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Acknowledgements. . . . . . . . . . . . . . . . xv
/ m! e# ^8 D- Z6 SChapter 1 Introduction . . . . . . . . . . . . . . 1
) f: C9 E+ u8 J" Q4 p t- {1.1 Additives . . . . . . . . . . . . . . . . . . . . . . . . 2
# ~4 E. Z1 e7 x& F3 l, N3 N1.1.1 Additive functionality . . . . . . . . . 3
6 j. ^! S- g2 @9 g1 ~) m1.2 Plastics formulations . . . . . . . . . . . . . . . 5
" M x) r, w$ q6 J1.2.1 Supply forms . . . . . . . . . . . . . . . 7! Y! ]: n- s$ @3 L, ]
1.2.2 Additive delivery . . . . . . . . . . . . 92 @# \) @4 A: \2 y3 l& b3 l/ T
1.3 Economic impact of polymer additives . . 9
% ~# ?; w3 }: d1.4 Analysis of plastics . . . . . . . . . . . . . . . . 11
* z4 u1 K- D$ w' W9 F5 Y6 l1.4.1 Regulations and standardisation . . 15
/ r* l, ?/ e/ u6 L* b1.4.2 Prior art . . . . . . . . . . . . . . . . . . . 17
- ~* w; r1 v! ?) U/ p {1.4.3 Databases . . . . . . . . . . . . . . . . . . 19
0 s! s; F3 d$ |4 y7 i1.4.4 Scope . . . . . . . . . . . . . . . . . . . . . 20" u+ f' P6 r5 Z% @% f, d+ ^* r
1.4.5 Chapter overview . . . . . . . . . . . . 22
- n" \; x8 @% l( N1.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 239 ^5 }. i( G6 x
1.5.1 Plastics additives . . . . . . . . . . . . . 235 _3 s( N' f* k
1.5.2 Processing technologies . . . . . . . . 23
3 E( J! U$ m# ~1.5.3 Instrumental analysis . . . . . . . . . . 23
/ s v7 K) b& [& J' E1.5.4 Polymer analysis . . . . . . . . . . . . . 246 f, y Q6 @8 n4 g5 U
1.5.5 Polymer/additive analysis . . . . . . 24, N v6 I3 u, ]) s9 @1 F
1.6 References . . . . . . . . . . . . . . . . . . . . . . . 24
) z+ x8 L( w5 gChapter 2 Deformulation Principles . . . . 29
; i% T6 ]" H5 ^3 ^/ E/ z2.1 Polymer identification . . . . . . . . . . . . . . 30
4 x5 p1 L; S% |7 I3 v# i2.2 Additive analysis of rubbers: ‘Best
' ?7 V8 A. A; ], k, V0 PPractice’ . . . . . . . . . . . . . . . . . . . . . . . . 32
/ N! ^* w# ^7 V ~2.3 Polymer extract analysis . . . . . . . . . . . . . 426 f( p! k: k3 a3 A, s# H, I- y
2.4 In situ polymer/additive analysis . . . . . . 46
9 c: F) M& Y9 R! I/ `$ w2.5 Class-specific polymer/additive analysis . 473 S* Z8 T0 S b1 Q# k; M
2.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 48
" L% y: t7 d$ C1 }" m2.6.1 Polymer identification . . . . . . . . . 482 }3 \/ ]/ Y9 F" { E2 e
2.6.2 Deformulation of rubbers . . . . . . 488 E7 d! ?, u m8 _5 s; y6 X f: A, |) \% D
2.6.3 Deformulation of polymers . . . . . 483 b1 \7 z( m3 o8 C. H4 s
2.7 References . . . . . . . . . . . . . . . . . . . . . . . 48
% E( A5 o9 u6 x- P! T4 TChapter 3 Sample Preparation! Z" t* m- \5 r8 o
Perspectives . . . . . . . . . . . . . . 51
* `5 ?; ?4 n/ H* w+ |+ X3.1 Solvents . . . . . . . . . . . . . . . . . . . . . . . . 54
! ?) R* Z9 E7 J$ \$ H! T( Q3.1.1 Polymer solubility criteria . . . . . . 55
8 T" Z* s& j9 `- O X3.1.2 Solubility parameters . . . . . . . . . . 554 e' X- N5 E# [0 G/ ^& C
