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  • 1990-1994  (14,714)
  • 1980-1984  (9,546)
  • Analytical Chemistry and Spectroscopy  (11,781)
  • General Chemistry  (10,763)
  • Physical Chemistry  (1,714)
  • Nuclear reactions
Material
Years
Year
Keywords
  • 201
    ISSN: 0935-6304
    Keywords: Enantioselective gas chromatography ; Cyclodextrin derivatives ; Polychlorinated pesticides ; Polychlorinated biphenyls (PCBs) ; Pyrethroid insecticides/Allethrin ; Organophosphorus pesticides/Acephate, Malaoxon ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The enantiomers of the polychlorinated polycyclic xenobiotics heptachlor, cis- and trans-chlordane, cis- and trans-heptachlorepoxide, oxychlordane, and bromocyclen have been resolved by gas chromatography with selectively substituted cyclodextrins. The order of elution of these compounds and of α-hexachlorocyclohexane (α-HCH) was determined by comparison with enantiomerically enriched reference compounds obtained by preparative enantioselective gas chromatography.A separation of the eight stereoisomers of the pyrethroid insecticide allethrin into seven peaks was achieved. Both trans-diastereomers were separated into their enantiomers and the order of elution could be determined by comparison with commercially available (S)-bioallethrin and trans-bioallethrin. Also one cis-diastereomer was separated, wheras the other cis-isomer could not be resolved. In addition 15 out of 19 stable atropisomeric polychlorinated biphenyls with 5, 6 and 7 chlorine substituents, some chiral organophosphorus pesticides, including acephate and malaoxon and the herbicide bromoacil were separated.
    Additional Material: 10 Ill.
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  • 202
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 713-718 
    ISSN: 0935-6304
    Keywords: Electrophoretic capillary chromatography ; Organic modifiers ; Hydrophobic association ; Capacity factors ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Very good separations of non-ionic organic compounds have been achieved by capillary zone electrophoresis (CZE) using a tetrahep-tylammonium salt as an additive in aqueous acetonitrile as solvent. A systematic study was undertaken to determine the effect of experimental parameters on electroosmotic mobility and electro-phoretic mobility. It was found that pH, acetonitrile concentration, and the type and concentration of quaternary ammonium salt are important experimental variables. Under appropriate conditions, the separation window was enlarged and a broad range of electrically neutral organics, including very hydrophobic compounds (e. g. poly-cyclic aromatic hydrocarbons) and fairly hydrophilic compounds were separated in a relatively short time. By adjusting the separation conditions, high resolution CZE of a specific group of neutral organic compounds could be achieved. A method for calculation of capacity factor was proposed and capacity factors for a variety of non-lonic organic compounds were calculated.
    Additional Material: 10 Ill.
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  • 203
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 729-731 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Electrospray mass spectrometry ; Sample concentration ; Peptides ; Drug metabolites ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
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  • 204
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 739-740 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 205
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 740-740 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 206
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 745-748 
    ISSN: 0935-6304
    Keywords: Organomercury compounds ; Capillary GC ; Atomic fluorescence detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Analysis of methyl- and ethylmercury (MM and EM) halides in biological and environmental samples is generally performed by gas chromatography with electron capture detection. Tedious sample work-up protocols and poor chromatographic response (using packed columns) have, however, shown the need for the development of new methods in this field.This paper reports a sensitive method, free from these deficiencies, for the determination of methyl- and ethylmercury. The organomercury compounds (MM and EM) are first released from the sample matrix, by the combined action of acidic potassium bromide and cupric ions, and then extracted into dichloromethane. The initial extracts are subjected to thiosulfate clean-up and the organomercury species are isolated as their chloride derivatives by addition of cupric chloride, and subsequent extraction into a small volume of organic solvent. Capillary GC coupled with atomic fluorescence detection provided excellent separation efficiencies for methyl- and ethylmercury and proved to be a very selective and sensitive technique. The absolute detection limit for both MM and EM was found to be 0.2 pg.
    Additional Material: 2 Ill.
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  • 207
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 120-120 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 208
    ISSN: 0935-6304
    Keywords: Two dimensional GC ; Heart cutting ; Retention index monitoring (RIM) ; Two-stage RIM ; GC-MS ; Selected ion monitoring ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two-stage capillary GC with two-stage retention index monitoring is an efficient analytical technique which can be used for detection and determination of small amounts of volatile compounds in complex mixtures of hundreds or thousands of other compounds. The system employs two capillary columns, coated with different stationary phases, connected on-line with the aid of a micro valve; the first column acts as a pre-separating unit from which unresolved fractions of interest are cut (transferred) into another column for final, interference-free separation of the compounds to be determined. This technique has been compared with selected ion monitoring capillary GC-MS using a hydrocarbon mixture as a test sample for comparing resolution, repeatability, and the practical usefulness of the techniques. Results indicate that two-stage capillary GC is very useful for mixtures containing compounds which produce mostly non-specific ions in the MS ion source whereas compounds producing specific ions can be easily analyzed by capillary GC - single ion monitoring MS even if they are not perfectly separated by a single capillary column.
    Additional Material: 7 Ill.
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  • 209
    ISSN: 0935-6304
    Keywords: High resolution capillary GC (HRCGC) ; HRCGC-MS ; Protein amino acids ; Non-protein amino acids ; Amino alcohols ; Hydroxycarboxylic acids ; tert-Butyldimethylsilyl (TBDMS) derivatives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A simple, single-step derivatization technique is presented for capillary GC-FID and GC-MS separation and identification of common protein and non-protein constituents of natural peptides as their tert-butyldimethylsilyl (TBDMS) derivatives. The tert-butyldimethyl-silylation of more than sixty compounds was accomplished with high yields and a single peak observed for each component. The TBDMS derivatives of both the protein and non-protein substances, moreover, exhibit excellent separation on apolar capillary columns and can be resolved completely using a polydimethylsiloxane or 5 % phenyl polydimethylsiloxane column and, complementarily, a 50 % phenyl polydimethylsiloxane column. Retention data and molar responses of the TBDMS derivatives on the polydimethylsiloxane column are compiled. Direct coupling of the 5 % phenyl polydimethylsiloxane column to an ion trap mass spectrometer enabled fast separation and identification of the investigated components, at nanomole to picomole levels, on the basis of retention and mass spectral data. The general usefulness of the method is demonstrated by research into new biologically active peptides isolated from entomopathogenic fungi.
