|
|
马上注册，结识高手，享用更多资源，轻松玩转三维网社区。
您需要 登录 才可以下载或查看，没有帐号？注册
x
Acknowledgements. . . . . . . . . . . . . . . . xv
' J; D+ Z" M, [, g: V! X7 mChapter 1 Introduction . . . . . . . . . . . . . . 16 ], ~! i! {8 D: m5 M
1.1 Additives . . . . . . . . . . . . . . . . . . . . . . . . 2
8 E, h# H+ Q' D0 j/ i1.1.1 Additive functionality . . . . . . . . . 3( x8 Y' [9 D. X3 k2 O/ l1 Q3 Y
1.2 Plastics formulations . . . . . . . . . . . . . . . 5$ F& | R( ] W0 O; Y& T8 |* _
1.2.1 Supply forms . . . . . . . . . . . . . . . 7) W" l3 X: E! q: R
1.2.2 Additive delivery . . . . . . . . . . . . 9. W, v! }5 j5 `3 ]
1.3 Economic impact of polymer additives . . 9
( i% a7 C: S( W, @( \8 M: |1.4 Analysis of plastics . . . . . . . . . . . . . . . . 11
; G: d7 _- X9 Z' N7 v1.4.1 Regulations and standardisation . . 157 b( }9 F/ s1 B( C: M
1.4.2 Prior art . . . . . . . . . . . . . . . . . . . 176 f$ _0 i. q* Q2 O" M
1.4.3 Databases . . . . . . . . . . . . . . . . . . 19
* W9 s, e3 N4 o+ x+ O! [) i2 W1.4.4 Scope . . . . . . . . . . . . . . . . . . . . . 20) [ O: Q2 B$ X8 d
1.4.5 Chapter overview . . . . . . . . . . . . 22
& H7 l" Y N! i( k+ N4 f* T6 c$ N1 Z1 ]1.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 23
: N/ H( A J. ]+ d; U7 A1.5.1 Plastics additives . . . . . . . . . . . . . 23
* o( n2 F' Z: N1 y+ R1.5.2 Processing technologies . . . . . . . . 23
4 E) ?5 ?6 _+ w; K1.5.3 Instrumental analysis . . . . . . . . . . 23
5 m) a' a, F! a; W% v! \ W1.5.4 Polymer analysis . . . . . . . . . . . . . 24% O7 v$ t6 x) u0 i* A9 l0 n" T6 l
1.5.5 Polymer/additive analysis . . . . . . 24
. U F9 n3 h7 V: Y2 c4 L8 t1.6 References . . . . . . . . . . . . . . . . . . . . . . . 24: m& ~8 X9 ]+ E
Chapter 2 Deformulation Principles . . . . 29, x0 F8 O8 K; k' g$ s
2.1 Polymer identification . . . . . . . . . . . . . . 30' }- _6 y% ~& i D; P
2.2 Additive analysis of rubbers: ‘Best
: \; t8 x. k5 e5 dPractice’ . . . . . . . . . . . . . . . . . . . . . . . . 326 ~; S0 Y9 {( |; V: i
2.3 Polymer extract analysis . . . . . . . . . . . . . 427 _! k3 l% F ^, f4 r
2.4 In situ polymer/additive analysis . . . . . . 46
2 Y( l+ u' x; e* A- f) p" M2.5 Class-specific polymer/additive analysis . 47
' R; v- t. u" q( v( l2.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 48
0 ~* y J6 F, l; I$ C2.6.1 Polymer identification . . . . . . . . . 48
8 b# g7 G- d6 p' t2 j3 W2 A2.6.2 Deformulation of rubbers . . . . . . 48! u4 d% A7 q9 L8 d! y7 J
2.6.3 Deformulation of polymers . . . . . 48
. u$ A5 U$ d/ ]! J; m5 k2.7 References . . . . . . . . . . . . . . . . . . . . . . . 48
8 R5 h8 o4 t: }! FChapter 3 Sample Preparation: |+ o) n# H6 x" ]* ^% K
Perspectives . . . . . . . . . . . . . . 513 D4 L1 ]7 ]; `1 {8 ~ Q) a
3.1 Solvents . . . . . . . . . . . . . . . . . . . . . . . . 54
$ h5 ?6 I' I% L. F; K3.1.1 Polymer solubility criteria . . . . . . 55( X" I- m( \8 {0 ^
