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Acknowledgements. . . . . . . . . . . . . . . . xv
2 {7 s( q6 k; _5 r9 I8 ^! l s& bChapter 1 Introduction . . . . . . . . . . . . . . 16 E" n; W; Q. P9 G1 j
1.1 Additives . . . . . . . . . . . . . . . . . . . . . . . . 2. o2 t8 |0 ~. ]
1.1.1 Additive functionality . . . . . . . . . 3" ~% e2 P" n& j" Z0 j
1.2 Plastics formulations . . . . . . . . . . . . . . . 5 R, l# x- N. M5 ` F6 j* B
1.2.1 Supply forms . . . . . . . . . . . . . . . 76 z% }& l \# X" ` G3 G( `) c
1.2.2 Additive delivery . . . . . . . . . . . . 9
6 v, Y" j3 m- Z }1.3 Economic impact of polymer additives . . 9; J: j! u% S" ^1 H$ k8 z; z2 e
1.4 Analysis of plastics . . . . . . . . . . . . . . . . 11
- |$ H; b5 B: z5 y5 L0 D% }; [" \! J7 x1.4.1 Regulations and standardisation . . 15
1 J) v" t1 B* D _% f0 h1.4.2 Prior art . . . . . . . . . . . . . . . . . . . 17
- |2 Z3 @2 h: \* J1.4.3 Databases . . . . . . . . . . . . . . . . . . 19( }- y6 p9 e3 |4 N" H9 ^% t9 S
1.4.4 Scope . . . . . . . . . . . . . . . . . . . . . 20
0 n$ q5 Q' Z" J8 Y$ w$ _1.4.5 Chapter overview . . . . . . . . . . . . 22. \* J+ Z9 z& i9 |7 E( j
1.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 23
1 P. c. C/ {0 D- j. R z1.5.1 Plastics additives . . . . . . . . . . . . . 23: V' Y1 j, d' }. ?" y
1.5.2 Processing technologies . . . . . . . . 23/ x% F$ A( T+ t- s0 @) l: K
1.5.3 Instrumental analysis . . . . . . . . . . 23
" R. B# e8 G, Z8 J! v+ E4 ?* @# D1.5.4 Polymer analysis . . . . . . . . . . . . . 24
2 k! r* s1 _. F! x: \3 c: U4 {1.5.5 Polymer/additive analysis . . . . . . 24
+ Q- t- v$ @; E1 H5 F y1.6 References . . . . . . . . . . . . . . . . . . . . . . . 24: m( Q4 G1 p+ t& i
Chapter 2 Deformulation Principles . . . . 29, {# G' P; U4 @2 X( z9 `6 Y/ i( z0 [
2.1 Polymer identification . . . . . . . . . . . . . . 30
8 x3 w7 L2 s5 o2.2 Additive analysis of rubbers: ‘Best3 Q( Z2 W9 h. C9 W
Practice’ . . . . . . . . . . . . . . . . . . . . . . . . 32
8 z4 e U* ?6 l2 c+ ~' w2.3 Polymer extract analysis . . . . . . . . . . . . . 42
3 x: |: {4 F1 I* m' P- s; i0 J2.4 In situ polymer/additive analysis . . . . . . 46
~8 F8 w. V4 l0 r7 B* ]2.5 Class-specific polymer/additive analysis . 47
0 v) ~0 K4 O% G; s. Z: ]$ w2.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 48% U! L/ v5 S: `' a! ~
2.6.1 Polymer identification . . . . . . . . . 48- J. N; r! o8 m N8 U5 a
2.6.2 Deformulation of rubbers . . . . . . 48
" L6 }3 E6 u* m4 F- E' `% L* w2.6.3 Deformulation of polymers . . . . . 48' |& W" P- L( v) U7 J
2.7 References . . . . . . . . . . . . . . . . . . . . . . . 48
6 p* @; R& C! X4 ]; s5 _6 p5 `Chapter 3 Sample Preparation
. J2 s2 {7 {1 K, ?! H' \* hPerspectives . . . . . . . . . . . . . . 51 |8 G$ D8 L3 K$ V9 ]9 W, ]
3.1 Solvents . . . . . . . . . . . . . . . . . . . . . . . . 54 ^: X6 q1 u1 U! Y7 G
