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Acknowledgements. . . . . . . . . . . . . . . . xv
' E5 t- s6 d9 w m+ F- Y7 bChapter 1 Introduction . . . . . . . . . . . . . . 1
+ w- }3 z0 [' R3 ~$ D# T1.1 Additives . . . . . . . . . . . . . . . . . . . . . . . . 22 }2 o2 i9 s" p
1.1.1 Additive functionality . . . . . . . . . 3$ M0 _* \2 ?' p+ [. g$ @3 Y- O4 S
1.2 Plastics formulations . . . . . . . . . . . . . . . 5* x9 p' e! b/ {* \- p, `! I8 D
1.2.1 Supply forms . . . . . . . . . . . . . . . 7) f5 J0 K+ J* F* Y9 j, a8 J& G- d; O
1.2.2 Additive delivery . . . . . . . . . . . . 9" @" [* e5 |' c) j! S
1.3 Economic impact of polymer additives . . 99 G+ p- y6 \2 m
1.4 Analysis of plastics . . . . . . . . . . . . . . . . 11
9 q% J Z: k0 L/ a1.4.1 Regulations and standardisation . . 15
4 Q5 H" f$ F: }3 ^1.4.2 Prior art . . . . . . . . . . . . . . . . . . . 17, s) n4 [5 L p( v3 \6 S) h' @& Y- ]
1.4.3 Databases . . . . . . . . . . . . . . . . . . 196 Q; p2 S+ S& c1 _/ I7 O
1.4.4 Scope . . . . . . . . . . . . . . . . . . . . . 20
2 y& J* X, D4 j# ^" H2 [; i1.4.5 Chapter overview . . . . . . . . . . . . 22- A6 g5 U, t0 h6 r7 C. Y* E
1.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 23) I& Z3 o. R' P! ^9 O! D. W
1.5.1 Plastics additives . . . . . . . . . . . . . 23
$ V& F. K, b- G3 G1.5.2 Processing technologies . . . . . . . . 232 h- K7 u% V( O p5 T. K
1.5.3 Instrumental analysis . . . . . . . . . . 23
- W2 Y+ F3 v# d2 ?! g1.5.4 Polymer analysis . . . . . . . . . . . . . 24
' k) l& r2 }* L1.5.5 Polymer/additive analysis . . . . . . 24$ F$ X- Z* J! P8 B6 k
1.6 References . . . . . . . . . . . . . . . . . . . . . . . 24
' y1 q/ ^$ `2 F. HChapter 2 Deformulation Principles . . . . 293 G) M6 R8 S$ |2 K! L$ j
2.1 Polymer identification . . . . . . . . . . . . . . 30
1 D8 i3 r6 F5 G- Z3 Y3 h2.2 Additive analysis of rubbers: ‘Best
! ` m6 X! q- K& Z& n9 X* Z& tPractice’ . . . . . . . . . . . . . . . . . . . . . . . . 32# D N0 X. \& ? s
2.3 Polymer extract analysis . . . . . . . . . . . . . 42$ P6 t* {5 O4 N) \& r: B
2.4 In situ polymer/additive analysis . . . . . . 46
& F5 T6 o2 |* |4 `2 @( e2.5 Class-specific polymer/additive analysis . 47 \1 w* r2 X/ c. a. @$ q4 T
2.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 48% `# ` P' g! ?8 n5 A
2.6.1 Polymer identification . . . . . . . . . 485 S2 h, K5 s9 B. y2 ^1 x7 P
2.6.2 Deformulation of rubbers . . . . . . 488 K: t, [: P4 J9 C% R/ ~& J7 [0 W5 q
2.6.3 Deformulation of polymers . . . . . 486 q7 [- C( f5 M( ]% k0 P" _
2.7 References . . . . . . . . . . . . . . . . . . . . . . . 48( s8 [- |% V1 ]8 z
Chapter 3 Sample Preparation% C: a* _2 k* u. I- D5 h
Perspectives . . . . . . . . . . . . . . 51
, w' V9 P* \9 T- T9 G3.1 Solvents . . . . . . . . . . . . . . . . . . . . . . . . 54, T. _ P+ U" ~% Q: J0 h
3.1.1 Polymer solubility criteria . . . . . . 55