    Additional Material: 6 Ill.
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  • 210
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 165-168 
    ISSN: 0935-6304
    Keywords: GC-MS ; Quantitation ; Selected fragments ; Sugars ; Carboxylic acids ; Citric acid ; Isocitric acid ; TMS derivatives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A GC-MS method has been developed for the analysis of the sugar and carboxylic acid content of citrus fruits, including the quantitation of isocitric acid in the presence of a large excess of citric acid. Optimum conditions have been determined for the analysis (from one solution, by one injection, on a 30 m DB-5 column) of the TMS oxime and/or TMS derivatives of sugars and acids obtained from various lemon, grapefruit, and orange samples. Quantitation was based on the monitoring of the total ion current and of selective fragments. The utility of the method has been demonstrated by the determination of isocitric acid in the presence of 10- to 200-fold excess of citric acid.
    Additional Material: 4 Ill.
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  • 211
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 177-179 
    ISSN: 0935-6304
    Keywords: Capillary GC ; High temperature analysis ; Novolac resins ; Epoxy resins ; Retention indices ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 212
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 191-192 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 213
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 193-193 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 214
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 251-254 
    ISSN: 0935-6304
    Keywords: Sulfur analysis ; Petroleum products ; Sulfur chemiluminescence detection ; Packed columns ; Supercritical fluid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Supercritical fluid chromatography using flameless sulfur chemiluminescence detection has been investigated for the analysis of sulfur compounds in petroleum products. The chromatography and detection system was easy to implement and exhibited good precision, linearity, selectivity, and sensitivity. A minimum detectable limit of 0.3 pg sulfur/s was obtained, and response to sulfur in different sulfur species was nearly equimolar.
    Additional Material: 7 Ill.
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  • 215
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 264-270 
    ISSN: 0935-6304
    Keywords: GC-MS ; Exhaust emissions ; Hydrocarbon emissions ; Photochemical smog ; Gasoline ; Spark-ignited engine ; Engine operating parameters, effect of ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactivities of engine-out exhaust hydrocarbon (HC) emissions in photochemical smog formation have been determined for three fuels (isooctane, an aromatic blend, and a gasoline) in a single-cylinder, spark-ignited engine. High resolution capillary GC was used to determine the mole fractions of the exhaust hydrocarbon species. Temperature programmed chromatography on a single capillary column was sufficient to separate the major exhaust species. A library of approximately 160 hydrocarbon species was used to identify typically 90-95 % of the HC species present. GC-MS was used selectively to verify peak assignments.The effect of engine operating parameters (fuel-to-air ratio, spark timing, and speed) on reactivity was examined. Engine operating parameters affect both total emissions [g/mile] and the specific atmospheric reactivity [g ozone/g HC emissions] of these emissions. Changing the operating parameters to control total emissions may not be as effective as expected in controlling the total reactivity [g ozone/mile] of the emissions because the specific reactivity can also change simultaneously. Effects of changes in operating parameters differ significantly as the type of fuel is varied. The ability to measure exhaust hydrocarbon species emissions accurately and quickly will increase in importance as reactivity-based emissions standards come into widespread use.
    Additional Material: 1 Ill.
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  • 216
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 280-282 
    ISSN: 0935-6304
    Keywords: Capillary column preparation ; Column polarity ; Immobilized phases ; Degree of immobilization ; Polyhydroxy stationary phase ; Polyglycidol (PG) ; Comparison with poly(ethylene glycol) 20M ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 217
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 287-288 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 218
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 288-288 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 219
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 308-311 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Mass selective detection ; Multidimensional GC-MSD ; Fish oil ; Furan fatty acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The separation and analysis of furan fatty acids and other minor component fatty acids present at very low concentrations in complex sample matrices, such as fish oil or lipids derived from liver and testes, require several pre-analytical separation steps if single column gas chromatography is to furnish sufficient resolution: after extraction and transesterification hydrogenation, urea complex precipitation and argentation TLC have been applied prior to GC analysis of furan fatty acids.By using multidimensional GC-MSD with cooled injection and flow-controlled column switching with intermediate cold trapping, it has been possible to identify directly the methyl esters of furan fatty acids without further pre-analytical separation.The most common of the furan fatty acids can be subdivided into two groups depending on whether they bear a propyl or pentyl side group in the 5-position of the furan ring. In addition to the eight furan fatty acids known to be present in fish oil, six new ones were identified, four with propyl substitution and two with pentyl substitution. Four have earlier been reported to be present in the hepatopancreas of crayfish and in fish tissue, whereas the propyl-substituted 16,19-epoxy-17,18-dimethyldocosa-16,18-dienoic acid and the pentyl-substituted furan fatty acid 6,9-epoxy-7-methyltetradeca-6,8-dienoic acid were hitherto unknown.
    Additional Material: 7 Ill.
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  • 220
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 339-342 
    ISSN: 0935-6304
    Keywords: Gas chromatography, GC ; Retention index ; Polycyclic aromatic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Theoretical procedures have been used to predict linear temperature-programmed retention indices for polycyclic aromatic compounds. It is possible to calculate such indices for polycyclic aromatic compounds in some practical situations in which the compounds cannot be eluted during a simple linear temperature program. The theory has been tested for a number of polycyclic aromatic hydrocarbon (PAHs) in single- and multi-plateau temperature-programmed gas chromatography with SE-52 as the stationary phase. This method will extend the applicability of linear retention indices for the identification of the isomers of polycyclic aromatic compounds.
    Additional Material: 4 Ill.
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  • 221
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 353-354 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 222
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 355-368 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 223
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 390-397 
    ISSN: 0935-6304
    Keywords: On-line coupled LC-GC ; Fuel product analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A review of the analysis of petroleum fuels, oils, tars and engine exhaust particulate extracts by on-line coupled LC-GC is presented.
    Additional Material: 8 Ill.
