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Acknowledgements. . . . . . . . . . . . . . . . xv
: g' ?/ F1 ?# FChapter 1 Introduction . . . . . . . . . . . . . . 1
1 z9 R1 Y+ u" H' G, I1.1 Additives . . . . . . . . . . . . . . . . . . . . . . . . 2+ H& q8 E1 J4 Q
1.1.1 Additive functionality . . . . . . . . . 3
1 c F+ g' e o5 a1.2 Plastics formulations . . . . . . . . . . . . . . . 5; Z7 w( A1 @8 c0 c# C5 v
1.2.1 Supply forms . . . . . . . . . . . . . . . 7" L: N4 x0 ?& B- R5 L: r6 ]
1.2.2 Additive delivery . . . . . . . . . . . . 9
, m( a0 z- l8 `; f* E1.3 Economic impact of polymer additives . . 97 L A. x2 B6 p" L
1.4 Analysis of plastics . . . . . . . . . . . . . . . . 11/ U# a% f4 d/ G
1.4.1 Regulations and standardisation . . 157 r6 {7 V/ j1 J ~4 y
1.4.2 Prior art . . . . . . . . . . . . . . . . . . . 17
% R# ]- `! @; N$ i. g( O5 N1.4.3 Databases . . . . . . . . . . . . . . . . . . 19
$ h& m' Z$ D7 ]3 [+ k1.4.4 Scope . . . . . . . . . . . . . . . . . . . . . 20
0 U# u& C( N0 I/ V+ j1.4.5 Chapter overview . . . . . . . . . . . . 22
1 T0 L' F- ^! E+ `' O5 w4 P1.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 23
' V( |# p5 F1 u- J- v% r5 T4 c6 J% ?1.5.1 Plastics additives . . . . . . . . . . . . . 23. a0 h6 y6 w) @/ N
1.5.2 Processing technologies . . . . . . . . 23- Q+ B2 B$ _+ F2 d9 e9 k: |
1.5.3 Instrumental analysis . . . . . . . . . . 23
, l/ _ }* o2 u1.5.4 Polymer analysis . . . . . . . . . . . . . 24: ~3 K# U9 `+ E; B. h
1.5.5 Polymer/additive analysis . . . . . . 24
- Q- p) n4 M# P# i# v1.6 References . . . . . . . . . . . . . . . . . . . . . . . 24 f r% k4 y) i- \ t- @
Chapter 2 Deformulation Principles . . . . 29! D& ^% U8 ]1 j% q( @7 U
2.1 Polymer identification . . . . . . . . . . . . . . 30* I! Q$ A+ T& r) e" w9 Y! w+ T
2.2 Additive analysis of rubbers: ‘Best f2 y: b3 |, B# G
Practice’ . . . . . . . . . . . . . . . . . . . . . . . . 32* v/ C. J' H) r0 T# ]( Y% [$ Z' w- A
2.3 Polymer extract analysis . . . . . . . . . . . . . 42
! e% V `( q! c& ]7 s. t2.4 In situ polymer/additive analysis . . . . . . 46- Z0 U: t+ D" p+ e
2.5 Class-specific polymer/additive analysis . 472 X6 g' L g2 H
2.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 48
# k1 ]3 h9 h% @5 E2.6.1 Polymer identification . . . . . . . . . 484 u3 h8 H7 I7 e1 U0 b [: U, j
2.6.2 Deformulation of rubbers . . . . . . 48
/ r, x* s# H, ?- w& N: d) J2.6.3 Deformulation of polymers . . . . . 48) m& O/ ~* Z& q+ Z V3 m2 |& i9 e
2.7 References . . . . . . . . . . . . . . . . . . . . . . . 48* l% P+ N( N8 L5 z2 N
Chapter 3 Sample Preparation$ u$ `, g5 Y! J) U/ I
Perspectives . . . . . . . . . . . . . . 51, E! M$ C4 `/ X# s4 k
3.1 Solvents . . . . . . . . . . . . . . . . . . . . . . . . 54, @4 A! W7 T' H# I
3.1.1 Polymer solubility criteria . . . . . . 559 |( h3 F" E/ [" n6 d
3.1.2 Solubility parameters . . . . . . . . . . 55, _' d) x% ?5 V) V* L
3.1.3 Polymer solutions . . . . . . . . . . . . 56
/ K- z) v+ [ w& S7 E2 C4 }3.2 Extraction strategy . . . . . . . . . . . . . . . . . 579 M6 q# y, J7 t$ M2 {
