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  • 1995-1999  (226)
  • 1996  (226)
  • Analytical Chemistry and Spectroscopy  (226)
  • Nuclear reactions
  • 1
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Biospectroscopy 2 (1996), S. 167-171 
    ISSN: 1075-4261
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Physics
    Notes: Fluorescence measurements of photosynthetic organisms and isolated proteins at ambient and low temperature have played an important role in understanding their function. When comparing fluorescence measurements at cryogenic temperatures, the differences in the scattering properties of frozen samples make it difficult to compare the fluorescence intensity of these samples. An internal emission standard can be used to scale the fluorescence intensity, compensating for these differences. We report the synthesis, purification and characterization of a luminescent terbium chelate complex for use as an internal emission standard for the study of photosystem II fluorescence at cryogenic temperatures. The ligand consists of a diethylenetriaminepentaacetic acid derivative where pyrimidine rings sensitize the terbium luminescence, overcoming the inherently low absorption of terbium. The chelated lanthanide remains in solution in the aqueous phase and does not interfere with photosystem II function. By scaling to the terbium emission, the fluorescence intensity of different samples can be readily compared. This chelate complex could also be used as an internal emission standard for studies of other proteins. © 1996 John Wiley & Sons, Inc.
    Additional Material: 5 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Biospectroscopy 2 (1996), S. 219-224 
    ISSN: 1075-4261
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Physics
    Notes: Cholestane is a fully saturated alkane with a structure analogous to cholesterol. We observed fluorescence emission from cholestane with a maximum near 235 nm when excited with picosecond laser pulses at 298 nm. The emission intensity of cholestane was found to depend on the square of the laser power, indicating the biphotonic process of two-photon excitation. The lifetime of cholestane in cyclopentane was found to be near 1.4 ns. Cholestane was found to be efficiently collisionally quenched by methanol and oxygen, as seen from decreased lifetime in the presence of these quenchers. These results suggest that cholestane or its analogs can be used as intrinsic probes in biologic systems. Two-photon excitation avoids the use of vacuum ultraviolet wavelength (130-170 nm), which requires special optics and exclusion of oxygen, and is generally incompatible with biologic samples. © 1996 John Wiley & Sons, Inc.
    Additional Material: 4 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 49-53 
    ISSN: 0935-6304
    Keywords: Polycyclic aromatic sulfur heterocycles ; Crude oil ; Oil maturity ; Fingerprinting ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is presented for the identification and quantification of C2-substituted benzothiophenes in crude oil. The method will enable analysis of the pattern of these compounds, for example as a basis for differentiating crude oils from one another (fingerprinting) and for investigation of their suitability as indicators of oil maturity. Here results are reported for five crudes from Iraq, Venezuela, Saudi Arabia, the former Soviet Union, and the North Sea. The aromatic fraction of the crudes was oxidized and the dioxides of the heterocycles separated according to the number of carbon atoms in the side chains. The final separation was by capillary GC with atomic emission or flame ionization detection. A fluorinated analog was synthesized and used as internal standard. The concentrations of 2,3-, 2,4-, 2,7-, and 3,7-dimethylbenzothiophene ranged between 11 and 272 ppm. Three other dimethylated benzothiophenes present in lower amounts were also identified.
    Additional Material: 4 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 66-66 
    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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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996) 
    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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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 80-84 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Specific detectors ; ECD/FPD response ratios ; Retention indices ; Identification on real samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A previous paper reported the possibility of using the ratio between the responses of two different specific detectors to a single compound (detector response ratio, DRR) as an identification criterion for that compound, in combination with its retention index.This article gives some applications of DRR in the identification of some pesticides in four different fruits (apples, apricots, strawberries, and peaches) in a range varying from 0.02 to 1.3 ppm, by means of their ECD/FPD DRRs. After clean-up GC analyses were performed on a single column with dual parallel detection; a personal computer system was used for data analysis.
    Additional Material: 4 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 225-226 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Chiral separation ; Ergot alkaloids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 234-236 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Trace analysis ; Automation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 244-244 
    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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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 105-110 
    ISSN: 0935-6304
    Keywords: HPLC-UV ; Baby food ; Apple pulp ; Pear pulp ; Diflubenzuron ; Ethiofencarb ; Teflubenzuron ; Triflumuron ; Triforine ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two distinct methods are described for determination of residues of ethiofencarb and triforine, and of diflubenzuron, teflubenzuron, and triflumuron at the 0.01 ppm level in apple and pear pulp used for baby food;recoveries are above 50%. Diflubenzuron, teflubenzuron, and triflumuron are extracted with a 1:1 mixture of dichloromethane and acetone, and the extracts are cleaned by SPE using C18 as stationary phase and methanol as mobile phase. Ethiofencarb and triforine are extracted with dichloromethane, and the extracts cleaned using the same stationary phase but a 1:1 mixture of acetonitrile and water as mobile phase. Analysis of both groups of pesticides is by isocratic HPLC - UV at 210 nm using an RP-18 column and acetonitrile-water as mobile phase.
    Additional Material: 3 Ill.
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  • 11
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 124-126 
    ISSN: 0935-6304
    Keywords: Reversed-phase HPLC ; Propionic antiinflammatory drugs ; Barbituric sedatives and hypnotics ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 12
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 129-129 
    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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  • 13
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 613-616 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Electrochemical detection ; End column detection ; Nickel electrode ; Carbohydrates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Carbohydrates were separated by capillary electrophoresis (CE) and detected electrochemically using a nickel microelectrode which was operated at a constant applied potential (∼0.6 V vs. Ag/AgCI). A simple capillary electrode holder design facilitated alignment between the separation capillary and the working microelectrode without the use of micro-positioning equipment. The separations were performed under alkaline conditions (pH 〉 11), matching the high pH requirements for amperometric detection at the nickel electrode. The analytical procedure developed showed detection limits for the carbohydrates studied in the micromolar range, showing a linear response in the range tested (micromolar to millimolar). The procedure was used to identify sugars in two real samples (i.e., urine and in a common beverage). The potential use of the system for the determination of amino acids was also demonstrated.
