.
If punched
as follows:

0.01

gm.

or

disc

flow

Use a punch
press
to remove
a 2 1/2
from
the center
of the laminate.

4.5.2

Weigh
0.01

5.1
5.1.1

the disc
inch.

CALCULATIONS

AND

Calculations.
Flow

by

to

0.001

laminate

and

inch

measure

flow

removal.

248

as

follows:

specified.

to

REPORTING
Calculate

flash

gm.

as

is

4.5.1

5.

the

the flash
down
to the original
size
with
being
careful
to avoid
removing
any
from
original
dimensions.

the

but

be

determined,

diameter

the

diameter

disc

to

5.1.i.1

Wet

flow.

Flow,

Calculate

Wt.

= W]

wet
- W_
W1

flow

as

follows:

100

where:
w I _ Original
weight,
gm.
W 2 = Weight
of laminate
after
pressing
before
flash
removal,
gm.
w 3 = Weight
after
flash
removal,
gm.
5.1.1.2

Dry

Flow.

Calculate

dry

Flow,

where
Flow

by

Wet

symbols

are

punched

disc.

flow.

Flow,

Wt.

W]
=

Wt.%

as

Calculate

flow
W_

specified

wet

flow

- RW 4 x
W1

as

follows:

- W_
W2
in

as

but

x 100

5.1.i.1

follows:

100

where:
W 1 = Original
weight,
gm.
W 4 = Weight
of 2.50
inch
disc,
R
_ Ratio
of area
of 4" x 4"
of 2.50 inch
disc

gm.
laminate

to

area

NOTE:
Punched
disc
flow.
Some
specifications
require
flow
ito be calculated
using
dry weight
in the
denominators.
This
is not
a standard
calculation
and
cannot
be defined
as a wet or dry
flow;
however,
the
calculation
is given
below
for reference:
Flow

NOTE:
5.2

Place

6.4

= W 1 - RW 4
RW 4
here,

but

i00

without

the

number.

Reporting.
Unless
otherwise
specified,
report
flow
to
three
significant
figures.
Test
results
should
be
considered
suspect
if the range
for triplicate
determinations
exceeds
2.5%
for flows
greater
than
10%.
For lower
flows,
tested
at 150 psi or greater,
the
range
of triplicate
flows
should
not
exceed
1.5%.

247

P-P-32
i.

Viscosity

- RDS

for

Prepregs,

by

Parallel

Disc

SCOPE

i.i

Prepreg

1.1.2

Run

Viscosity
Parameters

by

Parallel

(Operators

Temperature

1.1.2.2

Rate

1.1.2.3

% Strain
= 10% strain
for starting
temperature
to 70_C.
50% strain
for starting
temperature
excess
of 70C.

1.1.2.4

i0

Mode:

Cure

_otal
Time
C/min.
Time/test
1.1.2.5

Test:
50mm.

1.1.2.6

Geometry:

be

as

manual)

1.1.2.1

to

Plate

specified

in

Spec.

of

QPL

rad./sec
30C.
in

Sweep
140 minutes
2.0C
minutes
2.0 minutes/Test

Parallel
Plate:
25mm.
for
for epoxy/polyimides/phenolic

aldehyde-phenolic,

Gapsee below
Radius
- see 1.1.2.5

Gap
setting
must
be made
after
thermal
equilibration
of material
and plates.
After
equilibration,
set
force
normal
to 50% full
scale
and
read gap setting.
Use
50% force
nominal
gap
setting
for all
calculations.
1.1.2.7

Plot
X

Epoxy/Polyimide

axis

min.
max.

0
140

0
280

Y =

axis

min.
max.

IEO
IE5

IE2
1E7

Print:
n*, n I, n,
Paper:
Rheometerics
K&E Paper
1.2
1.2.1

Phenolic

Sample

time,
temperature,
rate
5 cycle
x 7 inch
Semi-log

#4662-10

Insertion

Set desired
temperature,
place
lower
parallel
plate
and return
machine.
Set oven
temperature
to allow
the prepreg
sample
to
as in 1.1.2.6.

248

prepreg
specimen
on
assembly
to test
to about
70C.
in order
become
pliable.
Set gap

1.3

Testing

Initiate

Shut

down

test

by

the

following

See
1.i.2.3
Cure
Mode
Parallel
Plate
See
1.1.2.3
i0 rad./sec.

