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Acknowledgements. . . . . . . . . . . . . . . . xv+ N& G1 z$ L* B1 p- I
Chapter 1 Introduction . . . . . . . . . . . . . . 1
. E( _& @7 V5 [1.1 Additives . . . . . . . . . . . . . . . . . . . . . . . . 23 m- z: U) i$ M* W6 s, x% H
1.1.1 Additive functionality . . . . . . . . . 3
& r2 ]; D2 f5 o9 @5 N8 K1.2 Plastics formulations . . . . . . . . . . . . . . . 5
: j# e* c" L' |* d) _6 Q+ F+ U1.2.1 Supply forms . . . . . . . . . . . . . . . 7
& ] X& b9 f7 r: P/ [' g8 Q1.2.2 Additive delivery . . . . . . . . . . . . 9
. l0 ^& x. I* G3 l- q1.3 Economic impact of polymer additives . . 9
0 a B2 F2 n. {, m1.4 Analysis of plastics . . . . . . . . . . . . . . . . 11
5 ^( o8 @# A' x6 w2 [1 B! G1.4.1 Regulations and standardisation . . 15
; e7 W. M1 b) i6 D0 y- H1.4.2 Prior art . . . . . . . . . . . . . . . . . . . 17
5 ~5 c5 F& d" t1 L# ]1.4.3 Databases . . . . . . . . . . . . . . . . . . 195 W Q- Z3 l: e% q5 N8 B& X
1.4.4 Scope . . . . . . . . . . . . . . . . . . . . . 20
0 Z+ B) ?: E/ ^% A6 N1.4.5 Chapter overview . . . . . . . . . . . . 22
9 ?6 |6 @; g6 }- _: e. B! J8 x1.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 23. x& j. J% t c
1.5.1 Plastics additives . . . . . . . . . . . . . 23
7 C1 G- F4 Z! P% M A5 f/ |1.5.2 Processing technologies . . . . . . . . 23
6 |+ r/ z* V- d K3 ]1.5.3 Instrumental analysis . . . . . . . . . . 234 @! N( Q) K, F! O$ e6 S
1.5.4 Polymer analysis . . . . . . . . . . . . . 24$ G) ?% O# D j# Y, [+ m! b
1.5.5 Polymer/additive analysis . . . . . . 24' D/ u$ t- C! ?9 G
1.6 References . . . . . . . . . . . . . . . . . . . . . . . 247 F1 z* g# `, c! [$ j
Chapter 2 Deformulation Principles . . . . 29
, n g# ]0 K; k$ t$ ], x2.1 Polymer identification . . . . . . . . . . . . . . 30+ [1 j# s: C0 p" c; L1 r
2.2 Additive analysis of rubbers: ‘Best
, S( z9 L) f: M3 D- A' B; mPractice’ . . . . . . . . . . . . . . . . . . . . . . . . 32
$ I' u$ \& I, q$ J2.3 Polymer extract analysis . . . . . . . . . . . . . 42
5 J1 {* H* z9 m2 c& f, V2.4 In situ polymer/additive analysis . . . . . . 469 z6 h8 B2 w/ t2 N& _3 Y
2.5 Class-specific polymer/additive analysis . 47& C, W5 _! J# F7 T) d
2.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 48
) V6 c- z4 r$ t Z% G! ], I2 Y0 p2.6.1 Polymer identification . . . . . . . . . 488 e6 R. P" v, Y. `9 A: t$ Y V
2.6.2 Deformulation of rubbers . . . . . . 48
$ s2 v2 W: Q( Y/ b! ?5 }2.6.3 Deformulation of polymers . . . . . 48% e) {8 ^4 R6 N2 `! E( c* R" C
2.7 References . . . . . . . . . . . . . . . . . . . . . . . 48
$ e" N( R: A F b$ CChapter 3 Sample Preparation
! d m% D& t: M. xPerspectives . . . . . . . . . . . . . . 514 [1 G9 \$ }) `/ B. h* i6 ^5 ~: g
3.1 Solvents . . . . . . . . . . . . . . . . . . . . . . . . 54