    Additional Material: 5 Ill.
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  • 14
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 639-642 
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; Gas chromatography ; Airborne particulate matter ; Nitroarenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Normal-phase HPLC has been applied to the separation of nitroarenes from dichloromethane extracts from airborne particulate matter samples collected in urban regions of Upper Silesia. GC-MS and capillary gas chromatography with NP detector analysis of the nitroarene fraction made it possible to identify and determine quantitatively those compounds which dominate in the organic matter emitted to the atmosphere in highly industrialized regions (2-nitrofluorene, isomeric nitroarenes of MW = 247, i.e. nitropyrene/nitrofluoranthene/nitroacephenanthrylene).
    Additional Material: 4 Ill.
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  • 15
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 643-646 
    ISSN: 0935-6304
    Keywords: Enantioselective gas chromatography ; Polysiloxane-anchored chiral crown ether stationary phase ; Chirasil-man-18C6-25 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 16
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 655-655 
    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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  • 17
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 655-656 
    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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  • 18
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996) 
    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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  • 19
    ISSN: 0935-6304
    Keywords: Chlorobiphenyl congeners ; Aroclors ; DB-XLB phase ; HP-5/HT-5 serial coupled phases ; GC-ECD ; GC-MS-SIM ; GC-Ion Trap MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Three HRGC systems (1: 30m DB-XLB capillary with MS-SIM detection; 2: 60m DB-XLB capillary with full-scan, ion-trap MS detection; and 3: Parallel dual-column DB-17 and series-coupled HP5/HT5 with ECD detection) were used to completely characterize multiple lots of 8 different-numbered Aroclor mixtures by quantitative calibration against 9 solutions containing primary standards of all 209 PCB congeners. Despite lower absolute sensitivity and more Aroclor congener coelutions than the dual-column ECD system, the MS systems enabled measurement of more congeners per Aroclor since their greater linear response range did not require dilution of samples and standards. Pairs of different lots of Aroclors 1248 and 1254 displayed markedly different proportions of congeners, and the 1254 pair displayed strong differences in the extent of ortho-chlorine substitution. The tables of congener weight percent distributions among Aroclors are more comprehensive and quantitatively precise than those of prior publications. However, the limitations of single-level calibration precluded measurement of all congeners to the ±10% accuracy desirable for establishing these Aroclors as secondary standards for comprehensive, quantitative congener-specific PCB analysis.
    Additional Material: 3 Ill.
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  • 20
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 691-695 
    ISSN: 0935-6304
    Keywords: HPLC ; Molecular sieve ; Cis-trans isomers ; Phenols ; Selectivity ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A molecular sieve known as Silicalite was used as the column packing for HPLC. Silicalite contains channels (or cavities) approximately 6 Å in diameter but, unlike most other molecular sieves, Silicalite is hydrophobic. The retention times of methyl ketones and substituted phenols containing n-alkyl groups increase with increasing chain length of the substituent. However, phenols with very bulky substituents appear to be excluded from the Silicalite channels and elute very quickly. Excellent separations were obtained for a number of compounds with only slight differences in chemical structure. These include phenol isomers with a primary- or secondary alkyl group, position isomers of substituted phenols, and aliphatic cis-trans isomers.
    Additional Material: 10 Ill.
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  • 21
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 229-233 
    ISSN: 0935-6304
    Keywords: Micellar electrokinetic chromatography (MEKC) ; D- and L-Amino acids ; On-column derivatization ; Chiral reagent (OPA/TATG) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 6 Ill.
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  • 22
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 243-243 
    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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  • 23
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996) 
    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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  • 24
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 373-376 
    ISSN: 0935-6304
    Keywords: Enantioselective gas chromatography ; Stable atropisomeric polychlorinated biphenyls (PCBs) ; Elution sequences ; Cyclodextrin derivatives ; Chirasil-Dex ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pure enantiomers of chiral (atropisomeric) polychlorinated biphenyls (PCBs) obtained by high-performance liquid chromatography were used to establish the gas chromatographic elution sequences of the (+)- and (-)-enantiomers of six PCB atropisomers on Chirasil-Dex. The elution order was found to be (-/+) for PCBs 84, 132, 136, and 176 and (+/-) for PCBs 135 and 174. The retention characteristics of all 19 tri- and tetra-ortho atropisomeric PCBs were also investigated. Nine of the atropisomers could be separated using this chiral selector. PCBs 95, 132, and 149 were completely resovled and PCBs 84, 91, 135, 136, 174, and 176 were partially separated (R = 0.7-0.9). All of the separated congeners are 2,3,6-substituted in at least one ring, and conversely - none of the congeners that lacks 2,3,6-substitution could be separated. Thus, chiral recognition and enantiomer separation seems to be strongly governed by 2,3,6-substitution.
    Additional Material: 2 Ill.
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  • 25
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 397-402 
    ISSN: 0935-6304
    Keywords: Solid phase deposition/supercritical fluid elution ; Pesticide recoveries ; Brackish water samples ; EPA method 525.1 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Application of solid phase deposition/supercitical fluid (SPD/SF) elution to real, brackish water samples, obtained from the Chesapeake Bay, has been investigated. The fortified (2ppb) brackish water samples contained suspended sediment, dissolved organic matter and salt. The sediment made post-deposition drying of the SPE disk difficult and the residual water interfered with analyte recovery. Attempts to dry the disk included increasing the vacuum drying time, use of a higher percent of modifier, and desiccation. The best results were obtained by first drying the disk for 10 min under a stream of nitrogen, followed by overnight desiccation, and finally, SF elution. The SF method required a 3 step, 42 min extraction which reduced organic solvent use by 60% compared to traditional elution. All but five analytes met EPA criteria when fresh desiccant was used to dry the disk; four of the unacceptable recoveries were presumably due to plasticizer contamination.
