Polymer characterization : laboratory techniques and analysis

254 Pages·1996·13.639 MB·English

by  Nicholas P Cheremisinoff

POLYMER
CHARACTERIZATION
Laboratory Techniques and Analysis
Nicholas P. Cheremisinoff, Ph.D.
NOYES PUBLICATIONS
We,hc.od, 11ew. l.ny, U.S.A.
thgirypoC 0 1996 yb seyoN snoitacilbuP
oN trap fo siht koob yam eb decudorper ro dezilitu ni
yna mrof ro yb yna ,snaem cinortcele ro ,lacinahcem
gnidulcni ,gniypocotohp gnidrocer ro yb yna -amrofni
noit egarots dna laveirter ,metsys tuohtiw noissimtep
ni gnitirw morf eht .rehsilbuP
yrarbiL fo ssergnoC golataC draC :rebmuN 96010912
:NBSI 0-8155-1403-4
detnirP ni eht detinU setatS
dehsilbuP ni eht detinU setatS fo aciremA yb
seyoN snoitacilbuP
369 weivriaF eunevA
,doowtseW weN yesreJ 07675
10987654321
yrarbiL fo ssergnoC noitacilbuP-ni-gnigolataC Data
,ffonisimerehC salohciN .P
remyloP noitaziretcarahc : yrotarobal seuqinhcet dna sisylana / yb
salohciN .P .ffonisimerehC
.p .mc
sedulcnI .xedni
NBSI O-8155-1403-4
1. .sisylanA--sremyloP .I .eltiT
QD139.P6C483 1996
620.1’92’0287--dc20 96-10912
PIC
Nicholas P. Cheremisinoff is a etavirp tnatlusnoc ot ,yrtsudni
,aimedaca and .tnemnrevog eH has ylraen ytnewt sraey fo
yrtsudni and deilppa hcraeser ecneirepxe ni ,sremotsale
citehtnys ,sleuf slacimehcortep ,gnirutcafunam and -norivne
latnem .lortnoc A lacimehc reenigne yb ,edart eh has derohtua
revo 100 gnireenigne skoobtxet and has detubirtnoc ylevisnetxe
ot eht lairtsudni .sserp eH is yltnerruc gnikrow rof eht detinU
setatS ycnegA rof lanoitanretnI tnempoleveD ni nretsaE
,eniarkU erehw eh is managing eht lairtsudnI Waste -eganaM
tnem .tcejorP .rD ffonisimerehC deviecer his ,.S.B M.S., and
.D.hP seerged morf noskralC egelloC fo .ygolonhceT
V
NOTICE
oT the tseb of ruo egdelwonk the noitamrofni ni siht -bup
noitacil si ;etarucca ,revewoh the rehsilbuP does ton emussa
yna ytilibisnopser or ytilibail for the ycarucca or ssenetelpmoc
of, or secneuqesnoc gnisira ,morf hcus .noitamrofni sihT koob
si dednetni for lanoitamrofni sesoprup .ylno noitneM of trade
seman or laicremmoc stcudorp does ton etutitsnoc tnemesrodne
or noitadnemmocer for esu yb the .rehsilbuP laniF -mreted
noitani of the ytilibatius of yna noitamrofni or tcudorp for esu
detalpmetnoc yb yna ,resu dna the rennam of that ,esu si the
elos ytilibisnopser of the .resu eW dnemmocer that enoyna -ni
gnidnet ot yler no yna noitadnemmocer of slairetam or -orp
serudec denoitnem ni siht noitacilbup dluohs yfsitas flesmih as
ot hcus ,ytilibatius dna that he nac teem lla elbacilppa ytefas
dna htlaeh .sdradnats
. . .
