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Acknowledgements. . . . . . . . . . . . . . . . xv2 t" v6 j9 h6 A8 s! J* `4 s
Chapter 1 Introduction . . . . . . . . . . . . . . 1
$ W% z' b# u1 Q; G1.1 Additives . . . . . . . . . . . . . . . . . . . . . . . . 2
. q* d" O9 r2 D' j1.1.1 Additive functionality . . . . . . . . . 3
: h( V3 f, I5 }$ \/ y' D1.2 Plastics formulations . . . . . . . . . . . . . . . 5$ k3 G& } b- j. p' D: Q) V
1.2.1 Supply forms . . . . . . . . . . . . . . . 7
6 A s1 S: x' z7 r* q1.2.2 Additive delivery . . . . . . . . . . . . 9
; w" [& g- I2 Y, |. z) X1.3 Economic impact of polymer additives . . 9, K9 K9 W% _" A+ k
1.4 Analysis of plastics . . . . . . . . . . . . . . . . 11
& y- S' j3 r6 E T1 v; T" ^* z1.4.1 Regulations and standardisation . . 151 Y( V9 a. G/ W3 b" T; N
1.4.2 Prior art . . . . . . . . . . . . . . . . . . . 17$ |/ b8 z# Y% X. B( n7 l {
1.4.3 Databases . . . . . . . . . . . . . . . . . . 195 Z8 x8 j! X Y1 U
1.4.4 Scope . . . . . . . . . . . . . . . . . . . . . 208 Q/ v3 G; e2 z- G3 U- P/ D
1.4.5 Chapter overview . . . . . . . . . . . . 22
2 E7 K: j/ Y$ ]. ?4 H6 W Y! A, J1.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 23
/ ]/ \% V( J0 t! D! |1.5.1 Plastics additives . . . . . . . . . . . . . 23
4 j4 x# [9 Q* b8 o1.5.2 Processing technologies . . . . . . . . 23
: m! r! H q1 `& X6 Z1.5.3 Instrumental analysis . . . . . . . . . . 237 Q# i5 \ K8 T& d" l
1.5.4 Polymer analysis . . . . . . . . . . . . . 24& h3 ~5 M0 F. u& C# l
1.5.5 Polymer/additive analysis . . . . . . 24 n+ }, p; n' v& d2 r
1.6 References . . . . . . . . . . . . . . . . . . . . . . . 24
* k3 ]& `" [2 ^1 A5 wChapter 2 Deformulation Principles . . . . 29
. D( e M" s& @2 | O2.1 Polymer identification . . . . . . . . . . . . . . 30, Z! b( \% s" V$ P2 o, p
2.2 Additive analysis of rubbers: ‘Best3 H+ [# e9 O2 ?7 f
Practice’ . . . . . . . . . . . . . . . . . . . . . . . . 323 s+ e# H2 d8 F" B
2.3 Polymer extract analysis . . . . . . . . . . . . . 42
( c' H$ c( O5 h3 a6 G2.4 In situ polymer/additive analysis . . . . . . 46. Q# ^2 d U' X1 h6 I6 M
2.5 Class-specific polymer/additive analysis . 47
! ^1 C; q* r; I% {) J' X4 ~2.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 48
0 u4 V7 ^& j' W) e P6 `8 {! c2.6.1 Polymer identification . . . . . . . . . 48
" K, h0 d( n8 {& `6 o4 b, ?2.6.2 Deformulation of rubbers . . . . . . 482 G2 Q* I4 E1 p$ r# j9 v4 D9 c) L
2.6.3 Deformulation of polymers . . . . . 48
. Z" S9 i, ^' o) G! }5 D& L( H2.7 References . . . . . . . . . . . . . . . . . . . . . . . 48; _' \5 R" y2 k) A
Chapter 3 Sample Preparation
/ v, j. S( A& Q4 G+ w# Q( MPerspectives . . . . . . . . . . . . . . 51
6 i' f6 G+ t. l& ?0 q7 h3.1 Solvents . . . . . . . . . . . . . . . . . . . . . . . . 542 k C% ]& N( W* V6 K
3.1.1 Polymer solubility criteria . . . . . . 55
