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Acknowledgements. . . . . . . . . . . . . . . . xv8 O+ \5 n9 |) u7 z6 M
Chapter 1 Introduction . . . . . . . . . . . . . . 1
, u) a' a$ d7 W! N d5 q6 H) q1.1 Additives . . . . . . . . . . . . . . . . . . . . . . . . 2' p; B! B: _: a! K# q, Y9 b! j
1.1.1 Additive functionality . . . . . . . . . 3: B# @ u5 S) J Q- }' K/ f# a
1.2 Plastics formulations . . . . . . . . . . . . . . . 5! P v8 d) B9 x- a
1.2.1 Supply forms . . . . . . . . . . . . . . . 7
( ]# N2 w$ y* x0 a- V- a! k% X1.2.2 Additive delivery . . . . . . . . . . . . 9
' j6 }+ O4 O+ E% b% o1.3 Economic impact of polymer additives . . 95 b8 M, U- R2 k
1.4 Analysis of plastics . . . . . . . . . . . . . . . . 11/ d9 S. m5 `. K# t0 e0 r/ B
1.4.1 Regulations and standardisation . . 150 M2 L2 |' r Q4 N- d
1.4.2 Prior art . . . . . . . . . . . . . . . . . . . 17
: X s) p1 k* j4 {1.4.3 Databases . . . . . . . . . . . . . . . . . . 19
9 B& K# T) U$ T) m1.4.4 Scope . . . . . . . . . . . . . . . . . . . . . 207 L: @2 ~5 h/ h$ |0 S
1.4.5 Chapter overview . . . . . . . . . . . . 22
" Q% Q# m" @. i0 f, d- W- L# m1.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 23
- N" W$ a5 s9 p, Q1.5.1 Plastics additives . . . . . . . . . . . . . 23/ N/ F: O$ @! \ E) y( L
1.5.2 Processing technologies . . . . . . . . 23
* Z& _# d+ |8 u9 J( ]3 X1.5.3 Instrumental analysis . . . . . . . . . . 23+ O+ s$ p' d$ L. m
1.5.4 Polymer analysis . . . . . . . . . . . . . 24
* U$ c* S' b% J9 b3 }% |1.5.5 Polymer/additive analysis . . . . . . 244 C/ o! ]& q* s' E
1.6 References . . . . . . . . . . . . . . . . . . . . . . . 24
b8 C8 Z: e1 T ?8 yChapter 2 Deformulation Principles . . . . 29( D' F' Z. |+ C5 Q7 L
2.1 Polymer identification . . . . . . . . . . . . . . 301 E- \8 P% T* f& A3 ]& L
2.2 Additive analysis of rubbers: ‘Best. B9 v4 l+ c3 a! z
Practice’ . . . . . . . . . . . . . . . . . . . . . . . . 32
# }9 n `7 v7 \6 @! A2.3 Polymer extract analysis . . . . . . . . . . . . . 42
( l; {! @/ Y7 m; j7 l$ d6 ?2.4 In situ polymer/additive analysis . . . . . . 46/ p4 O3 j% r2 \# {4 p
2.5 Class-specific polymer/additive analysis . 477 j) Q, A) W# d3 T* }0 s
2.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 481 |' K% i: A8 i) \# h
2.6.1 Polymer identification . . . . . . . . . 48
; K/ M, S/ a& B% `. G2.6.2 Deformulation of rubbers . . . . . . 48
5 `. A- x( _' V2.6.3 Deformulation of polymers . . . . . 486 K# d9 J }" A F% B
2.7 References . . . . . . . . . . . . . . . . . . . . . . . 48
$ U5 u8 c$ T; s* n! q" U) AChapter 3 Sample Preparation. d s, M/ E5 C, Z/ H
Perspectives . . . . . . . . . . . . . . 51' e E8 X' O' p
3.1 Solvents . . . . . . . . . . . . . . . . . . . . . . . . 547 E$ z) h+ i1 d: ?2 H7 L6 F
3.1.1 Polymer solubility criteria . . . . . . 550 s7 |: w+ j$ m, T, S( G/ i
3.1.2 Solubility parameters . . . . . . . . . . 552 m# V% n- R$ h( T4 f# l" H