5 ?4 t7 e& c+ D0 @- h8 b3.1.2 Solubility parameters . . . . . . . . . . 55
8 Q2 E& C: j4 ~7 |# ~5 M3.1.3 Polymer solutions . . . . . . . . . . . . 562 s4 ?4 X- O* V( W G5 i$ u
3.2 Extraction strategy . . . . . . . . . . . . . . . . . 57+ Q5 o1 _+ R7 C- i9 x, }
3.3 Conventional extraction technologies . . . 59( |1 Y+ X9 g6 h
3.3.1 Liquid–liquid extraction . . . . . . . 60
0 B) b9 g% n. ~. O$ u( d" Q8 m3.3.2 Liquid–solid extraction . . . . . . . . 602 O0 ?- {3 x- v
3.3.3 Classical solvent extractions of
5 S; ?: K/ T9 |& ]5 }additives from polymers . . . . . . . 61
) G5 f ^ c; C0 ]3.3.4 Sonication . . . . . . . . . . . . . . . . . 75
8 P( k6 j$ o- F/ T3.4 High-pressure solvent extraction methods 81
" l, _3 s* _' A9 T6 i% O3.4.1 Supercritical fluid technology . . . 81
w* N4 A, @3 q4 J9 y9 k% l" p+ B3.4.2 Analytical SFE . . . . . . . . . . . . . . 85
( K2 T Y6 J! a/ _0 _9 _3.4.3 Subcritical water extraction . . . . . 100
' c6 ~' x8 |& @3.4.4 Microwave technology . . . . . . . . 101
3 ^, u8 |9 S a6 p, o3.4.5 Microwave-assisted extractions . . 104
~ w* C0 r' J8 u3.4.6 Pressurised fluid extraction . . . . . 117
$ Y7 l `, p% q! t" G) J" r( [3.5 Sorbent extraction . . . . . . . . . . . . . . . . . 123' ~+ z' d6 Z% w+ s% u2 `
3.5.1 Solid-phase extraction . . . . . . . . . 124
1 B! } p2 V* C1 V+ E6 }. ~3.5.2 Solid-phase microextraction . . . . . 129
, r' {1 o& F2 v, e3.5.3 Stir bar sorptive extraction . . . . . 133
. G' `% ~. z/ d% R& ]* W F: _3.6 Methodological comparison of extraction7 [" g$ Z$ [: d1 K
methods. . . . . . . . . . . . . . . . . . . . . . . . . 134
& A2 X% A$ S4 X6 ?+ \/ C( V3.6.1 Experimental comparisons . . . . . . 136
6 R$ z- D5 b k! E- u7 d3.6.2 Extraction selectivity . . . . . . . . . . 138( P! M( {5 |0 d0 p5 k
3.6.3 ‘Nonextractable’ additive analysis 140
/ g+ W# {$ R3 P, n5 l3.7 Polymer/additive dissolution methods . . . 146
, X2 S0 w/ F) O* n/ ?' y, [% I3.8 Hydrolysis . . . . . . . . . . . . . . . . . . . . . . . 152 D7 K: i7 O z* z. \, G# i
3.9 Bibliography . . . . . . . . . . . . . . . . . . . . . 155
' y) u8 K. v3 W0 [3.9.1 Sampling and sample preparation 155
/ F! R* y! k" w3.9.2 Solvents/solubility . . . . . . . . . . . . 155
" H" a0 O1 b% a7 p* |3.9.3 Extraction methods . . . . . . . . . . . 156
: d% H$ L3 O' H4 V. \3.10 References . . . . . . . . . . . . . . . . . . . . . . . 156
" ]) L( o) s% _/ O, Z J- lvi Contents1 f1 I& q1 I# M. s. q9 Q
Chapter 4 Separation Techniques . . . . . . 171
8 v R% [3 C8 I( Y% M8 i' c4.1 Analytical detectors . . . . . . . . . . . . . . . . 177
( q. F$ R5 N8 Q+ y4.2 Gas chromatography . . . . . . . . . . . . . . . 1816 }" E1 w; K5 }# C- t
4.2.1 High-temperature gas
% p+ `0 |; }1 j. K% P& }4 {chromatography . . . . . . . . . . . . . 200- Q! d E8 q8 k+ Z
4.2.2 Headspace gas chromatography . . 202
% s4 R; R" c5 A! K0 L* t4.3 Supercritical fluid chromatography . . . . . 205" y) f3 ^ ~2 y. d o p