3.3 Conventional extraction technologies . . . 59+ [- }9 A9 t; O
3.3.1 Liquid–liquid extraction . . . . . . . 605 R( L) f U, e( O1 t" z% ^
3.3.2 Liquid–solid extraction . . . . . . . . 605 y; \/ J$ o6 P) U
3.3.3 Classical solvent extractions of( W! |5 s4 D% q' _; p
additives from polymers . . . . . . . 61! o5 I. I' v% q, k+ ^' ~; w( L
3.3.4 Sonication . . . . . . . . . . . . . . . . . 75
3 c7 j1 R. U9 a) Y3.4 High-pressure solvent extraction methods 81
' C+ u" d% J1 ?3.4.1 Supercritical fluid technology . . . 81
; q8 ~2 Z. P) I3.4.2 Analytical SFE . . . . . . . . . . . . . . 850 ~, W) g; A' Y& n* O
3.4.3 Subcritical water extraction . . . . . 100/ H+ {0 Q, K# {
3.4.4 Microwave technology . . . . . . . . 101$ }2 g2 C: h& o- v7 M
3.4.5 Microwave-assisted extractions . . 104) i B7 R' a1 A, i, I# T
3.4.6 Pressurised fluid extraction . . . . . 117! O+ q* V1 y" f/ N* t7 S
3.5 Sorbent extraction . . . . . . . . . . . . . . . . . 123- N* V" i2 D/ D3 o! L# y# y
3.5.1 Solid-phase extraction . . . . . . . . . 124
) \! `% z' E: e, ~1 }3.5.2 Solid-phase microextraction . . . . . 129
5 b: q( }( D. L3 t% c L3.5.3 Stir bar sorptive extraction . . . . . 133
" J9 _/ C6 w! y, R- U1 m3.6 Methodological comparison of extraction
$ F/ w$ M" d. `1 S9 u" wmethods. . . . . . . . . . . . . . . . . . . . . . . . . 134
9 M! b) f3 }& k/ n% B4 a/ L) e3.6.1 Experimental comparisons . . . . . . 136
7 Z. c E% a- J8 s6 p( |. }3.6.2 Extraction selectivity . . . . . . . . . . 138
7 [) Z( E! }9 w8 c3.6.3 ‘Nonextractable’ additive analysis 140
$ A" h$ P: Z: f+ ?0 `( D& R3.7 Polymer/additive dissolution methods . . . 146
" L5 L2 L1 L' y3 O3.8 Hydrolysis . . . . . . . . . . . . . . . . . . . . . . . 1523 V4 M0 o8 E8 B7 v" H7 H6 A
3.9 Bibliography . . . . . . . . . . . . . . . . . . . . . 155& C- [: g3 n/ n8 I" k' \
3.9.1 Sampling and sample preparation 155
" [7 T: J3 P, `* @3.9.2 Solvents/solubility . . . . . . . . . . . . 155
/ Z% m$ K% E2 ~" d/ `3.9.3 Extraction methods . . . . . . . . . . . 156
9 B3 D, m' M; Q, \+ F3.10 References . . . . . . . . . . . . . . . . . . . . . . . 1564 ~2 p9 |/ p3 x/ _" A, P+ A
vi Contents/ \. N& m& V% Y& C, c) e
Chapter 4 Separation Techniques . . . . . . 171
; q( g4 ~: z9 Q3 i! c7 f2 ?. |4 l0 L4.1 Analytical detectors . . . . . . . . . . . . . . . . 177
9 ~1 C% }+ A2 J8 s# u# y/ n4.2 Gas chromatography . . . . . . . . . . . . . . . 181
! u/ B2 W# v# ]0 Y4.2.1 High-temperature gas
) e) I- f5 B6 K1 o; k- kchromatography . . . . . . . . . . . . . 200
: ~+ _& W7 x5 ^( t4.2.2 Headspace gas chromatography . . 202
* S% e# ~; e* J# t& Z% D4.3 Supercritical fluid chromatography . . . . . 2055 A4 n b) f# }) e4 r
4.4 Liquid chromatography techniques . . . . . 2173 I8 |* `! x- O4 ]
4.4.1 Planar chromatographies . . . . . . . 218* n( L9 v X) n \5 B6 [
4.4.2 Column chromatographies . . . . . . 230
# \5 E) c; c% x7 c4.5 Capillary electrophoretic techniques . . . . 273) p2 J% l- |; e9 M/ \% d
4.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 278