3.1.3 Polymer solutions . . . . . . . . . . . . 56
: A' {, x/ ?/ O/ P9 h, u3.2 Extraction strategy . . . . . . . . . . . . . . . . . 57
8 j0 y0 ^: `# R" P( B# u3.3 Conventional extraction technologies . . . 59
( I9 p( a f2 }& q; q8 o4 ]% r3.3.1 Liquid–liquid extraction . . . . . . . 607 w9 H3 E+ Z4 R# s' f
3.3.2 Liquid–solid extraction . . . . . . . . 60
& f V( V5 T( m! k( g" Z7 q' [9 h3.3.3 Classical solvent extractions of; v m$ O! h. a( c
additives from polymers . . . . . . . 61
/ r3 I! i% f9 o1 A3.3.4 Sonication . . . . . . . . . . . . . . . . . 75
& `9 e) |3 M0 S! \, ~ J0 Y+ w2 ]- X3.4 High-pressure solvent extraction methods 81
! h, h1 E! B& o5 U! f: H3.4.1 Supercritical fluid technology . . . 813 H& J3 K4 K1 g8 j
3.4.2 Analytical SFE . . . . . . . . . . . . . . 85
9 ~* p4 I; Q" u% l, o; y3.4.3 Subcritical water extraction . . . . . 100
' L, l. T( T4 s, s" F. c/ `3.4.4 Microwave technology . . . . . . . . 101+ `; a. X' N* N
3.4.5 Microwave-assisted extractions . . 104' n# K8 M7 K( Q, ?! n# w7 Y
3.4.6 Pressurised fluid extraction . . . . . 117 ^* ^3 q4 f3 Q
3.5 Sorbent extraction . . . . . . . . . . . . . . . . . 123; \7 N* `$ A# d7 O- R( }
3.5.1 Solid-phase extraction . . . . . . . . . 124
; R4 @! \* t+ C1 m" P5 a2 x9 y: w6 e/ g- Z3.5.2 Solid-phase microextraction . . . . . 129/ f; v, R1 f8 {& H
3.5.3 Stir bar sorptive extraction . . . . . 1330 @5 h/ {8 D9 c) f5 o
3.6 Methodological comparison of extraction
# V, K, Q! I- O5 Tmethods. . . . . . . . . . . . . . . . . . . . . . . . . 134
" k. E" |0 _! t. ~2 o; U$ O3.6.1 Experimental comparisons . . . . . . 136
; W5 l9 H/ F3 d3.6.2 Extraction selectivity . . . . . . . . . . 138" k8 }/ v% U1 \
3.6.3 ‘Nonextractable’ additive analysis 140
$ j: Y& ~( u9 A" i; w( k3.7 Polymer/additive dissolution methods . . . 146
% Q P/ Z1 x" c5 g* b8 B3.8 Hydrolysis . . . . . . . . . . . . . . . . . . . . . . . 152
+ R" \0 g2 s \4 `$ b3.9 Bibliography . . . . . . . . . . . . . . . . . . . . . 155
; `1 h+ s) E8 b0 |# t4 v: t3.9.1 Sampling and sample preparation 155) X, `8 p; f# Q( j* c
3.9.2 Solvents/solubility . . . . . . . . . . . . 1558 l8 Q, f; p0 P; i
3.9.3 Extraction methods . . . . . . . . . . . 156# O$ M$ I5 \* }1 Q$ [1 n% ]
3.10 References . . . . . . . . . . . . . . . . . . . . . . . 1561 B: q0 q- Q: C. F8 X0 o- r! E
vi Contents
/ {' W+ m, D$ s3 r9 Y% ?! UChapter 4 Separation Techniques . . . . . . 171
0 u2 w4 {' Q; y" j2 z/ j4.1 Analytical detectors . . . . . . . . . . . . . . . . 177% {* x( J9 L/ d; [% t x m
4.2 Gas chromatography . . . . . . . . . . . . . . . 181
0 [( e; ?/ O% }# E1 O4.2.1 High-temperature gas
! I( y) L" J: w" V" Y% Mchromatography . . . . . . . . . . . . . 200
- e/ S1 l) [5 G5 l. @4.2.2 Headspace gas chromatography . . 2028 \$ N) ?8 w/ U( \0 t, j
4.3 Supercritical fluid chromatography . . . . . 205
