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Acknowledgements. . . . . . . . . . . . . . . . xv
, E. R( I$ j! I" d3 P1 mChapter 1 Introduction . . . . . . . . . . . . . . 1
1 c4 v& t8 l) L2 n1.1 Additives . . . . . . . . . . . . . . . . . . . . . . . . 2, g, e3 Y9 V3 u. h
1.1.1 Additive functionality . . . . . . . . . 3
`6 A1 t0 D2 |* m" Z( f1.2 Plastics formulations . . . . . . . . . . . . . . . 5
% E7 J H8 m/ s1.2.1 Supply forms . . . . . . . . . . . . . . . 7; O& @+ [" }- v, o* I8 i
1.2.2 Additive delivery . . . . . . . . . . . . 9
: ~) y' g! E$ s( O* g3 Y- w1.3 Economic impact of polymer additives . . 9
! N" w$ s- R3 t$ {/ @' g1.4 Analysis of plastics . . . . . . . . . . . . . . . . 11
* ]4 c7 R. [! I6 p, X8 v1.4.1 Regulations and standardisation . . 15
2 g6 p+ l$ v% S0 A a5 K1.4.2 Prior art . . . . . . . . . . . . . . . . . . . 171 ]; I4 r& Z, Y3 v8 T' m; ?0 D% k
1.4.3 Databases . . . . . . . . . . . . . . . . . . 19- l% v+ E( T2 ?5 [+ _
1.4.4 Scope . . . . . . . . . . . . . . . . . . . . . 20: H2 @1 ?" i; _- y
1.4.5 Chapter overview . . . . . . . . . . . . 223 k0 x7 D+ g; q; f8 E7 c1 X
1.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 23
; A1 \) l/ J( ^2 T- [/ O1.5.1 Plastics additives . . . . . . . . . . . . . 238 B' u& F8 S" _* A3 A1 Z0 `
1.5.2 Processing technologies . . . . . . . . 23
5 f& E+ [( R" W' J- @/ ~1.5.3 Instrumental analysis . . . . . . . . . . 238 z& |+ U% `/ N) R8 h, E
1.5.4 Polymer analysis . . . . . . . . . . . . . 241 W/ Y4 q$ ]! \( F, ~& C: C0 [- A" L
1.5.5 Polymer/additive analysis . . . . . . 247 n; R1 Q& ^6 `6 E( w- q
1.6 References . . . . . . . . . . . . . . . . . . . . . . . 24
+ S3 Z, c3 V) U7 }" {9 T9 DChapter 2 Deformulation Principles . . . . 29
, q' F8 q3 U5 k2.1 Polymer identification . . . . . . . . . . . . . . 30
2 l1 r* J4 T# Q( R2.2 Additive analysis of rubbers: ‘Best6 Q8 }3 j }( u4 y/ ?+ T# W }+ K
Practice’ . . . . . . . . . . . . . . . . . . . . . . . . 32% n& i9 h+ k+ n2 C
2.3 Polymer extract analysis . . . . . . . . . . . . . 42/ a7 U' u' B' |. R R/ P" \ r" r
2.4 In situ polymer/additive analysis . . . . . . 46* j0 x; t- z6 w
2.5 Class-specific polymer/additive analysis . 47
" Q7 h3 e% p9 ~! p i! o" m2.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 48
P" [' e: t! {! z2 _9 _6 z2.6.1 Polymer identification . . . . . . . . . 485 H/ i# n5 F5 w
2.6.2 Deformulation of rubbers . . . . . . 485 `$ O: g7 ]/ @5 x, k- n
2.6.3 Deformulation of polymers . . . . . 48
. j( x5 Z% O7 B% \2.7 References . . . . . . . . . . . . . . . . . . . . . . . 48
5 P+ W b4 W# j* S! l6 E, g6 M2 L9 EChapter 3 Sample Preparation& B+ a) l$ E5 m/ Q) r/ {
Perspectives . . . . . . . . . . . . . . 51
6 ?" S! j O8 l% r/ J( f3.1 Solvents . . . . . . . . . . . . . . . . . . . . . . . . 54
" V) Q" Q& w' w2 J. k Q( |- R3.1.1 Polymer solubility criteria . . . . . . 55
$ k5 a1 o# h& {# v# @3.1.2 Solubility parameters . . . . . . . . . . 554 c' a' A# t3 n# C" o L
3.1.3 Polymer solutions . . . . . . . . . . . . 56
. R6 t" g: Z6 F3.2 Extraction strategy . . . . . . . . . . . . . . . . . 57% Q/ z2 i- {1 w g7 ?9 e/ W. q2 {
3.3 Conventional extraction technologies . . . 59
1 k3 F) @0 N, b; [3.3.1 Liquid–liquid extraction . . . . . . . 60" T5 P2 i: i. ?8 [: K) m