3.1.3 Polymer solutions . . . . . . . . . . . . 56, q: v# V4 S2 x* _0 l/ \, |: `
3.2 Extraction strategy . . . . . . . . . . . . . . . . . 57
3 u: y, s( t" D; O6 _+ E) `- c3.3 Conventional extraction technologies . . . 59
5 Z' Z% c$ t4 u9 G3.3.1 Liquid–liquid extraction . . . . . . . 60
! Z! c2 i/ @; ]3.3.2 Liquid–solid extraction . . . . . . . . 60$ R% |- R8 [* O" A6 [. D/ r4 h
3.3.3 Classical solvent extractions of! N! r" {. U; v. j: @
additives from polymers . . . . . . . 61
_9 x8 ?; H7 Z- L3.3.4 Sonication . . . . . . . . . . . . . . . . . 754 S2 H4 w* x' F! Z; \
3.4 High-pressure solvent extraction methods 814 J1 t7 X" C# a4 V
3.4.1 Supercritical fluid technology . . . 81
* x2 v7 z2 m; @: q i3.4.2 Analytical SFE . . . . . . . . . . . . . . 85
: I$ n- E) D5 q, Z9 Y3.4.3 Subcritical water extraction . . . . . 100
% Q3 n: L5 J4 g k* k I3.4.4 Microwave technology . . . . . . . . 1017 S9 b9 [! f- K& j |& ^; E
3.4.5 Microwave-assisted extractions . . 104
: ?3 Q' F+ q* j$ w) \3.4.6 Pressurised fluid extraction . . . . . 117
. Z/ x/ Z$ F# c% w. S. Z3.5 Sorbent extraction . . . . . . . . . . . . . . . . . 123% E+ v0 f, P0 z! u1 e8 n; _1 m
3.5.1 Solid-phase extraction . . . . . . . . . 124
6 T1 C4 |' v* P- D3.5.2 Solid-phase microextraction . . . . . 129- t7 y9 E' N7 S& Y! ~# P- {
3.5.3 Stir bar sorptive extraction . . . . . 133
- ^! S, G0 c$ r8 Y4 \# q3.6 Methodological comparison of extraction
8 V; X; L$ b4 R1 @- f( @methods. . . . . . . . . . . . . . . . . . . . . . . . . 134
# U9 W) R3 a: z# p8 I3.6.1 Experimental comparisons . . . . . . 136
+ ^: _6 p; E1 N/ h6 ~1 ]3.6.2 Extraction selectivity . . . . . . . . . . 138& w8 M3 \3 s4 f! d7 |, \" L y
3.6.3 ‘Nonextractable’ additive analysis 140
+ v: v* f6 S. T3.7 Polymer/additive dissolution methods . . . 146, \+ V& i0 x( r& E1 ~7 E
3.8 Hydrolysis . . . . . . . . . . . . . . . . . . . . . . . 152# r2 T8 t6 K- U8 C# k4 u
3.9 Bibliography . . . . . . . . . . . . . . . . . . . . . 155
1 G6 m ?& \$ l* [3.9.1 Sampling and sample preparation 155
1 `6 ~& C; J6 [* S3.9.2 Solvents/solubility . . . . . . . . . . . . 1552 X5 Z4 M) a1 |' Q6 @
3.9.3 Extraction methods . . . . . . . . . . . 156
^. M+ C0 p- L8 Q7 f+ |, X3.10 References . . . . . . . . . . . . . . . . . . . . . . . 156& t! ~0 B `0 G; W! w
vi Contents8 W& i6 Y3 w7 E/ h) B
Chapter 4 Separation Techniques . . . . . . 171
7 c+ e* Q# r y% n4.1 Analytical detectors . . . . . . . . . . . . . . . . 1779 r, V: G4 b7 W/ I/ L
4.2 Gas chromatography . . . . . . . . . . . . . . . 181, b+ ?6 ?% D# p! [; J
4.2.1 High-temperature gas/ x- l' p8 O$ @, z# R6 R# ^
chromatography . . . . . . . . . . . . . 200
+ E6 v ]: {: V1 S1 E4.2.2 Headspace gas chromatography . . 202
) J) {6 Q5 w0 V0 `5 Y4.3 Supercritical fluid chromatography . . . . . 2050 X$ x3 \3 D3 y& c3 c. u0 r* L
