VII

Table of Contents
Part 1. Introduction and General Considerations 1. Preparatory Information 1.1. 1.2. 1.3. 1.4. 1.5. 1.6. 1.7. 1.8. 1.9. 1.10. 1.11. 1.12. Overview of a Chemical Analysis 3 Types of Operations Used in Sample Preparation 10 Some Theoretical Aspects of Phase Transfers 16 Introductory Approach to Theory of Distribution Equilibria 24 Some Aspects of Mass Transfer Processes 33 Characterization of Chromatographic Separations 43 General Characteristics of Separations 61 Elementary Discussion on Thermodynamic and Kinetic Factors in Chemical Reactions 66 Brief Survey on Molecular Interactions 69 Empirical and Estimated Parameters for Sample Preparation Problems... 77 Introductory Discussion on Precision, Accuracy, Sensitivity, and Limit of Detection in Chemical Analysis 94 Validation of an Analytical Method 107 References 1 108

2.

Sampling and Its Connection with Sample Preparation 2.1. 2.2. 2.3. 2.4. Relation of Sampling to Sample Preparation Representative Samples Techniques for Sample Collection Handling, Preservation, and Storage of Samples References 2 113 114 118 130 132

3.

Overview on Sample Preparation for Chromatography 3.1. 3.2. 3.3. 3.4. 3.5. 3.6. 3.7. 3.8. 3.9. The Role of Sample Preparation The Use of Preliminary Information for the Choice of a Sample Preparation Procedure Sample Homogenization and Dissolution Sample Cleanup, Fractionation, and Concentration Chemical Modifications of the Sample Other Types of Sample Modifications Differences in Sample Preparation for Different Chromatographic Techniques Quantitation Techniques in Chromatography and Their Relation to Sample Preparation Method Development in Sample Preparation References 3 137 141 146 147 152 153 154 156 159 163

viii

Table of Contents
4. Chromatography as the Core Step in an Analytical Process 4.1. 4.2. 4.3. 4.4. The Choice of the Core Analytical Technique Gas Chromatography as a Core Step in the Analytical Process Conventional High Performance Liquid Chromatography as a Core Analytical Technique Other Chromatography Types Used as a Core Analytical Technique References 4 165 169 182 201 209

5. Data Processing in Chromatographic Methods 5.1. 5.2. Information Gain from Chromatographic Data Qualitative and Quantitative Data from the Chromatographic Process References 5 213 214 218

6.

Automation in Sample Preparation 6.1. 6.2. Automation in the Instrumentation Used in Sample Preparation Computer Assisted Method Development References 6 219 221 221

Part 2. Sample Preparation Techniques Using Physical Processes 7. Mechanical Processing in Sample Preparation 7.1. 7.2. 7.3. 8 Grinding, Sieving, and Blending Filtration, Microfiltration, and Ultrafiltration Centrifugation References 7 225 238 241

Phase Transfer Separations Applied in Sample Preparations 8.1. 8.2. Distillation, Vaporization, and Drying Dissolution, Crystallization, and Precipitation References 8 243 255 265

9.

Headspace Sampling Techniques in Gas Chromatography 9.1. 9.2. 9.3. Static Headspace Techniques Dynamic Headspace Other Headspace Techniques References 9 267 272 283 285

ix

Table of Contents
10. Solvent Extraction 10.1. 10.2. 10.3. 10.4. 10.5. 10.6. Liquid-Liquid Extraction Conventional Liquid-Solid Extraction Accelerated Solvent Extraction Microwave-Assisted Solvent Extraction Simultaneous Distillation and Extraction Supercritical Solvent Extraction References 10 287 304 310 314 317 322 334

11. Sorbent Extraction 11.1. 11.2. 11.3. 11.4. Solid Phase Extraction Procedures Solid Phase Microextraction Matrix Solid Phase Dispersion Other Solid Phase Sample Preparation Techniques References 11 341 373 394 396 399

