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Acknowledgements. . . . . . . . . . . . . . . . xv
x, B( G; O. Z5 g; JChapter 1 Introduction . . . . . . . . . . . . . . 15 X( k" q* z v8 N4 y& f
1.1 Additives . . . . . . . . . . . . . . . . . . . . . . . . 23 j7 x D# M0 M; }) N4 n
1.1.1 Additive functionality . . . . . . . . . 30 U" U% g# W! |( S' {- I: M
1.2 Plastics formulations . . . . . . . . . . . . . . . 5 S3 W$ O1 K4 l7 q. Y, A" k& G$ v
1.2.1 Supply forms . . . . . . . . . . . . . . . 72 p8 Q. R) N" C; F
1.2.2 Additive delivery . . . . . . . . . . . . 9
- e9 [9 k6 ?" A7 @( d+ A1.3 Economic impact of polymer additives . . 99 s% B# p) E/ l: P- {& |0 `' m
1.4 Analysis of plastics . . . . . . . . . . . . . . . . 113 @ V d% Q' G: K) C8 D
1.4.1 Regulations and standardisation . . 15
9 u! w8 ~* b' R9 F1 d. o' e; d1.4.2 Prior art . . . . . . . . . . . . . . . . . . . 17
. H- Q+ E3 v! O) y2 K0 t1.4.3 Databases . . . . . . . . . . . . . . . . . . 19- s6 t: `1 R7 \# V# T7 k
1.4.4 Scope . . . . . . . . . . . . . . . . . . . . . 20
9 T$ V9 k1 n3 O1.4.5 Chapter overview . . . . . . . . . . . . 22- j' T- ^+ g4 p
1.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 23# _5 C( {9 i' e- Q
1.5.1 Plastics additives . . . . . . . . . . . . . 23
/ w: C! Z# f2 R" v( F2 B" A1.5.2 Processing technologies . . . . . . . . 23
* v5 I# |) \' q* e1.5.3 Instrumental analysis . . . . . . . . . . 23) e8 k4 |/ d) Q T1 H. F
1.5.4 Polymer analysis . . . . . . . . . . . . . 243 d) w" S! E. \* z( h
1.5.5 Polymer/additive analysis . . . . . . 242 G5 u& q2 s. f) r7 l! ~ k
1.6 References . . . . . . . . . . . . . . . . . . . . . . . 24
& I) f/ \: i$ |7 P2 Z* ]3 gChapter 2 Deformulation Principles . . . . 29! I( o1 V0 C5 {& V1 b4 R
2.1 Polymer identification . . . . . . . . . . . . . . 300 I/ Q! o1 z& V5 R0 P' J
2.2 Additive analysis of rubbers: ‘Best
7 Y# K! _! o' N" U: a2 B# T. x5 `. {Practice’ . . . . . . . . . . . . . . . . . . . . . . . . 32
& A2 A2 r& E+ u% w2.3 Polymer extract analysis . . . . . . . . . . . . . 424 s& ]7 @0 T! X) a5 r/ m
2.4 In situ polymer/additive analysis . . . . . . 46
5 l; p, B- k; A1 r* N2.5 Class-specific polymer/additive analysis . 470 X. r2 Z1 q+ b# s3 x
2.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 48
4 C& [) H( X5 E% W* N2.6.1 Polymer identification . . . . . . . . . 48
& q# s& q0 f- c+ [5 ]; `+ H/ P2.6.2 Deformulation of rubbers . . . . . . 48
0 ~: g% x6 E3 F6 d" G2.6.3 Deformulation of polymers . . . . . 48* s* F6 r: P; V; Z6 k/ c$ @
2.7 References . . . . . . . . . . . . . . . . . . . . . . . 48
) K9 n+ D5 V: N$ qChapter 3 Sample Preparation
! Y2 A# M* b5 o0 w- _5 TPerspectives . . . . . . . . . . . . . . 51 `- X; j E7 b+ O% _. |; ?9 C
3.1 Solvents . . . . . . . . . . . . . . . . . . . . . . . . 545 `3 ?$ I" L: B% f6 ?: g6 ^
3.1.1 Polymer solubility criteria . . . . . . 55