4.4 Liquid chromatography techniques . . . . . 217
' O m' P% c, ~8 F- g4.4.1 Planar chromatographies . . . . . . . 218
4 ]- [; F( O' B6 K' i& h2 G4.4.2 Column chromatographies . . . . . . 230
8 t* o$ V( {. K! B4.5 Capillary electrophoretic techniques . . . . 273
) _( z7 q' l7 ^2 [" W7 C4.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 2785 z2 L! d0 P* _0 \2 z
4.6.1 General texts . . . . . . . . . . . . . . . 278% M3 i# ?* Y" l. |+ d
4.6.2 Detectors . . . . . . . . . . . . . . . . . . 279
$ n# |. r8 h! D4 Z4.6.3 Gas chromatography . . . . . . . . . . 279! E& k4 r+ c4 u1 K i
4.6.4 Supercritical fluid chromatography 2798 P8 m u- r7 O, A2 e
4.6.5 Thin-layer chromatography . . . . . 279
! J6 x+ G/ { F X4 ]3 S4.6.6 Liquid chromatography . . . . . . . . 280
( f5 ]; s9 p: x3 z! X3 N4.6.7 Size-exclusion chromatography . . 280
) f! n5 K6 Y* H. A6 A+ g4.6.8 Ion chromatography . . . . . . . . . . 280 N0 \* T# g3 ^( v7 `3 _
4.6.9 Capillary electrophoretic2 _2 L9 b( l( X' W F
techniques . . . . . . . . . . . . . . . . . 280( W8 D. t6 g+ w. [" [1 n
4.7 References . . . . . . . . . . . . . . . . . . . . . . . 2814 W/ w- `* {6 z& |- G) L$ U
Chapter 5 Polymer/Additive Analysis:( C5 s. m0 Y; u" D5 W$ Z
The Spectroscopic Alternative 299! ]" k$ C3 U( q5 F3 w3 i
5.1 Ultraviolet/visible spectrophotometry . . . 302
- U8 V* C+ h/ \9 w% s4 ^5.2 Infrared spectroscopy . . . . . . . . . . . . . . . 311
! q9 p% v4 t/ J _/ B: Q5.3 Luminescence spectroscopy . . . . . . . . . . 318
4 D. W _# J! f5.4 High-resolution nuclear magnetic
6 F2 r8 f9 G4 M+ T# A+ Q3 E" sresonance spectroscopy . . . . . . . . . . . . . 3236 W( T; [) P6 C
5.4.1 Multidimensional NMR
3 B; C! ^7 U$ H3 h9 Bspectroscopy . . . . . . . . . . . . . . . . 336
3 |; i& F9 e) Z: C( @! f2 j. u Q5.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 342
3 D& l% j/ {- T+ Y5.5.1 General spectroscopy . . . . . . . . . 342
8 F0 {. r) N8 I T- {5.5.2 Ultraviolet/visible
+ x: i7 J+ V2 U( Lspectrophotometry . . . . . . . . . . . . 342) W, \) g, C+ c
5.5.3 Infrared spectroscopy . . . . . . . . . 342
9 X; p \2 O& [5 p! W: V. m5.5.4 Luminescence spectroscopy . . . . . 342; o% U6 a' C" i) ]9 d) N9 e
5.5.5 Nuclear magnetic resonance
! m& N& z% H3 L3 d9 r& H1 d+ Pspectroscopy . . . . . . . . . . . . . . . . 342
3 @$ Q2 }2 I! s+ \5.6 References . . . . . . . . . . . . . . . . . . . . . . . 342
+ |. ?0 O7 S3 d8 y5 `2 R% sChapter 6 Organic Mass-Spectrometric! n& f9 ~) n. V) G' j
Methods . . . . . . . . . . . . . . . . 349) h1 F( z7 @* ~/ |* [
6.1 Basic instrumentation . . . . . . . . . . . . . . . 351
1 |" u6 C; g$ ], e6 H {6.1.1 Inlet systems . . . . . . . . . . . . . . . . 352
$ A* t, k! r4 Y0 f! V% a6.1.2 Modes of detection . . . . . . . . . . . 3530 }; {; J' J7 d- g
6.1.3 Mass resolution . . . . . . . . . . . . . . 3543 L8 B3 l. U, u L
6.1.4 Isotope distributions . . . . . . . . . . 3547 W, V: N$ N; k& t$ e9 a. g" t