12. Chromatographic Procedures as Preliminary Separation 12.1. 12.2. 12.3. Gas Chromatography as a Sample Preparation Technique and Bidimensional GC Liquid Chromatography as a Sample Preparation Technique Size Exclusion Used in Sample Preparation References 12

403 408 415 420

13. Membrane Separations 13.1. 13.2. Gas Diffusion through Membranes and Stripping Reverse Osmosis and Dialysis References 13 423 425 431

14. Electroseparation Techniques in Sample Preparation 14.1. 14.2. Electrophoretic Techniques Other Electroseparation Techniques References 14 433 440 441

15. Other Separation Techniques in Sample Preparation 15.1. 15.2. Ion Exchange in Sample Preparation Other Techniques in Sample Preparation References 15 443 459 460

Table of Contents
Part 3. Sample Preparation Techniques Involving Chemical Modifications 16. Chemical Modifications for Dissolution and Fractionation 16.1. 16.2. Chemical Modifications for Sample Dissolution 463 Changes in pH and Chemical Modifications for Fractionation Purposes... 466 References 16 470

17. Purpose of Derivatization in Chromatographic Analysis 17.1. 17.2. 17.3. 17.4. 17.5. 17.6. 17.7. General Aspects Regarding Derivatization Preparation of the Sample for Derivatization and Common Derivatization Labware Derivatization for Improving Gas Chromatographic Process Derivatization for Improving Detection in GC Derivatization for Improving Mass Spectral Identification Derivatization for Improving Detection in HPLC and TLC Derivatization for Chiral Separations References 17 473 476 478 486 493 502 514 523

18. Chemical Reactions Used in Derivatization 18.1. 18.2. 18.3. 18.4. 18.5. 18.6. 18.7. 18.8. Reactions with Formation of Alkyl or Aryl Derivatives Silylation Reactions Acylation Reactions Reactions of Addition to Carbon-Heteroatom Multiple Bonds Used for Derivatization Derivatization Reactions with Formation of Cyclic Compounds Other Derivatization Reactions Derivatization Reactions Involving Solid Phase Reagents Derivatization on a Solid Support References 18 525 545 569 581 591 .613 623 629 631

19. Derivatization Reactions for Analytes with Various Functional Groups 19.1. 19.2. 19.3. 19.4. 19.5. 19.6. 19.7. 19.8. Derivatization of Compounds with Alcohols, Epoxide, or Ether Groups.... 639 Derivatization Reactions for Phenols 669 Derivatization Reactions for Thiols and Sulfides 675 Derivatization of Compounds with Amino and Other Nitrogen-Containing Groups 683 Derivatization of Aldehydes and Ketones 724 Derivatization of Carboxylic Acids 739 Derivatization of Amides, Esters, and Other Derivatives of Carboxylic Acids, and of Carbonic Acid 761 Derivatization of Other Types of Organic Groups and of Organometallic and Inorganic Compounds 776

XI

Table of Contents
19.9. Derivatization of Carbohydrates 19.10. Derivatization of Amino Acids and Related Compounds 19.11. Derivatization of Other Multifunctional Compounds References 19 20. Chemical Degradation of Polymers and Pyrolysis 20.1. 20.2. 20.3. 20.4. 20.5. 20.6. 20.7. Chemical Degradation of Polymeric Carbohydrates Chemical Degradation of Proteins for Analytical Purposes Chemical Degradation of other Macromolecular Compounds Overview of Analytical Pyrolysis Pyrolysis as a Chemical Modification Technique Instrumentation Used in Analytical Pyrolysis Application of Analytical Pyrolysis References 20 847 859 864 869 877 895 901 913 919 923 788 798 814 823