Temperature:
Mode:
Test:
% Strain:
Rate:
Start
1.4

the

after

test:

Press
reset
Remove
plates
and clean
Shut
down
power
to heat

in acetone
and torque

249

motor

sequence:

F-I
i.
i.i

Density

of

Cured

Material

SCOPE
The density
accordance

of the cured
material
with
the following.

shall

be

determined

in

PROCEDURE
2.1

Cut sufficient
plies
to produce
a test
panel
0.125
+ 0.025
by 4 inches
(minimum)
by 5 inches
(minimum),
mark
the warp
direction
and cure
panel
as
specified,
when
testing
tape
widths
which
are 4.0
inches
or less
prepare
a test
panel
whose
width
is equal
to that
of the tape.
The
outer
0.i00
inch
of the panel
shall
not
be used
for preparation
of the specimens.

2.2

Cut
a specimen
1-inch
by 1-inch
by panel
thickness
at
random
from the test
panel.
Wipe
the specimen
clean
using
methyl
ethyl
ketone
(MEK)
and allow
to air dry
20
minutes,
minimum,
before
testing.

2.3

Weigh
and
record
nearest
0.I mg.

2.4

Weigh
the specimen
in
weight
to the nearest
required
(W2).

NOTE:
water
water.
2.5

Weigh
if it

Calculate
Density

the weight
(Wl).

of

the

(gm./cc.)

using
=

in

air

to

water
at 73 + 3 OF.
and record
0.i mg. using
a wire
and sinker

specimen
in a suitable
is affected
by water
or

density

specimen

water

as

the

the
if

liquid
other
than
is lighter
than

follows:

0.9975
W]
(W l + W 3 - W2)

Where:
W 1 = weight
of specimen
in air,
gm.
w 2 = weight
of specimen,
wire
and sinker
suspended
in water,
gm.
w 3 - weight
of wire
and sinker
suspended
in water
the same depth
as in the W2 determination
to
the nearest
0.i mg.
2.6

Calculate

density

using
0.9975

Density

(gm./cc.)

other

liquids

W 1 S

=
(W 1 + W 3

250

- W2)

as

follows:

to

where:

Report
Limits
Minimum
Maximum

w I
W 2

=
=

W 3

the

weight
of
specimen
in air,
gm.
weight
of
specimen
and
wire
suspended
liquid,
gm.
weight
of wire
suspended
in the
liquid
same
depth
as
in the
W 2 determination,
predetermined
specific
gravity
of
the
73 + 3 _F.
density

to

the

nearest

(gm./cc)
1.40
1.52

251

0.01

gm./cc.

in

the

to the
gm.
liquid

at

F-2
i.
i.I

Residual

Volatile

Content

of

Cured

Material

SCOPE
The
residual
be determined

volatile
content
of
in accordance
with

the
the

cured
material
following:

shall

PROCEDURE
Cut
sufficient
plies
to produce
0.050
thickness
by 4 + 0.125
by
the panel
as specifie_
with
the

a test
panel
0.250
+
4 + 0.125
inches.
Cure
foTlowing
exceptions.

2.2

Apply
contact
pressure
for 30 + 5 seconds
and dump
pressure
for
2 cycles
before
slowly
applying
maximum
pressure.
(The material
shall
not be prestaged.)

2.3

When
testing
tape widths
which
are 4.0 inches
or less,
prepare
a test
panel
whose
width
is equal
to that
of the
tape.
The outer
0.i00
inch of the panel
shall
not be
used
for preparation
of the specimens.

2.4

Cut a specimen
1.000
+ 0.050
inch
by 1.000
+ 0.050
inch
by panel
thickness
from the center
2 inch
by 2 inch
section
of the test
panel.
Top and bottom
molded
surfaces
shall
not be machined.
Wipe
the specimen
clean
using
MEK
and allow
to air dry
20 minutes
minimum
before
testing.

2.5

Place
hours

the specimen
minimum.

in

a desiccator

2.6

Weigh
W 1

the

to

the

2.7

Place
the specimen
and stabilized
at
minutes;
condition
i0 F.for
24 hours

specimen

and

nearest

0.01

desiccate

gram

in an ai_ circulating
oven,
325 + i0 _F.for
approximately
the-specimen
at a temperature
minimum.

2.8

Remove
the
specimen
from the oven
and cool
desiccator
for approximately
30 minutes
or
specimen
reaches
room temperature.