3.1.2 Solubility parameters . . . . . . . . . . 55! g% O/ ^* ] Y0 j
3.1.3 Polymer solutions . . . . . . . . . . . . 56% d/ X u |9 H. B8 X* n1 x
3.2 Extraction strategy . . . . . . . . . . . . . . . . . 571 A5 o; G) L' R* z
3.3 Conventional extraction technologies . . . 59+ F$ k3 U+ a- d! m7 T
3.3.1 Liquid–liquid extraction . . . . . . . 60- ?0 X# G# q2 R9 ?
3.3.2 Liquid–solid extraction . . . . . . . . 605 B1 N5 U4 I3 {9 i, ?, f
3.3.3 Classical solvent extractions of
/ B! X% A2 c6 O# P% Radditives from polymers . . . . . . . 61
# B' N5 m) w) _2 c4 |3.3.4 Sonication . . . . . . . . . . . . . . . . . 75
9 C1 {) N9 `& w8 ~7 e3.4 High-pressure solvent extraction methods 81
2 M; {$ {% d* h3 u3.4.1 Supercritical fluid technology . . . 810 l' y; H! c) Z+ g9 B! b
3.4.2 Analytical SFE . . . . . . . . . . . . . . 85
! Q0 Z% J7 k; y- z; A3.4.3 Subcritical water extraction . . . . . 100
3 P1 _) y# l z' Z+ t3.4.4 Microwave technology . . . . . . . . 101
$ i, ]- [5 W! _( w- f3.4.5 Microwave-assisted extractions . . 104
& N+ R3 @! T3 k6 R: t3.4.6 Pressurised fluid extraction . . . . . 117
% c, [# e: R7 ^3.5 Sorbent extraction . . . . . . . . . . . . . . . . . 123$ m4 \# L) c9 f* {3 \: F1 x
3.5.1 Solid-phase extraction . . . . . . . . . 124
2 r N4 \3 `; k# A$ X w* Q3.5.2 Solid-phase microextraction . . . . . 129
/ x; Y8 H5 Y; J- \* t9 K3 j$ ~3.5.3 Stir bar sorptive extraction . . . . . 1330 d5 G2 ^% X! ]. V2 u( u
3.6 Methodological comparison of extraction
, i% k0 T+ R- m' \" Z# Hmethods. . . . . . . . . . . . . . . . . . . . . . . . . 134& G/ B% l; U7 L a; p2 y
3.6.1 Experimental comparisons . . . . . . 136+ I' i& u% H$ K% w t, @6 U3 F
3.6.2 Extraction selectivity . . . . . . . . . . 138
5 E% I2 M* k6 v8 e5 V1 \0 N3.6.3 ‘Nonextractable’ additive analysis 1407 n/ P% Y6 q3 r* x
3.7 Polymer/additive dissolution methods . . . 146
5 A3 _7 i. U3 m/ {% v3.8 Hydrolysis . . . . . . . . . . . . . . . . . . . . . . . 152
6 V' J1 r) v0 V6 x: N6 I# g3.9 Bibliography . . . . . . . . . . . . . . . . . . . . . 1555 q* {) A$ l; _8 P8 G4 l
3.9.1 Sampling and sample preparation 155- X( L; _5 p4 J& T% K6 w7 b
3.9.2 Solvents/solubility . . . . . . . . . . . . 155
- {: o. k+ c0 c: O7 v1 x' P: \3.9.3 Extraction methods . . . . . . . . . . . 156
5 V( Y" U+ b$ l* u2 F3.10 References . . . . . . . . . . . . . . . . . . . . . . . 156
2 Z/ Y# {' I! `9 L8 c5 r t& bvi Contents
; h3 @% x. p, f/ m+ i7 b1 nChapter 4 Separation Techniques . . . . . . 171' t/ r. }4 h# U b1 X5 e
4.1 Analytical detectors . . . . . . . . . . . . . . . . 177
# a; D8 K1 C( p- K4.2 Gas chromatography . . . . . . . . . . . . . . . 181
6 W, @4 {, K: t3 @. |3 k& o& @4.2.1 High-temperature gas3 U5 A3 C5 _+ l