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  • 224
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 522-526 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Precolumns ; Solvent focusing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In trace analysis by capillary GC it is often desirable to use larger than normal injection volumes to obtain sufficient sensitivity. This, however, results in a wider solvent peak and tailing, and may reduce column efficiency. This paper describes the use of a short length of a capillary precolumn coated with a stationary phase of polarity similar to that of the sample solvent and a film thickness greater than that of the analytical column; provided the right combination of polarities of injection solvent and liquid phases are used, the precolumn focuses the solvent band, thereby enabling the maximum injection volume to be increased without measurably reducing efficiency. Typical precolumn dimensions are 1 m length, 0.32 mm i.d., and 0.5 μm stationary phase film thickness. Using a precolumn increases the maximum injection volume up to 8 or 10 μl, or three times that appropriate for a conventional analytical column, with little or no loss in efficiency.
    Additional Material: 2 Ill.
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  • 225
    Electronic Resource
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 553-555 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Liquid - liquid extraction ; Vinegar ; Polyalcohol analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A capillary gas chromatographic method has been developed for the determination of glycerol, erythritol, arabitol, sorbitol, and inositol in vinegar. After addition of phenyl-β-glucopyranoside as internal standard, the sample was then dried and silylated. The analysis was performed both on the crude silylated sample and after liquid - liquid extraction. The repeatability of the two methods was evaluated on twenty three different types of vinegar and the extraction did not seriously affect the analysis. Extraction of the TMS-ethers enables elimination of a large number of interfering substances such as acids and polyphenols and so acts as a purification of the sample.
    Additional Material: 1 Ill.
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  • 226
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 556-556 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 227
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 561-562 
    ISSN: 0935-6304
    Keywords: Reversed phase LC ; Ion pair LC ; Quality assurance ; 2,5-Diaminobenzene-1,4-disulfonic acid ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 228
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 563-564 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Electrolysis ; Electrolytic effect ; pH Variation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 229
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 568-568 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 230
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 577-582 
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction (SFE) ; Supercritical fluid chromatography (SFC) ; Gas Chromatography (GC) ; On-line analysis ; Organochlorine pesticides ; Organophosphorus pesticides ; Fatty food samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An on-line SFE-chromatographic system, where SFE has been coupled with SFC and GC, was developed and utilized for trace analyses of organochlorine and organophosphorus pesticide residues from gram-sized complex sample matrices, such as chicken fat, ground beef, and lard. The SFE process and chromatographic techniques were instrumentally integrated for efficient and automated on-line analysis, having minimal sample handling between the sample preparation and separation steps. A cleanup step, incorporating packed column SFC, allowed the fractionation of relatively small-sized, non-polar pesticides from the co-extracted fatty materials. This permitted final high-resolution separation of analytes on a capillary GC column. Detection of pesticides was accomplished using selective electron-capture and nitrogen-phosphorus detectors. Pesticide concentrations determined with the on-line system were accurate and reproducible, for fatty samples containing both fortified and incurred pesticides. This method, utilizing supercritical carbon dioxide, was considerably faster and less laborious than the conventional analytical procedures based on liquid extraction.
    Additional Material: 6 Ill.
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  • 231
    ISSN: 0935-6304
    Keywords: Enantioselectivity ; Chlordane congeners ; o,p′-DDT ; Tandem capillary ; Environmental samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two capillary columns, one coated with 90 % biscyanopropyl 10 % phenylcyanopropylpolysiloxane (RTx 2330) the other with dimethyl-t-butyl-silylated β-cyclodextrin dissolved in 85 % methyl 15 % phenyl polysiloxane (PS-086), have, when employed in tandem, enabled the enantioselective separation of all the chiral chlordanes present in the fish oil reference material SRM 1588, without any overlap between enantiomers of different isomers. This capillary column combination is, furthermore, able to separate the enantiomers of other chiral polychlorinated pesticides such as o,p′-DDT, oxy-chlordane, a chiral nonachlor, and heptachlor exo-epoxide. It can be used to determine the enantiomer ratio of these compounds present in the low pg/g range in extracts of marine biota and ambient air.
    Additional Material: 4 Ill.
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  • 232
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 597-602 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Serially connected capillary columns ; Linear temperature programming ; Retention time prediction ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Systems formed by serial connection of capillary columns of different polarity were studied with methods previously used to predict the behavior of linked capillary columns under isothermal conditions and to obtain programmed temperature gas chromatography (PTGC) retention times of the individual columns starting from isothermal data. The two calculation methods were simultaneously applied in order to predict PTGC retention times of the series system starting from isothermal data obtained on the two individual columns. Experimental retention values measured using different temperature programs on the individual columns and on the series systems were found to agree with those calculated.
    Additional Material: 4 Ill.
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  • 233
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 613-615 
    ISSN: 0935-6304
    Keywords: Glass capillary column ; Trifluoroacetylated cyclodextrin ; γ-Lactones ; δ-Lactones ; Routine quality control ; GC-MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 234
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 622-622 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 235
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 17 (1994), S. 629-633 
    ISSN: 0935-6304
    Keywords: Chiral stationary phase ; Chiral separations ; HPLC ; N(1-Naphthyl)leucine ; N(5-Acenaphthyl)leucine ; Polysiloxane ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A π-basic, brush-type chiral stationary phase (CSP) derived from (S)-N-(1-naphthyl)leucine undecenyl ester has been shown to effectively separate the enantiomers of a broad array of π-acidic analytes. Armed with a mechanistic hypothesis as to how this CSP differentiates between the enantiomers of π-acidic derivatives of α-amino acids, the structure of this CSP was modified in a series of steps, each intended to enhance the enantioselectivity of the CSP. Specifically, brush-type CSPs were prepared from N-(5-naphthyl)leucine di-n-propyl amide and from N-(5-acenaphthyl)leucine di-n-propyl amide. The latter selector was also incorporated into a polysiloxane, then coated and bonded to silica. The rationale for each of the structural changes, and its effect on the enantioselectivity of the resulting CSP is described.
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  • 236
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    Journal of High Resolution Chromatography 17 (1994), S. 651-654 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Micellar electrokinetic capillary chromatography (MECC) ; β-Blockers ; Temperature control ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A home-made temperature control unit has been developed for a commercial capillary electrophoresis apparatus, the Waters Quanta 4000. The effect of the unit on the absolute migration times and peak areas of nine β-blockers is described. It was found that this homemade temperature control unit considerably (≥ 100 %) improved the repeatability of the separation.
