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Acknowledgements. . . . . . . . . . . . . . . . xv
4 [4 {6 H K+ t5 {! SChapter 1 Introduction . . . . . . . . . . . . . . 1. \; ?7 a: A7 ^: ?; U
1.1 Additives . . . . . . . . . . . . . . . . . . . . . . . . 2
, `% V* S! @3 R1.1.1 Additive functionality . . . . . . . . . 3
6 l; L8 [( K5 \8 g' V1.2 Plastics formulations . . . . . . . . . . . . . . . 5
3 @8 m% T. l6 @. P1.2.1 Supply forms . . . . . . . . . . . . . . . 7
6 x$ n6 Y* z5 Y% l; x1.2.2 Additive delivery . . . . . . . . . . . . 9) H( X$ S) s* c: P$ C
1.3 Economic impact of polymer additives . . 9
/ c0 l0 a. S% V; ]5 T& G1.4 Analysis of plastics . . . . . . . . . . . . . . . . 11" x1 N5 d; H) [) e* `
1.4.1 Regulations and standardisation . . 15
1 E# h, F9 B' i8 \' U' Q1.4.2 Prior art . . . . . . . . . . . . . . . . . . . 17
" ^$ _4 K' u& m5 d+ p1.4.3 Databases . . . . . . . . . . . . . . . . . . 19
2 ^5 k; N3 f; c6 s4 A4 @4 v! y1.4.4 Scope . . . . . . . . . . . . . . . . . . . . . 20* F( V* K$ w# U6 l2 P5 H' s
1.4.5 Chapter overview . . . . . . . . . . . . 22' F& V; f9 y; a8 h3 {- t: S
1.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 23' @: w% T' |( ^2 {4 Q
1.5.1 Plastics additives . . . . . . . . . . . . . 235 f* z% p- ]! x( @; i
1.5.2 Processing technologies . . . . . . . . 237 L# a7 I" f8 F
1.5.3 Instrumental analysis . . . . . . . . . . 23% X; O! [; ~% _8 t: d
1.5.4 Polymer analysis . . . . . . . . . . . . . 24
% ^0 O& ^8 j( J$ e; g; x1.5.5 Polymer/additive analysis . . . . . . 24( B) c) |* u$ Z, h3 u7 S
1.6 References . . . . . . . . . . . . . . . . . . . . . . . 24
* m% R9 b% \% Y5 f3 VChapter 2 Deformulation Principles . . . . 29( }) K- F, O( R$ [; x& u
2.1 Polymer identification . . . . . . . . . . . . . . 30! m e( H; y7 I# O% M
2.2 Additive analysis of rubbers: ‘Best
# w/ l2 u0 S/ F( u, ^Practice’ . . . . . . . . . . . . . . . . . . . . . . . . 32
6 ]; h0 E# i! X2.3 Polymer extract analysis . . . . . . . . . . . . . 42
# g4 g% \7 V; O6 @- o) \6 e$ V2.4 In situ polymer/additive analysis . . . . . . 46
8 m1 [ l0 n( t2.5 Class-specific polymer/additive analysis . 478 P1 i+ ?- q1 e4 K% L( ~# Y" z
2.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 48
$ }* S- a# c7 P! x X2.6.1 Polymer identification . . . . . . . . . 48
, k# P' E! ?# p& g* P* _' q2.6.2 Deformulation of rubbers . . . . . . 48
) a9 x6 E: S% p( _" Y" `) q2.6.3 Deformulation of polymers . . . . . 48% @# `/ t4 G% g4 k1 X S% e/ H
2.7 References . . . . . . . . . . . . . . . . . . . . . . . 48( b$ \2 ^* ?& N! b, w, d( M
Chapter 3 Sample Preparation1 ]$ F9 }" S% I4 x+ l1 a