! V9 M& b8 y) E9 K. Q+ I4.4 Liquid chromatography techniques . . . . . 217
8 y9 R2 L: X/ c4.4.1 Planar chromatographies . . . . . . . 218
- k$ h% x# W1 k" a4.4.2 Column chromatographies . . . . . . 230
+ b. ?5 d" {" @- M! u. ?/ d1 ?1 \4.5 Capillary electrophoretic techniques . . . . 273
& x$ Q! u, _9 T# g! X4.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 278
, F* S1 J! P# Y1 Y4.6.1 General texts . . . . . . . . . . . . . . . 278
' {& p& ` L r3 d4.6.2 Detectors . . . . . . . . . . . . . . . . . . 279
@$ G% r, o2 n1 U) N/ P- H4.6.3 Gas chromatography . . . . . . . . . . 279! O. s3 F5 n0 V) L6 c( |. G
4.6.4 Supercritical fluid chromatography 279) N, D6 S2 _7 O1 w. A
4.6.5 Thin-layer chromatography . . . . . 279
5 @. {+ V# T& B. C A) C4.6.6 Liquid chromatography . . . . . . . . 280- l' Q+ `- ` i2 D: H' |
4.6.7 Size-exclusion chromatography . . 280
& q9 Z Y: T; Y8 x: D4.6.8 Ion chromatography . . . . . . . . . . 280: X& R; P/ p K; Q2 O+ Y S% x
4.6.9 Capillary electrophoretic
1 x. h5 Z+ o# G T2 w7 U, V$ Utechniques . . . . . . . . . . . . . . . . . 280, e8 Q4 d, I3 r: b5 \- O6 U( z; z2 m9 f
4.7 References . . . . . . . . . . . . . . . . . . . . . . . 281
, {/ S; ]+ {. D, Q$ s# T/ f; kChapter 5 Polymer/Additive Analysis:
: ~, C% T9 K: P1 ^The Spectroscopic Alternative 299. a# U1 k/ S# }
5.1 Ultraviolet/visible spectrophotometry . . . 302
1 C) U {3 n7 L# C4 N; n( s5.2 Infrared spectroscopy . . . . . . . . . . . . . . . 311
9 i b- g6 f) Y+ J8 L, l5.3 Luminescence spectroscopy . . . . . . . . . . 3188 v- T6 w+ s( h2 a$ x2 Y$ R* I. b9 @
5.4 High-resolution nuclear magnetic; B$ a- [' v; ~+ R8 L9 D U
resonance spectroscopy . . . . . . . . . . . . . 3231 B6 u# D# T4 V
5.4.1 Multidimensional NMR
0 H0 W2 k8 b: O: Q, P2 h3 m, ?spectroscopy . . . . . . . . . . . . . . . . 336
6 r F9 c9 ?* b, }% Q' g! `) E5.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 342$ c! s9 Y' n8 z# Y
5.5.1 General spectroscopy . . . . . . . . . 342
: O7 S* X x5 B }5.5.2 Ultraviolet/visible1 M; ^2 I$ c, y5 h1 I
spectrophotometry . . . . . . . . . . . . 3423 G6 R, I/ p1 x! i% W, ^3 o
5.5.3 Infrared spectroscopy . . . . . . . . . 342+ C+ U# y" o/ u1 K: m
5.5.4 Luminescence spectroscopy . . . . . 342
: X" n# X( q9 ^3 s% C, L5.5.5 Nuclear magnetic resonance( i; N2 F4 N% `. ~4 o0 l: O" I$ w% @
spectroscopy . . . . . . . . . . . . . . . . 3429 u$ I0 b, x- o/ W9 E
5.6 References . . . . . . . . . . . . . . . . . . . . . . . 342! c0 v$ p+ S7 w! L
Chapter 6 Organic Mass-Spectrometric2 ], v( Q* v4 m7 a
Methods . . . . . . . . . . . . . . . . 349; a% z9 M- i, y5 q7 M5 ]8 A
6.1 Basic instrumentation . . . . . . . . . . . . . . . 351
) t- ], m; x. |, O6.1.1 Inlet systems . . . . . . . . . . . . . . . . 352* S1 L: Y: \4 b! M& Y4 x
6.1.2 Modes of detection . . . . . . . . . . . 353- s7 b4 F ?; D: S
6.1.3 Mass resolution . . . . . . . . . . . . . . 354