* n9 Z4 ]. Q v; n3 \3.1.1 Polymer solubility criteria . . . . . . 551 N6 y6 K5 L7 ^4 |
3.1.2 Solubility parameters . . . . . . . . . . 55
5 k# j! f! D) R% i0 j C3.1.3 Polymer solutions . . . . . . . . . . . . 56
3 B+ V/ c- p# r! D+ ^: u3.2 Extraction strategy . . . . . . . . . . . . . . . . . 57
$ ^$ I0 C5 W" e# x+ b. A! s) f3.3 Conventional extraction technologies . . . 59
" ?( w! y4 V+ e4 Z5 B4 C3.3.1 Liquid–liquid extraction . . . . . . . 600 f7 q4 z) q; L Q
3.3.2 Liquid–solid extraction . . . . . . . . 604 @$ b- m5 v8 y; f) K! i
3.3.3 Classical solvent extractions of
" T3 K# e( H/ e" b8 \( q! }: n3 v8 dadditives from polymers . . . . . . . 615 p ], K4 [& D/ D& g
3.3.4 Sonication . . . . . . . . . . . . . . . . . 75. R0 W1 j0 G1 o1 k# C. A2 H, E
3.4 High-pressure solvent extraction methods 81# x, J( E8 b/ D" A2 T
3.4.1 Supercritical fluid technology . . . 81
5 _* B) X/ B) t3 j5 ^, q3.4.2 Analytical SFE . . . . . . . . . . . . . . 85: ?& [$ T ~6 k& H4 l7 i: [
3.4.3 Subcritical water extraction . . . . . 100
; V0 P* U' Q5 n* z$ I; T9 G3.4.4 Microwave technology . . . . . . . . 101
3 s' c* v( C6 s8 M4 c1 r3.4.5 Microwave-assisted extractions . . 1045 C/ d. T5 a& o @% `- T
3.4.6 Pressurised fluid extraction . . . . . 117
0 B1 w' L$ ^7 m$ F$ O3.5 Sorbent extraction . . . . . . . . . . . . . . . . . 123; e7 S2 |: e" X( l
3.5.1 Solid-phase extraction . . . . . . . . . 124
" v) c# A0 G5 o% R3.5.2 Solid-phase microextraction . . . . . 129/ h& q3 @. K6 W. y% a& w
3.5.3 Stir bar sorptive extraction . . . . . 133" I; E/ i/ W: Y6 h, M' T9 e
3.6 Methodological comparison of extraction
5 X$ Y+ L3 t' z* g \/ Emethods. . . . . . . . . . . . . . . . . . . . . . . . . 134
+ l7 A, b" U5 F4 R3.6.1 Experimental comparisons . . . . . . 136
_$ g1 e) I& e, L% t5 M3.6.2 Extraction selectivity . . . . . . . . . . 1385 h* m! g; p0 t
3.6.3 ‘Nonextractable’ additive analysis 1403 R4 V* A3 w( r7 w X$ U
3.7 Polymer/additive dissolution methods . . . 146
' x% _9 R8 }* {3 }5 {1 T3.8 Hydrolysis . . . . . . . . . . . . . . . . . . . . . . . 152' C/ c" F% u+ j- N
3.9 Bibliography . . . . . . . . . . . . . . . . . . . . . 155
" I1 r3 Y; S- O8 f+ G" S( N. c1 {3.9.1 Sampling and sample preparation 155$ R6 w+ V/ i8 [$ o: J; W/ p& ]
3.9.2 Solvents/solubility . . . . . . . . . . . . 155
3 @; P! u$ J, g! a2 e3.9.3 Extraction methods . . . . . . . . . . . 1560 k+ w, V( v4 B0 J2 u
3.10 References . . . . . . . . . . . . . . . . . . . . . . . 156( _$ q2 S9 t& k
vi Contents7 e) C% ^) V! v& }7 J/ T
Chapter 4 Separation Techniques . . . . . . 1712 s/ `( l+ _2 h0 r) N" [
4.1 Analytical detectors . . . . . . . . . . . . . . . . 177" r5 I* x1 G: q' j$ G
4.2 Gas chromatography . . . . . . . . . . . . . . . 181