1 k, X8 {6 U1 s3.1.2 Solubility parameters . . . . . . . . . . 556 M ]% P$ l. n* Q
3.1.3 Polymer solutions . . . . . . . . . . . . 56
$ V( u/ W& i- U# e5 o+ g. f- @8 g3.2 Extraction strategy . . . . . . . . . . . . . . . . . 57
- o1 f; F) W. I! q2 p2 s3.3 Conventional extraction technologies . . . 59
: K$ M7 O; l+ D3.3.1 Liquid–liquid extraction . . . . . . . 60
. v! X5 X6 m7 W& J1 I% S3.3.2 Liquid–solid extraction . . . . . . . . 60
& Y% X# ?9 j9 l7 O% Q! n3.3.3 Classical solvent extractions of
5 f9 W1 k: ?1 g# ` w- }1 D# vadditives from polymers . . . . . . . 61% U$ B1 K8 Y8 t* s$ B
3.3.4 Sonication . . . . . . . . . . . . . . . . . 75# ~! p2 u3 f9 U- ^
3.4 High-pressure solvent extraction methods 81
1 P# Z7 G5 N8 l" D, H! F3.4.1 Supercritical fluid technology . . . 814 K2 P+ f$ G4 F( s# Q( G
3.4.2 Analytical SFE . . . . . . . . . . . . . . 85+ p0 T0 c# R; K6 J& c: m
3.4.3 Subcritical water extraction . . . . . 100) W k# U8 u' Z
3.4.4 Microwave technology . . . . . . . . 101 f5 V+ }! k% I/ Y
3.4.5 Microwave-assisted extractions . . 1047 c5 T* U. a3 y4 z0 N4 T- W0 s
3.4.6 Pressurised fluid extraction . . . . . 117
a& l$ [/ |" c# R3.5 Sorbent extraction . . . . . . . . . . . . . . . . . 123" j0 B2 W, @1 l/ \' ?( H" M
3.5.1 Solid-phase extraction . . . . . . . . . 124
4 i( M! Y" m7 n, P. m. k7 [3.5.2 Solid-phase microextraction . . . . . 129
3 a& P' l6 [4 J7 q- }3.5.3 Stir bar sorptive extraction . . . . . 133
9 ]8 P- c' r+ Y w v3 m5 ]% v1 D% y6 ]3.6 Methodological comparison of extraction
- q# M; x4 i2 o- Emethods. . . . . . . . . . . . . . . . . . . . . . . . . 134
8 f5 r4 v" H5 N$ K6 D3.6.1 Experimental comparisons . . . . . . 136
( F' U8 _3 \4 h7 D% N. p; y' d5 \3.6.2 Extraction selectivity . . . . . . . . . . 138
& l- _1 c% Q' z' B1 x" [, ^' v3.6.3 ‘Nonextractable’ additive analysis 140! e5 P9 [, p: y; b% g/ B* X( p
3.7 Polymer/additive dissolution methods . . . 146
' @( E2 F0 t, E C2 W3.8 Hydrolysis . . . . . . . . . . . . . . . . . . . . . . . 152
! u0 y4 t; O/ _2 N3.9 Bibliography . . . . . . . . . . . . . . . . . . . . . 155
; B4 W3 N& ]0 v. x3.9.1 Sampling and sample preparation 155
; o& D( @6 F+ Y& |# t6 v) J3 A6 U! B8 v3.9.2 Solvents/solubility . . . . . . . . . . . . 155+ p6 q9 ~; q# Z" R7 K; ^) q p
3.9.3 Extraction methods . . . . . . . . . . . 156# w% n* ?, C8 {/ J: H& g
3.10 References . . . . . . . . . . . . . . . . . . . . . . . 156
. }7 J- P( H6 mvi Contents
) }5 z, K- o8 t" c# vChapter 4 Separation Techniques . . . . . . 171
- D) T3 \# R, z0 J( O% E" W4.1 Analytical detectors . . . . . . . . . . . . . . . . 177. X, P9 E) a& K5 N
4.2 Gas chromatography . . . . . . . . . . . . . . . 181
3 T, T+ k$ u; |5 a, }; y4.2.1 High-temperature gas
, t) ?+ b7 j1 p2 Mchromatography . . . . . . . . . . . . . 200
7 `6 Q: e; d1 ^$ p, u2 j. T4.2.2 Headspace gas chromatography . . 2025 ?! c. R0 y$ ~1 ]) x; G1 M
