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PACKAGING ANO CONTAINERS

JamesS. SwinehartandRobertW.Hannah
The Perkin-ElmerCorporation
Infraredspectroscopyhasasignificantroletoplay
inthecontinuingquestofthepackagingandcontainer
industryformateriaistomeetdemandsforbetter
productprotection,betterappearance,andlowercosts.
Notonlywillinfraredspectraprovidelargeamounts
ofinformationaboutmateriaistobeusedinpackaging,
..butsuchspectracanbeobtainedrapidlyandeasily
..., withtheaidofavarietyofavailablesamplingtechniques
whichareapplicabtetosubstanceshavingwidely
differingphysicalproperties.
Amongthemanyusesofinfraredspectroscopy
inthepackagingindustryaresuchapplicationsasthe
detectionofimpuritiesintherawmateriaisused ina
formulation,qualitycontrolofcomponentsin
intermediateorfinishedproducts,andanalysisof
competitors'products.Whetherin research,quality
control,orinthesolutionofcustomerproblems,
thecontributionofinfraredcanbeamajorone.
Generally,forpositiveidentification,samplesshould
berelattvelypure,butoftentheycanbeidentifiedeven
whenimpure.Sometimes,evenminorimpuritiesofa
complexmixturecanberecognized.
r
TRANSMISSION SPECTRA
Inoneapplicationafoodpackagerwishedtoknow
- theidentityofapliabletransparentfilm.Thefilmwas
thinenoughsothatatransmissionspectrumcould
beobtained(Figure1) bysimplyplacingthefilm,
Figure1. Polyethylenewrap,Fllm.
..
..
lO
'.
justasitwasreceived,inthesamplebeamofan
infraredspectrophotometerandrecordingaspectrum.
Thefilmwasthenidentifiedbycomparisonwltha
collectionofpolymerreferencespectra.Itwasfound
~ ~ .. ~ ~ .
thatthespectrumoftheunknownfilmwasthesame
asthespectrumofpolyethylene.
Otheralkenes,suchaspolypropylene.havespectra
similartothatofpolyethylene.Certaindifferenees,
however,allowonetodistinguisheasilyamongthe
variousmembersoftheseries.Forexample,thespectra
ofpolyolefinsotherthanpolyethylenehaveoneor
moremoderatelystrongabsorptionsbetween1300and
80em-
1
duetoehainbranehing.Furthermore,the
spectraofalmostalipolyolefinsotherthanpolyethylene
haveamuehstrongerabsorptionat1380em-
l
than
thatshowninFigure1.Also.nootheralkenepolymer
hasastrongdoubletat725em-
l
.
Oftenanunknownmaterialisidentifiedfromits
infraredspeetrumbycomparingthefrequeneiesofthe
absorptionbandswiththefrequeneiesassoeiated
withpossiblestrueturalfeaturesoftheunknown,
Suehacomparisonoftenresultsinfasteridentification
ofanunknownbylimitingthenumberofreference
speetrathatmustbesearehed.
Afrequeney-structurecorrelationistheonlyway
anunknowncanbeidentifiedbyitsspectrumwhena
refereneespectrumofthematerialisunavailable.
Inthepresentexample,theidentificationofthefilm
byfrequency-structurecorrelationproceedsasfollows:
Theabsorptionbandsat2900,1460,and
1375em
1
areIrom aliphaticCH2 andCH3 groups.The
abseneeofanyothermoderateorstrongabsorptions
between4000and800cm-
1
suggestsanalkaneor
mixtureofalkanes.Thedoubletat725em-
1
indicates
thepreseneeofverylongalkanechains,withIiUle
ornobranching.Sinee,inadditiontoitsspeetral
characteristics,thefilmhasreasonablygoodmechanical
andtensilestrength.Itcanbeidentifiedaspolyethylene .
Evenwhenamaterialhasbeententativelyidentifiedby
frequency-structurecorrelation.comparisonwitha
spectrumofthesuspectedmaterialisusually
usedforconfirmation.
REFLECTANCE TECHNIQUES
Theforegoingexampleillustratesidentificationof
atransparentsample.Mostspectraareobtainedon
transparentsamples;however,techniquesareavailable
forobtainingspectraonopaquesamples.Figures2
and3arespectraofopaquesamplesobtainedby
usingreflectancetechniques.
Figure2. SpeclrumofunknownopaquesamplebyFMIR.
Figure3. SpaclrumofEpononIInplalebyspecularrefleclance.
