A 5523: 2012

Table of Contents
Page
Preface 1
1 Scope of Application 1
2 Normative Standard 1
3 Terms and Definitions 1
4 Types and Symbols 2
5 Chemical Composition 2
6 Carbon Equivalent 2
7 Mechanical Nature 3
7.1 Yield Point or Yield Strength, Tensile Strength and Elongation 3
7.2 Joint Tensile Strength of Linear Steel Sheet Pile 3
7.3 Charpy absorbed energy 3
8 Tolerance and dimensional tolerance and unit mass 3
9 Appearance 5
10 A test 6
10.1 Analysis test 6
10.2 Mechanical test 6
10.3 Joint tension test of straight steel sheet pile 7
11 Inspection 8
12 Re-examination 8
13 Display 8
14 Report 9
Annex A (normative) Nteel - Nitride Type Nitrogen Determination Method 10

(1)
5523: 2012
Foreword
This standard is based on the provisions of Article 12, Paragraph 1 applied mutatis mutandis
pursuant to Article 14 of the Industrial Standardization Act, Japan
From the Iron and Steel Federation (JISF), there is a proposal to amend the Japanese Industrial Standards
with the original industrial standards, and the Japanese Industry Standard
It is a Japanese Industrial Standard which was revised by the Minister of Economy, Trade and Industry
after deliberation by the investigation committee.

As a result, JIS A 5523 : 2006 was revised and replaced by this standard.
In addition, until April 19, 2013, JISMA based on the provisions of the relevant clauses such as
Article 19, Paragraph 1 of the Industrial Standardization Act
It can be done according to JIS A 5523 : 2006 in certification display certification .
This standard is a copyrighted work subject to copyright law.
To comply with this standard, there is a risk of falling under the use of the following patent rights,
etc. with respect to the hat form, so

Do so.

(Patent number) (Title of Invention) (Setting registration date)

1) No. 2689794 Asymmetric U-shaped steel sheet pile by hot rolling August 29, 1997
2) No. 2964933 How to place underground structure, asymmetric U-shaped steel sheet pile and
asymmetrical U-shaped steel sheet pile August 13, 1999
3) No. 3173389 Asymmetric U-shaped steel sheet pile and its hot rolling method March 30, 2001
4) 3458109 Hat type steel sheet pile August 1, 2003
5) No. 3488230 Rolled steel sheet pile October 31, 2003
6) No. 3488232 Rolled steel sheet pile October 31, 2003
7) No. 3488233 Hat type steel sheet pile October 31, 2003

The above-mentioned right holder of a patent right, etc. Shall implement the patent right etc. to any
person
under non-discriminatory and reasonable conditions
It is expressing that there is intention to give permission etc. However, for rights holders of other patents
etc. related to this standard
In addition, it is conditional on that the implementation is permitted under similar conditions.
It should be noted that conforming to this standard does not necessarily mean that the patent right is free
of charge
.
Some of this standard may conflict with patent rights etc. other than those indicated above. Minister of
Economy, Trade and Industry and Japan Industrial Market
The quasi-investigative committee is not responsible for confirmation concerning such patent rights etc.
Here, the term "patent right etc." means a patent right, a patent application after the application is opened,
or a utility model right.