Perspectives . . . . . . . . . . . . . . 51- J- ~4 h/ T0 R( O, L) P
3.1 Solvents . . . . . . . . . . . . . . . . . . . . . . . . 541 i" e' y; K; \8 L- {2 \/ W( j
3.1.1 Polymer solubility criteria . . . . . . 559 M' V, s" L4 t' T7 L2 Y
3.1.2 Solubility parameters . . . . . . . . . . 55% j2 W% p, K2 f |" c K
3.1.3 Polymer solutions . . . . . . . . . . . . 56
, O L- z2 Z% N' s. a3.2 Extraction strategy . . . . . . . . . . . . . . . . . 57+ R+ X7 v* t) s- j2 Q7 W
3.3 Conventional extraction technologies . . . 599 P0 C8 V/ |; k- R$ U" V9 v, Y
3.3.1 Liquid–liquid extraction . . . . . . . 60- M3 T% Y8 W! T: ]) a
3.3.2 Liquid–solid extraction . . . . . . . . 60$ A G3 @ B7 w) l2 o
3.3.3 Classical solvent extractions of
% [: A6 V5 i7 G) Fadditives from polymers . . . . . . . 61
2 p9 n6 s2 q% q* a- @- ]6 s3.3.4 Sonication . . . . . . . . . . . . . . . . . 75; }0 q, B& _7 ^
3.4 High-pressure solvent extraction methods 818 [# t3 p% k3 d5 C! |; g0 s# p( L& k
3.4.1 Supercritical fluid technology . . . 81+ U6 X" G/ k2 z2 P6 P
3.4.2 Analytical SFE . . . . . . . . . . . . . . 85- I3 E1 y. `- V5 A: S, G
3.4.3 Subcritical water extraction . . . . . 1002 t9 q6 Z4 l6 v5 r! P/ a. x
3.4.4 Microwave technology . . . . . . . . 101
2 K- r; h3 t* H: K2 a3.4.5 Microwave-assisted extractions . . 104" o) T0 w D" n7 e; y8 g5 `4 I% B
3.4.6 Pressurised fluid extraction . . . . . 117( T8 V; t' {6 [" z) n" L
3.5 Sorbent extraction . . . . . . . . . . . . . . . . . 123+ b' J1 e M# Q! A
3.5.1 Solid-phase extraction . . . . . . . . . 124
z' s' x) d: v3.5.2 Solid-phase microextraction . . . . . 129& D6 {* l/ a2 D+ _
3.5.3 Stir bar sorptive extraction . . . . . 1334 n& O4 }4 F, D$ V7 i
3.6 Methodological comparison of extraction" K7 K; [8 R3 u: j- f
methods. . . . . . . . . . . . . . . . . . . . . . . . . 134
0 s; {; m- p1 k3 [3 G7 }( I6 h3.6.1 Experimental comparisons . . . . . . 136
+ F- I4 ~# o: |, G2 l( C: Y3.6.2 Extraction selectivity . . . . . . . . . . 138+ W) H- l2 S' I8 g$ D% L1 J: s
3.6.3 ‘Nonextractable’ additive analysis 140
( k9 G+ ?+ C" P7 H3 }6 ]+ V( F3.7 Polymer/additive dissolution methods . . . 1464 _/ t. M0 J n ]; `
3.8 Hydrolysis . . . . . . . . . . . . . . . . . . . . . . . 152( ]4 ]: e3 A3 y2 t
3.9 Bibliography . . . . . . . . . . . . . . . . . . . . . 155
5 M, E! C' G% j. Y3 p. I3.9.1 Sampling and sample preparation 155
6 e( p J; B5 C8 T1 S3 E3.9.2 Solvents/solubility . . . . . . . . . . . . 155* n5 B/ a8 H1 J3 s7 C' K3 c3 p
3.9.3 Extraction methods . . . . . . . . . . . 156
8 |3 r1 B3 t9 [4 U( ?* w' C& t3.10 References . . . . . . . . . . . . . . . . . . . . . . . 156; f$ ~- B; ?: \0 G& ?* s: a4 L# ?