3.1.1 Polymer solubility criteria . . . . . . 55. M) \" l5 o& W4 K8 e
3.1.2 Solubility parameters . . . . . . . . . . 55
/ F# K& V# r! m- k3.1.3 Polymer solutions . . . . . . . . . . . . 56
. a2 h0 L# w$ q3.2 Extraction strategy . . . . . . . . . . . . . . . . . 57
0 m0 d3 Y6 \; \6 c8 g; a1 P3.3 Conventional extraction technologies . . . 591 J- v2 f# f4 v: K2 P0 T7 q
3.3.1 Liquid–liquid extraction . . . . . . . 604 E9 I6 u8 u1 q7 `
3.3.2 Liquid–solid extraction . . . . . . . . 60# y# Z X/ }! V$ [: b8 M
3.3.3 Classical solvent extractions of
! M0 @8 J8 V& ]0 {additives from polymers . . . . . . . 61
2 v. X+ a# g- p- a! T3.3.4 Sonication . . . . . . . . . . . . . . . . . 75- g, O) S* I2 R) ~
3.4 High-pressure solvent extraction methods 81
% V3 Z0 }( |' X3.4.1 Supercritical fluid technology . . . 81( K. y+ A$ G( F% y
3.4.2 Analytical SFE . . . . . . . . . . . . . . 85
% J1 m& S2 I5 ~+ a" `3.4.3 Subcritical water extraction . . . . . 100/ V; p, t" Q' }$ l; I& g8 `+ I+ L
3.4.4 Microwave technology . . . . . . . . 101. }! z; J: y. M/ V# Y) D a# R
3.4.5 Microwave-assisted extractions . . 104
' f0 A6 Q5 L! T) m4 f s3.4.6 Pressurised fluid extraction . . . . . 1178 @# I8 A: F& e$ w, B
3.5 Sorbent extraction . . . . . . . . . . . . . . . . . 123
1 i) |# @ I' U9 ^" {3.5.1 Solid-phase extraction . . . . . . . . . 124
) Q6 v3 z. A( q3.5.2 Solid-phase microextraction . . . . . 129
2 w- ^5 |$ r3 v4 f5 }1 V3 {, T6 I, C3.5.3 Stir bar sorptive extraction . . . . . 133
, t) C# Y) x9 ~/ v0 F/ i3.6 Methodological comparison of extraction' ~1 a* M n* w: }" T$ U: \7 w
methods. . . . . . . . . . . . . . . . . . . . . . . . . 1344 o+ u( t$ S: K% B& O
3.6.1 Experimental comparisons . . . . . . 136) {+ e8 P9 h0 M( C
3.6.2 Extraction selectivity . . . . . . . . . . 138# A+ L1 {9 M" k$ k, d- |4 S5 J1 U
3.6.3 ‘Nonextractable’ additive analysis 140. t" {. ^4 s, Z
3.7 Polymer/additive dissolution methods . . . 1460 M) M! ^2 m6 i. j1 d, M) X7 o
3.8 Hydrolysis . . . . . . . . . . . . . . . . . . . . . . . 152
# ^$ A5 K. A4 a& X1 P: U2 ^3.9 Bibliography . . . . . . . . . . . . . . . . . . . . . 155
- l- o: R: ]0 q% ]" ^0 v. s2 b2 i3.9.1 Sampling and sample preparation 155
# p" L' R% f6 |/ o, F! a8 J) b3.9.2 Solvents/solubility . . . . . . . . . . . . 1557 u4 \' q: ?0 J1 d5 S
3.9.3 Extraction methods . . . . . . . . . . . 156
- J$ ]6 B1 i" ]5 k3.10 References . . . . . . . . . . . . . . . . . . . . . . . 156
! m; v# Y; [; @7 U9 p2 d" bvi Contents" t% [" p- t$ S
Chapter 4 Separation Techniques . . . . . . 171
3 N% _( h) q0 c8 e2 T4.1 Analytical detectors . . . . . . . . . . . . . . . . 177
, B- Y, B7 l; z L& P4.2 Gas chromatography . . . . . . . . . . . . . . . 181
) B2 k) Z1 G& Y0 G- L4.2.1 High-temperature gas
3 f, [! m- G! bchromatography . . . . . . . . . . . . . 200, Q# s8 `$ C- A# _
4.2.2 Headspace gas chromatography . . 202& ?" r& e( a1 M# w& O( E