Thematerialwhichgavethespectrumshownin
Figure2wasatough,resilientwhitecoatingona
fiberboard.Toobtainthespectrum.asmaflpieceofthe
fiberboardwascutanditswhite-coatedsurfacepressed
againsHheKRS-5crystalinaFrustratedMultiple
InternaiReflectance(FMIR)Accessory.Theabsorptions
at2860and2920cm-
1
andtheabsenceofabsorptions
near3000em,1 andfrom1640to1500em,1 indieate
asaturatedaliphatiematerial.andthestrongabsorption
at1720em,1 indicatesanesterorketone.Thestrong
absorptionsat1220and1020cm'l,confirmtheester,
probablyanacetate,andfurtherverificationisprovided
bythestrongabsorptionat1360cm-
1
(symmetrie
methylbendnexttoacarbonyl)andtheabsorption
... _-------''''.... , ' ' ' ' ~ - - - - ~ ~ ~ - - - - --
at1432em-
1
(asymmetriemethyJbendnexttoa
carbonyl).Thedataindicatethatthecoatingisan
aliphaticacetatewithahighmolecularweight,probably
polyvinylacetateoroneofitscopolymers.Final (
confirmationthatthecoatingisindeedPVAiseasily
obtainedbycomparisonofthespectrumwitha
refereneespeetrumofpolyvinylacetate.
Figure3isthespeetrumofEponepoxyresin
ontinplate.Eventhoughthethieknessoftheeoating
waslessthan0.5mil,ausefulspectrumwasobtained
usingaPerkin-ElmerSpecularReflectanceAccessory
(partnumber186-0188),Thisaccessoryfocusesthe
samplebeamofthespectrophotometeronasample
placedontheaceessorysampleholdersothatthe
samplerefleetsradiationbaekintotheinstrument.
Ifthesampleisacoatingwhichispartiallyoreompletely
transparenttoinfraredradiationandisonarefleetive
substrate.theinfraredradiationpassesthroughthe
coatingandisrefleetedbacktothespectrophotometer. (
Atransmissionspectrumofthecoatingisthusobtained.
Sincethebeamisverysmallatthesamplepoint,
thereflectingsurfacecanbeeitherflator
somewhatcurved.
MEASUREMENT OF FILM THICKNESS
Wheneverabeamofradiationtravelsfromamedium
ofonerefractiveindexintoamediumwithadifferent
refractiveindex,partoftheenergyistransmitted- (
andpartisreflected.Figure4depictsafewofthe
muItipierefleetionsthatoccurwhen,forexample,
radlationpassesthroughatransparentpolymerfilm.
Figure4. PalhofradialionbelweenInnatsur1acesofaflImorcen.
Palhofreflecledradialionisdrawnaian angleloseparaleil
f tomIhaltransmilled.
Medium1 Medium2
Medium1 O
A B
C
.... -----
f--====--... ----- ~ - - ...---
D
~ ~ - - - - - d - - - - - - - ~
----REFLECTED
---TRANSMITTED
NoticethattherayABCDhastraveledapathlonger
thanrayABbytwicethefilmthickness,d.Thesetwo
raysinterferewitheachother,and,dependingon
theirwavelength,eitherreinforceoneanother,or (
interferedestructivelywithresultantattenuation.
Therelationbetweenfilmthickness,d,andwavelength
willdeterminewhetherthereisreinforcementor
attenuation,andasthespectrophotometerscans
throughsuccessivewavelengthsaseriesof"fringes"
)
. willbeproducedasreinforcementandattenuation
alternatewitheachother.
Figure5isatransmissionspectrumofafilmof
Saran,andexhibitstypicalinterferencefringes
superimposedonthecharacteristicabsorption
spectrum.Fringemaximaarelabeled"r"(for
reinforcement),andfringemnima"a"(forattenuation).
Figure5. Sa,an.
Interferencefringescanusuallyberecognizedand
differentiatedfromabsorptionbandsbecauseoftheir
uniformappearanceandbecausetheirpeaksand
valleysareevenlyspacedonalinearfrequencyscale.
Fromtheseinterferencefringesthethickness(d)
oftransparentfilmscanbepreciselymeasured.Thisis
danebysubstitutingthenumberofwavenumberunits
(VI - ['1) spannedbyagivennumberofinterference
fringes( m) intheequation:
thieknessoffilmin em d
where:
n= therefraetiveindexofthefilm(1.4forSaran).
InthespeetrumofSaran(Figure5) therearethree
,ringes(orthreecompletecycles)between
2760and1985cm
l
.
3 3
d= 2(1.4)(2760-1985) 2.8(775)
= 1.38x10.