6 Q4 h" w9 f* Q1 l4.6.1 General texts . . . . . . . . . . . . . . . 278) H3 I) F2 m# G% B6 Q+ J4 o' P
4.6.2 Detectors . . . . . . . . . . . . . . . . . . 279
8 Q- U' \: m; B4.6.3 Gas chromatography . . . . . . . . . . 279
* X0 H. T* L( o4.6.4 Supercritical fluid chromatography 279
. B! d6 p, U P' t k4.6.5 Thin-layer chromatography . . . . . 279
# L. m9 r8 o- s* m; v4.6.6 Liquid chromatography . . . . . . . . 280
9 O2 r) @" T( W! Q4 b* w; r4.6.7 Size-exclusion chromatography . . 280
" `2 C: h* ]. s* ]5 S, `6 W4.6.8 Ion chromatography . . . . . . . . . . 280
0 c, s* @/ K# j: A+ h' |4.6.9 Capillary electrophoretic
' k) M* G& H7 b$ Y$ x. Vtechniques . . . . . . . . . . . . . . . . . 280
. W6 v/ b# }" `% |0 N* y- g8 b' k4.7 References . . . . . . . . . . . . . . . . . . . . . . . 281& o- b0 r; T& C7 v
Chapter 5 Polymer/Additive Analysis:
" d# r& O. }/ r2 VThe Spectroscopic Alternative 299
# Z* i- S1 b: n4 B5.1 Ultraviolet/visible spectrophotometry . . . 302( Y5 S* V3 S1 Q) f. f/ x
5.2 Infrared spectroscopy . . . . . . . . . . . . . . . 311/ q& y) Z5 ]' D7 f
5.3 Luminescence spectroscopy . . . . . . . . . . 318- Y$ O; A# @3 ? |
5.4 High-resolution nuclear magnetic* W+ M( _% K% I6 a' _, C& }8 S4 p1 Y
resonance spectroscopy . . . . . . . . . . . . . 323
% A7 x! B6 v1 x) Y+ q5.4.1 Multidimensional NMR
, Y, h( {( T& q9 Q5 W8 Wspectroscopy . . . . . . . . . . . . . . . . 3368 Q2 k" C! ?" t6 v5 Y
5.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 342
9 c& Q! U6 j/ o8 ?5.5.1 General spectroscopy . . . . . . . . . 342( Z1 O {4 K: J
5.5.2 Ultraviolet/visible
J! T1 ^$ h1 f9 ~3 P2 Xspectrophotometry . . . . . . . . . . . . 3422 ]% c9 ~3 c; E, k5 o* z
5.5.3 Infrared spectroscopy . . . . . . . . . 342
, g x7 Y2 d5 x) X* I5.5.4 Luminescence spectroscopy . . . . . 342
+ A; F/ M, s d8 \5.5.5 Nuclear magnetic resonance Y+ g1 l9 e' S9 t' E
spectroscopy . . . . . . . . . . . . . . . . 342
, r9 f3 r% `9 _) ?) o0 G" s5.6 References . . . . . . . . . . . . . . . . . . . . . . . 342
' T3 t3 v7 A6 ]7 c @( E* l/ tChapter 6 Organic Mass-Spectrometric
# N _, ^8 c( Q5 T; {Methods . . . . . . . . . . . . . . . . 349: {4 Q& I! A. J( f& ^ X( J+ T
6.1 Basic instrumentation . . . . . . . . . . . . . . . 3515 _5 ?9 F4 U8 H3 v) u1 {8 o
6.1.1 Inlet systems . . . . . . . . . . . . . . . . 352: v0 _* S# `5 m- I, t4 V
6.1.2 Modes of detection . . . . . . . . . . . 353% ^- s) t% t- z9 t. R8 f
6.1.3 Mass resolution . . . . . . . . . . . . . . 354
( q; c" A9 w5 B: c/ R6.1.4 Isotope distributions . . . . . . . . . . 354
/ R% O% `4 s3 ?8 y( c/ r6.1.5 Accurate mass measurements. . . . 355
, m# h* E( Z2 m# z, x5 ?" H3 h; r1 F" x6.2 Ion sources . . . . . . . . . . . . . . . . . . . . . . 357. d4 P: @8 C; Q3 B0 M% i! z' l9 M
6.2.1 Electron impact ionisation . . . . . . 360
0 a! _) j3 L9 O6.2.2 Chemical ionisation . . . . . . . . . . . 362
9 u0 f. q0 A5 }* O" M6.2.3 Metastable atom bombardment . . 367
# s$ }! \: J9 B: @2 W! Q6.2.4 Fast atom bombardment . . . . . . . 3672 K& H- `4 ]5 m* q! z5 |, ]
6.2.5 Field ionisation . . . . . . . . . . . . . . 372