4 ?, [( ]1 A- o' ]& F3.1.2 Solubility parameters . . . . . . . . . . 55
! D/ g+ ^5 L6 y, E) I3.1.3 Polymer solutions . . . . . . . . . . . . 561 C1 o0 \. e' C" a4 t; J
3.2 Extraction strategy . . . . . . . . . . . . . . . . . 57
3 O* {3 V1 @8 W1 i) Y. [5 D0 Z3.3 Conventional extraction technologies . . . 59
) b1 Q0 a1 b3 x" ]3.3.1 Liquid–liquid extraction . . . . . . . 60
, H) K* b1 r: c9 Q2 O3.3.2 Liquid–solid extraction . . . . . . . . 60
: n6 m' S) k2 @- n+ C% a; N; d4 `: i3.3.3 Classical solvent extractions of
4 [+ U7 d8 g& S5 ~: x" zadditives from polymers . . . . . . . 61, ?1 M. o4 ~8 X
3.3.4 Sonication . . . . . . . . . . . . . . . . . 75$ p7 F$ l; D( x% i3 j" V+ e+ X
3.4 High-pressure solvent extraction methods 81
^5 C- r- K2 R l; B5 h3.4.1 Supercritical fluid technology . . . 81
2 W. X+ V, b# p6 b& V3 ^. j7 O3.4.2 Analytical SFE . . . . . . . . . . . . . . 85
7 `9 H) ~$ e* C0 U O2 g) T+ E3.4.3 Subcritical water extraction . . . . . 100: a0 c( R2 T: z; J; U; |' s
3.4.4 Microwave technology . . . . . . . . 101
' q+ p0 j* I0 z3.4.5 Microwave-assisted extractions . . 104: j$ l3 X, k% }! J
3.4.6 Pressurised fluid extraction . . . . . 117+ g. d4 E1 X' Q3 @
3.5 Sorbent extraction . . . . . . . . . . . . . . . . . 123, h- t {" f4 q- W1 W ^
3.5.1 Solid-phase extraction . . . . . . . . . 1244 E' I6 a' l& E& R
3.5.2 Solid-phase microextraction . . . . . 129
3 z+ y- @& X; J$ g( d3.5.3 Stir bar sorptive extraction . . . . . 133( u! W' R) D0 ?$ r
3.6 Methodological comparison of extraction0 O ], f3 Q- {
methods. . . . . . . . . . . . . . . . . . . . . . . . . 134
. p& s4 u4 X2 V$ H& T3.6.1 Experimental comparisons . . . . . . 1364 W& E2 ]& k( r! b* T. u9 _
3.6.2 Extraction selectivity . . . . . . . . . . 138% I0 {# \' F, s: d
3.6.3 ‘Nonextractable’ additive analysis 140
" c" i$ {: f6 m; v1 Q. o; X3.7 Polymer/additive dissolution methods . . . 146
9 n' p2 L( Y/ u. n z0 g. S' b3.8 Hydrolysis . . . . . . . . . . . . . . . . . . . . . . . 152
2 Q1 [+ j! O- Q# L, ]3.9 Bibliography . . . . . . . . . . . . . . . . . . . . . 155
, l2 E7 `8 n; x7 u& o% \3.9.1 Sampling and sample preparation 155
6 ]; b6 e3 u* d; W7 V) X3.9.2 Solvents/solubility . . . . . . . . . . . . 155+ c# c: d* n% F' q
3.9.3 Extraction methods . . . . . . . . . . . 1560 n4 o, g9 v" Y$ W
3.10 References . . . . . . . . . . . . . . . . . . . . . . . 1568 S/ b; }2 A! c; z
vi Contents
6 D/ f$ W% p% y! OChapter 4 Separation Techniques . . . . . . 171
4 a I+ k2 h9 Q3 d2 b" u' ~) D. L2 K/ D4.1 Analytical detectors . . . . . . . . . . . . . . . . 177
* q9 }, r) A, A- R. I4.2 Gas chromatography . . . . . . . . . . . . . . . 181& S% [2 |8 ?$ k6 V- M; `
4.2.1 High-temperature gas( b9 H1 O0 Q! y
chromatography . . . . . . . . . . . . . 200& G- z& n/ g: E4 T; c
4.2.2 Headspace gas chromatography . . 202