4.3 Supercritical fluid chromatography . . . . . 205
0 P4 f4 [& I7 l$ c& W" ~( W4.4 Liquid chromatography techniques . . . . . 217( _- i' U7 m) q2 g3 n
4.4.1 Planar chromatographies . . . . . . . 218) ^/ m0 ]5 J$ s8 W' U8 \) s
4.4.2 Column chromatographies . . . . . . 230
" G8 Q4 ~6 y @4.5 Capillary electrophoretic techniques . . . . 273/ d8 w% W. j$ X) @" n7 I. c" B
4.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 2780 N s& X. p, W' M4 X
4.6.1 General texts . . . . . . . . . . . . . . . 278+ T: [# }( n/ B" i; x* T3 ^
4.6.2 Detectors . . . . . . . . . . . . . . . . . . 2797 W% g, Q# ]9 A. s4 T2 m1 V
4.6.3 Gas chromatography . . . . . . . . . . 279" u! y; D* e; e' f V# H2 z
4.6.4 Supercritical fluid chromatography 279- ?2 D+ I7 Z' j! n
4.6.5 Thin-layer chromatography . . . . . 2799 j) V1 S$ z+ W' Q* F0 V
4.6.6 Liquid chromatography . . . . . . . . 280
8 N7 P7 `. B0 O3 x) P) Z4.6.7 Size-exclusion chromatography . . 2803 Z- U: m- v9 u6 p, t3 G
4.6.8 Ion chromatography . . . . . . . . . . 280
+ X' }6 n- ]9 t( J9 y1 f4.6.9 Capillary electrophoretic
4 j& `0 R4 d% t( Atechniques . . . . . . . . . . . . . . . . . 2800 x: A! e# b' w, Z+ p" q
4.7 References . . . . . . . . . . . . . . . . . . . . . . . 281
: z E! h+ |* CChapter 5 Polymer/Additive Analysis:: D9 m/ m- Y3 n; s, I( h" _
The Spectroscopic Alternative 2999 q/ x# g( g8 j) r! d3 T
5.1 Ultraviolet/visible spectrophotometry . . . 302; d( | p% ] T2 x6 @/ U# A# D6 z
5.2 Infrared spectroscopy . . . . . . . . . . . . . . . 311
/ p& }# p$ G% O4 W" J/ C5.3 Luminescence spectroscopy . . . . . . . . . . 318
9 x, P2 X, ^$ O+ I5.4 High-resolution nuclear magnetic7 L- v; F: x% t1 ]: f
resonance spectroscopy . . . . . . . . . . . . . 323
\6 q T6 X/ s5.4.1 Multidimensional NMR/ s8 J2 Q7 |, k& |
spectroscopy . . . . . . . . . . . . . . . . 336
2 F; B- L0 w$ `) ]" y5.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 342
! J7 I6 G6 y- `4 ?5.5.1 General spectroscopy . . . . . . . . . 342
+ _. @5 S) h; L5 k5.5.2 Ultraviolet/visible
, }8 B& e- d) E8 _spectrophotometry . . . . . . . . . . . . 3427 C: @# O9 F/ H6 I
5.5.3 Infrared spectroscopy . . . . . . . . . 342
# Y- c, y& i7 w& \! d) _5.5.4 Luminescence spectroscopy . . . . . 342
' F" l- v5 q2 ]+ R, \5.5.5 Nuclear magnetic resonance
, b* V6 v8 w q& Ispectroscopy . . . . . . . . . . . . . . . . 342& M5 C" Q" N* y8 C
5.6 References . . . . . . . . . . . . . . . . . . . . . . . 342
/ Y( O- Q _& e/ @( PChapter 6 Organic Mass-Spectrometric
1 [/ f8 f5 l. |/ s7 Q" J( wMethods . . . . . . . . . . . . . . . . 3493 w" j. o, i% |/ q+ |( B* R8 f
6.1 Basic instrumentation . . . . . . . . . . . . . . . 3516 x* D- M7 M2 B+ e7 {& Z
6.1.1 Inlet systems . . . . . . . . . . . . . . . . 352
* `, [ c2 Q, ^' l$ i6.1.2 Modes of detection . . . . . . . . . . . 3533 }* Q' q: [) d3 b0 P0 L
6.1.3 Mass resolution . . . . . . . . . . . . . . 354