. o' g$ w* o2 r6.2.6 Field desorption . . . . . . . . . . . . . 3745 Q: X1 u0 N- f# M+ R5 t
6.2.7 Thermospray ionisation . . . . . . . . 376. |5 z5 W. L! w0 C1 ^
6.2.8 Atmospheric pressure ionisation6 j( ~0 {! }' |2 x/ Q
techniques . . . . . . . . . . . . . . . . . 378
! }* i q7 J9 F9 u% ?9 w6.2.9 Desorption/ionisation methods . . . 383
8 O7 ^7 ]# O4 S/ u5 Q. U6.2.10 Photoionisation techniques. . . . . . 385+ L; v2 ^2 l4 ~! O4 H. y' x. P1 l
6.3 Mass analysers . . . . . . . . . . . . . . . . . . . 386
' y7 j* h% B+ t+ |% h, Y- Q6.3.1 Sector analysers . . . . . . . . . . . . . 387
( v% X1 J5 @! E; l& P) j1 X: `' j6.3.2 Quadrupole mass spectrometers . . 389
2 k8 a5 H& v4 K0 f0 L5 M5 g- |6.3.3 Time-of-flight mass spectrometry . 390
! H! I( c+ H' J6 H" v5 ]" X6.3.4 Quadrupole ion trap . . . . . . . . . . 393! I8 I* `9 w* b& P' ~# \
6.3.5 Fourier-transform ion-cyclotron5 g' o8 m0 f3 i8 ], E4 o
resonance mass spectrometry . . . . 3958 a9 |) A8 G9 {- v5 V; D3 E
6.3.6 Tandem mass spectrometry . . . . . 398
" ^# ?9 F1 u' J6.4 Direct mass-spectrometric polymer
* ^7 y6 Y7 K. h% @1 d' u9 B. u- K" bcompound analysis . . . . . . . . . . . . . . . . . 407
# |- r- }1 o [2 q6.5 Ion mobility spectrometry . . . . . . . . . . . 415
- U) G' g. G" b1 \! B9 v1 y0 j6.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 417) d9 {$ x; i& c) m$ m; E! m; f
6.6.1 Mass spectrometry (General) . . . . 417
6 k: ?- A$ U, ]$ N) Z( [6 Y6.6.2 Mass spectrometers . . . . . . . . . . . 417
5 ^& b' u! E7 N& u7 X7 {* N6 A9 o6.6.3 Ionisation modes . . . . . . . . . . . . . 417
2 o* \ f- H2 ~6 K' H- S6.7 References . . . . . . . . . . . . . . . . . . . . . . . 418" W1 j2 E$ a; Q, P
Chapter 7 Multihyphenation and
s+ R' J% U, C) s( PMultidimensionality in
S0 R5 {: ~: |; V. A* Z3 m0 LPolymer/Additive Analysis . . . 425- S# S& E8 H: \$ z* r z3 n: \7 s& d
7.1 Precolumn hyphenation . . . . . . . . . . . . . 428$ G# o% X+ Z( A7 ~, D& ]4 o! f
7.1.1 Chromatographic sampling
0 e9 V& u+ P) Z Q6 d5 Gmethods . . . . . . . . . . . . . . . . . . . 432
/ U7 a7 I. C s a7.2 Coupled sample. [0 p! G6 q; Y8 v* L' u
preparation – spectroscopy/spectrometry . 449) k X$ V8 S1 y- S) o
7.3 Postcolumn hyphenation . . . . . . . . . . . . . 452( G/ ]3 M7 o Q. E1 }: r
7.3.1 (Multi)hyphenated GC techniques 456# A( {, d& s4 i
7.3.2 (Multi)hyphenated SFC0 H- j3 V2 q" X6 a# u8 D; @4 n2 r
techniques . . . . . . . . . . . . . . . . . 475
5 L$ B. O6 E' t' H# m7.3.3 (Multi)hyphenated HPLC/ g% E& i2 H# ~/ l! ]8 t$ k: }( A
techniques . . . . . . . . . . . . . . . . . 489
( c3 Y2 L/ a) z6 U$ g" w2 G% _5 x7.3.4 Hyphenated SEC techniques . . . . 527
. r4 U+ Z/ a b$ _% g7.3.5 Hyphenated TLC techniques . . . . 5309 J6 c/ A9 A3 l, r. X
7.3.6 Hyphenated CE techniques . . . . . 543
% ]# A# B# U( GContents vii. u9 f0 W; ^% U% _' f3 H
7.4 Multidimensional chromatography . . . . . 545
) `: W: |- ~3 w7.4.1 Multidimensional gas
R) J3 W& }2 M" S7 p! B' x- i- {chromatography . . . . . . . . . . . . . 548
5 i$ H8 X/ j/ |0 t, V& [7.4.2 Multidimensional supercritical; {6 c L5 Y* e/ \: x" n5 K( }$ ?