2.9

Reweigh
w 2

2.10

Calculate
Percent

the

specimen

the

to

percent

volatiles

and

= W]

the

nearest

residual
- W2
W1

252

0.01

volatiles
(I00)

for

18

record

preheated
30
of 325

as

in the
until
the

gram.

as

Record

follows:

as

Where:
W1 W2 =

original
weight
of specimen
in grams
devolatilized
weight
of specimen
in

2.11

Report

residual

voaltiles

to

the

2.12

Limits

(percent

volatiles

by

weight)

Minimum
Maximum

2.5

253

nearest

0.01

grams
percent.

F-3
i.
i.i

2.

Compressive

Strength

of

Cured

Material

The compressive
accordance
with

strength
shall
the following:

be

determined

Prepregs

in

PROCEDURE
Cut
sufficient
plies
to produce
0.025
by 4 inches
(minimum)
by
mark
the warp
direction.
(All
direction.)

2.2

Cure
the plies
into
a panel
between
smooth
caul
plates
as follows:

2.2.1

Orient
aligned

2.2.2

Place
the
i0 degrees

2.2.3

Increase
allowing
edges.

the
the

Hold

pressure

The
not
Machine

a test panel
0.125
+
5 inches
(minimum)
and
pieces
aligned
in same

separator

film

on

plies
such
that warp
fibers
of each
ply
are
in the same
direction.
Mark
warp
direction.

the

Decrease

stack
F.

the

of

plies

pressure
resin
to

and

into

slowly
stage

and

outer
1/2 inch
of the
be used
for preparation
to

preset

to i000 +
to minimi[e

temperature

temperature

a specimen

a press

for

pressure

edges
of

at

325

50 psi.,
flash
at

120
to

15

ply

minutes.

ambient.

of the test
specimens.

theAdimensions"

Measure
the width
and thickness
of the
nearest
0.001
inch
in the gauge
section
and
record
the cross-section
area.
2.5

from

SCOPE

2.1

2.2.6

Made

panel

shall

--

specimen
to the
area.
Calculate

Place
the specimen
in the support
jig
(Figure
i),
centered
so the ends project
an even
amount
beyond
ends
of the Jig.
Tighten
finger
tight
only.

both

2.6

Place
the specimen
and the support
jig
in the testing
machine
and align
so that
the specimen
ends
are parallel
with
the surface
of the compression
tool.
Adjust
the
crosshead
of the testing
machine
until
it just
contacts
the top of the specimen.

2.7

Set
the speed
control
0.050
in./minute
and

at a cross
head
indicated
start
the machine.

254

rate

of

2.8

Record
the
the test.

2.9

Calculate
maximum

maximum

load

by

the

Report

compressive

2.11

Limits

(psi.)

strength

to

the

nearest

Warp
Direction
25,000
65,000

Minimum
Maximum
NOTES

specimen

during

the compressive
strength
by dividing
the
load
by the original
cross-section
area.

2.10

2.12

carried

FOR

FIG.

Note

1 - Cold

Note

Note

3 - Grind

i0

psi.

Fill
Direction
20,000
55,000

2
rolled

steel

- Furnished
four
steel
round
bead,
slotted,
surface

denoted

255

machine
length
"Gr"

screws
and
1-1/4
in.

nuts,

o
in

u')
0.0156

.,<.I

,"_t
I
i

,I

'1'

I _.

0.9375

t
I
I

c;,

I
_ I
r

p- 0.43,5-_1
i_ i,,
0.1675
I
I

I
II

II

I
i

II

ii
I!
'I

:,

I I

0. 500

I I

i l

Iii

Ii
I

I
I
I

II

II

II

:J

I
!

io

I!

Gr

I!

I
!
I

i!

2.000

I
I
I
I
I
,t
iI

I
I
i,

II

I,
il

il

I I

Iii

Ii
II
II

I I
ii
I

,_hi
li":'"
I

I I
i, I
I
I

I,
ii ,
iI
Ii
II
tl

II
i I

I
I

tl

I|

I I

'

|1

II

*1
tl

t,

0.18750
0.125
.,(

2.875

1 500

1.4375

Fig.

256

IG

r _

F-4
i.
I.i

Interlaminar

Shear

of

Cured

Material

SCOPE
The
interlaminar
accordance
with

shear
strength
the
following:

test

shall

be

in

PROCEDURE
Cut sufficient
plies
to produce
a
inch thick
across
the square
plies
of 1.5 + 0.25
in.

test
panel
of minimum

2.2

Spray
mold.

and

2.3

Cure
hours

at
+

2.4

After
test
room

cure,
remove
the mold
from the press,
panel
from
the mold
and allow
the panel
temperature.