3.3.2 Liquid–solid extraction . . . . . . . . 60
9 g- t1 Z6 f- P/ j+ s! `& h3.3.3 Classical solvent extractions of
- ~% u+ C c5 zadditives from polymers . . . . . . . 61; A. Q4 A# E4 {4 p0 q) v$ C
3.3.4 Sonication . . . . . . . . . . . . . . . . . 75
2 L1 n1 F: S+ D- Y1 R% o! j* R7 x! o3.4 High-pressure solvent extraction methods 810 Z. I8 a1 k4 V8 g
3.4.1 Supercritical fluid technology . . . 81
' ? b4 \8 J! R4 |+ d3.4.2 Analytical SFE . . . . . . . . . . . . . . 859 P. P9 ~2 S+ ]6 b4 P" c1 I
3.4.3 Subcritical water extraction . . . . . 100
) v, a7 \, i; v( }* K3 Q3 w- B$ d3.4.4 Microwave technology . . . . . . . . 101. {' x7 @/ |& D- W
3.4.5 Microwave-assisted extractions . . 104
9 F5 Z- W7 \% M0 S3.4.6 Pressurised fluid extraction . . . . . 117+ E& `7 i5 \% N ?4 m, u0 ]
3.5 Sorbent extraction . . . . . . . . . . . . . . . . . 123
& X$ ^9 P, N) C# z" H3 @2 M3.5.1 Solid-phase extraction . . . . . . . . . 124/ u5 |6 ^4 l3 I2 u! m% a0 Y- [
3.5.2 Solid-phase microextraction . . . . . 129
' w8 `+ ^- V/ z+ Y# X, |3.5.3 Stir bar sorptive extraction . . . . . 1337 `3 l6 g0 N2 `
3.6 Methodological comparison of extraction; [ z1 d2 p# N. i3 E# j
methods. . . . . . . . . . . . . . . . . . . . . . . . . 134
) b' d' [" t+ D3.6.1 Experimental comparisons . . . . . . 136, x u2 E5 h3 e6 U' k8 Q4 |5 h/ F
3.6.2 Extraction selectivity . . . . . . . . . . 138
. F2 R+ I) Z0 _0 G3.6.3 ‘Nonextractable’ additive analysis 140' B7 W$ ?- u1 d* B' H
3.7 Polymer/additive dissolution methods . . . 146
" a) R: i: A" u3 i3.8 Hydrolysis . . . . . . . . . . . . . . . . . . . . . . . 152
4 f' A# ?; `0 P( d: R3.9 Bibliography . . . . . . . . . . . . . . . . . . . . . 155
# F. i* L( x+ G, `' _3.9.1 Sampling and sample preparation 155
: I% f3 X+ [+ `! T" z8 n3.9.2 Solvents/solubility . . . . . . . . . . . . 1554 ~9 l% n4 P. P* c) G( J4 {3 s( i
3.9.3 Extraction methods . . . . . . . . . . . 156# \3 v; S+ I' ^$ s, D, |# c" e
3.10 References . . . . . . . . . . . . . . . . . . . . . . . 1568 v, m' v$ e: B1 R
vi Contents( ]! V& D6 g; u {+ ^3 N6 \% N
Chapter 4 Separation Techniques . . . . . . 171
0 ~/ p9 \$ g+ i' O* y7 s% A* D4.1 Analytical detectors . . . . . . . . . . . . . . . . 1777 ~7 o% w* s5 D+ n- B
4.2 Gas chromatography . . . . . . . . . . . . . . . 181
# P% `. q( g; W1 K% c: @) ]) Z# C4.2.1 High-temperature gas& u7 Y& _& x9 o( S, N$ V8 E! U
chromatography . . . . . . . . . . . . . 200; r) x9 b; D0 T- H) C
4.2.2 Headspace gas chromatography . . 202
( Y# i9 }0 C. F' f& r4.3 Supercritical fluid chromatography . . . . . 205
! n$ y8 A9 F# [) J& n4.4 Liquid chromatography techniques . . . . . 217 {* Q7 z7 X* j5 j
4.4.1 Planar chromatographies . . . . . . . 218
) M. S' d4 L1 M+ u4.4.2 Column chromatographies . . . . . . 2303 _7 R, f R, F0 ?1 W7 E( a
4.5 Capillary electrophoretic techniques . . . . 273
9 z' q8 r& D& Y9 g! V4.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 278
% [/ J$ ], ~! a2 d& |6 p' r( ]2 m# u4.6.1 General texts . . . . . . . . . . . . . . . 278% {- }2 w8 V7 `$ N* h3 @
4.6.2 Detectors . . . . . . . . . . . . . . . . . . 279
' F* x1 _# H7 p4 f9 T: K( B% M' [4.6.3 Gas chromatography . . . . . . . . . . 279& q- ^9 @/ ?; W) h9 I( ?