    Additional Material: 1 Ill.
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  • 26
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 413-416 
    ISSN: 0935-6304
    Keywords: Solubility ; Aroma compounds ; Capillary GC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
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  • 27
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 417-417 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 28
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 418-418 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 29
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 339-344 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Trace gas analysis ; Multichannel thick film silicone rubber traps ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Established standard methods for analyzing semi-volatile pollutants by capillary gas chromatography are cumbersome, time-consuming, and expensive. With the longer term aim of replacing the sample preparation procedures with convenient concertrating and thermal desorption steps, thick film silicone rubber traps were constructed in a novel multi-channel configuration. Tests were performed to determine breakthrough volumes and thermal desorption characteristics for total transfer of the trap contents to a capillary column. Initial results are very promising.
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  • 30
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 409-412 
    ISSN: 0935-6304
    Keywords: Micellar electrokinetic chromatography ; Rhei Rhizoma ; Scutellariae Radix ; Coptidis Rhizoma ; Bioactive constituents determination ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A capillary electrophoretic method for simultaneous determination of six bioactive ingredients (berberine, palmatine, baicalin, sennoside B, emodin, and sennoside A) in the Chinse herbal formula San-huang-hsieh-hsin-tang was established. A carrier composed of aqueous buffer solution (50 mM sodium cholate, 15 mM sodium dihydrogen phosphate, and 4.25 mM sodium borate)-acetonitrile (3:2) was found to be the most suitable electrolyte for this separation. Contents of these constituents in a non-pretreated methanol-water extract of San-huang-hsieh-hsin-tang sample could be easily determined within 20 min. The effects of borate, cholate, and organic modifier (acetonitrile) concentration of the carrier on the migration behavior of the solutes were also studied.
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  • 31
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 419-419 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 32
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Purge and trap extraction ; 1,2,4-TCB ; Environmental analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High resolution gas chromatography (HRGC) coupled to a “purge and trap” extraction-injection technique is described as a method of determining 1,2,4-trichlorobenzene in water at levels as low as parts-per-trillion (ppt). In order to investigate the interference from other volatile organic compounds (VOCs) several detection systems were compared: flame ionization, electron capture, and mass spectrometry-multiple ion detection. Concentrations ranging from 15 to 600 ng/L were analyzed in 20 ml standard aqueous solutions. The mean accuracy of the method varied from 89 to 103%, and its mean precision varied from ± 0.85 to ± 7.5 % for all detectors. The detection limits were 20 ng/L for FID, 2 ng/L for ECD and 0.5 ng/L for MID-MS detectors. The procedure was successfully applied to the analysis of industrial waste waters. The necessity of an appropriate internal standard to improve the quantitative determination and to determine possible losses or degradation of 1,2,4-trichlorobenzene during handling or storage is discussed.
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  • 33
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 34
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 492-496 
    ISSN: 0935-6304
    Keywords: High - speed capillary GC ; Carbon dioxide cryotrap ; Deactivated metal tubing ; Thermal decomposition ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ten different metal tubings were investigated for thermal decomposition of analytes when used as the trap tube in a cryotrap/thermodesorption inlet system. No noticeable sample decomposition of hydrocarbons, chlorinated hydrocarbons and a brominated hydrocarbon was observed for six of the tubings with hydrogen as the carrier gas. This observation may be partly attributed to the developed deactivation techniques that produce inert metal tubings that are being widely adopted by many column manufacturers, the different trap materials used in comparison to previous studies and the decreased sample residence time in the hot trap tube. A cryotrap using carbon dioxide was constructed and tested as a alternative to the previously used liquid nitrogen based systems. This cryotrap was able to trap compounds with a boiling point of 80°C.
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  • 35
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 497-502 
    ISSN: 0935-6304
    Keywords: α-Monoacetotriacylglycerides ; Celastraceae ; Fatty acids ; GLC ; GLC-(NCI)MS ; Maytenus seed oils ; OV-225-OH, OH-terminated ; SOP-50, methoxy-terminated ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The seed oils of three Maytenus species have been examined by high temperature GLC using SOP-50 (methoxy-terminated) and OV-225-OH (OH-terminated) glasscapillary columns. The main compounds (71-76%) could be identified as α-mono-acetotriacylglycerols by a combination of high temperature GLC-MS in negative chemical ionization mode with a CH4/N2O mixture as reactant gas and other spectroscopical methods (infrared, 1H- and 13C-nuclear magnetic resonance spectroscopy). The OV-225-OH phase demonstrated better separation properties that the SOP-50 phase for this substance class and up to eight species of α-monoacetotriacylglycerols could be separated. The content of usual triacyclglycerols was below 1%. The results of the analysis of the individual fatty acids as their methyl esters by GC and GC-MS are also presented.
    Additional Material: 2 Ill.