Symbols, Units, and Constants Index

923

INDEX

azeotropic distillation absolute capacity factor absolute retention time accuracy acid digestion acidity constants activation energy activity coefficient acyi halides adaptability to analyte volatility addition to a double bond adsorption constant AED (atomic emission detector) affinity sorbents Ag/AgCt electrode alcohols ALD (aroyl-luminescence detector) aldehydes Allyl-TMS (altyltrimethylsilane) alumina amides 45 44 95,98 464 540, 684, 739, 799 69 22 761 62 613 30 180, 486 357 196 639 180 724 546 276 761 azides azines azoles

247 761 604 600

B
B.E.T. isotherms basicity constants BASTFA (N.Obis(allyldimethylsilyl)tnfluoro-acetamide) batch extraction batch sample processing BDSA(bis(dimethylsilyl)acetamide) bidimensional GC bile acids binomial experiment blank sample blending boiling point bond energies bond energies for Si-X BOP (benzotriazol-1-yl-oxytris(dimethylamino)-phosphonium hexafluorophosphate) bottom (in distillation) breakthrough volume Vb BSA (N,0-bis(trimethylsilyl)-acetamide) BSB(N,0-bis(trimethylsilyl)-benzamide) BSC (N,0-bis(thmethylsilyl)-carbamate) BSF(N,N-bis(trimethylsilyl)formamide) BSS (bis(trimethylsilyl)sulfate) BSTFA (N,0-bis(trimethylsilyl)trifluoroacetamide) BSU(N,N'-bis(trimethylsilyl)urea) buffer solutions bulk chromatographic phases 31 684 554 287 219 555 113 667 117 159 225 80 872 561 520

amines amino acids amino alcohols amino phenols amino sugars analysis of volatiles analytes anhydrides APCI (atmospheric pressure ionization) aromatic ring substitutions Arrhenius reaction rate equation artifact formation in trimethytsilylation reactions artifacts in acylation artifacts in alkylation artifacts in distillation artifacts in liquid solid extraction artifacts in dynamic headspace ASE (accelerated solvent extraction) average azeotropic composition

683 710, 798 815 815 792 267 3 761 166, 199 620 69 564 580 541 247 256,265 272 310 95 22

244 276, 278, 343 546 546 546 547 547 547 547 466 178

C
C8 (silica base octyl sorbent) C18 (silica base octadecyl sorbent) X2 distribution CA (cellulose acetate) calibration standard capacity factor carbamates or urethanes 185 93, 185 98 233 156 28,48 772

924
661, 735, 788 579 582, 724 177 739 534 534 9 554 crystallization cumulative frequency distribution cyclic boronates cyclic phosphothionates cyclic siliconides cyclopropane containing carboxylic acids 263 96 610 610 606 759

Index

carbohydrates carbonyl azides in derivatization carbonyl compounds carborane stationary phase in GC carboxylic acids CCBBT(6-chloro-1-pchlorobenzensulfonyloxybenzotriazole) CD! (N.N'-carbodiimidazole) CE (capillary electrophoresis) CEDMSDEA (2cyanoethyldimethyl(diethyl)aminosilane) chain scission in pyrolysis charcoal sorbents charge transfer interactions chelating resins chemical potential chemiluminescencedetection in HPLC chemilumjnescence efficiency chirai chromatographic columns chiral reagents chirality

D
Dalton's law DCCI (dicydohexylcarbodiimide) 19 534 124 266 477 254 103 107 6 427 514 530 531 776 66 41,80 127 178,376 658 71 789 72 872 256 25 378 43 46 761 555 548 526 556 666 525