4.3 Supercritical fluid chromatography . . . . . 205- e( f5 V! v. `/ [) j
4.4 Liquid chromatography techniques . . . . . 217
& J) E4 S7 R# ]5 N4.4.1 Planar chromatographies . . . . . . . 2182 O$ O: V% y8 s+ F0 H& J
4.4.2 Column chromatographies . . . . . . 230
" M5 j) {! J U' m4.5 Capillary electrophoretic techniques . . . . 273( L* U) Q i% P( [1 O& U
4.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 2786 c" n: X& T% d9 i9 V( b
4.6.1 General texts . . . . . . . . . . . . . . . 278
; h0 _9 y1 O6 u5 \0 {9 z; h" V4.6.2 Detectors . . . . . . . . . . . . . . . . . . 2791 Y0 x; \' P- c. V1 S
4.6.3 Gas chromatography . . . . . . . . . . 279
( H) l- P0 d& O" |) W% K4.6.4 Supercritical fluid chromatography 279* C$ z' Z) O; x- a/ O! w
4.6.5 Thin-layer chromatography . . . . . 279: P# {% f; \- U# ?8 V' [
4.6.6 Liquid chromatography . . . . . . . . 2803 }5 M6 Z9 U' K, o2 q' j# D, e0 z" D
4.6.7 Size-exclusion chromatography . . 280
1 W( Q0 K9 Q6 m4.6.8 Ion chromatography . . . . . . . . . . 280& h, a' q5 l, ?. ^; F3 o
4.6.9 Capillary electrophoretic
$ ~/ b$ x8 J( @. H" wtechniques . . . . . . . . . . . . . . . . . 2803 j/ `6 `2 v- M; W; x
4.7 References . . . . . . . . . . . . . . . . . . . . . . . 2813 N, {$ A. N4 N. x% N$ B% F4 K
Chapter 5 Polymer/Additive Analysis:6 \4 R! M6 y* m$ @! c
The Spectroscopic Alternative 299
5 a# i1 N8 K$ u, i: a5.1 Ultraviolet/visible spectrophotometry . . . 302
+ M# x2 A3 {) l5 O, h: a5.2 Infrared spectroscopy . . . . . . . . . . . . . . . 311
- J3 m' K; U" Z* N6 @6 x6 i) g5 q5.3 Luminescence spectroscopy . . . . . . . . . . 318
$ E: l; d% Z6 E. H5 T0 L" t$ ^5.4 High-resolution nuclear magnetic
: s: H/ r# j) h. Kresonance spectroscopy . . . . . . . . . . . . . 323
+ G: I' h u) k& a. I9 a) ]8 a; P5.4.1 Multidimensional NMR' C5 M1 T/ M) y: F
spectroscopy . . . . . . . . . . . . . . . . 336
( v/ p9 A( W. d# L- P- u% ~5 L5.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 342
A& A a. V$ }) |5 s5.5.1 General spectroscopy . . . . . . . . . 342- P' U/ Z4 Q6 q7 l% |
5.5.2 Ultraviolet/visible
9 B. n& Q5 ?5 O& n; j% f2 Cspectrophotometry . . . . . . . . . . . . 342
% Q2 t5 ?: d. Y" ^: H2 ^: m5.5.3 Infrared spectroscopy . . . . . . . . . 342/ V3 ?& e5 z8 y5 s
5.5.4 Luminescence spectroscopy . . . . . 342) Z, a' J! A# f( o7 \. E
5.5.5 Nuclear magnetic resonance
B& h# ]' m+ t& V) Uspectroscopy . . . . . . . . . . . . . . . . 342
- `! C! L0 w: \ ^1 ?5.6 References . . . . . . . . . . . . . . . . . . . . . . . 342
3 @9 o" s6 @9 ?9 `; pChapter 6 Organic Mass-Spectrometric
: K; c- D6 B& i* ]5 P. W5 x. NMethods . . . . . . . . . . . . . . . . 349
z i, P4 n- w3 S! N6.1 Basic instrumentation . . . . . . . . . . . . . . . 3517 i3 P/ Q. E5 |0 V) M# C
6.1.1 Inlet systems . . . . . . . . . . . . . . . . 352
2 y8 b* a) |4 m+ x6.1.2 Modes of detection . . . . . . . . . . . 353