6.1.5 Accurate mass measurements. . . . 355' |/ e$ F+ g+ i( O; Y3 J+ _- q* b
6.2 Ion sources . . . . . . . . . . . . . . . . . . . . . . 357
) B" e5 B/ Y- n/ o. n: x) \6.2.1 Electron impact ionisation . . . . . . 360
6 F$ ]7 v, ]7 i2 \9 G3 \: z) @$ ~6.2.2 Chemical ionisation . . . . . . . . . . . 362' K$ Q/ ]$ b: j+ W4 G) d
6.2.3 Metastable atom bombardment . . 367. F. F4 @% ^& Y! Z( z% n6 n2 T, W
6.2.4 Fast atom bombardment . . . . . . . 367
7 l- K: g$ l, @. E/ E6.2.5 Field ionisation . . . . . . . . . . . . . . 3720 {' o+ ^. U, s% p7 k2 p/ p. |6 @
6.2.6 Field desorption . . . . . . . . . . . . . 374. V. f/ f3 Q6 u: n" L! ~' e
6.2.7 Thermospray ionisation . . . . . . . . 3760 E6 Z% [' v: e, o# d& v1 \) O0 k
6.2.8 Atmospheric pressure ionisation
! q; B4 Y4 f7 m5 Y% t; stechniques . . . . . . . . . . . . . . . . . 378: u$ s' u" Q% B3 l7 j% Y; X
6.2.9 Desorption/ionisation methods . . . 3831 ^9 W" Q1 D8 I" Y+ ^
6.2.10 Photoionisation techniques. . . . . . 385
0 m' a9 W+ D4 ], ?3 i6.3 Mass analysers . . . . . . . . . . . . . . . . . . . 386$ e4 B8 d) d1 A0 A% w" ?: P* [- B
6.3.1 Sector analysers . . . . . . . . . . . . . 387
# ^2 W3 j0 C. |7 j# p6.3.2 Quadrupole mass spectrometers . . 389
8 a; r# y: S, x% c- ^8 |6.3.3 Time-of-flight mass spectrometry . 390+ H, m4 r, |: n
6.3.4 Quadrupole ion trap . . . . . . . . . . 393
' C( F& y6 M& f* u D6.3.5 Fourier-transform ion-cyclotron
9 m; p9 M* `6 Q9 @ cresonance mass spectrometry . . . . 395' m: s! ~, V9 i4 S% {7 G
6.3.6 Tandem mass spectrometry . . . . . 398
4 C# h! `2 a* Z3 `# {6.4 Direct mass-spectrometric polymer: z7 ]4 J6 [1 ^; g$ U/ A) n+ e
compound analysis . . . . . . . . . . . . . . . . . 407+ l2 o J) J+ \9 o. s6 i4 M
6.5 Ion mobility spectrometry . . . . . . . . . . . 415
+ S0 g7 S# }/ w& t$ A1 @9 V6.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 417# \& V( ?/ a# A3 O( q
6.6.1 Mass spectrometry (General) . . . . 4173 I3 E. |& B( E' _
6.6.2 Mass spectrometers . . . . . . . . . . . 4175 Y, K) f- B# n4 U6 i4 M( }
6.6.3 Ionisation modes . . . . . . . . . . . . . 4178 [/ U7 W( t$ z6 ]) U# m3 S
6.7 References . . . . . . . . . . . . . . . . . . . . . . . 418% n; z8 u/ E g2 {, E" T, ~
Chapter 7 Multihyphenation and, F4 u) z9 R3 Z7 p/ E
Multidimensionality in" V( q& V, a! p o' Q% `" j; k
Polymer/Additive Analysis . . . 425
" h8 I( C' |' I* {( P2 H; E: z% L% R7.1 Precolumn hyphenation . . . . . . . . . . . . . 428) m- ~8 j" |- M5 H5 f8 c, O
7.1.1 Chromatographic sampling
0 h2 R2 @0 x# T( y: n7 ymethods . . . . . . . . . . . . . . . . . . . 432
: Z" Z+ y. i; n) |4 R* u: v7.2 Coupled sample
+ O! J3 Y- h' s5 U; P' O/ gpreparation – spectroscopy/spectrometry . 449
: M' a r+ u& ~% ~1 ]3 b7.3 Postcolumn hyphenation . . . . . . . . . . . . . 452
4 v S) W$ F. G. Q7.3.1 (Multi)hyphenated GC techniques 456
" E( D; T p! v5 u7.3.2 (Multi)hyphenated SFC