denuder tube 882 deproteinization 276 74 derivatization labware desiccants 455 14 detection limit determination limit 195,510 Dialog Corp. 195 519 dialysis _ diastereoisomers 520 Diazald (N-nitroso-N-methyl-p514 toluenesulfonamide) chloroformates 577 diazomethane generator dienes 157 chromatographic standard differential migrating processes chromatographic stationary phases (GC) 178 diffusion coefficient CI+ (positive ions chemical ionization) 217 Clausius-Clapeyron equation diffusive sampler 18,89, 252 closed-loop stripping 284 dimethyl polysiloxane diois CMDMCS 554 ((chloromethyl)dimethylchlorosilane) dipole-dipole interactions CMTMDS (1,3-bis(chloromethyl)-1,1,3,3- 554 tetramethyldisilazane) colloid solutions 263, 238 disaccharides concentration polarization 230, 427 dispersion interactions dissociation energies concentration process 148 dissolution concurrent sequential sample processingI 219 distribution constant conformers 516 distribution equilibrium in SPME continuous extraction 291 distribution process in gas convenience sampling 115 chromatography distribution process in HPLC core analytical process (step) 3,8 dithionic acid esters countercurrent separations 65 DMCS (dimethyldichlorosilane) countercurrent-with-reflux separations 66 DMCTMS (trimethylsilyl N,Ncritical point 18 dimethylcarbamate) 18,324 critical temperature DMF (dimethylformamide) DMIPCS (isopropyldimethylchlorosilane) crosscurrent processes 65 DMMCS (dimethylmonochlorosilane) 527 cryptands DMSO (dimethylsulfoxide) 177 cyanopropyl polysiloxane

Index

925

DNA (deoxyribonucleic acid) DNA sequencing dry ashing dry weight basis drying dynamic gas sampling dynamic headspace dynamic separations

821, 866 867 464 253 253,279 121 272 65

F
F distribution FAB (fast atom bombardment) Fick's first law Fick's second law FID (flame ionization detector) filter materials filter properties filtration finite interaction first law of thermodynamics first order reaction rate FLOROX (O-(pentafluorobenzyl)hydroxylarnine hydrochloride) fluorescence detection in HPLC fluorescence efficiency Florisii FPD (flame photometry detector) fraction of moles in the mobile phase fractional distillation fractionation fractionation capacity frequency factor FTIR (Fourier transform IR) 98 200 33 34 166,180, 486 231 229 226 77 14 68 586 193, 506 194 277 180 44 246 148 61 69 181

EA (electron affinities) EA (electron affinity) ECD (electron capture detector) EDAC (1 -(3-dimethyiaminopropyl)-3ethylcarbodiimide) Edman degradation effective plate number El+Jpqsitive ions electron ionization) electrochemical detection in HPLC electrochromatography electrode potential electrodialysis electrophoretic mobility ELSD (evaporative light-scattering detector) elutropic strength Emerson reaction emulsion formation enantiomers enrichment factor EPA (United States Environmental Protection Agency) epoxides equilibrium constant error-function error-function complement ES (electrospray) esters of carbonic acids estimation of distribution constants estimation of solubility ethers ETSA (ethyl trimethylsilylacetate) extensive variables external calibration standard external information extraction of ionic species extrathermodynamic estimations

489 488 180,492 535 862 51 217 195,512 209 196 440 435 200 48, 189 673 298 514 149 133 668 67, 451 37 37 166, 199 761 88,90 85 669 547 17 156 141 289 81

G
gamma function gas-liquid equilibrium gas-liquid partition gas-solid adsorption Gaussian bell curve GC (gas chromatography) GC columns GC injection techniques GC oven GC detectors GC-GC (bidimensional GC) Gibbs phase rule GIME (gas injection membrane extraction) glycosidic linkage GPC (gel permeation chromatography) gradient elution gradient temperature GC grinding guanidines 37 19 27 29 35 8 174, 177 171 173 179 403 17 424 855 202,416 57 58 225 773

926
166 half wave potential Hall (electrolytic conductivity detector) HCB (hexachlorobenzene) headspace height equivalent to a theoretical plate Henry's constant Henry's law heterocyclic amines HFBA (heptafluorobutyric anhydride) HID (helium ionization detector) HMDS (hexamethyldisilazane) HMDSO (hexamethyldisiloxane) Hofmann degradation homogenization HPLC (high performance liquid chromatography) HPLC columns hydrazides hydrazines hydrogen bond hydrolysis hydroxamic acids hydroxy acids hydroxylamines 197 180 321 267 51 90, 378 27 718 492, 572 180 547 547 622 146 182 185 769 722 74 619 771 816 723 keto acids ketones KovSts retention index Kuderna Danish (KD) evaporative concentrator IRD (infrared detector) ISO International Standardization Organization isocyanates isocyanates in derivatization isoelectric focusing isokinetic sampling isolated (closed) system isotachophoresis isothermal GC isothiocyanates in derivatization isotope labeling IUPAC (International Union of Pure and Applied Chemistry) 180 107

