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Acknowledgements. . . . . . . . . . . . . . . . xv
& _( M9 F# s. f mChapter 1 Introduction . . . . . . . . . . . . . . 1: d* C' J w! d* x
1.1 Additives . . . . . . . . . . . . . . . . . . . . . . . . 2
$ h. F0 _1 @. k* b1 }! q- J1.1.1 Additive functionality . . . . . . . . . 3
# f; e4 o1 Z, x; ? G1.2 Plastics formulations . . . . . . . . . . . . . . . 5: { ^: C5 @; a1 t8 ]
1.2.1 Supply forms . . . . . . . . . . . . . . . 74 R ?/ T% g0 C# z
1.2.2 Additive delivery . . . . . . . . . . . . 9
! S. S+ k$ _. G/ p" K W" P7 d1.3 Economic impact of polymer additives . . 9- h, D& O. G7 e9 B* G
1.4 Analysis of plastics . . . . . . . . . . . . . . . . 11
5 e5 F$ @# {+ z1.4.1 Regulations and standardisation . . 15
$ Z7 t+ f$ Q6 O1.4.2 Prior art . . . . . . . . . . . . . . . . . . . 175 G ?6 B% j- v, Q6 ]' C6 z
1.4.3 Databases . . . . . . . . . . . . . . . . . . 19
$ Q# g y9 n) P! K% w& I1.4.4 Scope . . . . . . . . . . . . . . . . . . . . . 20
+ u; W- v' A. r1.4.5 Chapter overview . . . . . . . . . . . . 22
5 E1 F" j& k4 [6 A$ M& R1.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 23) @& U, d2 \( [! ^
1.5.1 Plastics additives . . . . . . . . . . . . . 23
4 G' q! w3 Z' |* }1 u$ P1.5.2 Processing technologies . . . . . . . . 237 k$ y$ ?& |7 x2 A# U
1.5.3 Instrumental analysis . . . . . . . . . . 23( n1 ^$ V% m$ b* o' ~3 y; ]5 x9 m
1.5.4 Polymer analysis . . . . . . . . . . . . . 24
9 m" E. @2 u+ W' ]7 q1 o7 D1.5.5 Polymer/additive analysis . . . . . . 248 Z4 a( P9 B6 b/ {9 W. n- K
1.6 References . . . . . . . . . . . . . . . . . . . . . . . 24& b7 y0 g. d$ |& |, A4 A; Q4 {# n3 P
Chapter 2 Deformulation Principles . . . . 29
8 T T( H' z9 l2.1 Polymer identification . . . . . . . . . . . . . . 30
# K$ W+ t+ X" h% w5 [7 y# k2.2 Additive analysis of rubbers: ‘Best* m3 s$ b N7 s. X" A5 @. U" ]
Practice’ . . . . . . . . . . . . . . . . . . . . . . . . 329 J$ o% f- w3 w6 L; K
2.3 Polymer extract analysis . . . . . . . . . . . . . 420 Y! h' M0 p5 N$ `: K
2.4 In situ polymer/additive analysis . . . . . . 46
! H$ h3 G- w* C: ]' c, @/ B7 u* Q2.5 Class-specific polymer/additive analysis . 47) S8 B& x- w" h1 u* G
2.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 48
4 O; g3 g4 \ z v& ?! a2.6.1 Polymer identification . . . . . . . . . 48
9 R) f5 G) ^2 F! E/ V7 N' M2.6.2 Deformulation of rubbers . . . . . . 484 d0 |% n5 G- s; A
2.6.3 Deformulation of polymers . . . . . 486 \* K! C+ @9 `, L& r$ @
2.7 References . . . . . . . . . . . . . . . . . . . . . . . 482 T6 i/ C# D2 \
Chapter 3 Sample Preparation
" Q( h7 S! O8 {. j- k5 RPerspectives . . . . . . . . . . . . . . 51
8 f! H' L) T# \3 M! B0 E: y; @4 {3.1 Solvents . . . . . . . . . . . . . . . . . . . . . . . . 54& e3 a; K) [ s6 F& m& K# a
3.1.1 Polymer solubility criteria . . . . . . 55