0 a* ?. B; A# h: ?4 q1 r. j' M& \6.1.4 Isotope distributions . . . . . . . . . . 354: _% q5 J+ D2 s( k( m2 s
6.1.5 Accurate mass measurements. . . . 355
+ }) ]/ j4 n$ z, b& f1 b6.2 Ion sources . . . . . . . . . . . . . . . . . . . . . . 357( ]7 x% E" f! r7 A
6.2.1 Electron impact ionisation . . . . . . 360
, l* q/ q D9 U$ k- |6.2.2 Chemical ionisation . . . . . . . . . . . 362* E9 ^3 d, Y+ U# g( L+ e/ ^
6.2.3 Metastable atom bombardment . . 367
7 U! K% A) J3 r4 d" |% n' K6.2.4 Fast atom bombardment . . . . . . . 367( l' `7 X# i! _, s% \% B
6.2.5 Field ionisation . . . . . . . . . . . . . . 372 c" Q' l& a! k( k: x; q- I6 m2 F! j& e
6.2.6 Field desorption . . . . . . . . . . . . . 374" r# ^# |. x+ F# T" S9 Q
6.2.7 Thermospray ionisation . . . . . . . . 3769 | i t. C% O% [) f
6.2.8 Atmospheric pressure ionisation
! E/ k; p. \6 W0 D+ k: B) P6 B2 Ytechniques . . . . . . . . . . . . . . . . . 378
; s- W, Z, C2 @2 Q7 o0 M6.2.9 Desorption/ionisation methods . . . 383, `7 d2 C& u2 G1 e
6.2.10 Photoionisation techniques. . . . . . 385
+ g- r: Y( h" b6.3 Mass analysers . . . . . . . . . . . . . . . . . . . 386& x# ~& w' q9 N- _# p
6.3.1 Sector analysers . . . . . . . . . . . . . 387" F2 c* E: Y I F: D* w- Z `
6.3.2 Quadrupole mass spectrometers . . 389
. k! F, \& X: |2 O; J6 P9 u6.3.3 Time-of-flight mass spectrometry . 390" o& x; P+ X2 `; P) u5 ]3 X0 g
6.3.4 Quadrupole ion trap . . . . . . . . . . 393
: t1 a$ y/ }( `/ x6.3.5 Fourier-transform ion-cyclotron0 c. F1 E+ T W
resonance mass spectrometry . . . . 395
2 q" s2 ~. Y% n6.3.6 Tandem mass spectrometry . . . . . 398
/ o* P V2 i8 t. V2 o6.4 Direct mass-spectrometric polymer: A, V! X7 B* N) r
compound analysis . . . . . . . . . . . . . . . . . 407
& j: u3 [% ]" W. C, f/ w& p) l$ ~6.5 Ion mobility spectrometry . . . . . . . . . . . 415
/ N+ \& D) \+ z: v% P; W6.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 417/ ` I v8 ^" r4 Q4 d$ D
6.6.1 Mass spectrometry (General) . . . . 417% M7 l5 \, X/ y8 g4 T O' H
6.6.2 Mass spectrometers . . . . . . . . . . . 417. b! [" `+ h. R) y. m3 [' }
6.6.3 Ionisation modes . . . . . . . . . . . . . 417
f4 c) A0 }+ l( ?8 [0 Q, T# M- V1 t6.7 References . . . . . . . . . . . . . . . . . . . . . . . 418
) T& y2 m, a$ } Q) C# F6 eChapter 7 Multihyphenation and
N4 g8 |- D6 tMultidimensionality in
# u. t1 K; a1 Y+ A% U+ u5 YPolymer/Additive Analysis . . . 425
& {( l7 }, g/ T# {7.1 Precolumn hyphenation . . . . . . . . . . . . . 428
, x( g" R8 S1 O h+ r2 R. y7.1.1 Chromatographic sampling4 [ Q3 J6 P% e; c- x
methods . . . . . . . . . . . . . . . . . . . 432
, V5 e0 m* n, \( M4 G( _/ b7.2 Coupled sample- l+ Y4 A3 r$ \3 d
preparation – spectroscopy/spectrometry . 449
* m" T* R& P9 {2 n) D7.3 Postcolumn hyphenation . . . . . . . . . . . . . 4525 Z0 Z( C3 ?2 [- t- k3 o5 D) c; ]1 F
7.3.1 (Multi)hyphenated GC techniques 456