chromatography . . . . . . . . . . . . . 200! _. w ?' s% l5 X2 q: }3 A
4.2.2 Headspace gas chromatography . . 202
' X& c% _$ s! Q4.3 Supercritical fluid chromatography . . . . . 205
7 \) z0 J# W1 z1 P4.4 Liquid chromatography techniques . . . . . 2170 K+ g( }4 C! J- k4 ?: n: x
4.4.1 Planar chromatographies . . . . . . . 218
/ g4 H# t9 z5 u( d4.4.2 Column chromatographies . . . . . . 230, A s2 C3 N- J' L) g5 P& A2 a' K
4.5 Capillary electrophoretic techniques . . . . 273
* Z5 P8 ]! W" B$ v7 N4.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 278
& P; w# B3 ?6 V1 E+ W7 o$ H4.6.1 General texts . . . . . . . . . . . . . . . 278
4 c) n* F* [% x2 K8 h, r/ A) P4.6.2 Detectors . . . . . . . . . . . . . . . . . . 279
0 O. n# O' T9 _4 r+ w" L4.6.3 Gas chromatography . . . . . . . . . . 279
1 W9 i4 u, ?) \9 @7 g3 e$ j @7 F7 R4.6.4 Supercritical fluid chromatography 279& l4 f7 O/ U) M4 w5 {, O! `: i5 U
4.6.5 Thin-layer chromatography . . . . . 279
9 S; ~/ E0 ? ^6 W4.6.6 Liquid chromatography . . . . . . . . 2808 s- p9 N9 d) z( [9 z3 k
4.6.7 Size-exclusion chromatography . . 280' y( D4 I& D3 E
4.6.8 Ion chromatography . . . . . . . . . . 280" j$ {! K& A( ~$ y. U( G
4.6.9 Capillary electrophoretic
6 G' y: B% ^$ s- E3 Ztechniques . . . . . . . . . . . . . . . . . 280: C- K8 M. v3 B
4.7 References . . . . . . . . . . . . . . . . . . . . . . . 281
, D8 A4 c* o4 ^! h& _; ^Chapter 5 Polymer/Additive Analysis:
( t6 a: x$ r% ?6 g6 XThe Spectroscopic Alternative 299. K8 d! M& c+ R4 M
5.1 Ultraviolet/visible spectrophotometry . . . 302
0 o1 b( T4 n$ _5.2 Infrared spectroscopy . . . . . . . . . . . . . . . 311+ u# c% W# E) ?
5.3 Luminescence spectroscopy . . . . . . . . . . 3189 ^5 R' N, i, X I C, V% Z" F
5.4 High-resolution nuclear magnetic* s$ h$ I; m. x) }2 ]& X* J, ^
resonance spectroscopy . . . . . . . . . . . . . 323
$ `1 {. p6 A; s0 a: _' i) q- h5.4.1 Multidimensional NMR3 e/ t8 ~0 v; X9 N' }7 @- q
spectroscopy . . . . . . . . . . . . . . . . 336+ k# \( Y6 T! _* Q6 @7 b
5.5 Bibliography . . . . . . . . . . . . . . . . . . . . . 3420 B; k) \! I# \' E1 a7 @& Q' X' |
5.5.1 General spectroscopy . . . . . . . . . 342
' W+ l( T- y) s& y/ G' J. I- }8 D5.5.2 Ultraviolet/visible$ t) d+ c( G4 a$ s: [- Q- u
spectrophotometry . . . . . . . . . . . . 342* S& v9 q1 D; H5 s
5.5.3 Infrared spectroscopy . . . . . . . . . 342
4 ]7 v0 h2 O1 K9 O9 `+ m7 a% c% c1 t5.5.4 Luminescence spectroscopy . . . . . 342
" C6 }3 e2 V- a4 V" ?, m/ u5.5.5 Nuclear magnetic resonance
" c8 F( L' V) A( E2 r: M1 W- _spectroscopy . . . . . . . . . . . . . . . . 3423 }8 _2 _2 ~ h) p6 U( K
5.6 References . . . . . . . . . . . . . . . . . . . . . . . 342