4.6.4 Supercritical fluid chromatography 279
2 |; @! H. I2 l; O/ D# F4.6.5 Thin-layer chromatography . . . . . 279
8 \. ~1 @: n2 X2 r3 A# x4.6.6 Liquid chromatography . . . . . . . . 280
+ k" {9 p1 q7 H9 H9 V4.6.7 Size-exclusion chromatography . . 280( j+ X( B- h' ^" F. ^
4.6.8 Ion chromatography . . . . . . . . . . 2808 U* M& k% s5 Y& r* I& o
4.6.9 Capillary electrophoretic& k; [, G" U7 j$ v
techniques . . . . . . . . . . . . . . . . . 280( ]3 Z3 J: ?+ x6 Q& ?
4.7 References . . . . . . . . . . . . . . . . . . . . . . . 281" ]9 [$ M% {8 O% e1 i
Chapter 5 Polymer/Additive Analysis:
9 u( X+ A3 B4 L$ Q7 T# jThe Spectroscopic Alternative 299
( t! J, S( r) F/ o6 w( Y3 k1 a, f' s1 o5.1 Ultraviolet/visible spectrophotometry . . . 302 E& P& H% K$ c$ c
5.2 Infrared spectroscopy . . . . . . . . . . . . . . . 311
1 _& ~9 Y* m9 z6 m$ C& k7 S* i5.3 Luminescence spectroscopy . . . . . . . . . . 318
3 A" m$ ]( F( J* g+ x! D1 f( u8 Z5.4 High-resolution nuclear magnetic) c W1 Y2 e' C5 _, [0 d+ I# F/ o
resonance spectroscopy . . . . . . . . . . . . . 3234 W9 C: l5 _. k6 ~3 M* F( x7 m
5.4.1 Multidimensional NMR
# @6 e7 @8 V/ X- w3 x- Fspectroscopy . . . . . . . . . . . . . . . . 336
9 U; S: }& ]4 \+ _4 n( D8 Q5.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 342
. |, Y! z. l8 G+ `5.5.1 General spectroscopy . . . . . . . . . 342
/ u9 H6 `' Z: T9 O/ ^2 u" F1 Y5.5.2 Ultraviolet/visible
! \7 ~4 q6 y$ P0 j4 [2 Bspectrophotometry . . . . . . . . . . . . 342
z# D' [7 _" L5.5.3 Infrared spectroscopy . . . . . . . . . 342+ @9 O( T! \) q$ \+ B, B! z
5.5.4 Luminescence spectroscopy . . . . . 3428 |& Q# N* I# A W2 K1 {$ J
5.5.5 Nuclear magnetic resonance
' h& V4 a. n1 n" }$ @8 k3 i1 Cspectroscopy . . . . . . . . . . . . . . . . 342; M: p5 l6 l# e# g3 n
5.6 References . . . . . . . . . . . . . . . . . . . . . . . 3425 o5 N3 A' X, @
Chapter 6 Organic Mass-Spectrometric# l& ~+ K, ~6 I
Methods . . . . . . . . . . . . . . . . 349( Z4 {" v7 ]. P$ E5 E. K
6.1 Basic instrumentation . . . . . . . . . . . . . . . 351' ~" G) I# c4 t: ]9 `$ n# U
6.1.1 Inlet systems . . . . . . . . . . . . . . . . 3526 c$ Q8 f" i4 i* e) ~
6.1.2 Modes of detection . . . . . . . . . . . 353$ Y8 D) D1 W3 y" w
6.1.3 Mass resolution . . . . . . . . . . . . . . 354! {; H* H3 w; W( Q6 I8 S
6.1.4 Isotope distributions . . . . . . . . . . 354
$ u" v5 I8 U$ x; D- [) e6.1.5 Accurate mass measurements. . . . 3553 L" y! w2 Y; N; y3 \2 {) H
6.2 Ion sources . . . . . . . . . . . . . . . . . . . . . . 357
0 V! @0 r: C$ L6.2.1 Electron impact ionisation . . . . . . 360" o8 E6 ?3 l! B. ~8 ~; H6 n
6.2.2 Chemical ionisation . . . . . . . . . . . 362) o2 r* y5 J* {# D) m- w: c