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  • 36
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 515-519 
    ISSN: 0935-6304
    Keywords: Solid phase microextraction (SPME) ; Landfill soil ; VOC ; Headspace ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Solid phase microextraction (SPME) was applied in the development of a protocol for the analysis of a number of target organic compounds in landfill site samples. The selected analytes, including aromatic hydrocarbons, chlorinated hydrocarbous, and unsaturated compounds, were absorbed directly from a headspace sample above a soil layer onto a fused silica fiber. Following exposure, the fiber was thermally desorbed in the injection port of the gas chromatograph and eluted compounds were detected using a mass selective detector. The stability and sensitivity of the extraction technique were examined at five temperatures (22-60°C) using a 100μm polydimethylsiloxane fiber. Calibrations, using soil samples spiked with selected solvents (0.5-30 μg/g), were linear; trichloroethene (r2 = 0.992) and benzene (r2 = 0.998). SPME was applied to the examination of a municipal landfill where 8 sites were sampled, at three depths, resulting in the detection of xylene (maximum 2.8 μg/g) and a number of other non-target organic contaminants.
    Additional Material: 4 Ill.
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  • 37
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 534-534 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 38
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 674-678 
    ISSN: 0935-6304
    Keywords: Micellar electrokinetic chromatography (MEKC) ; Organic modifiers ; Alcohols ; Chain length ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The influence of alcohol modifiers with different chain length on the migration time window in micellar electrokinetic chromatography (MEKC) has been studied. Highly polar alcohols like methanol and 1-propanol are typical aqueous phase modifiers. Higher alcohols like 1-butanol, 1-pentanol and 1-hexanol influence the micellar structure and are considered as micellar phase modifiers. The effect of long chain alcohols is small because of their low applicable concentrations.
    Additional Material: 10 Ill.
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  • 39
    ISSN: 0935-6304
    Keywords: Programmed temperature vaporization injection ; Volatile organic compounds ; Isoprene ; Biogenic emissions ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method has been developed for the automated determination of C5—C10 and C2—C6 volatile organic compounds in urban and rural air, using programmed temperature vaporization injection from a sorbent tube trap. A single activated charcoal sorbent tube was repeatedly used to collect samples of air with trapped VOCs being subsequently desorbed onto either a wide bore dimethyl polysiloxane (C5—C10) or porous layer open tubular (C2—C6) gas chromatography column without use of intermediate cryogenic refocussing. The high flow rates of helium used during the analysis resulted in the sample tube being cleaned and ready to reuse following the analytical separation. Examples of analysis of aromatic VOCs in urban air, and biogenic emissions in rural air, collected in a Sitka Spruce forest are presented. Using this method it is possible to quasi-continuously monitor concentrations of VOCs in locations where high sensitivity in situ analysis is required, but where cryogenic coolants may not be readily available or desirable.
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  • 40
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 59-61 
    ISSN: 0935-6304
    Keywords: Steam chromatography ; Salt-water stationary phases ; Retention of alcohols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 41
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    Journal of High Resolution Chromatography 19 (1996), S. 65-65 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 42
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 117-120 
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction, SFE ; Solid phases ; Analyte breakthrough ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 43
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    Journal of High Resolution Chromatography 19 (1996), S. 121-123 
    ISSN: 0935-6304
    Keywords: 2-Alkyl-branched fatty acids ; Enantioselective gas chromatography ; Modified cyclodextrin ; Polysiloxanes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 44
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 45
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    Journal of High Resolution Chromatography 19 (1996), S. 131-136 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Kraft process liquors ; Inorganic anions ; Sulfur specification ; Direct and indirect detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Various sulfur containing anions (sulfate, sulfite, and thiosulfate) in Kraft pulping process liquors are determined by capillary electrophoresis. In addition, other inorganic anions (hydroxide, chloride, oxalate, carbonate) are analyzed with the developed method. Through optimization of the separation conditions it is possible to simultaneously determine these anionic species in pulping liquors with direct and indirect UV detection at 185, 214, and 254 nm. To ensure short separation times a migration of the anionic analytes in the same direction as the electroosmotic flow (co-electroosmotic CE) is established by reversal of the electroosmotic flow with 1,5-dimethyl-1,5-diazaundecamethylene polymethobromide (hexadimethrine bromide; HDB; polybrene™) which is added to the electrolyte as EOF modifier. The impact of acetonitrile as organic modifier to improve the selectivity of the anionic analytes is also investigated. The developed method is then applied to analyze and quantify various anions in pulping liquors (white and black liquors). By simultaneously determining the hydroxide concentration it is possible to calculate effective alkalinity and sulfidity with the measured concentrations without the need of volumetric methods.
    Additional Material: 9 Ill.
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  • 46
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    Journal of High Resolution Chromatography 19 (1996), S. 155-160 
    ISSN: 0935-6304
    Keywords: Solid phase microextraction (SPME) ; Headspace analysis ; Gastight syringe ; Water analysis ; Volatile organic compounds (VOCs) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Headspace solid phase microextraction (headspace SPME) has been demonstrated to be an excellent solvent-free sampling method. One of the major factors contributing to the success of headspace SPME is the concentrating effect of the fiber coating toward organic compounds. The affinity of the fiber coating toward very volatile analytes, such as chloromethane, may, however, not be large enough for detection at the parts per trillion concentration level. Static headspace analysis, on the other hand, is very effective for these very volatile compounds. As analyte volatility decreases, the sensitivity of static headspace analysis drops. The complementary nature of these two sampling methods can be exploited by combining the SPME device with a gastight syringe. The sensitivity of the new sampling device is better than that of SPME for very volatile compounds or that of static headspace analysis for less volatile compounds. This new method can sample a wide range of compounds from chloromethane (b.p. -24°C) to bromoform (b.p. 149°C) with estimated limits of detection at the low parts per trillion level.