# S2 N! \6 {5 _1 k3 Y4.3 Supercritical fluid chromatography . . . . . 205/ W( P& i% P Q
4.4 Liquid chromatography techniques . . . . . 217
- R ^0 h& Z0 |, [; q# c9 Y/ F4.4.1 Planar chromatographies . . . . . . . 2189 l) d0 v3 B- Z: @, j" O; O6 I$ z4 s
4.4.2 Column chromatographies . . . . . . 2304 C& f1 n" r2 W; \' K9 i; h* Y
4.5 Capillary electrophoretic techniques . . . . 273
) Y$ V; A5 m4 e1 P4.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 2788 Y' Q# v& `1 p# X/ Q
4.6.1 General texts . . . . . . . . . . . . . . . 278
: E, j. u! R8 Z4.6.2 Detectors . . . . . . . . . . . . . . . . . . 2796 s: D, \0 \2 y1 q9 Z' u
4.6.3 Gas chromatography . . . . . . . . . . 279
- H! r6 a7 p7 Y6 u3 ^4.6.4 Supercritical fluid chromatography 279- ~2 B1 J H% p m0 n! b. @
4.6.5 Thin-layer chromatography . . . . . 279% h9 M0 w! W8 A' L
4.6.6 Liquid chromatography . . . . . . . . 280
2 g7 L+ S# E7 h5 p8 t q4.6.7 Size-exclusion chromatography . . 280" Q7 @$ [1 D3 h7 W6 K6 J
4.6.8 Ion chromatography . . . . . . . . . . 280
& y9 S: t6 j+ k' H& _4.6.9 Capillary electrophoretic" U% k, k! ^% Z# j3 y/ O
techniques . . . . . . . . . . . . . . . . . 2802 X" L @$ |) h
4.7 References . . . . . . . . . . . . . . . . . . . . . . . 281- r; x: L2 X7 H9 m, p3 t
Chapter 5 Polymer/Additive Analysis:6 C; e- B5 d7 `" o4 m
The Spectroscopic Alternative 299( b; D& @. Z! Z9 W
5.1 Ultraviolet/visible spectrophotometry . . . 302
4 p$ F5 e! t2 l, G4 e$ f6 Z5.2 Infrared spectroscopy . . . . . . . . . . . . . . . 311) Y# ~5 _" `. J/ y1 o
5.3 Luminescence spectroscopy . . . . . . . . . . 318
+ r7 F, U0 ]8 r5.4 High-resolution nuclear magnetic/ @3 n2 x c6 z% D+ Y, ~$ i
resonance spectroscopy . . . . . . . . . . . . . 323$ b. w, l8 {9 T! X: g( \- j) _
5.4.1 Multidimensional NMR
. [. l1 H; ~- Dspectroscopy . . . . . . . . . . . . . . . . 336
: T( }2 J! i0 e: _) j8 f, f6 _5.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 342
& K4 K6 y9 L% D6 x) U2 B7 Y( y5.5.1 General spectroscopy . . . . . . . . . 342
! O; ]- U- r$ O( R" C1 |/ @' n3 W H5.5.2 Ultraviolet/visible& q* d% _, ?& ~, c. G' A9 p
spectrophotometry . . . . . . . . . . . . 342/ f* }2 b! b5 d4 W
5.5.3 Infrared spectroscopy . . . . . . . . . 342
" s' P5 z2 j1 J4 ^! s5.5.4 Luminescence spectroscopy . . . . . 342' K) z1 [* \" U5 {/ z/ c+ E+ d4 c, r8 p
5.5.5 Nuclear magnetic resonance
% e9 ]9 b& d, d8 ]* {0 Zspectroscopy . . . . . . . . . . . . . . . . 342
/ A! q4 A& \) l+ J- a5.6 References . . . . . . . . . . . . . . . . . . . . . . . 342
; g- N b3 R1 v) f. Z: m7 ]* o+ @Chapter 6 Organic Mass-Spectrometric/ C+ ^/ L: E9 {' {: j0 i& y/ L
Methods . . . . . . . . . . . . . . . . 3497 k7 g1 X" Z! J* u
6.1 Basic instrumentation . . . . . . . . . . . . . . . 3516 s5 D: U" i7 D- e
6.1.1 Inlet systems . . . . . . . . . . . . . . . . 352
. B2 m0 ~ C) q. d, }6.1.2 Modes of detection . . . . . . . . . . . 353