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  • 237
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    Journal of High Resolution Chromatography 17 (1994), S. 665-667 
    ISSN: 0935-6304
    Keywords: Capillary zone electrophoresis ; Indirect UV detection ; Sodium dodecyl sulfate ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: SDS (sodium dodecyl sulfate) has been quantitatively determined by capillary zone electrophoresis using a fused silica capillary and a 5 mM dihydroxybenzoic acid / sodium hydroxide buffer in 5% methanol solution at a pH of 8.1. The ion was detected by indirect UV absorption at 250 nm. Detection range was from 0.8 to 50 mg SDS/L. This rapid method requiring only small sample volumes was developed in support of an aquatic toxicology study in a simulated stream water and is applicable to waters containing common inorganic ions.
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  • 238
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    Journal of High Resolution Chromatography 17 (1994) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 239
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    Journal of High Resolution Chromatography 17 (1994), S. 753-755 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Nitrosamines ; Subambient temperature ; syn and anti isomers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The separation of a selected group of naturally occurring, heterocyclic nitrosoamino acids was achieved by capillary zone electrophoresis and the resolution of the syn and anti conformers improved as the temperature was lowered to 5 °C. The double peaks observed for each nitrosoamino acid are probably caused by the slow kinetics of conformational isomerism. The experimental setup consisted of a P/ACE 5510 electrophoresis system, a 57 cm polyacrylamidecoated capillary, and a 10 mM phosphate buffer, pH 7.2, containing 2 mM of 3-(N-N-dimethylmyristylammonio)propanesulfonate (DMMAPS) and 0.1% Tween 20. Our study shows that (a) the lower the temperature, the greater the resolution and the longer the migration times; and (b) different nitrosoamino acid conformers were resolved at different temperatures because of differences in the rate of isomerization. For example, the conformers of N-nitrosothiazolidine-4-carboxylic acid were partially resolved at 30 °C while those of N-nitrosoproline were well resolved at the same temperature.
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  • 240
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    Journal of High Resolution Chromatography 17 (1994), S. 765-769 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography ; Sector field mass spectrometry ; Capillary column ; Polymer additives ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An integral restrictor interface with jet separator for coupling capillary column supercritical fluid extraction - supercritical fluid chromatography with high resolution mass spectrometry (SFE-SFC-MS) has been built and used for the analysis of a fatty acid ester, and of polymer additives with a wide range of masses. The mobile phase used was supercritical carbon dioxide; a flame ionization detector (FID) was used in parallel with the mass spectrometer. Different SFC-MS interface operating conditions, e.g. temperature, restrictor position, flow rate, and sample transfer conditions were optimized to obtain good sensitivity and separation for these applications. In addition, the sensitivity of measurements performed with the direct insertion probe and by SFC-MS interface have been compared.
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  • 241
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    Journal of High Resolution Chromatography 17 (1994), S. 802-802 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 242
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    Journal of High Resolution Chromatography 17 (1994), S. 809-813 
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction (SFE) ; Capillary SFC ; On-line SFE-SFC ; Modified carbon dioxide ; Pesticides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary supercritical fluid chromatography has been directly coupled with supercritical fluid extraction using modified carbon dioxide. The mixed fluids were prepared with a single pump on-line mixing system. The most important step in the SFE-SFC interface was the elimination of the modifier solvent. This was achieved by use of a coupled trap, 0.1 mm i.d. and 0.53 mm i.d. capillary tubing connected in series, with the collected solutes refocused on the second (0.53 mm i.d.) trap before transfer into the separation column. This enabled complete elimination of various modifier solvents and high efficiency collection of the solutes. The effect of the modifier on trapping efficiency was investigated using methanol, ethanol, dichloromethane, hexane, and toluene at a variety of concentrations. n-Eicosane was, for example, trapped quantitatively by modified carbon dioxide containing up to 13 % (w/w) methanol. The use of the technique has been demonstrated by selective extraction of n-paraffins, fatty acid methyl esters, and alcohols from a silica matrix; the effect of different modifiers on the extraction of a mixture of pesticides from soil has also been investigated.
    Additional Material: 7 Ill.
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  • 243
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Atomic emission detection (AED) ; Programmed temperature vaporization (PTV) ; Nitro musks ; Human adipose tissue ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Atomic emission detection (AED) has been successfully applied to the determination of nitro musks in the fat of human adipose tissue by gas chromatography at trace concentration levels. Element specific detection with the AED combined with a clean-up procedure for nonpolar substances makes target screening analysis for lipophilic nitro aromatic compounds possible for the first time. The lack of sensitivity, especially in the AED nitrogen and oxygen trace, was compensated by higher concentration of the extracts and injection of larger sample volumes performed by cold programmed temperature vaporization (PTV) in the solvent split mode. The combination of the superior quantification properties of the atomic emission detector with large sample volume introduction makes the quantification of nitro musks down to the ppb level possible. All five nitro musks investigated exhibit linear dynamic ranges going down close to instrumental limits of detection. Moreover, organochlorine compounds could be sensitively detected in the same sample extract by the AED chlorine trace without any interferences from coeluting matrix compounds.
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  • 244
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    Journal of High Resolution Chromatography 17 (1994), S. 4-8 
    ISSN: 0935-6304
    Keywords: Micellar electrokinetic capillary chromatography (MECC) ; Cationic micelles ; DNA photoproducts ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Micellar electrokinetic capillary chromatography has been explored as an efficient and rapid method of separating the photoproducts of 2′-deoxyuridylyl-(3′-5′)-thymidine (i.e., cis-syn and trans-syn cyclobutane dimers, (6-4) photoproduct, and the related Dewar valence isomer) from normal nucleosides and nucleotides. Three cationic surfactants, dodecyl-, tetradecyl-, and hexadecyltrimethy-lammonium bromide were evaluated and the separations compared with those obtainable with the anionic surfactant, sodium dodecylsulfate. Optimum resolution of the dinucleoside monophosphate photoproducts was obtained using tetradecyltrimethylammonium bromide. By use of this detergent the photoproducts could also be separated from other normal constituents in less than 6 min at -25 kV. Dodecyl- and hexadecyltrimethylammonium bromide provided some separation between the various species but sodium dodecylsulfate did not separate the UV radiation-induced products from either the parent compound or other dinucleoside monophosphates. Increased interaction between negatively charged solutes and positively charged micelles accounts for the differences.