Q" X- t+ m, zChapter 6 Organic Mass-Spectrometric! p. G! y; `# O2 J8 m! O$ i4 J
Methods . . . . . . . . . . . . . . . . 349
% o) L5 W4 k1 m, C6.1 Basic instrumentation . . . . . . . . . . . . . . . 3510 S* l: U; `9 s$ g
6.1.1 Inlet systems . . . . . . . . . . . . . . . . 352 H' J; i0 U/ ]& y6 p9 z
6.1.2 Modes of detection . . . . . . . . . . . 353" R- U+ k% V4 @9 p- N [
6.1.3 Mass resolution . . . . . . . . . . . . . . 354
) ^* H9 C9 Q9 R X6.1.4 Isotope distributions . . . . . . . . . . 354
" l( I- K+ p( o) ]% l* J5 ?7 i$ L6.1.5 Accurate mass measurements. . . . 355$ U' E3 S# X* |' `" l9 a' V
6.2 Ion sources . . . . . . . . . . . . . . . . . . . . . . 3574 c" K P% F/ b% U! v) U
6.2.1 Electron impact ionisation . . . . . . 3603 b2 s9 Y% s T; {. b
6.2.2 Chemical ionisation . . . . . . . . . . . 3622 w. a, }0 I6 X$ t/ C
6.2.3 Metastable atom bombardment . . 3673 e7 b; i) Q0 D) u
6.2.4 Fast atom bombardment . . . . . . . 367
9 w- Y% W; ]# J7 }7 U6.2.5 Field ionisation . . . . . . . . . . . . . . 372
- q) e4 f5 ]7 R7 L( I# c6.2.6 Field desorption . . . . . . . . . . . . . 374
; I$ V/ E. M. c5 A6.2.7 Thermospray ionisation . . . . . . . . 3765 i8 C' M3 S, e1 j H4 ^+ ~) T, Y, @
6.2.8 Atmospheric pressure ionisation" ?& u* K1 f- L n2 h4 m
techniques . . . . . . . . . . . . . . . . . 378
' T% p+ C3 ^- \8 H' Q# R* m: J5 u1 b6.2.9 Desorption/ionisation methods . . . 383% g# Z5 F5 {6 ], [# G. t) S& `
6.2.10 Photoionisation techniques. . . . . . 3850 j3 A k$ R) n
6.3 Mass analysers . . . . . . . . . . . . . . . . . . . 386
6 @) H( \7 o& P, A" _, G6.3.1 Sector analysers . . . . . . . . . . . . . 387, p& k$ D O9 d6 @
6.3.2 Quadrupole mass spectrometers . . 389
( k+ p7 R' `- t& c6.3.3 Time-of-flight mass spectrometry . 390* v5 S; S& y2 Y( i
6.3.4 Quadrupole ion trap . . . . . . . . . . 393
^- u* N6 V: {! V2 f0 z# ]' r6.3.5 Fourier-transform ion-cyclotron
/ h" r% q$ K+ J* @+ X* Cresonance mass spectrometry . . . . 3950 q( y. D: F/ q7 I2 K8 f6 `
6.3.6 Tandem mass spectrometry . . . . . 3980 ]) c4 q4 N3 B5 V6 P
6.4 Direct mass-spectrometric polymer
/ R; K* P/ R0 [; ^6 |# m2 r' F! wcompound analysis . . . . . . . . . . . . . . . . . 407
; r6 L9 s( r% I; C: S2 B6.5 Ion mobility spectrometry . . . . . . . . . . . 415
+ i3 x. S( n: C6 K* F. E( @$ L6.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 417
+ O) S2 j! R: |$ j3 b6.6.1 Mass spectrometry (General) . . . . 417 s" c8 R+ [2 M
6.6.2 Mass spectrometers . . . . . . . . . . . 417
: D; K, Q( t# t$ T6.6.3 Ionisation modes . . . . . . . . . . . . . 417
1 o, W5 Y5 }7 N! u: B* L2 |6.7 References . . . . . . . . . . . . . . . . . . . . . . . 4180 C* R4 O4 w$ M" D f! L9 @3 q0 C) ?