, E8 ^1 U+ d6 W2 m5 ]4.2.1 High-temperature gas6 a* y, E3 e+ C; X' \! f
chromatography . . . . . . . . . . . . . 200- Q% T9 O6 L0 s( {$ A/ I
4.2.2 Headspace gas chromatography . . 202
/ q2 J" _4 C2 q4.3 Supercritical fluid chromatography . . . . . 205
n+ \+ i. ]% @9 Q: r1 s. U& A& C+ u4.4 Liquid chromatography techniques . . . . . 217# K- m0 A7 ]+ O) h9 Z% Q
4.4.1 Planar chromatographies . . . . . . . 2187 O7 {6 j% t4 ]7 R" n
4.4.2 Column chromatographies . . . . . . 230+ a; u: X% H5 a% K
4.5 Capillary electrophoretic techniques . . . . 273
6 H9 m& d) W/ d! ~+ l4.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 2781 E1 q% Z0 l' V5 L# x/ }
4.6.1 General texts . . . . . . . . . . . . . . . 278, \: f/ z3 h3 A! O' _6 r
4.6.2 Detectors . . . . . . . . . . . . . . . . . . 2790 t# y9 k% g9 q# C$ ~/ ?; W& \
4.6.3 Gas chromatography . . . . . . . . . . 279 O- p b7 g+ z/ n; P$ ~0 i
4.6.4 Supercritical fluid chromatography 2798 M, N' w; [$ Q
4.6.5 Thin-layer chromatography . . . . . 279' s# e2 U: i( ~
4.6.6 Liquid chromatography . . . . . . . . 280% q8 w! V1 ?5 V; Z! P/ C
4.6.7 Size-exclusion chromatography . . 280
* }" y' ~9 H. s8 m" I8 A4 [4 v7 ~+ Y4.6.8 Ion chromatography . . . . . . . . . . 280& A6 N/ }' P7 @
4.6.9 Capillary electrophoretic
, Z% H6 k, I" W0 p- W) dtechniques . . . . . . . . . . . . . . . . . 280
" M) z2 b/ m7 Q4 Q4.7 References . . . . . . . . . . . . . . . . . . . . . . . 281
# n: J3 X j1 k$ R( }+ J6 }Chapter 5 Polymer/Additive Analysis:
[3 @6 i' h0 }, }. [- |' z) tThe Spectroscopic Alternative 299* e6 H+ u4 Z" `" q
5.1 Ultraviolet/visible spectrophotometry . . . 302
7 t9 p7 U9 W; U( H9 y) Q$ D5.2 Infrared spectroscopy . . . . . . . . . . . . . . . 311
: I4 v8 b9 E3 y4 H5.3 Luminescence spectroscopy . . . . . . . . . . 318
4 b3 {" Y9 Z {+ f8 A2 H2 i! [5.4 High-resolution nuclear magnetic
* Y" W6 u5 j. f" b" @resonance spectroscopy . . . . . . . . . . . . . 323
s) N d1 y3 o4 T' r5.4.1 Multidimensional NMR0 r, L5 {3 ] n' H) u7 K
spectroscopy . . . . . . . . . . . . . . . . 336
9 N( Q8 R7 h& B5.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 342
9 A8 Z* t- l) ]& m5 [0 [$ G! v# }! {# p- l5.5.1 General spectroscopy . . . . . . . . . 342
: f0 y, d$ ]0 P, x6 P2 v5.5.2 Ultraviolet/visible. f6 f/ R+ r# p
spectrophotometry . . . . . . . . . . . . 342+ Z4 ^: V, O) {
5.5.3 Infrared spectroscopy . . . . . . . . . 342, q* d! w, A% {- u' P2 x$ t
5.5.4 Luminescence spectroscopy . . . . . 342
& G4 _" n5 Q% K* Z$ }/ O) t) c# W$ c7 R5.5.5 Nuclear magnetic resonance
: v2 U1 ^. D4 a2 Sspectroscopy . . . . . . . . . . . . . . . . 342, C; l( G" E" w2 t
5.6 References . . . . . . . . . . . . . . . . . . . . . . . 342 m/ U; F- n( K, a: @* o
Chapter 6 Organic Mass-Spectrometric