(1)
Japanese Industrial Standards JIS
A
5523:2012

Hot rolled steel sheet pile for welding

Weldable hot rolled steel sheet piles
preface

This standard was enacted in 2000 and since then revised in 2006 it has reached today. In the last
revision,
The shape was added, but since then, the necessity of adding high-strength steel and so on has been
increased and revised. This standard
Is specified for hot-rolled steel sheet piles, which are particularly excellent in weldability,
and carbon bonds not specified in JIS A 5528
Amount, free nitrogen and Charpy absorbed energy.
The corresponding international standards are not enacted at the present time.
1
Scope of application
This standard is a hot rolled steel sheet pile (hereinafter referred to as a steel sheet pile) used for soil
fastening, shutoff, foundation of a structure, and the like.
)so
It specifies what is especially excellent in weldability.
2
Normative standard
The following standards constitute a part of the provisions of this standard by quoting this standard. these
For undated references, the latest edition of the referenced document (including any amendments) applies.
) Is applied.
JIS G 0320
Molten steel analysis method for steel materials
JIS G 0321
Product analysis method of steel material and its allowable variation value
JIS G 0404
General delivery conditions of steel materials
JIS G 0415
Steel and steel products - inspection documents
JIS G 1201
Iron and steel - Method of analysis General rules
JIS G 1228
Iron and steel - Nitrogen determination method
JIS G 3192
Shape, size, mass and tolerance of hot rolled steel
JIS Z 2241
Metallic material tensile test method
JIS Z 2242
Charpy impact test method for metallic materials
3
Terms and definitions
The definitions of the main terms used in this standard are as follows.
3.1
Free nitrogen
Nitrogen precipitated in steel by combining with alloying elements (aluminum, titanium, vanadium etc) with
high affinity for nitrogen
Solid dissolved nitrogen in steel other than nitrogen (nitride type nitrogen) contained in the oxide.

(1)
2
A 5523
: 2012
Four
Types and symbols
There are three types of steel sheet piles,
See Table 1 .
Table 1 - Types of symbols
Types of symbols
SYW
295
SYW 390 SYW 430
Five
Chemical composition
The steel sheet pile was subjected to the test of 10.1 ,
See Table 2 .
Table 2 - Chemical Components
Unit%
Types of Symbols C
Si
Mn
P
S free nitrogen
a)
SYW
295
SYW 390 SYW 430
0.18 or less 0.55 or less 1.50 or less 0.040 or less 0.040 or less 0.006
0 or less
b)
If necessary, alloying elements other than this table may be added. Of the chemical components other than
this table, carbon equivalent specified in Clause 6
For the components included in the calculation formula of quantity, the test of 10.1 shall be conducted.
note
a)
Free nitrogen is determined as nitrogen obtained by subtracting nitriding nitrogen quantitative value from
the total nitrogen determination value in steel. In the total nitrogen determination method,
JIS G 1228
by. In the nitride type nitrogen determination method,
According to the steel-nitride type nitrogen determination method shown in Annex A. Nitride type
Determination of nitrogen is done by samples taken from the product. The value of the free nitrogen content
may be replaced with the total nitrogen content .
b)
For steel materials with free nitrogen above 0.006 0% and below 0.010 0%, strain aging (after applying
3% strain, at 250 ° C.
For 1 hour), Charpy impact test was carried out, and the result was
When Table 5 is satisfied, free nitrogen
May be 0.010 0% or less.
6
Carbon equivalent
The carbon equivalent of the steel sheet pile was calculated using the molten steel analysis value of 10.1
according to the formula (1)

(1)
See Table 3 .
14
V
Four
Mo
Five
Cr
40
Ni
twenty four
Si
6
Mn
C
eq
+
+
+
+
+
+
=
C
(1)
here,
C
eq
:
Carbon equivalent (
%
)
Table 3 - Carbon equivalent
Unit%
Types of symbols
Carbon equivalent
SYW 295 0.44 or less
SYW 390 0.45 or less
SYW 430 0.46 or less
According to the agreement between the delivering parties,
(2)
Is used,
In place of Table 3 , carbon equivalents may be agreed. However,
In this case,
(1)
The carbon equivalent by
Table 3 shall be satisfied.
15
Cu
Ni
Five
V
Mo
Cr
6
Mn

(1)
C
)
IIW
(
eq
+
+
+
+
+
+
=
C
(2)

3
A 5523
: 2012
here,
C
eq
(IIW)
:
IIW
1)
Carbon equivalence according to the equation (
%
)
note
1)
International Institute of Welding
7
mechanical nature
7.1
Yield point or yield strength, tensile strength and elongation
The steel sheet pile was subjected to a tensile test according to 10.2 , and its yield point or yield strength,
tensile strength and elongation,
See Table 4 .
Table 4 - Yield point or yield strength, tensile strength and elongation
Types of symbols
Yield point or yield strength
N / mm
2
Tensile strength
N / mm
2
Test pieces
Elongation
%
1A No. 18 or more
SYW 295
295 or more 450 or more
14B 24 or more
1A No. 16 or more
SYW 390
390 or more 490 or more