Index

776 579, 587 171 122 66 169 58 579, 587

498 4o

K
816 724 60, 176 252

L
Langmuir adsorption isotherm large volume sample introduction system LC (liquid chromatography) LC-GC (liquid chromatography-gas chromatography) LC-LC (liquid chromatography-liquid chromatography) least-squares fitting Lenard-Jones equation LIF (laser induced fluorescence) lignin limiting current intensity linearity of response lipids liquid membranes liquid sample collection liquid-liquid partition liquid-liquid partition of compounds simultaneously in ionic and nonionic form liquid-liquid partition of ion pairs liquid-solid equilibrium LLE (liquid-liquid extraction) load capacity LSE (liquid-solid extraction) LTPRI index lyophilization (freeze-drying)

30 171 182 412 409 100 73 194 865 199 102, 108 773 430 128 24 32 31 23 287 62 304 60 255

1 IC (ion chromatography) ICP (inductively coupled plasma) imino ethers immunoaffinity chromatography Immunoelectrophoresis indoles informational entropy inorganic compounds instrumentation in pyrolysis intensive variables internal standard ion exchange capacity ion exchange resins ion exchange SPE sorbents ion pair chromatography ionic strength intermolecular forces IPOTMS ((isopropenyloxy)trimethyl125,202 200 761 207 439 715 213 782 895 17 157 448 443 357 204 429 71 547

silane

Index

927

M
MAE (microwave assisted extraction) mass transfer by diffusion mass transfer by diffusion and convection matrix MBTFA (2,2,2-trifluoro-N-methyl-N(2,2,2-trifluoroacetyl)acetamide) MCE (mixed cellulose esters) McReynolds constant mean 315 33 39 3 574 233 176,485 95

nttriles nitrogen chemiluminescent detector NMR (nuclear magnetic resonance) non-Gaussian peaks nonaromatic cycle formation nonelectrolytes nonpolar SPE sorbents normal distribution NPD (nitrogen phosphorus detector) neuraminic acid nucleation nucleosides nucleotides number of peaks separated in a chromatogram NYL (nylon)

761 180 200 54 591 256 352 96 166, 180, 487 792 263 821 821 61 233

mean of the population 95 membrane materials 231 membrane properties 229 MESI (membrane extraction with sorbent 424 interface) 4 method Methyl-8 (N,N-dimethylformamide dimethyl acetal) microti Itration MIMS (membrane introduction mass spectrometry) MMTSP (1-methoxy-2-methyl-1trimethylsiloxypropene) modifiers in SFE moisture removal in SPE molar volume mole fraction molecular distillation molecular imprinted sorbents monosaccharides MOPAC (molecular orbital calculation package) moving boundary electrophoresis MS (mass spectroscopy or spectrometry) MSA (N-methyl-N-trimethylsilylacetamide) MSD (mass selective detector) MSDP (matrix solid phase dispersion) MSHFBA (N-methyl-Ntrimethylsilylheptafluorobutyr-amide) MSTFA (N-methyl-N-trimethylsilyltrifluoroacetamide) MTBSTFA (N-methyl-N-(tertbutyldimethylsilyl)-trifluoroacetamide) 532 226 424 547 327 358 26, 259 17 251 358 789 479,559 437 487,514 548 180 394 548 548 554

O
octanol/water partition coefficients ODS columns (octadecyl silica) on-line instrumentation OPA (o-phthalaldehyde) operational aspects of separations organometallic compounds OTT (open tubular trapping) overpotential oxidations and reductions oximes 81 185 220 597 64 782 398 198 615 723