Vlll
PREFACE
sihT emulov sedivorp na weivrevo fo remylop noitaziretcarahc
tset .sdohtem ehT sdohtem dna noitatnemurtsni debircsed
tneserper nredom lacitylana seuqinhcet lufesu ot ,srehcraeser
tcudorp tnempoleved ,stsilaiceps dna ytilauq lortnoc strepxe
ni remylop sisehtnys dna .gnirutcafunam ,sreenignE remylop
stsitneics dna snaicinhcet lliw dnif siht emulov lufesu ni
gnitceles sehcaorppa dna seuqinhcet elbacilppa ot -carahc
gniziret ,ralucelom ,lanoitisopmoc ,lacigoloehr dna -omreht
cimanyd seitreporp fo sremotsale dna .scitsalp
tI si laitnesse taht htob D&R seirotarobal as llew as ytilauq
lortnoc snoitcnuf eb desrev ni eht suoirav seuqinhcet debircsed
ni siht koob ni redro ot ylreporp ngised rieht stcudorp dna ot
erusne eht tsehgih ytilauq sremylop no eht tekram .ecalp sihT
emulov si ylralucitrap lufesu ni gnicudortni dradnats remylop
noitaziretcarahc yrotarobal seuqinhcet ot snaicinhcet dna -ne
sreenig gninnigeb rieht sreerac ni remylop gnirutcafunam dna
tcudorp tnempoleved areas.
A egral noitrop fo siht emulov si desirpmoc fo secidneppa
gnidivorp snoitinifed fo gnitset dna tcudorp noitaziretcarahc
.smret esehT snoitces are dednetni ot edivorp eht redaer htiw
a lacitcarp ecruos fo latnemadnuf .noitamrofni ehT rohtua
sehsiw ot dnetxe edutitarg ot adniL iksbezrtsaJ rof reh
ecnatsissa ni gnizinagro dna gnittesepyt siht .koob
salohciN .P ffonisimerehC
iiv
CONTENTS
1. CHROMATOGRAPHIC TECHNIQUES ............... 1
Chromatography for Analytical Analyses ............ 1
Gas Chromatography .......................... 1
lareneG .................................. 1
sepyT fo Gas yhpargotamorhC .................. 3
Liquid Chromatography ........................ 3
lareneG .................................. 3
sepyT fo diuqiL yhpargotamorhC ................ 5
epyT fo noitamrofnI deniatbO ................... 6
segatnavdA ................................ 7
segatnavdasiD .............................. 7
secnerefretnI ............................... 7
GPC/DRI ................................... 7
Gel Permeation Chromatography .................. 8
GPC/DRI/LALLS ............................ 10
GPC/DRI/VIS ............................... 11
GPC/DRI/UV ............................... 11
GPC/DRI/FTIR .............................. 15
Submitting Samples ......................... 15
2. THERMAL ANALYSIS .......................... 17
General Principles of Operation .................. 17
Thermal Analysis of Polymers ................... 19
Differential Scanning Calorimetry (DSC) .......... 20
ThermogravimetricA nalysis (TGA) .............. 20
Thermomechanical Analysis (TMA) .............. 20
Dynamic Mechanical Thermal Analysis (DMTA) .... 23
xi
stnetnoC
X
3. MICROSCOPY FOR POLYMER
CHARACTERIZATION .......................... 25
General Information .......................... 25
Non-Routine Techniques ....................... 27
4. ELEMENTAL AND STRUCTURAL
CHARACTERIZATION TESTS .................... 43
Atomic Absorption Spectroscopy ................. 43
Inductively Coupled Plasma Atomic Emission
Spectroscopy .............................. 45
Ion Chromatography (IC) ...................... 48
Ion Selective Electrodes (ISE) ................... 52
Mass Spectrometry (MS and GC/MS) ............. 55
Nuclear Magnetic Resonance Spectrometer .......... 60
elpmaS noitaraperP ......................... 62
dehsilbatsE sdohteM yb H‘ NMR ............... 63
Fourier Transform Infrared (FI’IR) ............... 64
Ultraviolet, Visible, and Infrared Spectrometry