(1)
14B 20 or more
1A No. 14 or more
SYW 430
430 or more 510 or more
14B issue 19 or more
Note 1
N / mm
2
= 1 MPa
7.2
Joint tensile strength of linear steel sheet pile
The straight steel sheet pile board was subjected to the test of 10.3 and its joint tensile strength
2)
, Thickness
10 mm
Less than
3.92 MN / m
Or more, thickness
10 mm
that's all
16 mm
Less than
5.88 MN / m
Or more.
note
2)
During the course of the joint tensile test of the steel sheet pile, the maximum load that the specimen
endured was changed to the width
1m
Converted value per unit.
7.3
Charpy absorbed energy
The steel sheet pile,
The impact test was carried out under the conditions shown in Table 5 in accordance with 10.2 , and the
Charpy absorbed energy thereof
Five
by.
The Charpy absorbed energy in Table 5 ,
3
The average value of the number of test pieces, JIS G 0404 of 9.6 (set test
Evaluation of results).
Table 5 - Charpy absorbed energy
Charpy absorbed energy
J
Height × width of specimen
Standard specimen
Sub size test piece
Types of symbols
Test temperature
a)

℃
10 × 10 mm
10 × 7.5 mm

(1)
10 × 5 mm
Test pieces
as well as
Test specimen collection
direction
b)
SYW
295
SYW 390 SYW 430
0 43 or more 32 or more 22 or more
V notch
rolling direction
note
a)
According to the agreement between the delivering parties, when conducting the test at a temperature
lower than these test temperatures, that
It may be replaced by the test temperature.
b)
According to the agreement between the delivery parties, in the case of conducting a test in the direction
perpendicular to the rolling direction, there is an approval of the orderer.
In this case, the rolling direction test may be omitted.
8
Tolerance and dimensional tolerance and unit mass
The shape, size and tolerance and unit mass shall be as follows.
a)
As for the sectional shape of the steel sheet pile,
U
Shape, linear shape,
Z
form,
H
Shape and hat shape, the nickname of each part,
Refer to Fig. 1 .

Four
A 5523
: 2012
b)
The joint of the steel sheet pile is sufficiently engaged at the time of driving and can be easily detached
when pulling it out
Only watertightness should be obtained.
c)
The tolerance of the shape and dimensions of the steel sheet pile,
See Table 6 .
d)
Unit weight depends on the agreement between the delivering parties.
e)
Depending on the designation of the orderer, drilling or accessory mounting may be carried out to hang the
steel sheet pile at the time of construction. This
In the case of inspection, display, etc. are based on the agreement between the delivering parties.
a)
U shape b) linear shape
c)
Z -shaped D) H -shaped

(1)
e)
Hat form
Figure 1 - Name of each part of the section

Five
A 5523
: 2012
Table 6 - Tolerance of shape and dimensions
Cross-sectional shape
item
Linear shape
U shape
Hat form
Z type
H type
width
± 4 mm
Effective width ≦ 400
± 4 mm
400 <effective width ≦ 500
± 5 mm
500 <effective width ≦ 600
+6 mm
-5 mm
+10 mm
-5 mm
+8 mm -
4 mm
± 4 mm
height
-
± 4%
± 5 mm
± 1.0%
Less than 10 mm
+1.5 mm -
0.7 mm
+1.0 mm -
0.3 mm
± 1.0 mm
10 mm or more and
less than 16 mm
+1.5 mm -
0.7 mm
+1.2 mm -
0.3 mm
± 1.2 mm
thickness
16 mm or more
-
+1.5 mm -
0.3 mm