P
PAH (polycyclic aromatic hydrocarbons) parachor parameters for solvent characterization partition coefficient PB (particle beam) PBM (probability based matching of mass spectra) PCB (polychlorinated biphenyls) 372 80 87 25 200,513 494 308 177,395 49 61 55

N
NCI (negative chemical ionization) Nernst equation NH2 sorbent (column) NHE (standard hydrogen electrode) 490 197 349 196

PDMS (polydimethylsiloxane) peak broadening peak capacity peak separation

928
peak width PEEK (polyetheretherketone) peptide bond formation peptides performance of SPE phases peracids permeate PES (polyethersutfone) PFPA (pentafluoropropionic anhydride) pH modification phase phase ratio phenols phosphate esters phosphonates PID (phototonization detector) Pirkle chiral chromatographic columns plate height polar SPE sorbents polarity parameter P' polarizability polymeric carbohydrates polyols population porous polymers precipitation precision prostaglandins proteins PS-DVB-EVB (polystyrenedivinylbenzne/ethylvinylbenzene) PS-DVB-NVP (polystyrenedivinylbenzne/N-vinytpyrrolidone) PTFE (potytretrafluoroethylene, teflon) PTV (programmed temperature vaporizer) purge and trap (P&T) purpose of analysis PVDF (polyvinylidene fluoride) pyridine pyrolytic elimination pyrolysis in the presence of reactants pyrolysis with derivatization pyrolysis of natural organic polymers pyrolysis of small molecules pyrolysis of synthetic polymers pyrroles 50 184 573 813, 861 351 761 235 233 492, 572 466, 476 12 46 669 778 778 166, 200 519 52 354 86 72,479 797, 847 658 95 270, 278 265 95, 101 818 813, 859 350 350 126 58,171 273 142 233 721 879 888 898 901 912 905 715 salting out sample sample capacity sample cleanup sample collection saturated solution SAX columns (strong anion exchange) SBSE (stir bar sorptive extraction) SCE (saturated calomel electrode) SCX columns (strong cation exchange) SDE (simultaneous distillation and extraction)

Index

Q
quantitation limit quaternary ammonium compounds 107 721

R
random error random sampling Raoult's (aw RCF (relative centrifugal force) reaction rate recovery reduced parameters refractive index rejection characteristic of membranes relative frequency of occurrence of random errors relative humidity repeatability representative samples representativeness of sampling reproducibility resolution response factor retention index in gas chromatography retention time retention volume reverse osmosis
Rf

94 113 15,21 238 68 108, 149 324 80, 191 230 96 253 108 114 115 108 56, 437 159 60 44 44 226,425 48 131 821,866 108 108

RH (relative humidity) RNA (ribonucleic acid) robustness ruggedness

S
260, 275, 297 95 57 147 118 256 185 396 196 185 318

Index

929

SDS-PAGE (sodium dodecyl sulfate polyacrylamide gels electrophoresis) SDVB (styrene-divinylbenzene, polymer) SEC (size exclusion chromatography) sensitivity separation factor

438

standard addition in quantitation standard deviation standard electrochemical potential standard error static and trapped headspace (S&THS) static gas sampling static separations steam distillation steam distillation and extraction stereoisomers steroids derivatization STOX (hydroxylamine hydrochloride) stratified sampling Student function sublimation substituted amides sugar acids sugar phosphates sulfates sulfides sulfonic acids sulfonyt derivatives sulfur chemiluminescence detector supersaturation syn-anti isomers systematic errors systematic sampling

158 95 196 96 284 121 65 248 318 514 665,818 586 114 97 264 761 792 792 780 675 780 578 180 262 514 94 114