; M+ c: ?) s! z3 ^. D- @; L$ {3.1.2 Solubility parameters . . . . . . . . . . 55; B# A! b8 x2 B: b- K8 ?; w% ^
3.1.3 Polymer solutions . . . . . . . . . . . . 568 z+ R, z" N) F/ P9 v! P0 ~
3.2 Extraction strategy . . . . . . . . . . . . . . . . . 57
0 p H9 E6 B; X2 \0 _3.3 Conventional extraction technologies . . . 59
6 g2 U4 J4 N; t. h+ g* B3.3.1 Liquid–liquid extraction . . . . . . . 60
7 g: i) ]% _5 G3.3.2 Liquid–solid extraction . . . . . . . . 60
7 k" r. ]' s5 V; \# M3.3.3 Classical solvent extractions of: V/ F. [3 {# O, h" D5 J
additives from polymers . . . . . . . 61
. B! W2 J& B$ U- ~; r* z- d+ ~3.3.4 Sonication . . . . . . . . . . . . . . . . . 75
% F+ z% R' ^2 \9 H3.4 High-pressure solvent extraction methods 81/ l+ S# Y0 ^6 b, x# D
3.4.1 Supercritical fluid technology . . . 81( U! C3 z6 F; ~6 R3 W J
3.4.2 Analytical SFE . . . . . . . . . . . . . . 85
$ q& _: J# P, T1 ~3 c. ~6 Y3.4.3 Subcritical water extraction . . . . . 100
/ u# r" Q0 h& a3.4.4 Microwave technology . . . . . . . . 101
9 [) {: \2 L3 v# L& y. D" H3.4.5 Microwave-assisted extractions . . 104
& Y- @. y. h2 e" m3.4.6 Pressurised fluid extraction . . . . . 117
# o1 ~, j4 Q0 f$ j5 x$ f& f. d3.5 Sorbent extraction . . . . . . . . . . . . . . . . . 123
& D0 G% f( ^; F$ M: z3.5.1 Solid-phase extraction . . . . . . . . . 124$ l; r" {/ } x( X4 m; I. k- x
3.5.2 Solid-phase microextraction . . . . . 1292 p3 u% Z. M2 [7 C, `7 U) e
3.5.3 Stir bar sorptive extraction . . . . . 133- M# J# ^+ j2 M3 i/ O
3.6 Methodological comparison of extraction* Q/ ^' l9 s. c! v8 _
methods. . . . . . . . . . . . . . . . . . . . . . . . . 134
1 m. _5 V# q0 w3.6.1 Experimental comparisons . . . . . . 136! r. @ Q6 Q+ e) F; O6 M
3.6.2 Extraction selectivity . . . . . . . . . . 138 c. b" ~/ v f0 G" a, F
3.6.3 ‘Nonextractable’ additive analysis 140
* m2 N/ o) g3 d7 P4 @9 a3.7 Polymer/additive dissolution methods . . . 146
?! ?6 Z* c( l* }6 p3.8 Hydrolysis . . . . . . . . . . . . . . . . . . . . . . . 152" @' V- o# }: o7 n1 A
3.9 Bibliography . . . . . . . . . . . . . . . . . . . . . 1552 o, U+ |- e# v: y1 B4 o( e: T
3.9.1 Sampling and sample preparation 155# F3 m) C6 x4 J4 Z: w
3.9.2 Solvents/solubility . . . . . . . . . . . . 1559 k- D+ l, ]1 K1 f! X/ t
3.9.3 Extraction methods . . . . . . . . . . . 156; P) v! m% O# I0 _3 _
3.10 References . . . . . . . . . . . . . . . . . . . . . . . 156% I% u# s; G8 T0 B' s
vi Contents
" G0 F9 V" I0 tChapter 4 Separation Techniques . . . . . . 171
+ g6 H% a3 ]" T, W4.1 Analytical detectors . . . . . . . . . . . . . . . . 1772 x# G; j; |$ N; y. a5 B+ e B+ \, |' G
4.2 Gas chromatography . . . . . . . . . . . . . . . 181: o0 N4 G1 x) X( @0 ?# t
4.2.1 High-temperature gas0 I7 K, G3 u# {& T- V. x4 Z! c( a
chromatography . . . . . . . . . . . . . 200
+ ^" S1 K. N7 E. C5 N% r4.2.2 Headspace gas chromatography . . 202