3
cm 0.53mils
Notethatinmakingthefringemeasurementthe
3000cm-
l
region,wherethesamplehasabsorption
bands.wasavoided.Whencountingfringes
itispreferabletochoosearegionwhichsfreeof
absorptionwhichmightotherwisemasktheprecise
locationoreventheactualnumberofmaxima
orminima.
REFERENCES
Furtherapplicationsofinfraredspectroscopythat
maybeofinteresttotechnicalpersonnelinthe
packagingandcontainerindustryarefoundin:
1.J.Fahrenfort,"AttenuatedTotalReflection,aNew
PrincipiefortheProductionofUsefullnfrared
ReflectionSpectraofOrganicCompounds."
SpectrochimicaActa17,698-709(1961).
2. R. W. Hannah,J.S. Swinehart,"Determiningthe
ThicknessofaSealedCellandPolymerFilm,"
ExperimentsinTechniques01InlraredSpectroscopy,
pp.3.1 - 3.6,Perkin-ElmerCorporation,
Norwalk,Connecticut(1968).
3. N.J.Harrick,"TotalInternaiReflectionandIts
ApplicationtoSurfaceStudies,"Annals01lheN.Y.
Acad.of Scences101,928-959(1963).
4. WalterMorris.Jr. "'dentificationofPackaging
MaterialbyInfraredReflectanceTechniques,"
Journal01Assn.DfOfticial AgriculturalChemists
48,497-501 (1965).
5. RichardA. Nyquist,"InfraredSpectraDfPlasticsand
Resins,"DowChemicalCompany,Midland,Michigan.
6. o ~ i s H.Sharpe."ObservationofMolecular
InteractionsinOrientedMonolayersbyInfrared
SpectroscopyInvolvingTotalInternaiReflection,"
ProceedingsoftheChem.Soc.,December1961,
page461.
7. W.W.Wendlandt,andH.G.Hecht,"Reflectance
Spectroscopy,"NewYork,IntersciencePublishers,
1966.
8. PaulA. Wilks,Jr.,andMayhewR. Iszard,"The
IdentificationofFibersandFabricsbyInternai
ReflectionSpectroseopy,"Mid-AmerieaSpeetroseopy
Symposium,June1964.(AvailablefromWilks
ScientificCorp.,So.Norwalk.Conn.06856).
9. InfraredApplicationsStudyNo.2. "Polymersand
Plastics,"ThePerkin-ElmerCorporation,Norwalk,
Connecticut(1968).
10. InfraredApplicationsStudyNo.5. "Waxes,"The
Perkin-ElmerCorporation,Norwalk,Connecticut
(1968).
11."InfraredSpectroscopy,ItsUseasanAnalytical
ToolintheFieldofPaintsandCoatings,"'bythe
InfraredSpectroscopyCommitteeoftheChicago
SocietyforPaintTechnologyFederationofSocieties
forPaintTechnology,1961.Reprintedfromthe
OfticialDigest,March1961.
AlIspectrashowninthisApplicationsStudywereobtainedona
Perkin-ElmerMode'700'ntraredSpectrophotometer.
/
-
3
Page 3-1
EXPERIMENT 3
Determ.ining the Thickness of a Sealed Cell and of a Polym.er Film.
OBJECTIVE
To determ.ine the thickness of a sealed liquid cell and of a polyrn.er
film. hy the interference fringe technique.
MATERIALS
A sealed cell (thickness 0.015 to 0.3 rn.rn.) and the polystyrene calibra-
tion film..
INTRODUCTION
The thickness of sealed cells is one of the basic quantities required
for quantitati ve analysis. The value should be verified from. tim.e to tim.e
since the thicknes s m.ay change due to a gradual erosion of the internal sur-
faces of the crystal windows in the cell. In addition to the thickness of cells,
the thickness of polym.er film.s is also im.portant both for quantitative analysis
of the filrn and for a knowledge of the thickness, itself.
The basis for the m.easurem.ent is the interference fringe pattern pro-
duced when the transrn.ission of the film. or em.pty cell is recorded over a
range of frequencies. This pattern, an effect of the wave nature of light, re-
sults from. the interaction between radiation which is reflected by the inner
surfaces and then transm.itted. Unless absorption occurs, m.ost of the radia-
tion a t any gi ven wa velength is transm.itted. A sm.all am.ount, however, is
reflected and then transrn.itted as shown in Figure 3-1, a sim.plified schem.atic
diagram./ The am.ount reflected depends on the difference in the refractive
indexes of the two m.aterials at the reflecting interface.