0 A$ F5 k4 N/ G' {! j1 M: s! k! S, j6.1.3 Mass resolution . . . . . . . . . . . . . . 354% Q2 b6 C; v# r
6.1.4 Isotope distributions . . . . . . . . . . 354) J- ?8 F5 ^9 O1 ?1 D7 r p
6.1.5 Accurate mass measurements. . . . 355
8 N9 s$ _; x. M! D; U3 E6.2 Ion sources . . . . . . . . . . . . . . . . . . . . . . 357
6 s1 u! ?1 x" Q/ X6 H4 v' A3 }$ \+ Z6.2.1 Electron impact ionisation . . . . . . 360/ k+ D7 \& n" z
6.2.2 Chemical ionisation . . . . . . . . . . . 362
5 b8 z8 C4 X; i6.2.3 Metastable atom bombardment . . 3671 W) w# N( E# k3 u) W- I
6.2.4 Fast atom bombardment . . . . . . . 3671 w4 p* Z! `! G$ Z1 B1 W; f
6.2.5 Field ionisation . . . . . . . . . . . . . . 372
' k8 I G6 S* l8 E- j$ `/ ~0 ~6.2.6 Field desorption . . . . . . . . . . . . . 374' `4 M, q" H; f5 P4 N( D, u' I0 e
6.2.7 Thermospray ionisation . . . . . . . . 376# a+ u/ n4 @4 M. H( T' m' |- G
6.2.8 Atmospheric pressure ionisation t' u" {9 c' r2 N% g4 f
techniques . . . . . . . . . . . . . . . . . 378
- x7 o0 X7 p0 m# P c6.2.9 Desorption/ionisation methods . . . 383; E* ?: U- y1 P. \2 E
6.2.10 Photoionisation techniques. . . . . . 385$ {, v, }# @+ m7 [! t9 L. u
6.3 Mass analysers . . . . . . . . . . . . . . . . . . . 386
, c+ g7 Z1 ]7 `. w1 R5 f6.3.1 Sector analysers . . . . . . . . . . . . . 387+ }0 C) u( e4 v( x) r
6.3.2 Quadrupole mass spectrometers . . 389
2 W) k, N% `$ i; d6.3.3 Time-of-flight mass spectrometry . 390
$ x7 ?# [; [& E' i6.3.4 Quadrupole ion trap . . . . . . . . . . 393) e' F& f" h+ D8 x- s& N* v
6.3.5 Fourier-transform ion-cyclotron
, m3 J3 ?& ^ {% vresonance mass spectrometry . . . . 395
8 x4 e" H: f& ~/ o. b0 J. h/ C! O6.3.6 Tandem mass spectrometry . . . . . 398
6 h; y4 }, v. }- C3 C6.4 Direct mass-spectrometric polymer9 U) A3 G j ^5 ?' @
compound analysis . . . . . . . . . . . . . . . . . 407
) P& e/ M- M8 P' J; L6.5 Ion mobility spectrometry . . . . . . . . . . . 415
/ W# [0 l: e9 G) k. @0 ]( c6.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 417# ^- O" F! Q2 ^7 X$ D8 [
6.6.1 Mass spectrometry (General) . . . . 417
" m: j% b1 s, a0 b) c( G2 l6.6.2 Mass spectrometers . . . . . . . . . . . 417& g4 e, f+ `) E1 d( s5 ]- w/ k
6.6.3 Ionisation modes . . . . . . . . . . . . . 4172 t7 O# Y9 ^# V8 X; r
6.7 References . . . . . . . . . . . . . . . . . . . . . . . 4188 V# }% ]3 [- ~" O
Chapter 7 Multihyphenation and+ U: I4 Q/ i; J! ?/ R/ l
Multidimensionality in0 n9 q' H6 J4 O# h: L
Polymer/Additive Analysis . . . 425; r% d8 |2 X3 Y& A
7.1 Precolumn hyphenation . . . . . . . . . . . . . 428
5 H; a: {) i c; _7.1.1 Chromatographic sampling
F! E4 Z5 s9 z3 [; {methods . . . . . . . . . . . . . . . . . . . 432
; F( A# w. t) X+ r @7.2 Coupled sample! y0 N N+ ]% X N0 ?5 E" L
preparation – spectroscopy/spectrometry . 449
7 G5 P; V8 j% B# `7.3 Postcolumn hyphenation . . . . . . . . . . . . . 452