(1)
± 1.5 mm
length
+ Not stipulated
0
Less than 10 m
Total length (m) × 0.15% or less
under
Overall length (m) ×
0.12% or less
Overall length (m) × 0.15% or less
Bend
a)
Ultra length 10 m
which obtain
[(Overall length - 10 m) x
0.10% + 15 mm] or less
Total length (m) × 0.10%
, however, 20 mm or less
under
[(Overall length - 10
m) x 0.10% +
12 mm] or less
[
(Total length - 10 m) x 0.10%
+ 15 mm] or less
Less than 10 m
Total length (m) × 0.20% or less
under
Overall length (m) ×
0.25% or less
Overall length (m) × 0.15% or less
warp
a)
Ultra length 10 m
which obtain
[(Overall length - 10 m) x
0.10% + 20 mm] or less
Total length (m) × 0.20%
, however, 20 mm or less
under
[(Overall length - 10
m) x 0.20% +
25 mm] or less
[
(Total length - 10 m) x 0.15%
+ 15 mm] or less
Right-angle cutting difference of cross section
4% or less of width

(1)
4% or less of height and width
Full width difference
-
In
the range of the end 1 m in the longitudinal direction,
the maximum and minimum of the full width
Is less than 4 mm
-
-
-
End curvature
b)
-

End curvature of edge 1 m in longitudinal direction is

less than 1.5 mm
-
-
-
Coupling angle (fitting) angle θ
c)
-
≧6°
≧4°
-
-
Where the tolerance of width, height and thickness is applied,
Refer to Fig. 1 . However, the width tolerance is a linear, U-shaped and hat-shaped field
In case of full width, in the case of Z shape it is applied to the whole piece width, in the case of H shape it
is applied to the width of the main body. In addition, the height tolerance is
applied to the total height in case of U shape and the height of the main body in case of H shape.
note
a)
The bending is parallel to the sheet pile wall, and the warpage is a direction perpendicular to the sheet
pile wall.
b)
End curvature shall be 1/2 of chord side measurement value or tangential side measurement value.
c)
Joint Kan (fit) engagement angle, FIG. 2 by.
9
appearance
The steel sheet pile must not have harmful drawbacks in use. However, the disadvantage which is harmful
in terms of use is the clause 9 of JIS G 3192
Or may be removed or repaired by an external appearance.

6
A 5523
: 2012
Ten
test
10.1
Analysis test

(1)
Analytical tests are as follows.
a)
General items of analytical tests and how to take analytical samples are according to Clause 8 (chemical
composition) of JIS G 0404 .
b)
Molten steel analysis method is according to JIS G 0320 .
c)
For the method of quantifying free nitrogen,
According to the steel-nitride type nitrogen determination method shown in Annex A.
d)
Determination of nitride type nitrogen in the determination of free nitrogen is based on the sample taken
from the product,
1
Fruit per molten steel
To apply. In this case, the method of collecting the analysis sample is according to Clause 4 (sampling
method for analysis) of JIS G 0321 . However
As a sample material, a tensile test piece after rupture may be used.
Figure 2 - Joint angle (fit) angle of U- shaped and hat-shaped steel sheet piles
10.2
Mechanical test
10.2.1
Test General
General items of mechanical tests are according to Clause 7 (General Request) and
Clause 9 (Mechanical Properties) of JIS G 0404 . Provided, however,
How taken of試材is JIS G 0404 of 7.6 in (specimen collection condition and the test piece)
A
The number of specimens and the sampling position
The collection direction is as follows.
a)
Number of tensile test specimens The number of tensile test specimens shall be the same for molten steel,
the same cross-sectional shape and the same cross-sectional dimensions
A set of tensile specimens
1
Collect individuals. However,
50 t
If it exceeds
2
Collect individuals.
b)
Number of Impact Test Specimens The number of impact test pieces shall be the same for the same molten
steel, the same cross-sectional shape and the same cross-sectional dimensions
One pair and the test material
1
Samples are taken and the test strips are taken from now
3
Collect individuals.
c)
Collection position and sampling direction of tensile specimen Tensile specimen shall be taken from the
position shown in Fig. 3 in parallel to the rolling direction.
If it can not be done according to Fig. 3 , it should be close to this.
d)
Sampling position impact test specimens for collecting sample material of the impact test piece,
FIG. 3 taken from the position shown in. Thickness of impact test piece
The sampling position in the direction,
Refer to Fig. 4 .
10.2.2

(1)
Test pieces
Tensile test specimens and impact test specimens shall be as follows.
a)
The tensile test pieces, JIS Z 2241 of
1A
Issue or
14B
Issue.
b)
Impact test pieces, JIS Z 2242 of
V
Make a notched specimen. If standard specimens can not be collected, the width is
7.5 mm
Or
5 mm
May be used.
10.2.3
Test method
a)
The method of tensile test shall be in accordance with JIS Z 2241 .