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  • 245
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    Journal of High Resolution Chromatography 17 (1994), S. 37-42 
    ISSN: 0935-6304
    Keywords: Deactivation of GC precolumns ; Water resistance of deactivation ; OV-1701 for deactivation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Deactivation of precolumns with an ultra thin film of OV-1701 provided inertness at least equal to silylation, but better resistance to water. Dynamic coating of the raw fused silica capillary is, furthermore, much faster than the hydrothermal treatment/silylation procedure.
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  • 246
    ISSN: 0935-6304
    Keywords: Chiral stationary phase ; Carbon dioxide-based mobile phases ; Dynamic chiral chromatography ; Fullerenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fast and efficient separations of chiral stereolabile compounds were obtained at very low temperature on a π-acid chiral stationary phase (R,R-DACH-DNB) using carbon dioxide-based mobile phases containing alcoholic polar modifiers.Furthermore, efficient separations of the newly discovered spherical carbon cluster buckminsterfullerene (C60) and the related higher fullerenes (C70, etc.) have been performed on the same stationary phase using eluents based on either n-hexane or carbon dioxide.
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  • 247
    ISSN: 0935-6304
    Keywords: Fused silica model substrates ; Adsorption characteristics ; Surface OH distribution ; Inverse gas-solid chromatography ; 29Si CP MAS NMR ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The possibilities of inverse gas-solid chromatography (IGC) in obtaining chromatographic data on fumed silica were examined. Aerosil A-200, a fused silica model substrate in 29Si nuclear magnetic resonance analysis, was trimethylsilylated to different degrees. IGC was used to very reproducibly determine the free specific energies of adsorption of several functionalized probe solutes. Hydrogen bonding solutes have a free specific energy of adsorption that is at least about 50% higher than that of non-hydrogen bonding probe solutes. NMR was used in combination with elemental analysis to calculate surface concentrations of the different chemical surface structures. IGC data and surface concentrations were combined in order to determine the contribution of each type of surface structure to the total free specific adsorption energy. It could be concluded that residual silanols from the reaction of dihydroxydi-siloxysiloxane (Q2 groups) with trimethylchlorosilane possess a higher adsorption activity than the silanols initially present.
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  • 248
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    Journal of High Resolution Chromatography 17 (1994), S. 95-97 
    ISSN: 0935-6304
    Keywords: Chemical warfare agents ; Microcolumn liquid chromatography ; Enantiomeric separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An improved interface for the on-line coupling of microcolumn liquid chromatography (micro-LC) with thermionic detection (TID) is described. Modifications have been made to enable separate adjustment of the eluent introduction and the detector flame temperature in order to improve the sensitivity and ease of use of the system.The micro-LC-TID was used for the chiral separation of the nerve agent O-ethyl S-2-diisopropylaminoethyl methylphosphonothioate (VX). Baseline separation for the enantiomers of VX was obtained on Chiralcel OD using 1% isopropanol in hexane as the eluent. The detection limit of VX using 60 nl injections is ca. 5 μg/ml (ppm range). However, when using large-volume injections (10 μl) the detection limit is ca. 25 ng/ml (ppb range).
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  • 249
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    Journal of High Resolution Chromatography 17 (1994), S. 102-103 
    ISSN: 0935-6304
    Keywords: HPLC ; Capillary electrophoresis (CE) ; Laser desorption mass spectrometry ; Synthetic peptides ; Purity determination ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 250
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    Journal of High Resolution Chromatography 17 (1994), S. 109-115 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 251
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    Journal of High Resolution Chromatography 17 (1994), S. 118-118 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 252
    ISSN: 0935-6304
    Keywords: Block polysiloxanes ; Functionalized polysiloxanes ; Chiral polysiloxanes ; Enantioselective stationary GC phase ; Polysiloxane synthesis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Trifluoroethyl ester-functionalized polysiloxanes can be prepared by block condensation of 3-dichloromethylsilyl-2-methylpropionic acid 2′,2′,2′-trifluoroethyl ester with 1,5-bis(diethylamino)hexamethyltrisiloxane or with disodium tetramethyldisiloxane-1,3-diolate. The functionalized polysiloxanes may serve as supports for a variety of selector groups; for instance, nucleophilic displacements with L-valine-t-butylamide or L-α-naphthylethylamine lead to chiral polysiloxanes in high yields and with high reproducibility. Imidazole accelerates the rate of nucleophilic displacement. Capillary columns coated with such chiral polysiloxanes exhibit high enantioselectivity and thermostability.
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  • 253
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    Journal of High Resolution Chromatography 17 (1994), S. 56-56 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 254
    ISSN: 0935-6304
    Keywords: Taxol ; Micellar electrokinetic chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 255
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    Journal of High Resolution Chromatography 17 (1994), S. 203-211 
    ISSN: 0935-6304
    Keywords: Simulated distillation ; Boiling point distribution ; Element-specific detectors ; Carbon number distribution ; Petroleum ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Information about the boiling point distribution of petroleum and its products is obtained either by actual distillation, or by analyses designed to simulate the distillation process. These analytical techniques are called simulated distillations. Simulated distillations are most often performed by gas or supercritical fluid chromatography. This paper reviews the use of gas and supercritical fluid chromatography for simulated distillation, and the development of element-specific detection coupled with these analyses.
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  • 256
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    Journal of High Resolution Chromatography 17 (1994), S. 237-244 
    ISSN: 0935-6304
    Keywords: Preparative liquid chromatography ; High resolution gas chromatography (HRGC) ; Alternative fuels ; Group-type fractionation ; Sugar cane bagasse upgrading ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An overview is presented of the analytical approaches developed by our research group over the last ten years for analysis of alternative fuel, both biomass and fossil. The alternative fuels are analyzed successively by PLC-8 (preparative liquid chromatography-group-type) fractionation and high resolution gas chromatography. Some of the possibilities for fractionation and characterization of alternative fuels are herein exemplified with sugar cane bagasse pyrolysis products.