/ _7 l4 d) I" C+ P3 b3 Z- w RMethods . . . . . . . . . . . . . . . . 349
, R/ }8 q* ]1 `' c$ G; N6.1 Basic instrumentation . . . . . . . . . . . . . . . 351
+ ~0 [6 \5 V0 V2 ^5 S6.1.1 Inlet systems . . . . . . . . . . . . . . . . 352
# n/ K8 q4 x# M+ o6.1.2 Modes of detection . . . . . . . . . . . 353
+ d- {( N- U! Y! v+ J( r2 g6.1.3 Mass resolution . . . . . . . . . . . . . . 354. v7 G, E- o% S
6.1.4 Isotope distributions . . . . . . . . . . 354# H' e, {6 y' E% @
6.1.5 Accurate mass measurements. . . . 355. w) r% e' h9 ^
6.2 Ion sources . . . . . . . . . . . . . . . . . . . . . . 357
2 ~, ~* i9 ^, b, j+ k" h6.2.1 Electron impact ionisation . . . . . . 360
5 h) x$ Z2 r. a; ]1 l* H0 m% Z6.2.2 Chemical ionisation . . . . . . . . . . . 362
: A# i7 y5 }3 b$ J9 y5 q6.2.3 Metastable atom bombardment . . 367/ E7 t1 G* H3 M( ^
6.2.4 Fast atom bombardment . . . . . . . 367; `" `& H( ?* j- C/ H1 r
6.2.5 Field ionisation . . . . . . . . . . . . . . 372
$ r' Y/ J: ^; W# H6.2.6 Field desorption . . . . . . . . . . . . . 374
. L: r1 _5 ~# P9 j6.2.7 Thermospray ionisation . . . . . . . . 376
6 z: d, n) b/ Z( h6.2.8 Atmospheric pressure ionisation
5 ?0 T4 m; r! g0 J. ?8 xtechniques . . . . . . . . . . . . . . . . . 3789 j& x) e( ?1 F) a) G% j/ S
6.2.9 Desorption/ionisation methods . . . 383; |4 H/ z/ N& ] }+ J" S
6.2.10 Photoionisation techniques. . . . . . 3859 x2 x! w. ^# ^% ^
6.3 Mass analysers . . . . . . . . . . . . . . . . . . . 386- T u0 S0 \# w r- \' Z7 H7 J! ^
6.3.1 Sector analysers . . . . . . . . . . . . . 387
# E/ L+ j2 m6 i) b6.3.2 Quadrupole mass spectrometers . . 389* z/ t% {1 v8 x) M7 w L- H a7 q
6.3.3 Time-of-flight mass spectrometry . 3900 @5 z' A6 r# L: L/ s
6.3.4 Quadrupole ion trap . . . . . . . . . . 393) L% Q1 e1 V, i }
6.3.5 Fourier-transform ion-cyclotron
$ N9 B/ ~. w7 w) i0 K3 qresonance mass spectrometry . . . . 395' ^; u! }' {3 c1 K3 T
6.3.6 Tandem mass spectrometry . . . . . 398
0 j+ H9 e d. t% ?9 }6 B6.4 Direct mass-spectrometric polymer& m' |; ^! l I
compound analysis . . . . . . . . . . . . . . . . . 407
5 b' n% Z& Z* R6.5 Ion mobility spectrometry . . . . . . . . . . . 4158 q( ~" I7 D; h a+ ~
6.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 417* [8 Q7 {3 h& Y* H" V( |2 \
6.6.1 Mass spectrometry (General) . . . . 417- C7 B0 U) w, [9 ^' K
6.6.2 Mass spectrometers . . . . . . . . . . . 417
8 d M, B H1 U) a/ n+ f6.6.3 Ionisation modes . . . . . . . . . . . . . 417* j+ l# l6 E# e5 u) J
6.7 References . . . . . . . . . . . . . . . . . . . . . . . 418, \5 l5 b( I* _
Chapter 7 Multihyphenation and. f* D3 c2 B' B) q+ }) k' r6 {
Multidimensionality in
- o/ s+ w( @% n& _- @2 K% {Polymer/Additive Analysis . . . 425
C! @4 J0 R! v6 u, S. Z7.1 Precolumn hyphenation . . . . . . . . . . . . . 428) P1 r P8 J* S ?