' a9 [0 _" G" H5 b* v( M0 W7.3.2 (Multi)hyphenated SFC- E- W' e' Y* J( z& {+ \8 {
techniques . . . . . . . . . . . . . . . . . 475) e+ i) A# }( ^* O3 Q# k
7.3.3 (Multi)hyphenated HPLC
' ]+ \5 K' Y" w8 b/ stechniques . . . . . . . . . . . . . . . . . 489' U5 ^7 e* B0 W8 U3 y! E& ~
7.3.4 Hyphenated SEC techniques . . . . 527
1 ?! [- N/ n3 m8 E6 A) |7.3.5 Hyphenated TLC techniques . . . . 530
4 E8 M# Z7 t1 n; @6 F7.3.6 Hyphenated CE techniques . . . . . 543
2 O7 q. D9 Q, b8 O& OContents vii
2 [' | I1 ^% L, T7 S; z7.4 Multidimensional chromatography . . . . . 545
3 @9 s9 G$ }4 X3 ^7.4.1 Multidimensional gas* v+ M7 L, A/ a: N* s, O: v
chromatography . . . . . . . . . . . . . 548
0 g" B; M4 \% n! ?! J8 o9 `9 D1 b6 N: G. K7.4.2 Multidimensional supercritical% V0 `7 d0 I4 L- Y1 v
fluid chromatography . . . . . . . . . 5505 u' u; e8 U1 t* i# a+ _4 N9 a; z
7.4.3 Multidimensional liquid( o3 X1 n7 l9 W# S: f( n" L% C
chromatography . . . . . . . . . . . . . 550
]8 P6 h M3 r7.4.4 Multidimensional thin-layer
" B- B) E9 X( } K/ uchromatography . . . . . . . . . . . . . 558
5 x, K4 N) h: d: J, p7 t7.5 Multidimensional spectroscopy . . . . . . . . 560. t5 x# C* ?$ r0 z* k3 U% @+ ~
7.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 562
1 ~3 Y( v+ n4 |% C" D- g9 J7.6.1 General . . . . . . . . . . . . . . . . . . . 562+ B- F, d: c5 O5 f! t
7.6.2 Multihyphenation and
! [2 X9 u+ r0 Q9 O; k/ Gmultidimensionality . . . . . . . . . . . 563' S% g7 M# t" `* ?+ v. H0 F
7.6.3 Precolumn hyphenation . . . . . . . . 563
" M$ `3 E: H. t+ Q4 A* J( S7.6.4 Postcolumn hyphenation . . . . . . . 563
8 [+ P7 I7 B# c7.6.5 Multidimensional chromatography 563
7 e8 }) y' g% P* e$ `% h7.6.6 Multidimensional spectroscopy . . 5634 x3 D8 W+ w1 B% n0 q4 ~: F
7.7 References 564
6 p' {& ?3 p+ B6 P5 v* ~9 RChapter 8 Inorganic and Element
4 e7 Y) E( s1 ]% uAnalytical Methods . . . . . . . . 585
6 W: N `1 }. ~5 F8.1 Element analytical protocols . . . . . . . . . . 587
) D1 f2 \( B4 x+ Q4 D& S8.1.1 Element analytical pretreatment/ K$ C9 N1 L+ k4 ^3 D: ^, ]
protocols . . . . . . . . . . . . . . . . . . 588
8 H( l' [, r: M% {( H8.1.2 Elemental analysis methods . . . . . 589 ]; g$ f1 C! n2 [0 p
8.2 Sample destruction for classical elemental
" W5 j6 L$ o# p: n/ C. Manalysis . . . . . . . . . . . . . . . . . . . . . . . . . 5915 ~7 x; X) _5 }$ u9 s# u4 S8 y
8.2.1 Combustion analysis . . . . . . . . . . 593
2 q8 h, J) E) x- \0 ^8.2.2 Wet matrix digestion . . . . . . . . . . 597
. w6 j3 ?+ u9 _ ~; M8.2.3 Fusion methods . . . . . . . . . . . . . . 604) V7 A$ k* d5 K
8.3 Analytical atomic spectrometry . . . . . . . . 6052 f* T) |3 N; q" ?8 {- p
8.3.1 Atomic absorption spectrometry . 608
) k2 G' P7 z0 l7 u! t8.3.2 Atomic emission spectrometry . . . 613
& y8 I. p, A9 c3 ^ ]4 t/ X8.3.3 Atomic fluorescence spectrometry 624 |
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