8 P6 F( `& J2 K" w5 \' h5 J, E+ D4.3 Supercritical fluid chromatography . . . . . 2050 o! L8 u( e/ q# u
4.4 Liquid chromatography techniques . . . . . 217- C4 n5 h4 Q$ Q5 u/ j
4.4.1 Planar chromatographies . . . . . . . 218
) E+ \* q3 o4 Y+ E( h2 g1 J# p4.4.2 Column chromatographies . . . . . . 230* q+ X/ ~ E9 `# x5 e
4.5 Capillary electrophoretic techniques . . . . 273
7 W" G" T& K! j: a6 t8 ~4.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 278
$ [5 O* N+ Z* p3 H1 w4.6.1 General texts . . . . . . . . . . . . . . . 278: s' V( K7 }* t% p0 b9 K1 S
4.6.2 Detectors . . . . . . . . . . . . . . . . . . 279
z: M0 i) j4 W$ ?4.6.3 Gas chromatography . . . . . . . . . . 279, b7 D6 t ^# R9 ~3 _1 s. U
4.6.4 Supercritical fluid chromatography 279
/ V4 X* V: O& K( {( f4 c& T; `4.6.5 Thin-layer chromatography . . . . . 279
0 D2 `/ h; l5 z" r% F, o4.6.6 Liquid chromatography . . . . . . . . 280/ ]& R* t1 J* I" L% a e; g
4.6.7 Size-exclusion chromatography . . 280+ N; ~# f$ X2 h- N" y* D
4.6.8 Ion chromatography . . . . . . . . . . 2804 U- h3 `% J1 x) _9 y5 _6 G) E/ V
4.6.9 Capillary electrophoretic
|5 n+ \6 k+ }7 d& I& ]techniques . . . . . . . . . . . . . . . . . 2807 n# k/ x9 Y) W
4.7 References . . . . . . . . . . . . . . . . . . . . . . . 281
8 i3 @0 ^/ i+ RChapter 5 Polymer/Additive Analysis:
3 \1 D( c5 y& q8 L' ^! O1 a+ wThe Spectroscopic Alternative 299& z) B' w( w& g0 b* A f6 @! l
5.1 Ultraviolet/visible spectrophotometry . . . 302
, b4 d8 m. O( H2 `. u/ i4 J5.2 Infrared spectroscopy . . . . . . . . . . . . . . . 3115 A) E6 ~9 J! Z: ], }# w, _: f
5.3 Luminescence spectroscopy . . . . . . . . . . 318
# M* V3 c( |5 E! p. h8 l5.4 High-resolution nuclear magnetic
9 |) ~7 b4 v& v5 J- rresonance spectroscopy . . . . . . . . . . . . . 323
+ O, Q6 [. j: M$ O5.4.1 Multidimensional NMR
5 n. k" x o' e- Yspectroscopy . . . . . . . . . . . . . . . . 336
r" i# S* G# ~- R5.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 342
3 u; L. r5 G0 z( Y5.5.1 General spectroscopy . . . . . . . . . 342, k) Y$ t- L2 Z& E
5.5.2 Ultraviolet/visible' u. H3 c0 W8 f+ ^7 s8 d) i
spectrophotometry . . . . . . . . . . . . 342
9 s1 Y' `0 l4 w+ r0 z5.5.3 Infrared spectroscopy . . . . . . . . . 342+ v. o' N' q: K/ q- w) Q
5.5.4 Luminescence spectroscopy . . . . . 342
4 C) L" f6 t+ q x% {5.5.5 Nuclear magnetic resonance) }2 {! `& P h
spectroscopy . . . . . . . . . . . . . . . . 342* O* Q h s9 A# @4 y! n
5.6 References . . . . . . . . . . . . . . . . . . . . . . . 342
1 E# |) ~# b2 p6 |7 C0 EChapter 6 Organic Mass-Spectrometric
) L" y' P7 w2 P9 Q `% ZMethods . . . . . . . . . . . . . . . . 349
0 c/ q9 y2 w$ ?0 b" @+ ~- \6.1 Basic instrumentation . . . . . . . . . . . . . . . 351
# K. X* x+ B8 u: g6.1.1 Inlet systems . . . . . . . . . . . . . . . . 352- e! S! `* P1 _7 ?& [% z
6.1.2 Modes of detection . . . . . . . . . . . 353