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  • 257
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    Keywords: Capillary electrophoresis ; EOF ; Sample loading ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 258
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    Journal of High Resolution Chromatography 17 (1994), S. 671-673 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Sample loading ; Concentration ; Drug metabolism ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 259
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    Journal of High Resolution Chromatography 17 (1994), S. 682-682 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 260
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    Journal of High Resolution Chromatography 17 (1994), S. 695-699 
    ISSN: 0935-6304
    Keywords: High resolution gas chromatography ; Sulfur chemiluminescence detection ; Chromatographic injection profile ; Gaseous injection ; Sulfur gases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A one meter stainless steel capillary column coated with a 20μm film of polydimethylsiloxane was used to replace the Teflon gas sampling loop of a HRGC - flameless SCD system. This column trap was equilibrated with the gaseous sample and then purged with carrier gas while being sequentially, resistively heated in ten 10 cm sections. The sequential heating of the 10cm sections was timed such that the velocity of the moving heated zone was approximately the same as the velocity of the carrier gas. The thick stationary phase film served to retard the front end of the injection band while the ballistic heating accelerated the back end. The net result was focusing of the injection, which gave rise to a narrower injection profile than that obtained with the original Teflon loop.
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  • 261
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    Journal of High Resolution Chromatography 17 (1994), S. 705-712 
    ISSN: 0935-6304
    Keywords: High performance liquid Chromatography ; Zirconia-based ion exchange ; Proteins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of non-porous, microspherical zirconia-based stationary phases with surface bound cationic functions have been introduced and evaluated in ion exchange chromatography of proteins and small acidic solutes. Different surface modification procedures were evaluated in the covalent attachment of weak, strong or hybrid anion exchange moieties on the surface of non-porous zirconia micropar-ticles. N,N-Diethylaminoethanol (DEAE) was used as the weak anion exchange ligand while glycidyltrimethylammonium chloride, which was covalently attached to poly(vinyl alcohol) layer (PVAN) on the zirconia surface, constituted the strong anion exchange moiety. Partially quaternarized poly(ethyleneimine) hydroxyethylated (PEI) was used as the hybrid type of anion exchange coating. DEAE-zir-conia microparticles acted as purely cation exchange stationary phases toward basic proteins indicating the predominance of electron donor-electron acceptor interaction (EDA) with surface exposed zirconium sites as well as cation exchange mechanism via electrostatic interaction with unreacted and unshielded hydroxyl groups. PVAN-zirconia stationary phase exhibited anion exchange chromatographic properties toward acidic proteins, but EDA interaction has stayed as an important contributor to solute retention despite the presence of a relatively thick layer of poly(vinyl alcohol) on the surface of the zirconia particles. The modification of zirconia surface with partially quaternarized PEI proved to be the most effective approach to minimize Lewis acidic metallic properties of the support. In fact, PEI-zirconia stationary phase operated as an anion exchanger toward acidic proteins and other small acidic solutes.
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  • 262
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    Journal of High Resolution Chromatography 17 (1994), S. 727-728 
    ISSN: 0935-6304
    Keywords: Trichloroacetyl pentyl β-cyclodextrin ; Enantioselective GC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 263
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    Journal of High Resolution Chromatography 17 (1994), S. 731-732 
    ISSN: 0935-6304
    Keywords: Micellar electrokinetic chromatography ; Lanthanide luminescence ; Steroids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 264
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    Journal of High Resolution Chromatography 17 (1994), S. 735-738 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Silica-bonded cation exchangers ; Amino acids ; TBDMS derivatives ; Clean-up ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
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  • 265
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    Journal of High Resolution Chromatography 17 (1994), S. 831-838 
    ISSN: 0935-6304
    Keywords: GC ; GC-MS ; Dehydration of sterols ; Sterenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Samples of maize, rapeseed, soyabean, sunflower, and palm oils, collected at different stages in their respective refining processes, have been analyzed for the presence of dehydrated sterols (sterenes). A total of fifteen compounds were detected. Four have been characterized using model systems designed to investigate their formation. Their elemental composition, and that of the other eleven sterenes, was determined by high resolution mass spectrometry and structures assigned to a further six compounds. These included the -3,5-, -2,5-, -4,6-,-3,5,22-, and -4,6,22- sterenes. Sterenes were not present in crude or alkali neutralized oils. Bleaching introduced a maximum concentration of 5 μg g-1 of total sterenes into the edible oils. Deodorization is the dominant stage in sterene production resulting in a maximum total concentration of 163 μg g-1. This increased concentration arises due to dehydration of the sterols and considerable isomerism of the sterenes.
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  • 266
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    Journal of High Resolution Chromatography 17 (1994), S. 865-865 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 267
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    Journal of High Resolution Chromatography 17 (1994), S. 866-866 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 268
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    Journal of High Resolution Chromatography 17 (1994), S. 868-868 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 269
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    Biological Mass Spectrometry 29 (1994), S. 1-10 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Biological Mass Spectrometry 29 (1994), S. 55-56 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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    Biological Mass Spectrometry 29 (1994) 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
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  • 272
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    Biological Mass Spectrometry 29 (1994), S. i 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 273
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    Biological Mass Spectrometry 29 (1994), S. 85-89 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Survivor-ion mass spectrometry is used to distinguish stereoisomeric cis- and trans-4-methylcyclohexanol. The method involves producing ions by electron impact ionization and submitting them without mass selection to collisional neutralization and reionization, followed by selective monitoring of non-dissociating ions. The differences in the electron impact mass spectra of the stereoisomers, due to the different fragment ion elemental compositions and structures, are highlighted by collisional neutralization with Xe, NO and CH3SSCH3, followed by reionization with oxygen. The differences in the survivor-ion spectra are due to different neutralization efficiencies of the isobaric and isomeric ions produced by electron impact ionization, different stabilities of the intermediate neutral species, different reionization efficiencies and reionized ion stabilities. Neutralization-reionization spectra of the C7H12+., C6H9+, C3H6O+. and C3H5O+ ions from stereoisomeric 4-methylcyclohexanols are also reported.