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  • 47
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    Journal of High Resolution Chromatography 19 (1996), S. 169-175 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography ; Open tubular columns ; Retention behavior ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The elucidation of the detailed mechanism of retention in supercritical fluid chromatography (SFC) is a complex problem, especially for high-density supercritical fluid mobile phases. Martire and Boehm developed a theory of SFC retention based on a statistical thermodynamic treatment, and introduced a density-squared equation for retention in SFC: In k = a + b/T + cρ + dρ/T + eρ2/T. In this paper the systems n-alkane-polydimethylsiloxane-CO2 and n-carboxylic acid methyl ester-polydimethylsiloxane-CO2 have been treated using the method introduced by Martire and Boehm. In the ranges of reduced temperature from 1.079 to 1.293 and reduced SF mobile phase density from 0.705 to 1.632, two problems were discovered in the treatment of SFC retention behavior by the method of Martire and Boehm: (1) the experimental value of the site of CO2 in the lattice field, ra, of the two systems was ca 0.9, which is obviously different from the theoretical values of 3.6 or 5.4; and (2) the difference between experimental and calculated retention values increased with increasing SF mobile phase density. The minimum in SFC retention predicted by Martire and Boehm was not observed. On the basis of some assumptions and the experimental data, the following retention equation was derived: In k = a + b/T + cρ + dρ/T + eρ2/T + fρ3/T + gρ4/T. This equation was consistent with the experimental data and can conveniently be used to explain other SFC retention behavior.
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  • 48
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    Journal of High Resolution Chromatography 19 (1996), S. 535-542 
    ISSN: 0935-6304
    Keywords: On-line LC-GC coupling ; Fully concurrent eluent evaporation ; Sample pretreatment ; Residue analysis ; Complex biological matrices ; Pyrethroid insecticide ; Acrinathrin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The following paper presents a fast, selective, sensitive, and automated procedure for the residue analysis of the pyrethroid insecticide acrinathrin in various fruit samples by on-line combination of Liquid Chromatography (LC) with capillary Gas Chromatography (GC) and an Electron-Capture Detector (ECD). The loop-type interface and Fully Concurrent Solvent Evaporation (FCSE) were chosen due to their ease of use and low volatility of acrinathrin. Commercially available LC diol columns with small internal diameters (2.1 mm) provided the selectivity required for the separation of the solute from matrix components and permitted the transfer of fraction volumes up to 500 μl into the retention gap, located inside the gas chromatograph. Optimization of the operating conditions with standard solutions showed the influence of the GC initial transfer temperature on the response of acrinathrin and the quantitative nature of the transfer was established by liquid scintillation counting. The linearity and precision were studied with the aid of calibration plots, whereas quantitative recoveries of the analyte (at least 95 %) were determined in spiked fruits. Compared to the corresponding off-line technique, the on-line approach allows us to reach lower detection limits (ppb level when 20 μl LC injections are performed) with excellent repeatability between 0.6 and 6.6 %. Moreover, the integrated analytical set-up is robust, less time-consuming and subsequently brings a marked improvement in the sample preparation step of complex biological matrices. Finally, the versatility of the system renders it highly suitable for the determination of other similar pyrethroids in order to develop a multiresidue method.
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  • 49
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    Journal of High Resolution Chromatography 19 (1996), S. 571-576 
    ISSN: 0935-6304
    Keywords: Hollow fiber membranes ; Water analysis ; Volatile organic compounds ; Trace enrichment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
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  • 50
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    Journal of High Resolution Chromatography 19 (1996), S. 111-116 
    ISSN: 0935-6304
    Keywords: Polynuclear aromatic hydrocarbons ; Liquid chromatography ; Alcohols ; Micelles ; Enviromental samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method for the separation of polycyclic aromatic hydrocarbons (PAHs) by high-performance liquid chromatography using a hybrid micellar mobile phase is described. The detection of PAHs was carried out using the fluorescence method with programmable excitation and emission wavelength. The method is applied to the analysis of several environmental samples (sea water, sediments, limpets, sea worms) and several of these compounds are quantitated at concentration below 70 ng L-1(kg-1) in the original samples.
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  • 51
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    Journal of High Resolution Chromatography 19 (1996), S. 588-590 
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction ; Water samples ; Polycyclic aromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
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  • 52
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    Journal of High Resolution Chromatography 19 (1996), S. 143-150 
    ISSN: 0935-6304
    Keywords: Capillary zone electrophoresis ; Cyclodextrin ; Aromatic carboxylic acids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method using capillary zone electrophoresis has been developed for separation of a series of isomeric benzene polycarboxylic acids. The separation was found to depend largely on the geometry of the acids and their degree of ionization as well as on the buffer pH and composition. The presence of additives to the buffer such as cyclodextrin and cationic surfactants was found necessary for complete resolution of all the isomers.
    Additional Material: 14 Ill.
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  • 53
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    Journal of High Resolution Chromatography 19 (1996), S. 257-262 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Solid-phase microextraction ; Food analysis ; Wine bouquet ; Monoterpenes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The extraction, identification, and quantification of wine aroma compounds are preliminary steps required for further investigation of wine quality, i.e. determination of the varieties of grapes used, the production process, and the origin and age of the wine. This paper deals with the optimization of solid-phase microextraction for the determination of compounds which produce wine bouquet. Optimum operating conditions have been determined to obtain high reproducibility at low cost and with low time-consumption. Several factors influencing the equilibrium of the aroma compounds between the sample and the fiber must be taken into account, including length of contact time between the two phases involved, speed of agitation of the sample, the matrix in which the process takes place, and, furthermore, the place, duration, and temperature of desorption in the injector of the chromatograph.
    Additional Material: 8 Ill.
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  • 54
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    Journal of High Resolution Chromatography 19 (1996), S. 272-276 
    ISSN: 0935-6304
    Keywords: Capillary gas-solid chromatography ; PLOT column ; Correlation equations for retention values ; Carbon dioxide as carrier gas ; Separation of hydrocarbon gases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In capillary gas-solid chromatography where interactions between solute and carrier gas and adsorption of the solute on the surface of the adsorbent are considered to be imperfect, it has been shown that chromatographic retention is determined largely by adsorption processes. It has been established that correlation relationships k(P2)=A k(P1) + B, where k is the retention factor, and A and B are equation constants, was valid for use of different carrier gases P1 and P2. Column efficiency could be improved by use of carbon dioxide. The advantages of using carbon dioxide as the carrier gas were investigated.