7.1.1 Chromatographic sampling
/ S$ X1 q5 c) G- Z" N4 a7 amethods . . . . . . . . . . . . . . . . . . . 432
) X, i L i: Q% t* v7.2 Coupled sample
3 g6 m1 t9 _5 @! e, mpreparation – spectroscopy/spectrometry . 449
. ~; L7 k0 t$ G7.3 Postcolumn hyphenation . . . . . . . . . . . . . 452
1 |5 {- m4 n" G5 m6 U7.3.1 (Multi)hyphenated GC techniques 456
# u, W9 u; ^9 e4 d9 E! H7.3.2 (Multi)hyphenated SFC: |9 T# p+ J& m3 \+ J$ s; X
techniques . . . . . . . . . . . . . . . . . 4758 t4 l4 W M% \
7.3.3 (Multi)hyphenated HPLC
: S l8 _' j# A5 Y; Ztechniques . . . . . . . . . . . . . . . . . 489/ L' ]3 I# E" J
7.3.4 Hyphenated SEC techniques . . . . 5276 `' K, T g- B
7.3.5 Hyphenated TLC techniques . . . . 530# e9 `1 ^. k$ ~1 v3 A* Z
7.3.6 Hyphenated CE techniques . . . . . 543* c- S* j# A, V+ K# h, A
Contents vii, c D6 C5 D; s6 [4 O" s' K
7.4 Multidimensional chromatography . . . . . 545
3 k7 S1 I5 r n+ O7.4.1 Multidimensional gas
. _ s9 s9 D- ychromatography . . . . . . . . . . . . . 548
% ]' Y3 a( [/ I8 L6 @# i& w) O7.4.2 Multidimensional supercritical
3 ?6 X: @* W. r6 V G% x# ofluid chromatography . . . . . . . . . 550
( g3 @8 U& q7 o% u7.4.3 Multidimensional liquid9 t/ P% i7 T% }! Y
chromatography . . . . . . . . . . . . . 5506 v, d+ N3 f5 D) L' @+ i8 j
7.4.4 Multidimensional thin-layer& p6 s: s: r- B: o+ W- Q
chromatography . . . . . . . . . . . . . 558
0 Q" `$ z, A$ Z7.5 Multidimensional spectroscopy . . . . . . . . 560+ I$ s+ x) v+ Z/ T+ T) P( F
7.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 562! s% }8 ^* K, s: ]$ a
7.6.1 General . . . . . . . . . . . . . . . . . . . 5627 n) m0 x0 c# ?2 z A$ N
7.6.2 Multihyphenation and! W3 j# c% }- h- p9 F7 G
multidimensionality . . . . . . . . . . . 563
* W. m+ f8 ?/ w& s7.6.3 Precolumn hyphenation . . . . . . . . 563
) v0 s; H' E5 R4 u8 D3 M7.6.4 Postcolumn hyphenation . . . . . . . 563- }: D. n: n# e0 H6 y! e ~8 _
7.6.5 Multidimensional chromatography 563
6 B3 M+ R% N3 S) z: S9 x) C" Z7.6.6 Multidimensional spectroscopy . . 563
) d/ n" S, z/ y9 u: P+ I- I7.7 References 564
0 e% {2 p# v$ Y& ]3 {) @* x7 wChapter 8 Inorganic and Element' ~: d# m1 J. n y
Analytical Methods . . . . . . . . 585
. O, c' j1 j) ~- j$ H8.1 Element analytical protocols . . . . . . . . . . 5877 X H! a8 x3 f, y* A
8.1.1 Element analytical pretreatment
1 ^- t& J' R% }( r, q- L# N! h& Hprotocols . . . . . . . . . . . . . . . . . . 588
6 R* x, k5 w/ R% \) e! J8.1.2 Elemental analysis methods . . . . . 589
0 J, B2 F, v3 l# ~6 I5 b8.2 Sample destruction for classical elemental0 ^% g- C. i( a
analysis . . . . . . . . . . . . . . . . . . . . . . . . . 591
' {+ G8 H# G# i! _2 g$ A* F8.2.1 Combustion analysis . . . . . . . . . . 593+ B9 ?$ n6 K! R$ B. ~2 W
8.2.2 Wet matrix digestion . . . . . . . . . . 597: r' s) w3 d ^8 X
8.2.3 Fusion methods . . . . . . . . . . . . . . 604/ V! M8 n" e- E
8.3 Analytical atomic spectrometry . . . . . . . . 605
& W' u2 n0 {( m, g8.3.1 Atomic absorption spectrometry . 608
p& c8 `8 h* ~6 B; t: E' R+ |0 I8.3.2 Atomic emission spectrometry . . . 613; P' r( j" a1 e
8.3.3 Atomic fluorescence spectrometry 624 |
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