6.2.3 Metastable atom bombardment . . 367$ g5 _) d+ y# [$ l( m# `; s( R2 r
6.2.4 Fast atom bombardment . . . . . . . 367
7 }& k& b& u/ ~/ ~0 D- s* X5 [5 X8 m6.2.5 Field ionisation . . . . . . . . . . . . . . 3729 ]; q: L9 g4 ?* k
6.2.6 Field desorption . . . . . . . . . . . . . 374! Z. x* P7 y# m! v, }
6.2.7 Thermospray ionisation . . . . . . . . 376
; H! B- b! {& b$ t$ n) @- v6.2.8 Atmospheric pressure ionisation' Q) J. Z N" i' A3 W
techniques . . . . . . . . . . . . . . . . . 378
7 f( @5 x8 D6 v. D4 H1 W' k' s3 f$ ?6.2.9 Desorption/ionisation methods . . . 3833 ^$ i6 I' Y/ O, \7 I
6.2.10 Photoionisation techniques. . . . . . 385
& v0 g9 Z3 b. Y+ x6.3 Mass analysers . . . . . . . . . . . . . . . . . . . 386
7 N2 Y* y0 I2 S; i3 v6.3.1 Sector analysers . . . . . . . . . . . . . 387: w5 t' {1 E( h- Q/ k. R6 d
6.3.2 Quadrupole mass spectrometers . . 3895 H( S8 D4 f8 e+ \, v
6.3.3 Time-of-flight mass spectrometry . 390( B4 y. A, E. o( O0 d/ Q- h U1 C
6.3.4 Quadrupole ion trap . . . . . . . . . . 393
+ t, A9 U0 E7 n6 ~3 ?) K2 c! z6.3.5 Fourier-transform ion-cyclotron3 k% \! W& F: p% o8 c
resonance mass spectrometry . . . . 395
) C% r+ `' u- O+ v9 J6.3.6 Tandem mass spectrometry . . . . . 398
/ S0 t6 _$ L7 I! A% H6.4 Direct mass-spectrometric polymer
' W2 L7 e/ o: ?2 ~( lcompound analysis . . . . . . . . . . . . . . . . . 407
6 z+ v( C0 z& {. I" ]+ Z1 R6.5 Ion mobility spectrometry . . . . . . . . . . . 4155 d) H0 K, z R9 S
6.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 417
5 s! U- g0 h) p. q( R6.6.1 Mass spectrometry (General) . . . . 417
1 M# h2 X) f' @. v' g& C. N! s6.6.2 Mass spectrometers . . . . . . . . . . . 417
7 T' E0 ]2 G& Q" ^6.6.3 Ionisation modes . . . . . . . . . . . . . 4170 s3 V- o' W" B* \" ?% X# p8 i
6.7 References . . . . . . . . . . . . . . . . . . . . . . . 418% a4 S3 ]* e, ^2 C6 s; }
Chapter 7 Multihyphenation and1 o2 [" U# f9 w) }( g0 W L3 {
Multidimensionality in w' A* p5 K% q
Polymer/Additive Analysis . . . 425+ P8 j! @6 G6 V9 T. }' E( _! Z
7.1 Precolumn hyphenation . . . . . . . . . . . . . 428) T; \6 C6 h9 R: V& m3 i
7.1.1 Chromatographic sampling; z9 t( c- t s" z( Q
methods . . . . . . . . . . . . . . . . . . . 432/ R2 L% `9 p) i: ]; x0 c
7.2 Coupled sample$ E8 b& x+ e+ P/ Z! H6 d& n
preparation – spectroscopy/spectrometry . 449
4 \% X [. T" E2 Z* p7.3 Postcolumn hyphenation . . . . . . . . . . . . . 452
, ?! m, \" c, R0 E/ ?* [) K- w7.3.1 (Multi)hyphenated GC techniques 456 K& @* `, @# }% J- |/ _. A
7.3.2 (Multi)hyphenated SFC
! J. _/ d) t$ m8 {% x( H* V6 Atechniques . . . . . . . . . . . . . . . . . 475, k5 z9 ?4 I" ^
7.3.3 (Multi)hyphenated HPLC6 }9 C! T, s( G9 Q& @# h) A