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  • 55
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    Journal of High Resolution Chromatography 19 (1996), S. 165-168 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Liquid chromatography ; Solvent venting ; Cholesterol ; Pig fat ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two methods for determination of cholesterol in fat and muscle of pig were evaluated: extraction with chloroform:methanol (2:1, v/v) followed by saponification (method 1) and direct saponification (method 2). HPLC and GC were used to determine cholesterol concentrations. GC analysis was performed with a capillary column of 100 μm using a PTV injector in the modes of cold split and solvent venting. Cholesterol was analyzed without derivatization. Both methods of extraction did not present significant differences (p 〉 0.01). Sample analysis by GC with solvent venting injection and HPLC showed the lowest % r.s.d. but GC in the cold split mode allowed to obtain a shorter analysis time. Cholesterol concentrations obtained by HPLC were not statistically different from the results obtained by GC with solvent venting injection and were slightly lower than those previously reported. Cholesterol concentrations in fat and muscle tissues respectively ranged from 52 to 77 mg/100 g and from 55 to 65 mg/100 g.
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  • 56
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    Journal of High Resolution Chromatography 19 (1996) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 57
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    Journal of High Resolution Chromatography 19 (1996), S. 183-188 
    ISSN: 0935-6304
    Keywords: Chelating agents ; Complexation ; Capillary zone electrophoresis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A capillary electrophoretic method has been developed which achieves rapid quantitative separation and determination of ethylenediaminetetraacetic acid, N-(2-hydroxyethyl)ethylenediaminetriacetic acid, diethylenetriaminepentaacetic acid, ethylenediaminediacetic acid, and nitrilotriacetic acid in Hanford tank waste simulant (TWS). Direct UV detection of Cu2+/chelator complexes is used to achieve enhanced sensitivity. The qualitative and quantitative reliability of the method and the quality of separations, as given by efficiency and resolution, is presented. In addition, the limits of detection and linearity of detector response with concentration are given for each chelator. The selection of Cu as the UV-absorbing species over other transition metals present in the waste is discussed.
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  • 58
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    Journal of High Resolution Chromatography 19 (1996), S. 200-206 
    ISSN: 0935-6304
    Keywords: High performance liquid chromatography ; High resolution gas chromatography ; Capillary zone electrophoresis ; Carbamate ; Carbaryl ; Carbofuran ; Tobacco ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Determination of carbamate residues in tobacco samples was carried out by three different methods, two having been described in the literature and one developed for the purpose of this work. The extracts were analyzed by HRGC-FID (using derivatization), by HPLC-RP with photodiode array detection and by Capillary Zone Electrophoresis (CZE) with UV detection. The extraction method developed used in conjunction with capillary zone electrophoresis showed to be the most suitable for carbamate residue analysis in real tobacco samples. The developed method presented better recovery results in relation to the others. CZE allowed the determination of carbamate residue in real tobacco sample while HPLC and HRGC could not do this, due to co-elution problems.
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  • 59
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    Journal of High Resolution Chromatography 19 (1996), S. 224-224 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 60
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    Journal of High Resolution Chromatography 19 (1996), S. 224-224 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 61
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    Journal of High Resolution Chromatography 19 (1996), S. 696-696 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 62
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    Journal of High Resolution Chromatography 19 (1996), S. 696-696 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 63
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    Journal of High Resolution Chromatography 19 (1996), S. 703-705 
    ISSN: 0935-6304
    Keywords: Drug-related impurities ; Capillary electrophoresis (CE) ; Betamethasone sodium phosphate ; Bromhexine hydrochloride ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 64
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    Journal of High Resolution Chromatography 19 (1996), S. 709-709 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 65
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    Journal of High Resolution Chromatography 19 (1996), S. 245-245 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 66
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    Journal of High Resolution Chromatography 19 (1996), S. 284-284 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 67
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    Journal of High Resolution Chromatography 19 (1996), S. 285-290 
    ISSN: 0935-6304
    Keywords: High speed GC ; Computer-aided GC design ; Instrument evaluation ; Instrument model ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Several commercially available chromatographs have been evaluated with respect to their ability to support high speed chromatography. Both autoinjection and trap and thermal pulse injection are both found to be suitable procedures to deliver the required narrow sample injection peak widths. However, even with the appropriate injectors in place, the systems are burdened with relatively slow data acquisition rates and large amplifier time constants that further degrade system performance and make them unsuitable for the high speed chromatography discussed herein. The study was conducted using a computer implemented model of a gas chromatograph's output.
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  • 68
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    Journal of High Resolution Chromatography 19 (1996), S. 298-300 
    ISSN: 0935-6304
    Keywords: Dynamic head space ; Coffee berry ; Identification ; Hypothenemus hampei ; Plant-insect relationship ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Tab.
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  • 69
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    Journal of High Resolution Chromatography 19 (1996), S. 277-283 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Coupled columns ; Four factor optimization ; Simplex method ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Optimization of a gas chromatographic system with two capillary columns coupled in series in a single oven for the linear temperature programmed separation of a mixture of C1—C10 hydrocarbons has been carried out using the simplex optimization method. The following four selectivity parameters were optimized: the initial temperature of the oven; the initial hold time; the temperature programmed rate; and the pressure at the mid-point of the system. The optimization procedure was monitored by the Cp criterion.
    Additional Material: 3 Ill.