vi Contents
- x6 U; z" M. h8 J" t5 z: PChapter 4 Separation Techniques . . . . . . 171- y$ [7 n( a7 p" g
4.1 Analytical detectors . . . . . . . . . . . . . . . . 177' k/ a- C- N; b' w7 [+ u4 L
4.2 Gas chromatography . . . . . . . . . . . . . . . 181& {3 O9 ~/ w* _6 c
4.2.1 High-temperature gas
5 F$ E; U+ N/ Qchromatography . . . . . . . . . . . . . 200
/ F) Q* B9 [& I s/ V( z4.2.2 Headspace gas chromatography . . 2022 u6 ^6 w, Q- ], u
4.3 Supercritical fluid chromatography . . . . . 205) b+ e% {, |# N: y2 y9 m( ~
4.4 Liquid chromatography techniques . . . . . 217
S( Q" W/ @. @+ v7 k' L4.4.1 Planar chromatographies . . . . . . . 218" @- n+ w, i' G+ P' n* G" H( Z# {
4.4.2 Column chromatographies . . . . . . 230
3 j# ^& }8 K3 R5 g4 j; A4 C4.5 Capillary electrophoretic techniques . . . . 273) Y4 \$ x; g; Q T
4.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 278
$ k/ q5 [8 L& o7 M7 v4.6.1 General texts . . . . . . . . . . . . . . . 278
N6 ~; F* s% B4 O k6 P# U4.6.2 Detectors . . . . . . . . . . . . . . . . . . 2790 z* f' S" l( U2 ^
4.6.3 Gas chromatography . . . . . . . . . . 2792 w5 _4 b$ u) @8 A/ ^5 X
4.6.4 Supercritical fluid chromatography 279
( @' F: K& ], f8 k6 ^ I4.6.5 Thin-layer chromatography . . . . . 279% d7 V! c/ S6 v* j4 [3 w
4.6.6 Liquid chromatography . . . . . . . . 280
- {- U. H' J; q4.6.7 Size-exclusion chromatography . . 280
+ T7 n: Q5 c. W* F$ J8 W6 B8 C8 m4.6.8 Ion chromatography . . . . . . . . . . 280
0 C" z3 {/ y5 V8 n- \- @4 S4.6.9 Capillary electrophoretic
# J1 {7 e- C; R$ Y% C0 Gtechniques . . . . . . . . . . . . . . . . . 280; ]: _. N4 J5 W W4 M! U6 v0 g
4.7 References . . . . . . . . . . . . . . . . . . . . . . . 2811 M5 @6 I. i' [& L
Chapter 5 Polymer/Additive Analysis:( y1 [5 I+ X' j5 ~! P" E- ]1 w
The Spectroscopic Alternative 299
- W. B0 ^3 p% } {5.1 Ultraviolet/visible spectrophotometry . . . 302
* \, C; j9 q" Y- C! M/ b3 e8 Z! \5.2 Infrared spectroscopy . . . . . . . . . . . . . . . 311$ }+ L! d; i& ~5 ~# F- ~ l8 H
5.3 Luminescence spectroscopy . . . . . . . . . . 318: N* K1 m4 }+ J7 x) S
5.4 High-resolution nuclear magnetic' a9 \- b0 u; _* q! j, e8 I6 ~* R7 g
resonance spectroscopy . . . . . . . . . . . . . 323
- H7 h. k% b1 p$ x3 G9 Y/ b) F: |5.4.1 Multidimensional NMR
! q4 O) j3 o. ]) i6 vspectroscopy . . . . . . . . . . . . . . . . 336% \, x K; s" I' _- h+ X
5.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 342
+ t% y% L$ o2 ]% r! r1 y3 q; ]1 E8 b5.5.1 General spectroscopy . . . . . . . . . 3420 ?( r3 L* d' Q3 W
5.5.2 Ultraviolet/visible
% i* \% {: c% l+ l8 P) n( H, H1 Espectrophotometry . . . . . . . . . . . . 342& x( w1 X8 o- S1 O, a
5.5.3 Infrared spectroscopy . . . . . . . . . 342( w% O% ^* H6 ~1 |% H/ G& k
5.5.4 Luminescence spectroscopy . . . . . 342) P3 G* l& g5 _# W u/ l7 p
5.5.5 Nuclear magnetic resonance
: D; H- }- x% [; ^& ^, b% tspectroscopy . . . . . . . . . . . . . . . . 342
7 f' g- e! ?: e8 I1 X) u5.6 References . . . . . . . . . . . . . . . . . . . . . . . 342
7 g% O) w; @& p9 v! Z. d# B: S# \' NChapter 6 Organic Mass-Spectrometric! R5 P. p8 g5 u
Methods . . . . . . . . . . . . . . . . 349
9 d# t# D4 g: @5 \5 X$ C6.1 Basic instrumentation . . . . . . . . . . . . . . . 3515 w/ M% Z+ X e: P' D* a$ I
6.1.1 Inlet systems . . . . . . . . . . . . . . . . 352
6 `/ m$ {1 @8 S& O/ E8 k) ^, h3 n6.1.2 Modes of detection . . . . . . . . . . . 353
/ k- X# N d7 Q$ e6.1.3 Mass resolution . . . . . . . . . . . . . . 354
" |, h. L$ a) L2 l# g0 y6.1.4 Isotope distributions . . . . . . . . . . 354
, p1 m m& q7 e* G$ a; n6.1.5 Accurate mass measurements. . . . 355; y; K6 |8 S* }
6.2 Ion sources . . . . . . . . . . . . . . . . . . . . . . 357- `; x8 X: s$ B5 e' _9 L2 X
6.2.1 Electron impact ionisation . . . . . . 360" t; J0 l, N) D+ H2 t# r
6.2.2 Chemical ionisation . . . . . . . . . . . 362
5 y i; h5 n# M2 h. r! _6.2.3 Metastable atom bombardment . . 3673 w9 W4 [. ?5 V" F B6 Q0 J