$ C- t3 T5 _6 T6.1.3 Mass resolution . . . . . . . . . . . . . . 354
* Z% L% Y4 b# C3 V; T" G [. f6.1.4 Isotope distributions . . . . . . . . . . 354 F, C) C: L+ ^/ }
6.1.5 Accurate mass measurements. . . . 355' f2 Q' n3 F# ]+ l' p! K
6.2 Ion sources . . . . . . . . . . . . . . . . . . . . . . 357
0 o+ w( b# c% z: b6.2.1 Electron impact ionisation . . . . . . 3600 \6 U" O7 i3 S! F1 M7 Y
6.2.2 Chemical ionisation . . . . . . . . . . . 3629 M& j4 B( Z' t9 `4 R/ R% E: G
6.2.3 Metastable atom bombardment . . 367
3 c2 K2 w3 A2 |% [) P6.2.4 Fast atom bombardment . . . . . . . 367
& U+ v8 H% C% q+ e6.2.5 Field ionisation . . . . . . . . . . . . . . 372
5 g/ E: G" L" O: ?( y1 g6.2.6 Field desorption . . . . . . . . . . . . . 374
( M! R3 {3 C S& o6.2.7 Thermospray ionisation . . . . . . . . 376
: h3 f( l4 F' P G4 W- D8 L8 B6.2.8 Atmospheric pressure ionisation( g1 P4 E8 b+ K9 J/ w7 r' n
techniques . . . . . . . . . . . . . . . . . 378 T* ]! ?# D) p3 g. D% v
6.2.9 Desorption/ionisation methods . . . 383, F6 `& I+ E, c2 F+ V5 | t
6.2.10 Photoionisation techniques. . . . . . 3851 Q# w* h% c+ G8 |4 N; X$ t
6.3 Mass analysers . . . . . . . . . . . . . . . . . . . 386. S$ S0 X5 O# d! f; n, ^' ^
6.3.1 Sector analysers . . . . . . . . . . . . . 387
1 M/ {+ |9 I% F; \1 L# @6.3.2 Quadrupole mass spectrometers . . 389
% i, S2 a- y& ?& w0 [6.3.3 Time-of-flight mass spectrometry . 390
, N' p9 {" D2 w2 t' w$ N, b) I/ W6.3.4 Quadrupole ion trap . . . . . . . . . . 393# [8 b) r; v, L+ h: R) K$ G8 Y
6.3.5 Fourier-transform ion-cyclotron ]/ `4 D$ B* d- U
resonance mass spectrometry . . . . 395
9 i: B4 o7 ?& [5 L6.3.6 Tandem mass spectrometry . . . . . 398+ K( j8 J0 i6 t
6.4 Direct mass-spectrometric polymer
+ X. H1 V. V0 D# ecompound analysis . . . . . . . . . . . . . . . . . 4078 q0 R+ i8 u: G1 @0 W
6.5 Ion mobility spectrometry . . . . . . . . . . . 415
% f, Q6 E* l p& P6.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 417, h- N+ ?) E; {! S- J) A
6.6.1 Mass spectrometry (General) . . . . 417* K% F& C! j j3 }- [
6.6.2 Mass spectrometers . . . . . . . . . . . 417
6 ]7 E+ I2 n1 P3 T; k# g6.6.3 Ionisation modes . . . . . . . . . . . . . 417- b! C S6 o& E
6.7 References . . . . . . . . . . . . . . . . . . . . . . . 418
0 [) `! X8 u! A7 v z. DChapter 7 Multihyphenation and
7 v( L. z# ~0 Y4 [3 mMultidimensionality in
`! ]. _+ l7 @- s: GPolymer/Additive Analysis . . . 425( S8 K+ \ c* |+ x! w% D! ^3 I
7.1 Precolumn hyphenation . . . . . . . . . . . . . 428
- n* @4 o8 m0 G" W. p- _& H; l; {7.1.1 Chromatographic sampling( F. H3 y1 r8 B2 M9 U5 r
methods . . . . . . . . . . . . . . . . . . . 432& R2 y: R8 p% F3 G& b, V9 Y
7.2 Coupled sample
- e m5 O4 n; F# V' w1 r+ ]preparation – spectroscopy/spectrometry . 449" P4 ^' D% E. K0 O) f! B
7.3 Postcolumn hyphenation . . . . . . . . . . . . . 4526 @) J! Y' `# `8 K' a+ a