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  • 70
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. VII 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 71
    ISSN: 0935-6304
    Keywords: Electrokinetic chromatography (EKC) ; Anionic cyclodextrins ; Enantiomer separation ; Pseudo-stationary Phase ; Neutral racemates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Separations of neutral and basic racemates were performed using five different anionic cyclodextrin (CD) derivatives as chiral selectors, viz. carboxymethylated β-CD, β-CD phosphate sodium salt, sulfobutyl ether β-CD sodium salt, carboxymethylated γ-CD, and γ-CD phosphate sodium salt. For the separation of neutral racemates, an untreated fused silica capillary was employed and various neutral racemates were successfully separated. Since the pH of the buffer affected the electroosmotic flow (EOF), the resolution was improved by changing the buffer pH. A polyacrylamide coated capillary was employed for the separation of basic racemates to suppress EOF and to prevent adsorption of cationic analyte on the capillary surface. By choosing an appropriate type and concentration of anionic CD, about 40 basic racemates were successfully separated. Some rough binding constants of basic analytes with an anionic β-CD were measured to discuss the optimum concentration of the CD. The migration direction was dependent on the binding constants and the concentration of the CD. The analyte strongly bound to the anionic CD migrated towards the anode but the weakly bound one moved towards the cathode. Anionic γ-CDs were also very useful for the separation of basic enantiomers. Five neutral CDs were employed as chiral selectors to compare selectivity between charged and neutral CDs, and eleven racemates could only be resolved using anionic CDs. The separation of some basic racemates in human plasma was also described. The direct injection of plasma samples was possible for some enantiomers that did not interact strongly with plasma proteins.
    Additional Material: 10 Ill.
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  • 72
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    Journal of High Resolution Chromatography 19 (1996), S. 462-462 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 73
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 464-464 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 74
    Electronic Resource
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 469-471 
    ISSN: 0935-6304
    Keywords: Microextration ; GC/MS ; Chlorobenzenes ; Water samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 75
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 377-382 
    ISSN: 0935-6304
    Keywords: Capillary chromatography ; Boiling points prediction ; Identification ; Chlorobenzenes ; Phenols ; Programmed temperature ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Quantitative correlations between physicochemical parameters and structure of various solutes and their gas chromatographic behavior were investigated in order to predict the retention values. The identification of unknown samples in gas chromatographic routine analysis of environmental samples is enhanced by the use of these correlations in conjuction with other chromatographic methods and with mass spectrometry. The boiling points of many compounds are easily found in literature and therefore their correlation with retention values obtained in isothermal or programmed temperature analysis permit restriction of the choice of names of unknown compound to within a narrow range. The correlation between the boiling points and the retention times of chloro- and bromo-benzenes and of some chloro- and nitro- substituted phenols was investigated on non-polar capillary columns and permitted the tentative identification of many compounds belonging to these homologous series.
    Additional Material: 3 Ill.
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  • 76
    ISSN: 0935-6304
    Keywords: Multidimensional gas chromatography (MDGC) ; Chiral polychlorinated biphenyls (PCBs) ; Enantiomeric ratio ; Shark ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chiral 2,2′,3,5′,6-pentachlorobiphenyl (PCB 95), 2,2′,3,3′,4,6′-hexachlorobiphnyl (PCB 132) and 2,2′,3,4′,5′,6-hexachlorobiphenyl (PCB 149) were quantified in Atlantic Ocean shark liver samples (C. coelolepis) by gas chromatography-mass spectrometry (GC-MS) and their enantiomeric ratios were studied by multidimensional gas chromatography (MDGC) with an achiral-chiral column combination and detected by ECD and MS/SIM. The concentration range of the chiral PCBs was from 2 to 6 ng/g (fresh weight), which represents 2-6 % of the total PCB mean concentration. The investigations revealed a small enantiomeric bias of PCB 132 in most of the samples studied (ER = 0.75-0.89, ee = 6-14%), while PCB 95 and PCB 149 were present in racemic or almost racemic form.
    Additional Material: 2 Ill.
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  • 77
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 403-408 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Cryogenic trapping ; Capillary ; Focusing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cryogenic trapping of solutes leads to narrowing of the chromatographic band. By placing the trap at the end of a capillary column, it is possible to study the effectiveness of the trap in terms of producing a sharpened elution profile. The trap may be heated by supplementary heating, but here convective heating from the GC oven is employed simply by turning off the cryogenic coolant. It is estimated that it takes about 50 s for the trap to heat up sufficiently to allow trapped solute to be remobilized, although this depends upon the oven temperature and thermal mass of the trap. It can also be shown that the more volatile solutes mobilize faster from the trap in this particular mode of operation. The recovery of trapped components shows that there is essentially quantitative trapping, and the solutes are trapped just at the leading edge of the trap.
    Additional Material: 4 Ill.
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  • 78
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    Journal of High Resolution Chromatography 19 (1996), S. 420-420 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 79
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996) 
    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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  • 80
    Electronic Resource
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 449-456 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography (SFC) ; Packed columns ; Pressure drop ; Selectivity ; Resolution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The influence of pressure drop on retention, selectivity, plate height and resolution was investigated systematically in packed supercritical fluid chromatography (SFC) using pure carbon dioxide as the mobile phase. Numerical methods developed previously which enabled the prediction of pressure gradients, diffusivities, capacity factors, plate heights and resolutions along the length of the column were used for the model calculations. The effects of inlet pressure and supercritical fluid flow rate on selectivity and resolution are studied. In packed column SFC with pure carbon dioxide as the mobile phase, the pressure drop can have a significant effect on resolution. The flow rate is shown to have a larger effect than generally realized. The calculated data are shown to be in good agreement with the experimental results. Finally, the variation of the chromatographic parameters along a 5.5 meter long model SFC column is illustrated. The possibilities and limitations of using long packed columns in SFC are discussed. It is demonstrated that long columns with large plate numbers do not necessarily yield better separations.