The reflected radiation, as finally transm.itted, m.ay be exactly in
phase with the radiation not reflected, it m.ay be exactly out of phase, or it
m.ay be som.ewhere in between. li in phase. reinforcem.ent occurs and the
cell (or filrn.) transm.ission is m.axim.um.; if out of phase, destructive inter-
ference occurs and the transm.ission is m.inim.urn. Between the m.axim.a and
m.inirn.a, the transm.ission changes gradually with frequency as radiation
which is neither entirely in phase nor entirely out of phase interacts. As the
spectrophotom.eter scans the cell or film. transrn.ission at one wavelength
after another, a wavy interference fringe pattern em.erges such as that
shown in Figure 3-3 or Figure 3-4.
Page 3- 2
-_ ....
c - - - .... - - .... - -
-- REFLECTEO --- - - - - REFlECTED
TRANSMITTED TRANSMITTED
Fig. 3-1 - Pathof radiation between Fig. 3-2 - Wave patterns for trans-
the inner surfaces of a filITl or cell. rnitted and reflected portions of radia-
Pathof reflected radiation is drawn tion when cell thickness, d, is such
atanang1e to separate itfroITl tha t that 2d ITl the in-phase condition
transrrtted. for a fringe ITlaxiITluITl. The reflected
radiation, as finally transrnitted, is
in phase with that transrnitted directly.
The thickness, d, ofa cellor filITl can be ca1culatedfroITl data obtained
frOITl the fringe pattern by using Equations 1 and 2, be10w.
.o..m -10
4
For cells: d = 2(v1- 2) Equation1
v
For fi1ITls: d = Equation Z
where: d =thickness, inITlicrons ()l)'
vI := frequency atwhichfirstITlaxiITlurn (or ITliniITluITl)
occurs, inwavenuITlber units.
v2 = frequency at which lastrnaxiITlurn (or ITliniITluITl)
occurs, inwavenurnber units.
6rn:= nurnber ofITlaxiITla (or rniniITla) in the interval
froITl vl to vZ. a whole nurnber.
n =index of refractionfor the filITl.
The use of these equations should becoITle apparentwhen perforITling the Pro-
cedure whichfollows. These equations and their origin are discussed in
ITlore detailin the Discussionfollowing the Procedure.
Page 3- 3
PROCEDURE
Part I - Thicknes s of a Sealed Cell
Place an empty sealed cell (nominal thickness 0.015 to 0.3 mm), in
good condition, in the sample beam and obtain the spectrum from 4000 to
650 em-I. The spectrum produced should be similar to that shown in Figure
3- 3 except for the spacing between minima or maxima. The calculation, based
on Equation 1, is demonstrated on the figure with appropriate values of .o.m,
vI and vz. Note that as many fringes as possible are counted in order to re-
duce the effect of errors in measuring vl and vz.
Part II Thickness of a Polymer FUm
Place the polystyrene calibration film in the sample beam oi the in-
strument. Obtain a spectrum irom 4000 to 650 em-I. The curve should be
similar to that shown in Figure 3-4. The interierence iringes used in the
calculation are noted on the curve. In this case, Equation Z should be used.
A refractive index value of 1. 6 was used for polystyrene. The operator should
be able to verify that his polystyrene film is approximately the same thickness
as determined in the example.
DISCUSSION
The phase relation between radiation transmitted straight through a
cell (or film) and that reflected by the inner suriaces and then transmitted
depends on several factors. In the case of the Model 700, where the rays of
incident radiaton are perpendicular, on the a verage, to the cell (or film) sur-
faces, the phase relation depends on the cell or film thickness, d, the radiation
fREQUENCY (eM')
4000 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 650
100 . I . f--
dH - .. . '\AI\/\f.IAIlIf\Af\f\r..f\I'A ,I\/,A 1_
90!, ; . , I ': ;; I I' . "'. "!... v. .. v VIV . '" y .. U . JI'"
,"Ter r" i' 7 .. , y
Fig. 3-3 - Fringe pattern obtained for an empty O. 1 mm thick sealed cell
Page 3-4
FREQUENCY (CM')
4000 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 650
100
_; l
90
ri
i
' ,
70
- l
1 I
I:,
l __<
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10 lL
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,
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I II
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-
f---- ....---'
,rI';

.00
'I -
.05
-1-'-'
" , .. .. _... - ," , . '>l_'

l
-I''''" ---
c- .,
_., ...
I
..
I
..


I' r'
I i
I,
'I
j"-

-\12
..__.
. _- ..... ..