# Y. t* s# V( G# ^: n' g7.3.1 (Multi)hyphenated GC techniques 456$ _$ R5 h) t% P
7.3.2 (Multi)hyphenated SFC# b" Q, {$ U: w, ^: Q N% i( d! L! w
techniques . . . . . . . . . . . . . . . . . 475+ G( F L3 r+ B
7.3.3 (Multi)hyphenated HPLC
- o. q6 W3 U3 K1 Ntechniques . . . . . . . . . . . . . . . . . 489, j# e2 I9 F7 b( \: D. T. ?+ ^
7.3.4 Hyphenated SEC techniques . . . . 5272 ]1 b( g0 d% N6 [5 j6 ~& Y0 a
7.3.5 Hyphenated TLC techniques . . . . 530
, X% y' C" s) t3 Q% a* L7.3.6 Hyphenated CE techniques . . . . . 5438 w) J, l+ p6 r
Contents vii/ e! }$ o2 C: N6 x% M |' y" Q( f
7.4 Multidimensional chromatography . . . . . 545
6 A. X/ e: [# c7.4.1 Multidimensional gas
% k5 N! g7 x G0 {chromatography . . . . . . . . . . . . . 548
( \4 h; p0 W9 t. |- D% D7.4.2 Multidimensional supercritical, }1 ?5 b' h' p! ~" j
fluid chromatography . . . . . . . . . 550
/ b, i+ w$ } u1 r$ v7.4.3 Multidimensional liquid
5 b4 N. l5 [- D! [0 s3 I) k- achromatography . . . . . . . . . . . . . 550) v3 T- [. f* K% {1 ?2 h
7.4.4 Multidimensional thin-layer# O7 r5 Q* Y K- S
chromatography . . . . . . . . . . . . . 558
9 y& A1 c" s$ @1 T0 n/ C7.5 Multidimensional spectroscopy . . . . . . . . 5606 M1 a8 O; B, a5 u
7.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 562; ~4 H* Y" H5 q3 B. Q& B |! t
7.6.1 General . . . . . . . . . . . . . . . . . . . 562
4 S" I! N2 H0 y1 _! x7.6.2 Multihyphenation and
! F9 u5 L6 J" T4 z; u- H' F; @# _multidimensionality . . . . . . . . . . . 563
2 l- c. ]# a+ z" [' P! q0 P/ k7.6.3 Precolumn hyphenation . . . . . . . . 563
5 U+ x: |+ w$ B% p7.6.4 Postcolumn hyphenation . . . . . . . 563
9 k* j! d- k5 x7.6.5 Multidimensional chromatography 563
9 c" H3 n1 @/ D6 o/ @5 ~7.6.6 Multidimensional spectroscopy . . 563
7 E, O/ m/ W/ L+ b' M' A) c7 v7.7 References 564% }2 |5 _# s7 F& o
Chapter 8 Inorganic and Element
) x" D* K/ j/ QAnalytical Methods . . . . . . . . 585
2 m% G. F8 \' S/ f5 X8 I8.1 Element analytical protocols . . . . . . . . . . 5875 k5 l1 L' i/ W6 q
8.1.1 Element analytical pretreatment2 B- _, ~, |* e( p, h. a
protocols . . . . . . . . . . . . . . . . . . 588
' W2 y9 I3 s4 S( |7 Q: D4 a* O; t8.1.2 Elemental analysis methods . . . . . 589
: M) L9 s* i7 J" e$ o8.2 Sample destruction for classical elemental8 |7 g) g- N& S* ? o& {
analysis . . . . . . . . . . . . . . . . . . . . . . . . . 591
. S G, _. K" w1 }: [8.2.1 Combustion analysis . . . . . . . . . . 593+ @/ r8 m. w7 y+ ~) X
8.2.2 Wet matrix digestion . . . . . . . . . . 597( t: t- F: ~4 c; \: n
8.2.3 Fusion methods . . . . . . . . . . . . . . 604
7 \2 y, j. }) V) a, m8.3 Analytical atomic spectrometry . . . . . . . . 605
% a/ R* ]/ X$ [$ T/ X8.3.1 Atomic absorption spectrometry . 608
5 k8 t7 S, O0 m8.3.2 Atomic emission spectrometry . . . 613) y6 o, E0 u0 D6 h3 q: R _
8.3.3 Atomic fluorescence spectrometry 624 |
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