7
A 5523
: 2012
b)
The method of impact test is according to JIS Z 2242 .
Figure 3 - Picking position of test specimens for tensile test specimens and shock specimens
Unit mm
Figure 4 - Thickness sampling position of impact specimen
10.3
Joint tension test of straight steel sheet pile
The joint tensile test of linear steel sheet pile shall be as follows.
a)
The joint tensile test specimen was made of the same molten steel, one set at right angles to the rolling
direction for the same cross-sectional dimension
2
Collect individuals. in this case,
1
The dimensions of the test pieces are about width
100 mm
, About length
300 mm
, And represent the joints on both sides of the steel sheet pile
Collect one set of specimens each with a joint on one side.
b)
The method of the joint tensile test is based on JIS Z 2241 to measure the strength of joint breakaway
(when the test specimen has broken before the joint disengages
And its breaking strength) is measured. In this case, the test piece
As shown in Fig . 5 , the joint is engaged and the tensile shaft and
It was set so that the axis of the specimen was parallel to the axis of the specimen, and the grip interval
was
400 mm
Or more.

8
A 5523

(1)
: 2012
Figure 5 - Test piece set state
11
Inspection
The examination is as follows.
a)
General matters of inspection shall be in accordance with JIS G 0404 .
b)
Chemical components shall conform to clause 5 .
c)
The carbon equivalent shall comply with Clause 6 .
d)
Mechanical properties shall conform to clause 7 .
e)
Shape and dimensions shall comply with Clause 8 .
f)
Appearance shall conform to clause 9 .
12
re-examination
Re-examination shall be as follows.
a)
Tensile steel sheet pile which did not pass the test or joint tensile test, JIS G 0404 of 9.8 retried by (retest)
You may make an exam and decide whether to accept or not.
b)
Steel materials whose impact tests did not pass in accordance with JIS G 0404 , 9.6 (evaluation of the
result of the group test), are as specified in JIS G 0404
9.8
(Re-test) to determine the acceptance or rejection.
13
display
The steel sheet pile that passed the inspection shows the following items for each steel sheet pile in an
appropriate manner that does not easily disappear until the start of hammering
Must be indicated. However, in the case of obtaining the approval of the orderer, part of it may be omitted.
a)
Types of symbols
b)
Molten steel number or inspection number
c)
Abbreviations indicating the shape and dimensions (or cross-section performance) (abbreviations agreed
between the delivering parties)
d)
Length (expressed in meters.
)
e)
Manufacturer name or its abbreviation

9
A 5523
: 2012
14
report
The report shall be in accordance with Clause 13 (Report) of JIS G 0404 , and the manufacturer
shall comply with the requirements of JIS G 0415
Table 1 (Total of inspection documents
On the table
3.1.B

(1)
(Inspection certificate
3.1.B
) To the orderer. If the ordering person makes another inspection document
When requesting, you must request the manufacturer at the time of ordering. Report on free nitrogen
content,
Please state that it satisfies Table 2 , or note in Table 2
a)
Strain Age Charpy impact test conducted on the basis of
Experiment result
This is done by describing that the values specified in Table 5 are satisfied. The value of total nitrogen
content is shown in the table
2
If the nitrogen value is satisfied, the total nitrogen content may be reported instead of the free nitrogen
content.
Incidentally,
Table 2 alloy elements contained in and carbon equivalent formula, and Table 2 Table by
footnote 2 chemical components other than
, The content of the alloying element must be reported.