93 201, 416 102 21, 29, 55 , 289 sequential sample processing 219 SFC (supercritical fluid chromatography) 208 323 SFE (supercritical fluid or solvent extraction) short path thermal desorption 284 side group reactions is pyrolysis 886 sieving 225 105 signal to noise ratio S/N 346 silica base sorbents 277 silica gel 181 SIM (single ion monitoring) 65 single contact separations SN1 mechanism 540 540, 560 SN2 mechanism solid sample collection 129 85,256 solubility solubility parameter 26, 259 solubility product 261 427 solute loss in reverse osmosis 86, 260, solvent polarity 298, 363 86, 298, solvent properties 363,476 188 solvent solubility in water 139 solvent-free sample preparation 852 solvolysis solvophobic interactions 75 Soxhlet extraction Soxtec extractor SPE (solid phase extraction) SPE accessories (formats) SPE fibers specific rotation specificity/selectivity SPME (solid phase microextraction) spray and trap stability static headspace (SHS) 307 309 153, 341 365 377 517 108 271, 374, 899 284 108, 260 267

T
98 t-test TBDMCS(tert-butyldimethylchlorosilane) 554 554 TBDMS triflate (tert-butyldimethylsilyl trifluoromethanesulfonate) TBDMSacac(4-tert-butyldimethylsiloxy-3 - 5 5 4 penten-2-one) 554 TBDMSI (1-(terfbutyldimethylsilyl)imidazole) TBDPCS (terf-butyldiphenyichlorosilane) 554 168, 178. TCD (thermal conductivity detector) 486 322 TCDD (tetrachlorodibenzo-p-dioxin) TCEP (1,2,3-tris(2-cyanoethoxy)propane;) 176 270 teabag headspace 4 technique

930

Index

techniques for gas collection TFAA (trifluqroacetic anhydride) theoretical plate height theoretical plate number thermochemolysis thermodynamic distribution constant tertiary amines THF (tetrahydrofuran) thiocyanates thiohydantoins thiols THT (total heating time) tie line (in distillation) TLC (thin layer chromatography)

120 492,572 53 51 890 24 721 476 761 812 675 869 244 207

ureas UV-Vis (ultraviolet-visible)

761 191,504

V
vacuum distillation validation van Deemter equation van der Waals forces vapor-liquid equilibrium vaporization viscosity VOC (volatile organic compounds) 247 107 53 70, 480 19 251 41,228 119,267

Z
zeolites zeta potential 277 166

TMAAc (tetramethylammonium acetate) 536 TMAH (tetramethylammonium hydroxide]) 536 547 TMBS (bromotrimethylsilane) 547 TMCS (chlorotrimethylsilane) TMDS (1,1,3,3-tertamethyldisilazane) 555 547 TMIS (iodotrimethylsilane) I M S (trimethyisilyl) 545 548 TMSA (N-trimethylsilylacetamide) TMSacac((4-trimethylsiloxy-3-pentene-2 - 5 4 8 one or (trimethyisilyl enol of acetylacetone)) 548 TMSCN (trimethyisilyl cyanide) TMSDEA(N,N-diethyl-N-trimethylsilyl547 amine) 547 TMSDMA (N.N-dimethyl-Ntrimethylsilylamine) TMSI (TMSIM) (N-trimethylsilylimidazole) 549 TMSO (3-trimethylsilyl-2-oxazolidinone) 549 TMSPI (N-trimethylsilylpiperidine) 549 TMSTCA (trimethyisilyl trichloroacetate) 549 TMSTF (TMS triflate) (trimethyisilyl 549 trifluoromethanesulfonate) (triflate) 554 TMTBS-CI (cyclotetramethylene-terfbutylchlorosilane) 536 TMTFTH (trimethyttrifluoro-m-tolyl ammonium hydroxide) 556 TPDMDS (1,3-dimethyH, 1,3,3tetraphenyldisifazane) TPSA (triphenylsilylamine) 556 transesterifi cation 537 TRT (temperature rise time) 869 TS (thermospray) 166,200, 513 TsOH (toluenesulfonic acid) 663

ultrafiltration unsaturated acids

226 759