?% T7 K! R: i- M" ]! }techniques . . . . . . . . . . . . . . . . . 475
1 Z7 y& m( z- |7.3.3 (Multi)hyphenated HPLC
) s$ r9 f/ r% b! N/ x( ]+ z: T, ?1 mtechniques . . . . . . . . . . . . . . . . . 489$ W- q# \6 |8 |. G1 d, A D
7.3.4 Hyphenated SEC techniques . . . . 527 Z. l3 U- w5 d1 ^4 s/ b) a
7.3.5 Hyphenated TLC techniques . . . . 530- z6 T1 m1 l V6 ?& e
7.3.6 Hyphenated CE techniques . . . . . 543
; B. r9 [- s, J) }6 l( B9 N bContents vii3 q4 [( U, h4 X$ ~$ e4 U, z: A
7.4 Multidimensional chromatography . . . . . 545
I3 E. d8 }$ p8 B1 E* h7.4.1 Multidimensional gas! \/ E, d& d9 N# R9 O2 d
chromatography . . . . . . . . . . . . . 548
8 n A# @, M/ P" H6 R: R7.4.2 Multidimensional supercritical# E2 z6 K# {# h8 Y- w+ [
fluid chromatography . . . . . . . . . 5500 e' v) ^& I1 i- ?9 g# T
7.4.3 Multidimensional liquid
/ M) X' C/ h8 x/ a) A8 lchromatography . . . . . . . . . . . . . 550, Q1 m+ x& V( d8 i
7.4.4 Multidimensional thin-layer- p; v3 K* F# B/ ^
chromatography . . . . . . . . . . . . . 558* {! u5 Q9 S. I1 l6 K2 A. w, x# b' s; q
7.5 Multidimensional spectroscopy . . . . . . . . 560$ Q' S- ^1 a* j3 @2 [' ]9 ^7 [
7.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 562
: H5 l8 f/ k. o- \, w$ o+ I7.6.1 General . . . . . . . . . . . . . . . . . . . 562" ^. J( G* Y! ~: F
7.6.2 Multihyphenation and- R3 F5 L7 w4 ?, {) h! f6 ]" ]
multidimensionality . . . . . . . . . . . 5633 v& _9 S$ c0 }7 f6 A( g: u; ?9 F
7.6.3 Precolumn hyphenation . . . . . . . . 563) A% a) ?% K' U: O0 g
7.6.4 Postcolumn hyphenation . . . . . . . 5631 R7 Q: ?; ^) [1 [* }
7.6.5 Multidimensional chromatography 563
3 W* X: _% \. S9 W l* b) { }7.6.6 Multidimensional spectroscopy . . 563
8 _: y7 n ?$ V1 T2 @7.7 References 5641 w- w# L# n& \+ A. m" W1 Q
Chapter 8 Inorganic and Element
- ~' U. v0 ]2 v+ L/ m' fAnalytical Methods . . . . . . . . 585
9 i( g& P; c* o1 c8.1 Element analytical protocols . . . . . . . . . . 587* l# U! K6 r, [! `3 k: R& _) U" N
8.1.1 Element analytical pretreatment
) v/ L5 m5 d4 I$ X& Gprotocols . . . . . . . . . . . . . . . . . . 588/ ?& Z$ }$ }: Q" @! l1 ?
8.1.2 Elemental analysis methods . . . . . 589, E8 J$ F$ D# e% L- A
8.2 Sample destruction for classical elemental" v5 U9 k Q$ y \% }5 _+ M8 i
analysis . . . . . . . . . . . . . . . . . . . . . . . . . 591
$ C/ Y; S. t& S( [! E7 l- g+ M; c- T6 R8.2.1 Combustion analysis . . . . . . . . . . 593- F0 w( ]2 \) A# K
8.2.2 Wet matrix digestion . . . . . . . . . . 597
- N2 |$ ?7 c) }( v1 s* ]8.2.3 Fusion methods . . . . . . . . . . . . . . 604: a0 o' A7 W) I0 e6 t2 a
8.3 Analytical atomic spectrometry . . . . . . . . 605
) s1 Q& S! R+ k( P4 ]' f! s8.3.1 Atomic absorption spectrometry . 608- |! i+ ]- K; J( L- G* a
8.3.2 Atomic emission spectrometry . . . 613
/ f; _2 h1 k- V D$ L: \& T& X2 W8.3.3 Atomic fluorescence spectrometry 624 |
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