techniques . . . . . . . . . . . . . . . . . 489' \, e/ B5 j6 w: k. V+ S
7.3.4 Hyphenated SEC techniques . . . . 527$ |3 E/ Y# X) ^0 X( z' |* u
7.3.5 Hyphenated TLC techniques . . . . 530
9 C) F5 g! i; K$ E, Q- ^6 }7.3.6 Hyphenated CE techniques . . . . . 543
/ c+ S6 Y7 k/ |( X) W# a. |4 yContents vii
0 a8 f, i6 @) P( k$ x1 t5 z7.4 Multidimensional chromatography . . . . . 545
5 c0 i: \8 E* n7.4.1 Multidimensional gas
: S9 N& W/ Q$ X1 n+ qchromatography . . . . . . . . . . . . . 548
. W" U7 l5 x2 X/ T% y& t4 A2 l7.4.2 Multidimensional supercritical. C0 q: E* R9 w/ R& K
fluid chromatography . . . . . . . . . 550
1 m- i' B2 b# t7 Q) s5 g9 w7.4.3 Multidimensional liquid5 ~4 q& F8 j8 H, Z3 z
chromatography . . . . . . . . . . . . . 550$ r( @( F# w4 y6 t
7.4.4 Multidimensional thin-layer
6 J; |, F( p! `" o- k& Qchromatography . . . . . . . . . . . . . 558
4 d9 F+ M, ]+ g3 ?7.5 Multidimensional spectroscopy . . . . . . . . 5601 y+ p# B/ B# O% h7 g" x
7.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 562' k; B N: Z, |6 V. f# P2 H3 Q% k [, x5 Z
7.6.1 General . . . . . . . . . . . . . . . . . . . 562
" @: I0 U* W$ E r; Y- y7.6.2 Multihyphenation and) |0 Z2 `/ V2 C3 o. \/ G# c. i% S
multidimensionality . . . . . . . . . . . 563' T' e: ^) B+ b
7.6.3 Precolumn hyphenation . . . . . . . . 5635 Q5 J W2 f; _2 Y
7.6.4 Postcolumn hyphenation . . . . . . . 563& `& \2 h. p" e" N! |; e
7.6.5 Multidimensional chromatography 563
- y- X* W( N5 u3 P& y! j' s7.6.6 Multidimensional spectroscopy . . 5631 m" x+ x( z% p% u
7.7 References 564- A Q6 L6 l5 }4 G4 q& }! k
Chapter 8 Inorganic and Element7 ^) h) [8 |& }0 W6 [# I
Analytical Methods . . . . . . . . 585
8 ~, c; K+ j7 F2 k8.1 Element analytical protocols . . . . . . . . . . 587
/ z, h, e% k7 T t8.1.1 Element analytical pretreatment
8 _2 h* L8 c0 D! O" ] yprotocols . . . . . . . . . . . . . . . . . . 5888 t# E7 s2 P" N# S" ~! Q
8.1.2 Elemental analysis methods . . . . . 589& h: e X- p/ Z
8.2 Sample destruction for classical elemental! @0 J' d$ p+ \' g: T+ g
analysis . . . . . . . . . . . . . . . . . . . . . . . . . 591
8 F' B* ^7 A* A+ a2 F& }8.2.1 Combustion analysis . . . . . . . . . . 593
% b" a' p2 D( f$ y8.2.2 Wet matrix digestion . . . . . . . . . . 5974 u: d5 G8 j0 h. ?
8.2.3 Fusion methods . . . . . . . . . . . . . . 604
$ g8 u( l9 s5 _' V' r8.3 Analytical atomic spectrometry . . . . . . . . 6052 g" U6 U. x$ k/ s: c, x
8.3.1 Atomic absorption spectrometry . 608% l1 u+ b$ R: x' q% t$ T% {
8.3.2 Atomic emission spectrometry . . . 613
4 `% T4 }, M7 b) l/ ]8.3.3 Atomic fluorescence spectrometry 624 |
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