2.5

Cut
a specimen
of sufficient
size
to produce
a 0.375
inch
diameter
by 1.125
inch minimum
length
finished
specimen
with
the length
being
perpendicular
to the plies
from
the
test
panel.

2.6

Center
the specimen
to
specimen
perpendicular
specimens
to a diameter
diameter.

2.7

Measure
the diameter
the cross-sectional

2.8

Place
the specimen
in
double-shear
jig shown

2.9

Place
the shear
fixture
and pin
the ends
of the

the

mold

with

release

i000
+ 50 psi.
15 minutes.

agent

and

325

of the test
area
(A).
the
in

degrees

specimen

0.375-inch
Figure
I.

F.

into

for

remove
the
to cool
to

2.11

Record
the maximum
the test
and record
Calculations:

load
carried
as L, lb.

Interlaminar

(psi.)

= L/2A

257

the

calculate

three

machine,

indicated
crosshead
and test.
by

and

diameter

in the testing
fixture.

Set
the machine
at an
to 0.025
inch-per-mlnute

shear

plies

get the length

of the cylindrical
to the plies
and machine
the
of 0.375
+ 0.000/-0.002
inch

2.10

2.12

+ i0

layup

1.5 + 0.25
dimensions

speed

specimen

plate

align,

of

0.015

during

Where:
L

the
maximum
load
carried
during
testing
in pounds
The
original
cross-sectional
specimen
in square
inches.

2.13

Report

the

2.14

Limits

(psi.)

minimum
maximum

interlaminar

shear

2,400
6,500

258

to

by

the

the
area

nearest

specimen
of

i0

the

psi.

259

F-5
i.
i.i

2.1

Thermal

Conductivity

Thermal
conductivity
with
ASTM
C 177 and

Prepare
follows:

a test

2.1.2

Increase
allowing
edges.

panel

the stack
i0 F.
the
the

shall
be determined
as follows:

of

of

The
for

the

outer
1/2
preparation

required

plies

pressure
resin
to

Hold
the pressure
and
or 1 hour
per inch of
Decrease

slowly
stage

in

and

test

specimen

accordance

Report
thermal
hr.
F.
Limits

Minimum
Maximum

(BTU./ft.

conductivity

hr.

for
which

panel

to

be

shall
the

50 psi.,
flash
at

260

15
is

ambient.

shall

not

reported

be

nearest

9.00
0.01

Across
0.10
i.i

Ply

ply

minutes,
greater.

to

OF)
With
Ply
0.10
1.1

as

at

120
ever

pressure

shall

cure

preset

to i000
+
to minimi_e

of the test
specimens.

thickness

and

a press

temperature
thickness,

temperature
inch
of

size

into

Data
for thermal
conductivity
temperature
of 250 + 20F.
Maximum

2.5

Material

PROCEDURE

Place
325 +

2.2

Cured

SCOPE

2.1.1

2.1.3

of

be

for

used

inches.
BTU./ft.

F-6
i.
i.I

2.1

Coefficient

The
coefficient
in accordance

Prepare
follows:

of
with

a test

2.1.2

Increase
allowing
edges.

the

thermal
ASTM
E

panel

stack

the
the

of

of

of

Cured

expansion
228 and as

The
not

the

required

plies

pressure
resin
to

Hold
the pressure
and
or 1 hour
per
inch of
Decrease

Material

shall
be
follows:

size

into

slowly
stage

determined

and

outer
1/2 inch of the
be used
for preparation

test

specimen

Report
coefficient
0.01
in./in.
OF x
Limits

Minimum
Maximum

(in./in.

OF

thickness

of_thermal
i0 -b.
x

50 psi.,
flash
at

to

shall
expansion

be

be

to

281

Ply

With

Ply
2.0
9.0

325

ply

minutes,
greater.

ambient.
panel

reported

4.0

10 -6 )
Across
5.0
20.0

15

of the test
specimens.
shall
OF.

as

at

for 120 +
whichever-is

pressure

edges
of

cure

preset

to 1000
+
to minimi_e

temperature
thickness,

temperature

and

a press

Data
for coefficient
of expansion
temperature
range
from
75 to 400
Maximum

2.5

Expansion

PROCEDURE

Place
OF.