4.4 Liquid chromatography techniques . . . . . 217
1 N- ^, t) B! e: t/ v: \& A4.4.1 Planar chromatographies . . . . . . . 218
8 G- H& ]5 L$ N+ c; ?, W' S; V& ]4.4.2 Column chromatographies . . . . . . 230* Y$ w4 f6 i$ C
4.5 Capillary electrophoretic techniques . . . . 273
1 Q& R" M" i, F) d4.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 2788 G5 T% s( r7 c9 \
4.6.1 General texts . . . . . . . . . . . . . . . 2785 N5 z1 o) N/ `, V+ S3 ^
4.6.2 Detectors . . . . . . . . . . . . . . . . . . 2795 \" }# B- j. @! V" S9 d
4.6.3 Gas chromatography . . . . . . . . . . 279, G, n+ L. V, ]
4.6.4 Supercritical fluid chromatography 279) @2 t8 B D8 p5 T& E" W! o9 l: J
4.6.5 Thin-layer chromatography . . . . . 279& {- f {) Z$ n7 ?
4.6.6 Liquid chromatography . . . . . . . . 280$ u9 a; y8 ^0 `% f" q( b, O
4.6.7 Size-exclusion chromatography . . 280& R/ [4 _# {4 b% C }! k- O2 Y: F4 Z
4.6.8 Ion chromatography . . . . . . . . . . 280
; e; n9 i* Y6 r6 b4.6.9 Capillary electrophoretic$ o6 F m* ] j6 @6 a
techniques . . . . . . . . . . . . . . . . . 280; `2 O, e, ]( u- P
4.7 References . . . . . . . . . . . . . . . . . . . . . . . 281$ _; a/ E! M% s
Chapter 5 Polymer/Additive Analysis:
0 r6 o/ {0 `0 R* H, X$ Q' A% ]The Spectroscopic Alternative 2991 S# F$ i) Y% \) G6 c
5.1 Ultraviolet/visible spectrophotometry . . . 302
/ Y$ p& E" a- i4 f/ N4 G5.2 Infrared spectroscopy . . . . . . . . . . . . . . . 311$ N1 V6 Z/ S! h
5.3 Luminescence spectroscopy . . . . . . . . . . 318: ^$ G3 K |6 [8 T
5.4 High-resolution nuclear magnetic
5 h9 h8 H4 k" Z, |resonance spectroscopy . . . . . . . . . . . . . 323' d$ P) c& @: O
5.4.1 Multidimensional NMR
" y6 b6 r4 o- j/ ]spectroscopy . . . . . . . . . . . . . . . . 336) j* K W! z; B, _. t& Y2 p
5.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 3421 @0 S8 |6 I: J& P3 L) H
5.5.1 General spectroscopy . . . . . . . . . 342
, Z8 h1 F( d1 m7 T3 z5.5.2 Ultraviolet/visible
% e! l/ S! x2 g1 a# K) h" @6 Tspectrophotometry . . . . . . . . . . . . 342; r# c" X( i' Q! [! |* x9 v
5.5.3 Infrared spectroscopy . . . . . . . . . 3428 A$ T; V. h6 h- ]
5.5.4 Luminescence spectroscopy . . . . . 342
. \3 F1 k( _9 v0 q% R8 t5.5.5 Nuclear magnetic resonance
. C! F9 E1 t; ^; V/ P* T5 b7 tspectroscopy . . . . . . . . . . . . . . . . 3423 n& _8 F8 a; a5 |0 w
5.6 References . . . . . . . . . . . . . . . . . . . . . . . 342
# u* r I1 q* q' YChapter 6 Organic Mass-Spectrometric% e8 W, k1 V- q7 I" ~' K& N
Methods . . . . . . . . . . . . . . . . 349: L( x3 U6 k/ o" @- r F2 y
6.1 Basic instrumentation . . . . . . . . . . . . . . . 3512 T: y- A2 }0 J+ e% h2 y
6.1.1 Inlet systems . . . . . . . . . . . . . . . . 352
) ^9 o6 E: Y$ D# }" I, i9 a6.1.2 Modes of detection . . . . . . . . . . . 3533 I* v4 {' a: d) [4 a* ^
6.1.3 Mass resolution . . . . . . . . . . . . . . 354 W1 u8 v# H) D+ d# ]( D% k7 u) U, O