4 |: b/ X$ b. y8 p9 q" o1 \6.1.4 Isotope distributions . . . . . . . . . . 354
4 N& o8 Q! m7 w! P: Z6.1.5 Accurate mass measurements. . . . 355 b, ?0 |8 v! H1 ~& T; y' K
6.2 Ion sources . . . . . . . . . . . . . . . . . . . . . . 357& F0 b* g0 ]& _3 y% y" h
6.2.1 Electron impact ionisation . . . . . . 360
( s5 B$ b" M0 z6.2.2 Chemical ionisation . . . . . . . . . . . 362
7 S3 u0 e0 v( F. G' f, x6.2.3 Metastable atom bombardment . . 367
& k; h0 C8 n- |2 k% m6.2.4 Fast atom bombardment . . . . . . . 3678 ]3 j4 U+ B' ?$ ]7 c+ f9 S. f8 H( `( Q
6.2.5 Field ionisation . . . . . . . . . . . . . . 372
2 o' ^( y, F4 `/ z6.2.6 Field desorption . . . . . . . . . . . . . 3740 H6 K/ f+ a1 [* ]* M& {
6.2.7 Thermospray ionisation . . . . . . . . 376
& B* c; Q! `5 E8 }) O/ {! W6.2.8 Atmospheric pressure ionisation
4 \* s: F$ B4 q2 {techniques . . . . . . . . . . . . . . . . . 378
7 h2 N0 U9 S+ U' H) E# t6.2.9 Desorption/ionisation methods . . . 3832 W/ {5 H$ v, A; `% @& R0 r4 O/ y
6.2.10 Photoionisation techniques. . . . . . 385
: X$ | E+ V/ }6 M q; w6.3 Mass analysers . . . . . . . . . . . . . . . . . . . 3869 |' z4 ?$ ^$ C" v8 G% @, \
6.3.1 Sector analysers . . . . . . . . . . . . . 387
' j! X y: S; H4 Z0 A2 L6.3.2 Quadrupole mass spectrometers . . 389% ]4 z% \# X7 s( \! h
6.3.3 Time-of-flight mass spectrometry . 390 I i: p6 o5 [ N. z: W8 s7 }
6.3.4 Quadrupole ion trap . . . . . . . . . . 393
$ J1 b) J4 D3 H7 R" J6.3.5 Fourier-transform ion-cyclotron! e h& c+ Q# g- p; G
resonance mass spectrometry . . . . 395
3 U2 K! W6 l; [: r6.3.6 Tandem mass spectrometry . . . . . 398
! {/ p2 A$ u9 R. n) r6.4 Direct mass-spectrometric polymer
! c1 ~' b6 g, V% Ocompound analysis . . . . . . . . . . . . . . . . . 407
# m& d/ |' Q2 p# f6.5 Ion mobility spectrometry . . . . . . . . . . . 4150 p% w8 p$ {( B( H5 z- v- {0 Z) |" ^
6.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 417
1 H( G# a6 s" |+ u# V6.6.1 Mass spectrometry (General) . . . . 4177 _- S: o( U6 h8 n1 i
6.6.2 Mass spectrometers . . . . . . . . . . . 417
8 L; D; }$ P* K8 G6.6.3 Ionisation modes . . . . . . . . . . . . . 417
3 G" r: `" F% d) m6.7 References . . . . . . . . . . . . . . . . . . . . . . . 418( |$ g9 [, i- T7 Z+ \
Chapter 7 Multihyphenation and) D1 G$ h, O0 v M# P6 y
Multidimensionality in% J7 t" Q t! c Y4 T
Polymer/Additive Analysis . . . 425; x% r9 Y# [, S- D2 c9 {/ q5 _
7.1 Precolumn hyphenation . . . . . . . . . . . . . 428
# m' _$ U0 _6 s7.1.1 Chromatographic sampling
0 k7 B: J( f' z6 y2 r: `6 Z8 umethods . . . . . . . . . . . . . . . . . . . 432
" j+ b2 a- y3 k7.2 Coupled sample
2 u& B8 q2 z5 R5 G8 B. M( }9 Ipreparation – spectroscopy/spectrometry . 449& j% {7 r# u2 q
7.3 Postcolumn hyphenation . . . . . . . . . . . . . 452
! Q9 A/ k% b$ }6 D7.3.1 (Multi)hyphenated GC techniques 456
! ^' P5 s0 P4 d3 i) T2 S7.3.2 (Multi)hyphenated SFC; Q2 N/ u1 S/ @# p% A1 A7 d- O