* S% D5 J) g! h3 J: o2 a6.1.3 Mass resolution . . . . . . . . . . . . . . 354
) l; m: T: m* r) V, x1 Y6.1.4 Isotope distributions . . . . . . . . . . 354
+ `/ |+ {, ?& ]: \. q7 s! g6.1.5 Accurate mass measurements. . . . 355
% K* U- @8 Z9 v: y- h3 A" \6.2 Ion sources . . . . . . . . . . . . . . . . . . . . . . 357
K6 T% X1 ]- M6.2.1 Electron impact ionisation . . . . . . 360
8 R9 l* k) `. Y; J" m& _" g6.2.2 Chemical ionisation . . . . . . . . . . . 362
* |( A1 I: C* v* \& B6 x6 q/ p% B6.2.3 Metastable atom bombardment . . 367
8 p! T4 `$ K) P6.2.4 Fast atom bombardment . . . . . . . 367
7 ]' U: `7 Q; `6.2.5 Field ionisation . . . . . . . . . . . . . . 3724 |3 l" z9 [7 F( ]3 C& K7 f
6.2.6 Field desorption . . . . . . . . . . . . . 3743 \8 {6 p4 y& I6 Q8 J
6.2.7 Thermospray ionisation . . . . . . . . 376
' z& N( K' m* S6.2.8 Atmospheric pressure ionisation1 C( u- j# E* G# m, }. E/ P
techniques . . . . . . . . . . . . . . . . . 378
9 D6 d# R; y' }/ r6.2.9 Desorption/ionisation methods . . . 3839 |6 r+ W7 q9 ]6 B* G- w4 k8 `
6.2.10 Photoionisation techniques. . . . . . 385) ] l+ V7 R7 {' R: R/ W
6.3 Mass analysers . . . . . . . . . . . . . . . . . . . 3867 N9 W2 ^, ]0 J! {9 m
6.3.1 Sector analysers . . . . . . . . . . . . . 387) v6 z% r- n9 V B
6.3.2 Quadrupole mass spectrometers . . 389
( G: G0 G' W) Y5 }6.3.3 Time-of-flight mass spectrometry . 390
) E6 |$ P8 J. G4 X6.3.4 Quadrupole ion trap . . . . . . . . . . 393# e! {! u/ A& \5 k7 S; B" N
6.3.5 Fourier-transform ion-cyclotron8 w; D; ]) N" m5 Y: \8 ^! N* y2 k
resonance mass spectrometry . . . . 3954 A8 E; ]; P' R ^, r" h
6.3.6 Tandem mass spectrometry . . . . . 398
[3 }6 \ ?+ {- c6.4 Direct mass-spectrometric polymer
6 l/ z; p% |1 B. [. c% q8 }compound analysis . . . . . . . . . . . . . . . . . 407. [+ L! A( e: h% O6 K
6.5 Ion mobility spectrometry . . . . . . . . . . . 415
, U3 T/ ~* R6 {6 ?6.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 417
/ ~- I3 |' I9 y9 U8 \6.6.1 Mass spectrometry (General) . . . . 417
( v) W, ?' P. b* p1 Q7 m8 x7 s6.6.2 Mass spectrometers . . . . . . . . . . . 4173 h% w4 \5 a9 U: [, g( }
6.6.3 Ionisation modes . . . . . . . . . . . . . 4170 [" w6 U8 _" X) I
6.7 References . . . . . . . . . . . . . . . . . . . . . . . 418
: \6 `/ R. B! o7 Q& ]Chapter 7 Multihyphenation and
) S/ F! `6 G7 l$ L6 x8 vMultidimensionality in" A- e4 V: i. `7 D
Polymer/Additive Analysis . . . 425( ]. k' o. B4 m/ }4 @" j
7.1 Precolumn hyphenation . . . . . . . . . . . . . 428& X) J9 H3 v) o" E: p; A
7.1.1 Chromatographic sampling- A+ G' M- Z" M+ a! r
methods . . . . . . . . . . . . . . . . . . . 4327 v% W' z* M2 F7 r/ n/ G
7.2 Coupled sample
7 P: `7 z% r$ v/ S! @preparation – spectroscopy/spectrometry . 449
# l( {; M6 h( N; o& r) |7.3 Postcolumn hyphenation . . . . . . . . . . . . . 4528 l# t: P% G6 k; M# J
7.3.1 (Multi)hyphenated GC techniques 456