6.1.4 Isotope distributions . . . . . . . . . . 354
7 m8 ]$ e/ C. Z' a6.1.5 Accurate mass measurements. . . . 355
* |7 D$ H+ ]0 m- @+ `6.2 Ion sources . . . . . . . . . . . . . . . . . . . . . . 357
9 {( ^ D( ]# ~$ E" M! l! ]6.2.1 Electron impact ionisation . . . . . . 360
) u8 v( u; e8 f/ d6 s1 Q0 {5 A1 t6.2.2 Chemical ionisation . . . . . . . . . . . 3624 R4 Z/ x) m, ~- |' z+ I- K, `
6.2.3 Metastable atom bombardment . . 3674 a' F7 m7 _3 P# @ w$ x
6.2.4 Fast atom bombardment . . . . . . . 367! s' m3 U/ O$ ?9 r
6.2.5 Field ionisation . . . . . . . . . . . . . . 372
- t( q4 `8 Z9 e# D ]6.2.6 Field desorption . . . . . . . . . . . . . 374
' A( o7 l9 ~8 o( X7 X# m) X6.2.7 Thermospray ionisation . . . . . . . . 376" `1 w$ k. J0 e$ R6 T6 S5 E4 [
6.2.8 Atmospheric pressure ionisation; U: y4 G+ w x3 W7 s9 u3 {
techniques . . . . . . . . . . . . . . . . . 378+ P, K0 a4 {. N+ L# O3 [
6.2.9 Desorption/ionisation methods . . . 3834 I; Q5 b. U9 M! `4 v- Q( [# ~' p
6.2.10 Photoionisation techniques. . . . . . 3859 n3 N! s K+ S* [! \
6.3 Mass analysers . . . . . . . . . . . . . . . . . . . 386
& q0 O& k3 w; k% _# a- x6.3.1 Sector analysers . . . . . . . . . . . . . 3871 X/ f8 i1 B x2 \& T( |; h
6.3.2 Quadrupole mass spectrometers . . 389
$ r ~2 s/ w' Y* y* `1 l6.3.3 Time-of-flight mass spectrometry . 390
2 u7 R0 E# L- Z4 q) f5 }0 q6.3.4 Quadrupole ion trap . . . . . . . . . . 393
( j7 l/ T( d/ Y/ O, l2 }7 _* {6.3.5 Fourier-transform ion-cyclotron
3 F5 t" Z* e1 R7 {/ P6 h2 ?resonance mass spectrometry . . . . 395
' `3 y( C7 {4 }+ W+ I) [& Y, L6.3.6 Tandem mass spectrometry . . . . . 398# h+ C$ m! G5 u: j
6.4 Direct mass-spectrometric polymer
0 Y3 [0 w6 h/ J$ G2 ]compound analysis . . . . . . . . . . . . . . . . . 407
7 A+ f b& z2 a6.5 Ion mobility spectrometry . . . . . . . . . . . 415. U+ h8 g* B2 l7 H' R
6.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 417, `5 E$ [! A! F) X5 H3 j
6.6.1 Mass spectrometry (General) . . . . 4175 n3 w# B, z7 K
6.6.2 Mass spectrometers . . . . . . . . . . . 417
; c4 j7 S+ Y& y! Q+ l6 }; n6.6.3 Ionisation modes . . . . . . . . . . . . . 4178 W1 s# I( d6 I
6.7 References . . . . . . . . . . . . . . . . . . . . . . . 418/ X3 x# b) W; k# h8 z7 _
Chapter 7 Multihyphenation and& c5 R( p# j! M* ] C) }1 H
Multidimensionality in& i+ b* O! X, p3 Y& ]% A
Polymer/Additive Analysis . . . 425
# d' x7 D, j& _4 }1 o7.1 Precolumn hyphenation . . . . . . . . . . . . . 428
* J! |" S: b/ j+ g' E' a7.1.1 Chromatographic sampling
# {$ q8 D5 s9 Dmethods . . . . . . . . . . . . . . . . . . . 432
* Y* [3 {: y/ |7.2 Coupled sample
3 @1 } a. G& M& s& g4 @3 d% _preparation – spectroscopy/spectrometry . 449/ {, \0 p0 e) ?9 X1 a
7.3 Postcolumn hyphenation . . . . . . . . . . . . . 4522 |$ G( @) W$ s; g
7.3.1 (Multi)hyphenated GC techniques 456
/ H. r- o! H+ K; ?7.3.2 (Multi)hyphenated SFC