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  • 274
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    Biological Mass Spectrometry 29 (1994), S. 106-107 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 275
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electron-capture negative-ion chemical Ionization mass spectra of 36 35Cl mono- and di-labelled penta- and hexachlorobiphenyls were studied. Under the conditions of the analyses, the dechlorination of these congeners probably proceeds through electrophilic hydrogen atom attachment followed by rapid loss of the chlorine atom at the same position. These dechlorination reactions occur regioselectively. When present, ortho-chlorines are lost preferentially to meta- and para-chlorines. The extent of the dechlorination reaction, as seen by the relative abundance of the [MH — Cl]- ions, decreases with increasing number of ortho-chlorines.
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  • 276
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    Biological Mass Spectrometry 29 (1994), S. 153-154 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 277
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    Biological Mass Spectrometry 29 (1994) 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
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  • 278
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    Biological Mass Spectrometry 29 (1994), S. 176-185 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The metastable dissociation of the methoxymethyl cation and a number of its deuterium and 13C variants was examined using a reverse-geometry double-focusing mass spectrometer. The loss of methane from the methoxymethyl cation clearly showed a composite peak shape which, when deconvoluted, revealed a bimodal kinetic energy release distribution in the resulting formyl cations. Labelling experiments revealed that the two carbon atoms and all hydrogens become equivalent on the time-scale of the unimolecular dissociation lifetime of the decomposing ion. A small deuterium isotope effect was found which can be rationalized on the basis of zero point energy effects. The bimodal kinetic energy release distribution was shown, with the aid of a four-sector instrument, to be due to the production of both formyl cation (with a large kinetic energy release) and isoformyl cation (with a much smaller kinetic energy release). The methoxymethyl cation was also prepared with a precisely defined amount of internal energy in a Fourier transform ion cyclotron resonance (FTICR) spectrometer by the reaction of methyl cation with formaldehyde. Experiments with 13C and deuterium labelling revealed that the dissociation to formyl cation of the methoxymethyl cations formed in the low-pressure FTICR cell by reaction of methyl cation with formaldehyde is accompanied by complete scrambling of the carbons and incomplete scrambling of the hydrogens. Ab initio calculations were carried out which identified and characterized each of the stable minima and transition states for the appropriate reactions. The calculations were fully consistent with the mechanism deduced on the basis of the experimental data.
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  • 279
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    Biological Mass Spectrometry 29 (1994), S. 211-211 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 280
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    Biological Mass Spectrometry 29 (1994), S. 226-231 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Liquid chromatography/Thermabeam mass spectrometry/mass spectrometry was carried out on the starting material, 2-nitro-2′hydroxy-5′-acetylazobenzene (1) and the intermediate N-oxide (2) formed by dithionite reduction of the starting material (1). The mass spectra of (1) and the intermediate (2) showed an abundant fragment ion that corresponds to that of 2-(2′-hydroxy-5′-acetylphenyl)benzotriazole (3). These results show that 3 could be formed from both 1 and 2. The formation of 3 in the gas phase is analogous to the chemical reduction processes of the 2-nitroazobenzene derivative 1 and the N-oxide 2 in solution.
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  • 281
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    Biological Mass Spectrometry 29 (1994), S. 272-272 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 282
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    Biological Mass Spectrometry 29 (1994), S. 273-276 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The dipole moments of a series of substituted benzene radical cations were evaluated on the basis of mass displacements from the expected instrumental value by ion trap experiments. Mass displacements represent a direct measure of the total polarizability, giving access to both the electronic and dipolar polarizabilities, depending on the characteristics of the analyte under investigation. A linear relationship was found between the dipolar polarizabilities and the dipole moments of the corresponding neutrals.
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  • 283
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    Biological Mass Spectrometry 29 (1994), S. 295-302 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mass spectral behaviour of nine 1,3-dioxolanes, seven 1,3-dithiolanes and seven 1,3-oxathiolanes was studied under chemical ionization conditions with ammonia, isobutane, methane, acetone, acetone-d6 or pentan-3-one as reagent gas. The proton affinity of the first members in each series was not large enough for ammonia to protonate them; instead, the ionization took place through unstable [M + NH4]+ ions. Isobutane, which gave rise to abundant [M + H]+ ions in all cases, was the best reagent gas for the determination of the molecular mass. Methane chemical ionization caused extensive fragmentations either through ring cleavage or through the elimination of the largest substituent from ring positions 2 as a neutral hydrocarbon. The ketones used as reagent gas reacted to form adduct ions. In the case of dioxolanes and oxathiolanes, the [M + RCO]+ adduct ion decomposed through ring opening and then, as a consequence of intramolecular nucleophilic substitution, through the elimination of a neutral carbonyl compound. Resonance-stabilized dioxolanylium and oxathiolanylium ions were obtained for dioxolanes and oxathiolanes, respectively. This reaction was almost non-existent for the dithiolanes.
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  • 284
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    Topics: Chemistry and Pharmacology
    Notes: The electron impact ionization mass spectra of 4,5-bis(alkylthio)-1,3-dithiole-2-thiones and their 1,2-dithiole-3-thione isomers were studied by accurate mass measurements and linked scans. The relative abundance of ions formed following the extrusion of S2, CS or CS2 allows an unambiguous isomer differentiation. Isomerization of molecular ions was studied by means of metastable ion analysis and collision-induced dissociation. The order of reactivity was analogous to that observed in isomerization under photochemical conditions.
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    Biological Mass Spectrometry 29 (1994) 
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    Biological Mass Spectrometry 29 (1994), S. 382-390 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The neutral products arising during the collisionally activated dissociation of protonated oligopeptides (MH+) are post-ionized by collision and detected in neutral fragment-reionization (+NfR+) mass spectra. For the isomeric tripeptides Ala-Gly-Gly, Gly-Ala-Gly and Gly-Gly-Ala, the amino acid and dipeptide losses from the C-terminus and the diketopiperazine losses from the N-terminus allow for differentiation. These neutral fragments are identified in the corresponding +NfR+ spectra by comparison to reference collision-induced dissociative ionization (CIDI) mass spectra of individual amino acids, dipeptides and diketopiperazines. Peptides with distinct C-termini but otherwise identical sequences are found to yield +NfR+ products that are characteristic of the respective C-terminal amino acid. This is demonstrated for several peptide pairs, including leucine- and methionine-enkephalin. In general, +NfR+ spectra are dominated by the heavier neutral losses; further, +NfR+ and CIDI cause extensive dissociation, indicating that the collisional ionization process imparts high average internal energies.