(UV, Vis, IR) .............................. 64
X-Ray Fluorescence Spectrometry ................ 73
Potentiometric Titrations ....................... 78
Neutron Activation Analysis ..................... 80
5. RHEOMETRY ................................. 83
Rheometrics System IV ........................ 83
Capillary Rheometry .......................... 85
Torque Rheometry ........................... 87
6. CHEMICAL ANALYSIS OF POLYMERS ............ 97
Comminution, Separation, and Identification ........ 97
Stabilizer Identification ....................... 100
Polymer Identification ........................ 102
APPENDIX A: ABBREVIATIONS OF POLYMERS . . . . . . . 105
APPENDIX B: GLOSSARY OF POLYMERS
AND TESTING . . . . . . . . . . . . . . . , . . . . . . . . . . . . . . . . . . 107
APPENDIX C: PROFESSIONAL AND TESTING
ORGANIZATIONS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117
American National Standards Institute (ANSI) . . . . . . 117
stnetnoC ix
American Society for Testing and
Materials (ASTM) ......................... 117
Food and Drug Administration (FDA) ............ 118
National Bureau of Standards (NBS) ............. 119
National Electrical Manufacturers
Association (NEMA) ........................ 119
National Fire Protection Association (NFPA) ....... 120
National Sanitation Foundation (NSF) ............ 120
Plastics Technical Evaluation Center (Plastec) ...... 121
Society of Plastics Engineers (SPE) ............... 122
Society of Plastics Industry (SPI) ................ 122
Underwriters Laboratories (UL) ................. 123
APPENDIX D: GLOSSARY OF ENGINEERING AND MATERIALS
TERMS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 125
INDEX . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 235
CIHPARGOTAMORHC SEUQINHCET
1
YHPARGOTAMORHC ROF LACITYLANA SESYLANA
yhpargotamorhC yam eb denifed as eht noitarapes fo ralucelom serutxim
yb noitubirtsid neewteb owt ro erom ,sesahp eno esahp gnieb yllaitnesse
lanoisnemid-owt (a )ecafrus dna eht gniniamer ,esahp ro gnieb a klub
esahp thguorb otni tcatnoc ni a tnerruc-retnuoc noihsaf htiw eht -owt
lanoisnemid .esahp suoiraV sepyt fo lacisyhp setats fo yhpargotamorhc
are ,elbissop gnidneped no eht sesahp .devlovni
yhpargotamorhC si dedivid otni owt niam .sehcnarb enO hcnarb si
sag ,yhpargotamorhc eht rehto si diuqil .yhpargotamorhc diuqiL
yhpargotamorhc nac eb rehtruf dedividbus as nwohs ni erugiF 1.
ehT ecneuqes fo cihpargotamorhc no.itarapes si as :swollof A elpmas
si decalp at eht pot fo a nmuloc erehw sti stnenopmoc are debros dna
debrosed yb a carrier. sihT gninoititrap ssecorp srucco yldetaeper as eht
elpmas sevom sdrawot eht teltuo fo eht .nmuloc hcaE etulos slevart at
sti nwo rate hguorht eht ,nmuloc ,yltneuqesnoc a dnab gnitneserper hcae
etulos lliw mrof no eht .nmuloc A rotceted dehcatta ot eht s’nmuloc
teltuo sdnopser ot hcae .dnab ehT tuptuo fo rotceted esnopser susrev
emit si dellac a .margotamorhc ehT emit fo ecnegreme seifitnedi eht
,tnenopmoc dna eht kaep area senifed sti ,noitartnecnoc desab no
noitarbilac htiw nwonk .sdnuopmoc
SAG YHPARGOTAMORHC
General
fI eht gnivom esahp si a ,sag neht eht euqinhcet si dellac sag
yhpargotamorhc (GC). nI sag yhpargotamorhc eht elpmas si yllausu
1
CHROMATOGRAPHY
GAS LIQUID
+l
GLC GSC LLC LSC ION
EXCHANGE
I I
PC TLC EXCLU! Sl[ ON
GEL
PERMEATION
GEL
FILTRATION
Figure 1. Shows types of chromatographic operations.
. _, - _ .- _ - .___ ,.._ _- _ ___. __. . . . -