2.2

Thermal

SCOPE

2.1.1

2.1.3

of

shall

for

inches.

the

nearest

F-7
i.

Flexural

of

Cured

Material

SCOPE

i.i

Strength

Flexural
strength
ASTM
D 790,
Method

shall
be determined
I, and as follows:

in

accordance

with

test

and

PROCEDURE

2.1

Cut
sufficient
mark
the warp
Cure

the

plies
to
direction.

plies

Orient
aligned

into

prepare

a panel

required

as

panel

follows:

plies
such
that
warp
fibers
of each
ply
are
in the
same direction.
Mark
warp
direction.

2.2.2

Place
325 +

2.2.3

Increase
allowing
edges.

the stack
10 F.
the
the

of

plies

pressure
resin
to

into

slowly
stage

a press

preset

to I000 +
to minimi_e

at

50 psi.,
flash
at

ply

2.2.4

Hold
the pressure
and
or 1 hour
per inch
of

2.2.5

Decrease
the temperature
and pressure
to ambient.
outer
1/2 inch of the edges
of the test
panel
shall
be used
for preparation
of specimens.

2.3

Maximum

2.4

Report

flexural

2.5

Limits

(psi.)

Minimum
Maximum

test

specimen

temperature
thickness,

thickness

strength

to

Warp
Direction
25,000
55,000

the

for 120 +
whichever-is

shall

be

nearest

Fill
Direction
20,000
55,000

262

0.25
i0

psi.

15

minutes,
greater.

inch.

The
not

F-8
i.
I.i

2.1

Tensile

Strength

of

Cured

Material

SCOPE
Tensile
ASTM
D

strength
shall
be
638 and as follows:

determined

in

accordance

with

PROCEDURE
Prepare
follows:

a test

panel

2.1.1

Orient
aligned

2.1.2

Place
the stack
325 + i0 OF.

2.1.3

Increase
allowing
edges.

of

the

required

size

plies
such that
warp
fibers
of
in the same
direction
Mark

the
the

of

plies

pressure
resin
to

into

slowly
stage

a press

to I000 +
to minimize

and

each
warp
preset

cure

as

ply are
direction
at

50 psi.,
flash
at

ply

2.1.4

Hold
the pressure
and
or 1 hour
per
inch of

2.1.5

Decrease
the temperature
and pressure
to ambient
outer
1/2 inch of the edges
of the test
panel
shall
be used
for preparation
of specimens.

2.2

2.3

temperature
thickness,

for 120 +
whichever-is

15

minutes,
greater

A thickness
of up to 025
inch
can be used
for test
specimens
Report
each
determination
and the average
three
specimens
to the nearest
i0 psi.
Limits

Minimum
Maximum

(psi.)
Warp
Direction
15,000
40,000

Fill
Direction
10,000
35,000

263

The
not

of

F-9

Dry

I.

SCOPE

I.I

Resin

Content

Cured

EQUIPMENT

AND

for
the
carbon

determination
reinforced

MATERIALS

Burners,

2.2

Test

2.3

Vacuum

2.4

Manometer

2.5

Condenser,

2.6

Clamps

2.7

Rubber

stoppers

2.8

Vacuum

tubing

2.9

Press
310
+

Fisher

tubes,

vycor,

25

200

mm.

source
or

vacuum

cold

fo_
10_F

2.10

Desiccator

2.11

Cutting

2.12

Balance,

2.13

Timer

gauge

finger

type

molding
carbon
bars
and
i000
+ I00
psi.

assembly

for

cutting

analytical,

0.0001

1/2"

carbon
gm.

1/2"

at

5";

least

bars

sensitivity

SAMPLING

3.1

Sample
size.
is required.

3.2

Number
of
determinations.
run
duplicate
determinations
Preparation
Cutting.
1/2
inch

3.3.2

Material

This
method
describes
a procedure
of
the
dry
resin
content
in molded
aldehyde
phenolic
plastics.

2.1

3.

of

Staging.
reduce
system

of
Cut
by
5

broadgoods

test

sample

Unless
on

inches

by

otherwise
each
sample.

20

inches

specified,

specimens.

32 rectangles
inches.

Stage
the
flow.
Staging
and
flow
and

32

from

the

rectangles
at
time
is dependent
must
be
determined

264

prepreg

255 +
upon
from

measuring

5F.
to
resin
experience.

3.3.3

4.