7.3.1 (Multi)hyphenated GC techniques 456
& J! }- q. k6 O$ o A4 r6 V' T7.3.2 (Multi)hyphenated SFC) U. }% ^; p, F& @
techniques . . . . . . . . . . . . . . . . . 4753 l5 C; o: g$ h8 ]: J/ c
7.3.3 (Multi)hyphenated HPLC
! Y& @# ?( c3 u/ Utechniques . . . . . . . . . . . . . . . . . 489% S* Z! r2 `5 K6 F0 W( @
7.3.4 Hyphenated SEC techniques . . . . 527
5 @5 b2 t3 p/ G3 J7.3.5 Hyphenated TLC techniques . . . . 530
: n- r$ `! w2 F* C: `7.3.6 Hyphenated CE techniques . . . . . 543
6 N- t6 D2 G- D5 J9 h6 pContents vii! U; k( `; ?% ^) _8 a% G8 O+ I
7.4 Multidimensional chromatography . . . . . 545/ e; c6 j6 v0 d5 u4 |4 Z
7.4.1 Multidimensional gas
& h( m% w4 s3 z3 qchromatography . . . . . . . . . . . . . 548
) i4 @: q2 T$ c5 j' G' g2 N% Q; [7.4.2 Multidimensional supercritical) C) `0 F8 X8 A
fluid chromatography . . . . . . . . . 550( d/ M3 V! @6 w* T2 Q
7.4.3 Multidimensional liquid
# \+ R5 ^; l" a7 W& g k4 ]chromatography . . . . . . . . . . . . . 550: U0 O3 Q: w8 g, n8 P6 S4 }5 J
7.4.4 Multidimensional thin-layer( C+ `% o! t+ Y$ B% a
chromatography . . . . . . . . . . . . . 558
$ U! P, U: K+ C: Z/ t4 R: U+ B0 C7.5 Multidimensional spectroscopy . . . . . . . . 5608 h7 I' w( Z8 q+ f
7.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 562
' L# O( G" `1 u ~. y7.6.1 General . . . . . . . . . . . . . . . . . . . 5623 i5 n( W) h j7 r- d6 W& z# ?
7.6.2 Multihyphenation and
3 U- \( a! O% @+ Kmultidimensionality . . . . . . . . . . . 563
- M3 k0 b; _/ }: J7.6.3 Precolumn hyphenation . . . . . . . . 563
* d% U" z5 U% p( U3 R7.6.4 Postcolumn hyphenation . . . . . . . 563
; [/ {4 b& r# q* ^7.6.5 Multidimensional chromatography 563' X2 f; \! R2 ]! h5 `3 b F
7.6.6 Multidimensional spectroscopy . . 5638 w; }7 E0 l7 ?+ {2 `+ c) K2 Q
7.7 References 564! U" ]3 A d# b5 M; r0 Q+ N
Chapter 8 Inorganic and Element
0 z0 b) Z4 }) B" w" h7 m& X/ \Analytical Methods . . . . . . . . 5855 q, |+ V5 m2 F8 D8 R6 ?% I
8.1 Element analytical protocols . . . . . . . . . . 587' t0 r: v- J3 n$ L
8.1.1 Element analytical pretreatment( n1 _1 U8 D c% o6 E! H
protocols . . . . . . . . . . . . . . . . . . 588
t9 N) [3 z: X8.1.2 Elemental analysis methods . . . . . 589
) p) I( w; h4 H0 v9 A8.2 Sample destruction for classical elemental/ P: [5 p4 T6 j
analysis . . . . . . . . . . . . . . . . . . . . . . . . . 591
/ |3 a: u, f5 k/ [. q8.2.1 Combustion analysis . . . . . . . . . . 593
$ t( X0 M( r0 [/ J! V# d8.2.2 Wet matrix digestion . . . . . . . . . . 597% z9 W9 S. \7 r4 m' |
8.2.3 Fusion methods . . . . . . . . . . . . . . 604
3 C) b: O, U7 q9 j- J8.3 Analytical atomic spectrometry . . . . . . . . 6054 t' O6 a% v, c8 z+ B. p
8.3.1 Atomic absorption spectrometry . 608
j* R8 @3 h! Q2 ]8.3.2 Atomic emission spectrometry . . . 613" p" [3 y8 Y9 C$ y9 j
8.3.3 Atomic fluorescence spectrometry 624 |
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