techniques . . . . . . . . . . . . . . . . . 475
' h; u: }$ q* Y! H5 ]7.3.3 (Multi)hyphenated HPLC
# O" g, }, X, Etechniques . . . . . . . . . . . . . . . . . 489
' S$ V7 I* W- z7.3.4 Hyphenated SEC techniques . . . . 5273 _4 Y( C6 M# Q2 r" B" l3 Z3 R
7.3.5 Hyphenated TLC techniques . . . . 530
+ \, x8 b# J* y( ^& J4 `7.3.6 Hyphenated CE techniques . . . . . 543
[7 p5 O* r B# \- n* vContents vii- d( N- I, L$ Z% ~! Z* Y
7.4 Multidimensional chromatography . . . . . 545
( n# C) M. `$ q* n, l! }7.4.1 Multidimensional gas( n$ K8 y( E, m6 G
chromatography . . . . . . . . . . . . . 548
2 h' N3 ~8 s; g& K3 I5 `7.4.2 Multidimensional supercritical
) m; v5 ]" g- C0 u Q: X- wfluid chromatography . . . . . . . . . 550
$ ?7 j6 x9 }' O3 y1 p7.4.3 Multidimensional liquid
7 ?, d7 L$ p8 m& y( Cchromatography . . . . . . . . . . . . . 550
& q& u* H2 G& l; c8 p/ ~7.4.4 Multidimensional thin-layer
! ^# f0 @& M/ }& ]/ l7 ~* ?chromatography . . . . . . . . . . . . . 558
8 H; ~. z7 V- l6 n) J0 |; i7.5 Multidimensional spectroscopy . . . . . . . . 5608 w$ O- X( ]+ q: I% I, `& s1 \8 I' U6 Z
7.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 562
8 Q; I5 B! E4 m2 Y' w; z7.6.1 General . . . . . . . . . . . . . . . . . . . 562; s7 k4 f {& [1 W7 j0 P( d0 t- M7 r% a
7.6.2 Multihyphenation and
" v: e/ x6 ], C- U7 j# p* R! u5 \multidimensionality . . . . . . . . . . . 563
* t3 k- |5 L5 K, g3 M7.6.3 Precolumn hyphenation . . . . . . . . 563
8 g, Q& V- |0 ^3 L& `9 y$ H7 |7.6.4 Postcolumn hyphenation . . . . . . . 563- v2 Z: K% \' z+ D
7.6.5 Multidimensional chromatography 563
3 ~4 V: e& k, o N" x7.6.6 Multidimensional spectroscopy . . 563& v3 b3 [: K( U; V
7.7 References 564
* ]. i/ Y9 \# M0 iChapter 8 Inorganic and Element
: c% p% \- B* |* C- M$ G* c! BAnalytical Methods . . . . . . . . 585
' h9 X. Y k5 M6 V7 m8.1 Element analytical protocols . . . . . . . . . . 587
* C7 L$ T/ n) |0 X* J1 k8.1.1 Element analytical pretreatment
" h: P( M; X- P" s# r6 S6 Qprotocols . . . . . . . . . . . . . . . . . . 588
+ b: {7 r7 N& J! r$ Y$ S# r% d8.1.2 Elemental analysis methods . . . . . 589
U5 ]2 Y+ ~4 P1 C- U& S! W8.2 Sample destruction for classical elemental
6 e3 R& ^% [1 P) ]analysis . . . . . . . . . . . . . . . . . . . . . . . . . 5916 a" J: F E2 l. T- S' }4 u
8.2.1 Combustion analysis . . . . . . . . . . 593
, {1 W( ?1 h& }! q+ N1 O/ O+ N8 D1 `8.2.2 Wet matrix digestion . . . . . . . . . . 5976 B0 @9 W; S0 Z4 {) r
8.2.3 Fusion methods . . . . . . . . . . . . . . 604
3 ~4 v3 ?. Q) G" \. P8.3 Analytical atomic spectrometry . . . . . . . . 605
) J1 B i1 h2 O) Q9 z0 E- S8.3.1 Atomic absorption spectrometry . 608
/ D8 ]9 a! T) {1 X& ^1 [8.3.2 Atomic emission spectrometry . . . 613
" W! y$ N5 d4 a8.3.3 Atomic fluorescence spectrometry 624 |
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