Molding.
Using
the
32 rectangles,
mold
a bar
1/2"
x
1/2"
x 5" +
1/32".
Cure
the specimen
at 310 + 10F.
and
1900
+-i00
psi.
for 15 + 1 minutes.
If the_e
is
any resin-flash,
begin
again
and use
a longer
staging
time.
Cut
the bar into approximately
three
equal
lengths.
Tag
and store
in a desiccator.
PROCEDURE

4.1

Setting
up apparatus.
Set up the apparatus
as shown
in
Figure
i.
Weigh
the test
specimen
to 0.01
g.
Place
the
test
specimen
in the vycor
test
tube
and attach
the tube
to the side
arm of the vacuum
flask.
All
joints
must
be
air tight.
Start
the vacuum
pump,
evacuate
the system,
and check
for air leaks
by shutting
the valve
leading
to
the vacuum
pump.
The leak
rate
should
be less
than
five
millimeters
of Hg per minute
(0.2 inch)
as measured
by a
manometer
or vacuum
gauge.

4.2

Pyrolysis.
With
the vacuum
on and the pressure
stabilized,
place
the Fisher
burners
under
the
specimen
so that
the
flame
area
covers
it completely.
Continue
pyrolysis
for
30 minutes,
or until
the manometer
or
vacuum
gauge
reading
is the same
as it was
before
pyrolysis,
whichever
is longest.

4.3

Cooling
Sample.
When
pyrolysis
is complete,
turn
off the
burners
and allow
the specimen
to cool
under
vacuum
to
room
temperature.
When
the specimen
is cool,
turn
the
vacuum
off,
and carefully
let air into
the system
to
restore
pressure
equilibrium.

4.4

Reweighing
specimen.
vacuum
flask.
Weigh
cooled
to ambient,
or
when
convenient.

5.
5.1

CALCULATIONS

AND

Calculations.
the sample
% DRC

as

(i.00

Remove
the vycor
test
tube
from
the
the specimen
to 0.01
gm. when
transfer
to a desiccator
and weigh

REPORTING

Calculate
follows:
- W2/WI)

the

i00

dry

resin

content

(DRC)

of

where:
W1
W2
K

=
=
=

weight
of sample
before
pyrolysis,
g.
weight
of sample
after
pyrolysis,
g.
constant
peculiar
to material
being
tested,
which
must
come
from
prepreg
manufacturer.

265

5.2

Reporting.
Unless
otherwise
specified,
round
off
and
report
dry
resin
content
to the nearest
0.01%
on
worksheets
and to the nearest
unit
in the designated
place
for figures
on final
reports.
Duplicate
determinations
should
be considered
suspect
if they
differ
by more
than
0.2%.

6.0

NOTES:
Number
specimens
may
are completely

of specimens
per tube.
Two or more
be put
in a tube
so long
as all specimens
covered
by the flame
from
the burners.

266

F-10
1.
I.i

2.
2.1

Residual

Volatiles

Method
for
laminates.
EQUIPMENT

Laboratory
325F.
_

2.1.3

Analytical

2.1.4

4"

2.1.5

Laboratory

2.1.6

Carbide

3.1

4.
4.1

Material

residual

volatile

in

cured

MATERIALS

Equipment

2.1.2

3.

determining

AND

Laboratory

2.2.1

Cured

SCOPE

2.1.1

2.2

of

4"

forced

air

oven,

press,
hydraulic,
5F.
capability
balance,
steel

0.0001

325F.+

5F.

capability

16,000

lbs.

gm.

50

lbs.,

sensitivity

templates

knife
bladed

table

saw

or

hack

saw

Materials
Teflon

coated

glass

cloth

release

fabric

SAMPLING
Sample
size:
The sample
shall
be large
enough
so that
the required
number
of 4" x 4" plies,
cut on the bias,
may
be obtained
to make
a laminate
0.250"
thick.
PROCEDURE
Laminate:
Using
4" x 4" template,
cut reauired
number
of
plies
on the bias.
Stack
and load
at 325F
+ 5F,
press
between
Teflon
coated
glass
cloth
release
material.
Apply
contact
pressure
for 30 seconds
+ 2 seconds,
dump
press;
repeat
twice
and apply
I,_00
+-50
psi for four
hours
+ i0 minutes
at 325F.
+ 15_F.
--Remove
laminate
from
p[ess,
remove
flash
i" pieces
from
laminate

4.1.1

Cut

i"

4"

center

4.1.2

Cut
one

three
i" x
end without

4.1.3

Desiccate

with-knife,
as follows:

strip

i" pieces
trimming

parallel

and cut three

i"
(Refer
to Figure
to

two

from
this
strip,
outside
edge.

pieces.