Ten
A 5523
: 2012
Annex A
(Normative)
Steel-nitride type nitrogen determination method
A.1
Scope of application
This annex is a method for quantitative determination of nitride type nitrogen in steel products to determine
the free nitrogen content specified in the main body
Regulate. However, silicon nitride is not quantitated as nitride type nitrogen in this method.
A.2
General information
General matters common to analysis methods are according to JIS G 1201 .
A.3
Abstract
After decomposing the iron, which is the matrix of the sample, by an appropriate method, the residue is
passed through a polycarbonate membrane filter
Filter through. The collected residue was decomposed with sulfuric acid and potassium sulfate, and this
solution was treated with sodium hydroxide
After steam distillation, the distilled ammonia is absorbed in boric acid, water or dilute sulfuric acid, and the
ammonia in the absorption solution
Of ammonia with an amidosulfuric acid titration method, bis (
1-
Phenyl
-3-
Methyl
-Five-
Pyrazolone) absorptiometry method or Indofe
It is determined by Norblue Absorption Photometry.
A.4
reagent
Reagents are as follows.
A.4.1
Sulfate
A.4.2
Potassium sulfate

(1)
A.4.3
methanol
A.4.4
Methyl acetate
A.4.5
Bromine-methanol solution
Ten %
(Volume fraction)
methanol
135 mL
Using a measuring cylinder to weighed Erlenmeyer flask (
300 mL
). bromine
15 mL
Scale with a measuring cylinder or a cone-type liquid meter and stir. This solution is added immediately
before use
Prepare.
A.4.6
Bromine-methyl acetate solution
Ten %
(Volume fraction)
Methyl acetate
135 mL
Using a measuring cylinder to weighed Erlenmeyer flask (
300 mL
). bromine
15 mL
Scale with a measuring cylinder or a cone-type liquid meter and stir. This solution is added immediately
before use
Prepare.
A.4.7
Iodine-methanol solution
0.14 g / mL
Iodine
42 g
1)
Weigh the beakers (
300 mL
). Add methanol and stir, add the whole amount
300 mL
1)
. This solution is prepared just before use.
note
1)
Depending on usage, weighing amount and total amount may be changed according to this ratio.
A.4.8
Tetramethylammonium chloride ( TMAC ) - acetylacetone - methanol electrolyte
TMAC 5 g
On a scale, acetylacetone
50 mL
With a measuring cylinder or a cone type liquid volume meter
Bekkatto beaker (
500 mL
). Add methanol and stir, add the whole amount
500 mL
.

(1)
11
A 5523
: 2012
This solution is prepared just before use.
A.5
operation
A.5.1
Separation of nitride type nitrogen
Separation of nitride type nitrogen is according to one of the following.
a)
Iodine-methanol method
1)
sample
1
~
5g
To
1 mg
Carried up to the digit of the dried common dry flask Erlenmeyer flask (
500 mL
)
Sample
1g
For every
50 mL
Add iodine-methanol solution ( A.4.7 ). The amount of sample taken out was nitrogen
The amount of nitrogen calculated from the predicted content rate of the nitride of nitrogen is within the
applicable range of the nitrogen determination method of JIS G 1228
As shown in FIG. Dry common common paddle condenser Cooler is installed and in about a water bath
60
Heat to ℃
. While warming, stir the solution using ultrasonic equipment or magnetic stirrer. Deposition during
decomposition
If it occurs, increase the amount of iodine-methanol solution. When decomposition of the base material is
completed, flask from the water bath
Take out and cool.
2)
Polycarbonate membrane filter (
47 mm
φ, pore size
0.2 μm
), The solution was suction filtered, and the residue
Collect on the filter. Wash with methanol until no coloring of the filter is observed.
3)
Remove the filter from the suction filter and dry the filter at room temperature.
b)
Bromine-methyl acetate method
1)
sample
1
~
5g
To
1 mg
Carried up to the digit of the dried common dry flask Erlenmeyer flask (