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    Biological Mass Spectrometry 29 (1994) 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Topics: Chemistry and Pharmacology
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  • 288
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    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Methanol exchanges its hydroxyl hydrogen with deuteriums in ionized propene during the formation of protonated methanol. This exchange is attributed to the interconversion [CH3CH=CH2+. HOCH3⇌][CH2 ⋅CHCH2 +H2OCH3] in single collisions. The exchange in this ion-molecule reaction is analogous to that observed in the formation of protonated methanol from ionized 2-methylpropanol, supporting the intermediacy of ion-neutral complexes in the final step of the latter reaction. Ion-molecule reactions were studied using a Fourier transform mass spectrometer.
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    Biological Mass Spectrometry 29 (1994) 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Biological Mass Spectrometry 29 (1994), S. 458-462 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method for the direct identification of organic inclusions in graphite on the basis of field desorption mass spectrometry is proposed, based on the possibility of using a fractured graphite sample as a field emitter. Under such circumstances, the organic inclusions adsorbed on the surface of the microcrystallites of modified graphites may be directly field desorbed and identified by their mass spectra without any pretreatment of the sample. Two differently modified types of graphite were analysed by this method and the nature of the admixtures was established: one sample appeared to contain a mixture of polymethylsiloxanes and the other and blend of dyes. For the latter sample, temperature fractionation of admixed substances was performed and the presence of three individual dyes was established. Such features of field desorption as the production of abundant molecular ions with negligible fragmentation and the possibility of obtaining of mass thermograms greatly facilitate the identification of individual components of mixture inclusions.
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    Biological Mass Spectrometry 29 (1994), S. 483-490 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The collision-induced decomposition (CID) mass spectra of the protonated and cationized molecules of a number of carbohydrate antibiotics of RMM ranging from 700 to 1500 were studied by means of a four-sector mass spectrometer with a floated collision cell. Helium and argon were used as collision gases. This work illustrates that cationized rather than protonated carbohydrate antibiotics give an increased yield of high-mass ions of diagnostic value. Further, when helium is replaced by argon as collision gas, differences in the CID spectra of MH+ ions become apparent only for molecules of RMM 〉 1400 whereas for [M + Na]+ ions differences are observed for molecules of RMM as low as 1000. These results have been attributed to the deposition of more internal energy in the precursor ion when argon is used, resulting in increased fragmentation.
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    Biological Mass Spectrometry 29 (1994), S. 496-498 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The stereochemistry of six pairs of diastereomeric chlorin derivatives was investigated by electron impact (EI), fast atom bombardment (FAB) and direct chemical ionization DCI mass spectrometry. It was demonstrated that FAB and EI mass spectrometry are convenient and rapid methods for distinguishing between diastereomeric chlorin derivatives due to their different fragmentation patterns.
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    Biological Mass Spectrometry 29 (1994), S. 516-516 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Topics: Chemistry and Pharmacology
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    Biological Mass Spectrometry 29 (1994), S. 526-532 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Several proteins in the relative molecular mass (RMM) range 1150-29000 are examined by means of both positive electrospray and matrix-assisted laser desorption/ionization mass spectrometry. Accuracy of the measured RMMs, resolution and overall sensitivity are discussed. The presence of more than one component in a number of the investigated compounds permitted the assessment of both desorption methods for the analysis of mixtures. Solvent-induced conformational changes are linked to charge-state distribution shifts observed in some positive electrospray mass spectra.
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    Biological Mass Spectrometry 29 (1994), S. 553-555 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Negative-ion fast atom bombardment mass spectrometry and metastable ion studies were applied to the characterization of three isomeric fluorine-containing sugars. Peculiar fragmentation processes were evidenced for each isomer, enabling their differentiation. Comparison with the behaviour of a non-fluorinated analogue allowed investigation of the role of fluorine in the decomposition processes of these compounds.
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    Biological Mass Spectrometry 29 (1994), S. 578-578 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No. Abstract.
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    Biological Mass Spectrometry 29 (1994) 
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  • 298
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    Biological Mass Spectrometry 29 (1994), S. 607-614 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two n-heptane-precipitated asphaltene samples, characterized by elemental analysis and nuclear magnetic resonance spectrometry, were fractionated according to relative molecular size by gel permeation chromatography (GPC). Both the whole asphaltene samples and their fractions were analysed by pyrolysis/gas chromatography/mass spectrometry. The data obtained from the pyrograms (average side-chain length, aromaticity index, sulphur compounds vs. aliphatic compounds, presence of SO2 and CO2) demonstrated that, in the case of asphaltenes, GPC fractionation results in the separation of different chemical structures ranging from lower molecular mass, highly aromatic and polar compounds to higher molecular mass, less polar and aromatic compounds.
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    Biological Mass Spectrometry 29 (1994), S. 625-631 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Electron impact (EI), chemical ionization and negative-ion chemical ionization (NCI) mass spectra of 1,4-dinitroglycoluril (DINGU), its 15N- and 2H-labeled analogues and the dimethyl-substituted derivatives were recorded. Tandem mass spectrometry with collision induced dissociation was used to study the fragmentation pathways of these compounds. It was found that the main EI fragmentation processes of DINGU are due to the cleavage of C—N bonds and some rearrangement reactions.
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  • 300
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    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Side-reactions often occur during peptide synthesis resulting in modified amino acid moieties. To identify these residues, liquid secondary ion/collision-induced dissociation mass spectra were recorded. The main fragments are generated by cleavage of the peptide bond. To facilitate interpretation of the spectra and assignment of the structure, a simple, but flexible and efficient, computer program is presented. The program allows the verification of the correct structure of the synthesized peptides and the deduction of the type of side-products formed, such as alkylation of tryptophan residues.
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