Chapter 7 Multihyphenation and! G3 [4 u* A+ a1 N- p' e% b4 ]9 w
Multidimensionality in
1 L" K' ?# A4 x1 s; nPolymer/Additive Analysis . . . 425
$ a3 G* h! A' M$ m$ T) q" g7.1 Precolumn hyphenation . . . . . . . . . . . . . 428
6 K, L) J# A, a# l7.1.1 Chromatographic sampling
* B- S! t0 Q+ M5 l' umethods . . . . . . . . . . . . . . . . . . . 432
, h0 I! G/ o# {7.2 Coupled sample( m* \ Z3 N) _& T
preparation – spectroscopy/spectrometry . 4498 @: ?% T# u# I! F
7.3 Postcolumn hyphenation . . . . . . . . . . . . . 452+ A$ _3 E; X# {2 i+ s
7.3.1 (Multi)hyphenated GC techniques 456! Q( E3 C' e8 @
7.3.2 (Multi)hyphenated SFC4 R! ?* ]" a0 B L& f: e5 C
techniques . . . . . . . . . . . . . . . . . 475
7 C% w3 l* ?/ S m7.3.3 (Multi)hyphenated HPLC4 Z: c- g" E" V) _2 j- D! `
techniques . . . . . . . . . . . . . . . . . 489! x: d/ y; o0 O
7.3.4 Hyphenated SEC techniques . . . . 527
[$ @) E9 G1 p6 B$ c/ r1 ~7.3.5 Hyphenated TLC techniques . . . . 530& t/ B/ @1 T- t2 Z1 y
7.3.6 Hyphenated CE techniques . . . . . 5436 f4 }7 H( e, J/ h
Contents vii6 \& d) `7 n+ {$ {& H z1 Z
7.4 Multidimensional chromatography . . . . . 545
6 a! e. v: p w. I7.4.1 Multidimensional gas
! V$ q, c; l! `) c2 S% c( G) z6 U. fchromatography . . . . . . . . . . . . . 5484 j6 A _. X& b0 L, _' A
7.4.2 Multidimensional supercritical5 p* e# f5 P o" I0 R6 ?
fluid chromatography . . . . . . . . . 550
N) w+ d6 Z4 U; t0 V; E; U7.4.3 Multidimensional liquid$ }; t( I& | t3 X' _4 ]9 k: i5 o
chromatography . . . . . . . . . . . . . 550
3 }6 v; N: h. u4 ?0 V& T7.4.4 Multidimensional thin-layer
+ I' m/ u* Y q9 ?' U: Bchromatography . . . . . . . . . . . . . 558
u( I6 t, ~0 ?9 i0 F) R. e7.5 Multidimensional spectroscopy . . . . . . . . 5602 x6 H* w% C* e: R+ Z
7.6 Bibliography . . . . . . . . . . . . . . . . . . . . . 562& P/ n. U7 q) p; O. O
7.6.1 General . . . . . . . . . . . . . . . . . . . 562
1 S5 h& T0 }' e1 W7.6.2 Multihyphenation and8 z9 t5 T4 R% ~$ L3 Z" R
multidimensionality . . . . . . . . . . . 563
' y9 r8 j- L1 s0 w- n0 R7.6.3 Precolumn hyphenation . . . . . . . . 563
0 F% x" |9 I( ]0 e$ q) D7.6.4 Postcolumn hyphenation . . . . . . . 563. e8 _' }- z; K2 g& |' p) \/ j- Q/ D
7.6.5 Multidimensional chromatography 563
$ B$ e% y4 a: {; f O+ D1 a- P' [7.6.6 Multidimensional spectroscopy . . 563
) i+ m) r" `; a/ G+ @2 M) N7.7 References 564
5 a) V- g" u; T7 }3 y1 P1 MChapter 8 Inorganic and Element# |% Q6 p" B" z0 m) l5 R0 E3 a1 U, i
Analytical Methods . . . . . . . . 585' L& g! X4 O6 ~% B- i; e8 U. f
8.1 Element analytical protocols . . . . . . . . . . 587
& C+ g5 @3 ?9 h# c ~8.1.1 Element analytical pretreatment/ B1 J. P! L, ^" y+ d+ t8 v* V
protocols . . . . . . . . . . . . . . . . . . 5880 ~1 ?+ s, p! z4 p% O
8.1.2 Elemental analysis methods . . . . . 589
$ p9 m/ c, Y8 a6 s: D: { p8.2 Sample destruction for classical elemental# {0 d( F, H, _4 \
analysis . . . . . . . . . . . . . . . . . . . . . . . . . 5919 r) z8 k: m6 F/ j$ E$ V
8.2.1 Combustion analysis . . . . . . . . . . 5938 C2 }! Q. o( r# T5 D/ @
8.2.2 Wet matrix digestion . . . . . . . . . . 597/ Y* s( o" V2 m( X9 }
8.2.3 Fusion methods . . . . . . . . . . . . . . 604
# ?! q; Y; R }8.3 Analytical atomic spectrometry . . . . . . . . 6051 a$ x( t2 I) O
8.3.1 Atomic absorption spectrometry . 6082 G6 D8 t* R) F' S6 I Z0 W
8.3.2 Atomic emission spectrometry . . . 613
( e1 A3 ?8 ]* m# m# {* C0 q: E8.3.3 Atomic fluorescence spectrometry 624 |
|
[复制链接]
发表于 2007-9-14 08:35:42