" p$ K) ~0 [/ J6 V7 x* Dtechniques . . . . . . . . . . . . . . . . . 475# ~: Z0 k. B! [. U+ ?8 ]. u
7.3.3 (Multi)hyphenated HPLC
- _8 ?! C$ m9 }! P) {4 stechniques . . . . . . . . . . . . . . . . . 489 x0 O, t; \1 E5 F1 B7 R ?: |: o
7.3.4 Hyphenated SEC techniques . . . . 527- t K4 `! b: q/ K# k* b
7.3.5 Hyphenated TLC techniques . . . . 530
2 b- x3 J0 _; z7 O4 r. M/ {& v7 j0 V7.3.6 Hyphenated CE techniques . . . . . 543
& H& n3 }: p5 k4 A a* iContents vii; c: J* x4 w% y5 V3 @+ b7 N2 B
7.4 Multidimensional chromatography . . . . . 545
7 T8 H4 W2 A! O4 w$ l7.4.1 Multidimensional gas
9 G; T4 m, L4 b. Gchromatography . . . . . . . . . . . . . 548
* B# [- ]8 T$ x# J7.4.2 Multidimensional supercritical% L" t+ s9 y7 C* {6 z$ O7 m
fluid chromatography . . . . . . . . . 550* v j) T+ f( M, I3 U. N
7.4.3 Multidimensional liquid: @3 A5 |$ m, a& G9 C$ e$ p
chromatography . . . . . . . . . . . . . 550
1 I# K& d& S2 S1 @+ E: P7.4.4 Multidimensional thin-layer3 i/ j9 k& `9 {: f
chromatography . . . . . . . . . . . . . 5586 s% o( ~! ^8 Y4 f
7.5 Multidimensional spectroscopy . . . . . . . . 560
) F- Y D: ~4 p; b# a7.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 562" r& X1 o# k8 F5 t T% @+ x
7.6.1 General . . . . . . . . . . . . . . . . . . . 562
* w1 Q' o: P, V- _. m2 i7.6.2 Multihyphenation and
* D! S6 G- [4 ], m$ Wmultidimensionality . . . . . . . . . . . 563
3 K d+ x3 e3 v& `7.6.3 Precolumn hyphenation . . . . . . . . 563: E1 ], V0 |1 L
7.6.4 Postcolumn hyphenation . . . . . . . 563
! [! o- ~( L6 a; m7.6.5 Multidimensional chromatography 563
3 A1 v5 G I0 h( \& }' s9 c4 y7.6.6 Multidimensional spectroscopy . . 563. H8 V. f3 b$ U
7.7 References 564; \) y/ M/ [4 W4 s
Chapter 8 Inorganic and Element$ p9 P7 k# e$ D+ R
Analytical Methods . . . . . . . . 5857 }, N( G7 e) u3 D2 b
8.1 Element analytical protocols . . . . . . . . . . 587- ^ |5 y. q/ Z: a( k# M
8.1.1 Element analytical pretreatment. S" l1 y" ^: i- H$ f' V( y: a% ?. i
protocols . . . . . . . . . . . . . . . . . . 588
/ g% U; H5 n9 m+ X- }7 H8 E2 b8.1.2 Elemental analysis methods . . . . . 589
! A2 |) p. ~( {+ M H0 r2 I0 E8.2 Sample destruction for classical elemental2 K# y! q5 D: @& L0 A6 ]
analysis . . . . . . . . . . . . . . . . . . . . . . . . . 591( r( m2 z2 D2 m* w1 p7 D* N, y I
8.2.1 Combustion analysis . . . . . . . . . . 593
# t) `% K- T, l5 t0 W8 J8.2.2 Wet matrix digestion . . . . . . . . . . 597" c0 C" V* N0 X$ }( d
8.2.3 Fusion methods . . . . . . . . . . . . . . 604& n2 l0 b8 ?- c1 C3 h
8.3 Analytical atomic spectrometry . . . . . . . . 605% @/ X7 K# X5 F w/ J D" O% V
8.3.1 Atomic absorption spectrometry . 6089 L4 q, ?4 ?+ O7 N! c% s! d( D
8.3.2 Atomic emission spectrometry . . . 613& X/ J0 g2 {5 A0 |: D! t8 O$ s
8.3.3 Atomic fluorescence spectrometry 624 |
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