6.2.4 Fast atom bombardment . . . . . . . 367
2 R, l B# J+ [! ^; B$ l7 q6.2.5 Field ionisation . . . . . . . . . . . . . . 3728 D- @. G6 P, B. ?$ r
6.2.6 Field desorption . . . . . . . . . . . . . 374
6 W$ }, Q: q8 }, Z/ v* v' c( C6.2.7 Thermospray ionisation . . . . . . . . 376& |0 t* F. @. ?" b7 F3 M( y; H0 ?
6.2.8 Atmospheric pressure ionisation
- X4 m4 y' x. I/ E2 t' Ytechniques . . . . . . . . . . . . . . . . . 3781 t# y; V" o. c* s( q
6.2.9 Desorption/ionisation methods . . . 383
- O$ M9 l0 ^8 w) M1 x) K6.2.10 Photoionisation techniques. . . . . . 385
! r% R$ ^9 e8 J1 X; f$ c6.3 Mass analysers . . . . . . . . . . . . . . . . . . . 3860 _" K' N& R* n, z' E
6.3.1 Sector analysers . . . . . . . . . . . . . 387
. i: {* A" l- g! u4 ~5 z- y6.3.2 Quadrupole mass spectrometers . . 389
; {7 d) g6 ?7 E u' ~" D6.3.3 Time-of-flight mass spectrometry . 390
3 y7 U: ~9 R: ~+ L! C8 X$ H6.3.4 Quadrupole ion trap . . . . . . . . . . 3935 R/ j& a0 A6 Q8 o% _3 ?
6.3.5 Fourier-transform ion-cyclotron, ]# L! Y; l9 J/ c! f4 n; p: d9 s
resonance mass spectrometry . . . . 395: u7 Y5 P- k# Y/ i O
6.3.6 Tandem mass spectrometry . . . . . 398
' q2 V9 q; c4 M3 h4 g! M6.4 Direct mass-spectrometric polymer8 N! @0 L( c% r" @
compound analysis . . . . . . . . . . . . . . . . . 4070 Z/ {- k6 \4 o0 j' ~, M* n
6.5 Ion mobility spectrometry . . . . . . . . . . . 415
, N: P6 A$ e) \" U6 [6.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 417
8 N1 O' J4 i4 B. i$ @0 I9 I1 z6.6.1 Mass spectrometry (General) . . . . 417
7 }( y: j* b* c8 o7 m1 A6.6.2 Mass spectrometers . . . . . . . . . . . 4176 k; |9 r+ d; H9 r/ f+ q
6.6.3 Ionisation modes . . . . . . . . . . . . . 417 Z: B! a9 Q& x% @& p6 H$ {. o
6.7 References . . . . . . . . . . . . . . . . . . . . . . . 418
# T+ m9 \) @6 u! vChapter 7 Multihyphenation and
* R4 b5 S5 z) X% t1 _; e, ^Multidimensionality in
! x1 a; |- U$ ]: h/ hPolymer/Additive Analysis . . . 425
1 [5 {8 t) |4 C4 M0 ^0 \- }* f7.1 Precolumn hyphenation . . . . . . . . . . . . . 4283 _: n4 G6 }: W# F! Q f! J7 Y
7.1.1 Chromatographic sampling
# v" M* i0 L. ]methods . . . . . . . . . . . . . . . . . . . 432
6 e9 H" A; f0 S" o+ X7.2 Coupled sample
8 C9 L+ F2 n+ V! T* E- Apreparation – spectroscopy/spectrometry . 449
& O# d. E1 H; e9 }7.3 Postcolumn hyphenation . . . . . . . . . . . . . 452
* p) W6 T, Q8 p7 D7.3.1 (Multi)hyphenated GC techniques 456
! E/ }, j6 T. k5 X7.3.2 (Multi)hyphenated SFC1 Z: A, o' C& A# H
techniques . . . . . . . . . . . . . . . . . 475
# k4 z8 D; E6 G. B' Q5 L7.3.3 (Multi)hyphenated HPLC
7 [ m! H2 p# O/ x5 t' mtechniques . . . . . . . . . . . . . . . . . 489" l( G0 l( I& y4 q6 u