1
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i2ns-'zp-40tl- -
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rum1
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o
Fig. 3-4 Fringepatternobtained with the 0.05 mm thickpolysty
rene calibration saITlple
wavelength, , and inthe case ofa filITl, the indexof refraction, n. lithe
phase relationship andwavelengthareknown, therefore, itis possible to de-
terITline the thickness of an eITlpty celL liinaddition, the index of refraction
for a film is known, thenits thickness can also be found. Exceptfor the in-
dex of refrachon, aIl of this information is available in the fringe patternof
the cellorfilITl transmission. On the other hand, if the filITl thickness is
known from SOITle other measurement, the refractive indexmay be determined.
Figure 3-2 is a modification of Figure 3-1 showing the relation bctwcen
cell thickness and phase ina simplifiedfashion. Here, the cell thickness, d,
is made equal to one wavelength, or d ::: . The reflectedwave travels a dis-
tance 2d farther than the wave not reflected. lithe distance 2d is equal to m
(where m is any whole nUITlber) the reflected and nonreflected waves wiIl eITlerge
frOITl the cell cavity in phase, and the fringe patternwiU show a maximurn; a
ITliniITlUITl will occur when 2d (ITl +1/2). We now have a ITlatheITlatical rela-
tionship between cell thickness and wavelengthwhich is related directly to the
fringe pattern. For any ITlaxiITluITl, the cell thickness is:
d = mi\
Equation 3
2
However, the fringe pattern does not gi ve a value for m directly. It
does showthe wavelengths atwhich various ITlaxirna occur. Since the value
ofITl changes by 1 for adjacentITlaxiITla (or ITlinima), the following relations
can be establishedfor two differentITlaxiITla inthe fringe pattern:
1J2.
Page 3- 5
rnl"l
= 2d (for rna x irnum
1)
rn2"2
= 2d (for rna x irnum 2)
rnl-rn2
2d
-
2d
"1 "2
Solving for d:
d =
"1"2 (rn 1-rn
2
)
2("2-"1)
DITl, then:
Equation 4
Note that in Equation 4, the quantity (.ITl) corresponds to the nUITlber of
ITlaxiITla between wavelengths "1 and "2. For an eITlpty cell, the value of
d depends only on the wavelengths a t which the two chosen ITlaxiITla occur and
the nUITlber of ITlaxITla between theITl.
When the thickness of a filITl ITlust be ITleasured, the nUITlber of waves
in the filITl depends on the index of refraction, n. This value ITlust be obtained
frOITl a handbook or other source. Equaton 3 now becoITles
rn"
d =
2n
and Equation 4 becoITles:
Equation 5
Generally, Equa tions 4 and 5 will enable the user of the Model 700 to
determine the thickness of a cell or filITl. Both equations, however, are based
on the preITlise that the incident radiation is propagated in a direction perpendi-
cular to the flITl or cell surfaces (angle of incidence = 00), which is the normal
situation in the Model 700. If the angle of incidence, f/J. were not 00, it would
be necessary to use the general equation for thickness, which is:
d =
Equation 6
This reduces to when (/> 0.
Page 3- 6
Throughout the discussion above, the calculation cf cell or filITl
ness is based on a unit of wavelength (in the infrared, the ITlicron). It s ITlore
convenient to ITlake the calculation using wavenUITlber units when using the
Mode1700. For any given wavelength, the corresponding wavenuITlber is the
nUI1l.ber of waves which will occur in one c(;nL1nlcLer. li 'ii <.::knglh, \, j.:>
given in ITlicrons, the usual unit for infrared radiation, then the correspondng
wavenurnber is 10
4
/1-. waves per centITleter (CITl- 1).
When wavenuITlber units are used, Equations 1 through 6 ITlust be ITlodi-
fied. Equation 3 for cell thickness, based on n = 1, at a fringe ITlaxiITluITl
becoITles:
10
4
m
d , whe re d is ln ITl c rons;
Equation 7
2v
If d s In centiMeters, then:
m
d =
2v
Equation 1 for cell thicknes 5, based on n ::- 1, becoITle s:
Equation 8 d =
Equation 2 for filITl thickness, based on n I- 1, becoITles:
Am
Equation 9
Equation 6 o ~ fi1ITl thickness, based on n I- 1, and an angle of incidence (j) I 0,
becoITles:
=
6m
Equation 10
d =
d
_ ... _____ _ _ _ _ _ _ M t __
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ex:>
N
25
20
15
10
5
..-
m
N
O
-5
1
4000 3500 3000 2500 2000
Wavenumbers(cm-1
1.0
m
<
l"-
M
..-
~
<
1.0
..-
..-
M
<O
a
<O
m
1000 500
..-
1500

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