( f: W( a! h0 r2 y/ [. k2 ]5 N7.3.2 (Multi)hyphenated SFC
# s% h2 J U& d5 \$ l n6 Ntechniques . . . . . . . . . . . . . . . . . 475
4 ^3 }. C* D f7.3.3 (Multi)hyphenated HPLC- p) Q% F T2 M* j6 u
techniques . . . . . . . . . . . . . . . . . 489) r& U- v# R" i4 |' Z
7.3.4 Hyphenated SEC techniques . . . . 527- p! ], S0 }5 ]. x* r
7.3.5 Hyphenated TLC techniques . . . . 5300 r) y- o7 o/ g: V
7.3.6 Hyphenated CE techniques . . . . . 5438 N w8 [! D" j: C
Contents vii4 z2 {& ?6 r* q# F
7.4 Multidimensional chromatography . . . . . 545
/ m, d) L' J3 |# X8 L2 a# G7.4.1 Multidimensional gas
' `! n5 e7 ~( E, F- z& ychromatography . . . . . . . . . . . . . 548) U4 m/ N4 ~( l ?1 q
7.4.2 Multidimensional supercritical
) J/ s7 l8 x& }9 O3 S: H& ~' nfluid chromatography . . . . . . . . . 550 k& m& e6 h( w0 t
7.4.3 Multidimensional liquid, \9 A1 |) n M J, J" b
chromatography . . . . . . . . . . . . . 5500 A8 H9 \+ c6 J/ }: F5 R
7.4.4 Multidimensional thin-layer/ k, _0 Y1 ~6 T$ h: ?
chromatography . . . . . . . . . . . . . 558) k" D2 l0 {) b' A6 h
7.5 Multidimensional spectroscopy . . . . . . . . 560" k; V1 n9 g3 k9 h
7.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 562* E& K5 _; }2 L' a. X
7.6.1 General . . . . . . . . . . . . . . . . . . . 562/ A; [ C: k5 W4 z
7.6.2 Multihyphenation and5 j6 U4 h2 V0 G1 } `) L
multidimensionality . . . . . . . . . . . 563
1 o) R3 {9 D" Q, m$ h7.6.3 Precolumn hyphenation . . . . . . . . 5632 s( T2 Q4 j n1 M
7.6.4 Postcolumn hyphenation . . . . . . . 563' _+ J5 ^% J* M- e: O) L
7.6.5 Multidimensional chromatography 563
8 Q4 V0 {, R; q2 V5 a7.6.6 Multidimensional spectroscopy . . 563; m, C o" O7 q4 ^; _, A
7.7 References 564
/ A9 F8 C5 k4 P" ] s% r2 OChapter 8 Inorganic and Element
3 l8 O* L; x. g, ~6 Z6 _Analytical Methods . . . . . . . . 585
% A$ g0 y9 y7 @+ S8.1 Element analytical protocols . . . . . . . . . . 5872 k s+ _9 l. P3 o4 J$ R. H2 x
8.1.1 Element analytical pretreatment
J! W9 K2 J/ N+ P2 x2 ]protocols . . . . . . . . . . . . . . . . . . 588
. x+ R% ]5 d. `+ a8.1.2 Elemental analysis methods . . . . . 589# a- L9 E5 ^" Q! Z4 L
8.2 Sample destruction for classical elemental Z2 R( v: g* J
analysis . . . . . . . . . . . . . . . . . . . . . . . . . 591 ]$ Y" y0 h: N9 |: N
8.2.1 Combustion analysis . . . . . . . . . . 593. E7 ]; H5 J2 K4 w& b& h7 r
8.2.2 Wet matrix digestion . . . . . . . . . . 597
0 v) I% {* n- H4 M8.2.3 Fusion methods . . . . . . . . . . . . . . 604
U$ D. M% t6 n: N5 E8.3 Analytical atomic spectrometry . . . . . . . . 605
/ G# F; Y9 O$ N2 N: U' ], @& o8.3.1 Atomic absorption spectrometry . 608
7 w; u+ U! ]$ O. V% {8.3.2 Atomic emission spectrometry . . . 613, o6 a7 ?' I1 A; D) o3 S0 K& u, y3 P
8.3.3 Atomic fluorescence spectrometry 624 |
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