7.3.4 Hyphenated SEC techniques . . . . 527
* s* d+ L- B2 Z( M+ l7 h7.3.5 Hyphenated TLC techniques . . . . 5301 j4 K+ A7 V0 ^
7.3.6 Hyphenated CE techniques . . . . . 543. C& k# E" q# ]
Contents vii
% N8 Q; q, H) C ?3 z" i7 F7.4 Multidimensional chromatography . . . . . 545
% {8 K5 }' r' s \ K7.4.1 Multidimensional gas
2 @6 W7 w% F1 T7 C" l5 Xchromatography . . . . . . . . . . . . . 548+ |% t4 t) o) v
7.4.2 Multidimensional supercritical! D% p: x$ N( Z9 H3 M; K8 ~) q% B& b
fluid chromatography . . . . . . . . . 550
9 y( o' b0 I: @: Q# a3 W7.4.3 Multidimensional liquid1 y: u2 R% @& s6 J
chromatography . . . . . . . . . . . . . 5500 _$ B; \; i( A2 |0 ]' j L6 w2 ~
7.4.4 Multidimensional thin-layer+ }( `$ |" k k& v8 N9 p C E
chromatography . . . . . . . . . . . . . 558$ |8 d$ S% _5 i2 c
7.5 Multidimensional spectroscopy . . . . . . . . 560
0 O, B" [, F+ f+ S' A7.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 562
7 p; V {5 o; g- `+ v( {2 d/ s9 v7.6.1 General . . . . . . . . . . . . . . . . . . . 5627 d0 S* |/ P0 O$ }
7.6.2 Multihyphenation and" b) q3 L* S* R7 C( e
multidimensionality . . . . . . . . . . . 563$ G- w; r4 y% ]; O5 L
7.6.3 Precolumn hyphenation . . . . . . . . 5633 z- J% P {$ i- N. O
7.6.4 Postcolumn hyphenation . . . . . . . 563
" R+ U3 ^1 e' p+ [7 V7.6.5 Multidimensional chromatography 563
. Y& s8 ^) v0 W; g7.6.6 Multidimensional spectroscopy . . 5635 `( a8 t, t6 J. k7 O
7.7 References 564) u2 ?/ W j; `4 M
Chapter 8 Inorganic and Element
$ }; M2 N- F c; tAnalytical Methods . . . . . . . . 5859 _" C$ \: {: v6 l3 i" @
8.1 Element analytical protocols . . . . . . . . . . 587
5 G+ U, O$ d, N8.1.1 Element analytical pretreatment
1 ]. M! i& l/ D4 C: U/ R6 rprotocols . . . . . . . . . . . . . . . . . . 588
# N$ X1 @; h* ?2 y5 e8.1.2 Elemental analysis methods . . . . . 589- {# M5 e3 ~' ~. h7 e, a9 p& g9 }/ z
8.2 Sample destruction for classical elemental
+ N2 _1 m/ M$ ?7 U/ canalysis . . . . . . . . . . . . . . . . . . . . . . . . . 591
. J8 V x9 }5 x# d/ v8.2.1 Combustion analysis . . . . . . . . . . 593
. |( S$ n, x5 [$ E8 f8.2.2 Wet matrix digestion . . . . . . . . . . 597* J2 e/ h* f9 ^+ b. K1 h! K9 d
8.2.3 Fusion methods . . . . . . . . . . . . . . 604
, {1 d) D% ~# O) ]& Z8.3 Analytical atomic spectrometry . . . . . . . . 605
. `. V2 X% g! M, s" v; [8.3.1 Atomic absorption spectrometry . 608
; V% s+ G$ ?1 o. D8.3.2 Atomic emission spectrometry . . . 613/ r ?. f6 d6 g5 }+ b$ d1 x, i/ f
8.3.3 Atomic fluorescence spectrometry 624 |
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