267

outer

x
i)

edges.

starting

at

4.2

Test
for Residual
Volatiles:
Each
sample
described
above,
afer
desiccation
for a minimum
of 18 hours,
is
weighed.
This
is sample
weight.
Samples
are placed
in
forced
air oven
for four hours
+ I0 minutes
at 325F.
+
15VF.,
removed
and weighed
hot.Four-hour
weight
loss-is
calculated:
Weight

4.3

5.1

Initial

Sample

Wt.

- Hot

Wt.

= Weight
Sample

after

Residual

Volatile

of

each

sample

Residual

Volatile

of

mat.

= Arithmetic
Average
three
samples

4 hrs.

Loss
Weight

of

Tolerances:
0.2_0"
325VF
1,0Q0
325UF.

Loss

Laminate
Thickness,
Press,
+ 15F.
psi.
Press
+ 5%
oven,
+ 108 F.

5%

REPORTING
Report

Residual

Volatile

to

268

2 significant

figures.

100%

above

I.

I.

i.

4.
i.

4.

Fig.

269

F-If
i.
i.i

2.
2.1

Linear

Thermal

of

Cured

Material

Using

DSC

SCOPE
.
This
is a method
for the determination
of linear
al expansion
using
the differential
scanning
calorimeter.
The
thermal
expansion
of plastic
is
reversible.
Upon
it are superimposed
changes
in length
due to changes
in moisture
content,
degree
of
polymerization,
loss
of plasticizer
or solvents,
release
of stresses
or other
factors
which
are mainly
irreversible.
This method
of test
is intended
to yield
the linear
thermal
expansion
excluding
these
incidental
factors.
In general,
it will
not be possible
to exclude
all of these
spurious
factors
and thus
the method
can be
expected
to give
only
approximate
values.
This
method
is
an adaptation
of ASTM
E228-71.
EQUIPMENT

AND

MATERIALS

Equipment.

2.1.1

Differential
manual

2.1.2

DSC

2.1.3

Helium

3.

Expansion

Scanning

User's

Calorimeter

and

an

operators

Manual

Gas

source

SAMPLING

3.1

Preparation.
All
samples
shall
be cut or shaped
from
moldings,
castings,
or laminates
by methods
under
conditions
that
give
a minimum
of strains
or molecular
anisotropy.

3.2

Dimensions.
Samples
shall
be 1/4
by 1/4
with
the ends machined
flat
and parallel
tolerances.

4.

by 1/4 inches
with
0.005
inch

PROCEDURE

4.1

Calibrate

4.2

Turn

4.3

Set

4.4

Measure
0.0001

4.5

Place
sample
direction

on

the
the

DSC

helium

approximate
sample
inch

as

user's

atmosphere

upper
height,

into

per

the

and

lower

width,

TMS

(DSC)

270

manual
or

other

gas

as

specified

temperatures
and

thickness

apparatus,

to

nearest

noting

the

ply

Zero

out

Raise
2F.per
4.8

4.9

the

chart

temperature
minute.

Cool
sample
is
reached.
minute.

to
Hold

upper
upper

limit
limit

at
40F.+
5F.
Hold
at-lower

Repeat
steps
4.7
and
first
cycle
of heating
condition
the
sample.

per
minute
limit
for

4.8
three
(3)
and
cooling.

4.10

Measure
heating

the
temperature
difference
or
cooling
period.

4.11

Measure
heating

the
and

5.1

CALCULATIONS

shrinkage
cooling
AND

difference
periods
with

40F.+
+ 0.5F.

until
lower
minutes
+

times.
This

at

limit
0.5

Disregard
was
done

the

end

at
the
end
each
cycle.

of

of

the
to

each

the

REPORTING

Calculations:
Calculate
the
thermal
expansion
as
follows:
E

at
a rate
of
for
5 minutes

coefficient

of

linear

L
LxT

where:

delta

coefficient
in./in./F,

of
thermal
x i0 -_

L
T

=
=

test
length
of specimen
at
room
temp.,
inch
temperature
difference,
OF.,
over
which
the
change
in length
was
measured
Average
of change
in length
due
to heating
and
cooling.

271

expansion,