fluid chromatography . . . . . . . . . 5508 A: H9 X: l9 T( x- V2 {+ B
7.4.3 Multidimensional liquid
9 L7 F0 U8 n% H' p' Gchromatography . . . . . . . . . . . . . 550) h- B' @' d0 U
7.4.4 Multidimensional thin-layer1 j' h$ Z* j9 I5 Q; d W
chromatography . . . . . . . . . . . . . 558
; p$ j. {, A' l# L* x8 Q7.5 Multidimensional spectroscopy . . . . . . . . 560
- i+ p5 Q( V. U7 `+ T7.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 5623 B8 V% b7 u5 m9 p' v
7.6.1 General . . . . . . . . . . . . . . . . . . . 5625 Y3 K$ j/ L& R0 E; Q& j Y
7.6.2 Multihyphenation and
0 N, u) s( [, T6 h1 ~/ lmultidimensionality . . . . . . . . . . . 563
" m3 N* B6 h7 E0 X0 P1 h1 ]7.6.3 Precolumn hyphenation . . . . . . . . 5631 R# N+ o( q8 {7 T6 G" G, w, X
7.6.4 Postcolumn hyphenation . . . . . . . 5634 Z c6 y! \+ W
7.6.5 Multidimensional chromatography 563
1 u5 l3 i9 ^3 g4 i, Y, f" J7.6.6 Multidimensional spectroscopy . . 563 a \* h% ]7 ^5 S8 N* _
7.7 References 564
$ E' L6 [% |1 c& k7 T @& ?7 B2 kChapter 8 Inorganic and Element/ o* Q0 e8 T% f' o; M2 F+ e
Analytical Methods . . . . . . . . 585/ @* U! z/ x: @5 N. d' s
8.1 Element analytical protocols . . . . . . . . . . 587
5 s5 w: [4 J; E9 ^4 j( j8.1.1 Element analytical pretreatment
# N3 N3 ^1 a/ j# u+ cprotocols . . . . . . . . . . . . . . . . . . 588
+ z7 }9 M# K: T# p& o8.1.2 Elemental analysis methods . . . . . 589. N1 u; U8 J5 h9 U' a$ p: u6 L( C5 f: m
8.2 Sample destruction for classical elemental7 U$ U; `6 ]* y& Y: p
analysis . . . . . . . . . . . . . . . . . . . . . . . . . 5917 \- W$ t4 Q" |) E6 T9 f
8.2.1 Combustion analysis . . . . . . . . . . 593
; _( |$ d/ [. g* O1 y3 |2 m, F8.2.2 Wet matrix digestion . . . . . . . . . . 597( T7 M) u# g* n
8.2.3 Fusion methods . . . . . . . . . . . . . . 604$ d* Z1 \* W7 i0 \
8.3 Analytical atomic spectrometry . . . . . . . . 605
! I/ A# Q0 o+ H, ?1 f8.3.1 Atomic absorption spectrometry . 608. M8 Y9 K8 `+ y* h B* }1 s1 T
8.3.2 Atomic emission spectrometry . . . 613
0 L- R8 Q8 R/ g# X' c8.3.3 Atomic fluorescence spectrometry 624 |
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