(1)
300 mL
)
The bromine-methyl acetate solution ( A.4.6 )
150 mL
. The amount of dust in the specimen was estimated from the nitride type nitrogen
It is decided that the amount of nitrogen calculated from the content is within the applicable range of the
nitrogen determination method of JIS G 1228 to be applied
It is fixed. Attach a dry common grinding coiled condenser and disassemble at room temperature. During
disassembly, ultrasonic equipment
Stir the solution using a magnetic stirrer.
2)
Polycarbonate membrane filter (
47 mm
φ, pore size
0.2 μm
), The solution was suction filtered, and the residue
Collect on the filter. Wash with methyl acetate until no coloring of the filter is observed.
3)
Remove the filter from the suction filter and dry the filter at room temperature.
c)
Bromine-methanol method
1)
sample
1
~
5g
To
1 mg
Carried up to the digit of the dried common dry flask Erlenmeyer flask (
300 mL
)
Bromine-methanol solution ( A.4.5 )
150 mL
. The amount of dust in the specimen was estimated from the nitride type nitrogen
It is decided that the amount of nitrogen calculated from the content is within the applicable range of the
nitrogen determination method of JIS G 1228 to be applied
It is fixed. Attach a common companion duct cooler and disassemble at room temperature. During
disassembly, ultrasonic equipment or magnetic
Stir the solution using an agitator.
2)
Polycarbonate membrane filter (
47 mm
φ, pore size
0.2 μm
), The solution was suction filtered, and the residue
Collect on the filter. Wash with methanol until no coloring of the filter is observed.
3)
Remove the filter from the suction filter and dry the filter at room temperature.
d)
Constant potential electrolysis
1)
The surface of a specimen cut out into a block having an appropriate size was rubbed with abrasive paper
P120
~
P400
) And polished

(1)
After ultrasonic washing in methanol and drying, weigh the mass.
2)
Samples are preliminarily stored
TMAC
- Acetylacetone - Methanol Electrolyte ( A.4.8 )
500 mL
In an electrolytic cell
With a platinum wire or fixed with a magnet to form an anode, platinum or copper as a cathode and a
constant potential electrolyzer
Electrolysis is performed at a predetermined potential by using the apparatus to dissolve the base
material. The dissolution amount of the base material is,
1g
To the extent of
2)
.

12
A 5523
: 2012
note
2)
100
mA
so
1
When electrolyzed for about a hour, about
0.1 g
Is dissolved.
3)
After the electrolysis was completed, the sample was taken out from the electrolytic cell and dried in a
beaker (
200 mL
), And the sample completely
Methanol is added until it is immersed and ultrasonic washing is performed to sift off the deposits
remaining. Polycarbonate
Membrane filter (
47 mm
φ, pore size
0.2 μm
), The washing solution of the sample and the electrolytic solution were suction filtered,
Collect the residue on the filter.
Wash with methanol until no coloring of the filter is observed.
Four)
Remove the filter from the suction filter and dry the filter at room temperature.
Five)
After thoroughly washing the sample with methanol and drying, the mass was weighed, subtracted from
the mass obtained in 1) , and the sample
Dissolve amount.
A.5.2
Resolve residue
A.5.1 a)
, A.5.1 b) , A.5.1 c) or A.5.1 The residue obtained in d) is added to each polycarbonate membrane filter
Square flask (
300 mL
), And potassium sulfate
10 g

(1)
And sulfate
20 mL
. Gently heat to remove moisture
After evaporation, placing a funnel on the mouth of the flask and heating it, about
1
Time Generate white smoke of sulfuric acid, leave residue etc.
To solve. After cooling to room temperature, water
100 mL
Is added little by little, boil for a while to remove sulfur dioxide. A room
Cool to warm.
A.5.3
Determination of nitrogen
A.5.2
The determination of nitrogen in the solution obtained in
a)
Ammonia Distillation Separation Amidosulfuric Acid Titration Method Annex 1 of JIS G 1228 .
b)
Ammonia distillation separated bis ( 1- phenyl -3- methyl -5- pyrazolone) absorption spectrophotometric
method Annex 2 of JIS G 1228
According to.
c)
Ammonia Distillation Separation Indophenol Blue Absorption Photometric Method According to
Annex 3 of JIS G 1228 .

(1)