    Additional Material: 7 Ill.
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  • 81
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 585-587 
    ISSN: 0935-6304
    Keywords: Enantioselective gas chromatography ; Volatiles ; 2-Heptanol ; Ethyl benzoate ; (E)-Hex-2-enal ; 1-Terpinen-4-oI ; Rubus glaucus ; Rosaceae ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Tab.
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  • 82
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 591-594 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Formaldehyde ; Acetaldehyde ; Nickel catalyst ; Flame ionization detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 83
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 622-626 
    ISSN: 0935-6304
    Keywords: Multidimensional capillary chromatography ; Polychlorinated biphenyls ; PCBs ; Congener ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Multidimensional chromatography was used to resolve the specific chlorobiphenyl (CB) congeners 28, 52, 101, 118, 138, 153, and 180 in technical aroclor standards. Single column analysis of polychlorinated biphenyls (PCBs) results in co-elution of key congeners with other components in the mixture; therefore using two columns of different selectivity was necessary to enhance the resolution achievable on just one column. The HT8 column (8% phenylpolycarborane-siloxane phase) has been reported to have specific selectivity characteristics for improved PCB separation. When coupled with a BPX5 column (5% phenylpolysiloxane-silphenylene phase), it has been shown here to provide unambiguous identification of 7 marker compounds which are used to monitor PCB occurrence and distribution. All seven marker CBs are present in aroclor 1254, and by adjusting the size of the heartcut window, it was possible to obtain resolution of the marker congeners from other congeners. Single column analysis is unable to achieve this result. This offers an alternative to GC-MS analysis.
    Additional Material: 3 Ill.
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  • 84
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 633-638 
    ISSN: 0935-6304
    Keywords: High performance liquid chromatography ; Solid phase extraction ; Low molecular weight aliphatic amines ; Fluorescamine (Fluram) ; Environmental waters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A high resolution liquid chromatographic method is described for determination of low molecular weight (LMW) aliphatic amines in environmental waters. The analytes after isolation are derivatized by fluram and separated with isocratic elution on octyl (C8) column, followed by fluorimetric detection in 395/495 nm. Different isolation procedures such as octadecylsilane (ODS) and strong cation exchanger (SCX) solid phase extraction (SPE) cartridges and Amberlite CG-120 resin were evaluated. The quantitative characteristics such as recovery, linear dynamic range, correlation coefficient, limit of detection (LOD), and relative standard deviation (RSD) are presented. Using this method, aliphatic amines were analyzed in rain and tap water as well as in waste water.
    Additional Material: 4 Ill.
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  • 85
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 700-702 
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction, SFE ; HPLC ; On-line coupling ; Triazines ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 2 Ill.
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  • 86
    ISSN: 0935-6304
    Keywords: HPLC of phenols ; Dianthus caryophyllus ; Carnation vascular wilt ; Fusarium oxysporum f. sp. dianthi ; Root phenolic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Ill.
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  • 87
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 32-36 
    ISSN: 0935-6304
    Keywords: Alumina PLOT column ; Column selectivity ; Hydrocarbon gases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Alumina-coated porous layer open tubular (PLOT) columns are widely used for analyses of light hydrocarbons (C1 to C6). There is, however, a need for improved selectivity for complex analyses such as the determination of impurities in high purity petrochemical products. Some commercial alumina PLOT columns do not have sufficient selectivity for such analyses. The selectivity of four commercial alumina PLOT columns is evaluated for analyses of propylene and ethylene, and differences in column selectivity discussed. Requirements of column selectivity and retention are presented for several applications including the analysis of refinery gas, transformer oil gas, and fuel gas.
    Additional Material: 5 Ill.
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  • 88
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    Journal of High Resolution Chromatography 19 (1996), S. 37-42 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The headspace gas in static headspace gas chromatography contains mostly saturated water vapor. In the case of the cryofocusing enrichment technique this may cause baseline distortion in the early part of the chromatogram or may even lead to ice-plugging of the capillary column. A water-trap is described in which the water vapor is removed from the headspace gas before entering the cryo-trap. The water trap is packed with lithium chloride on a porous support and is regenerated after each analysis by heating under backflush conditions. It therefore can be used for automatic operation. Data are given for the precision and accuracy, and some practical examples, for environmental and flavor analysis are shown.
    Additional Material: 6 Ill.
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  • 89
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. iii 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 90
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 69-79 
    ISSN: 0935-6304
    Keywords: Large volume injection ; PTV injector ; Water analysis ; River sediment ; Pesticides ; Polycyclic aromatic hydrocarbons (PAHs) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Temperature programmable (PTV) injectors with packed widebore (ca. 3.5 mm i.d.) liners are used for large volume injection in capillary gas chromatography with the aim to simplify and/or improve off-line sample pretreatment proecdures. A simple procedure for optimization of large volume PTV injection is described. The system performance, i.e. linearity and repeatability, is evaluated for polar nitrogen/phosphorus containing pesticides (PTV-GC-NPD) and organochlorine pesticides (PTV-GC-ECD) in river water extracts as well as for polycyclic aromatic hydrocarbons (PAHs) in river sediment (PTV-GC-MS).
    Additional Material: 8 Ill.
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  • 91
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 85-90 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A windowless pulsed discharge photoionization detector (PDPID) is described which uses the emission spectra from the discharge in helium and Ar/Kr doped helium. The emission from helium is a continuum ranging from 13.5-17.7 eV which ionizes all compounds except neon. The emission from 5.4% Ar/He ranges from 9.3-11.8 eV and ionizes most organic compounds and many inorganic compounds. The emission from 1.36% Kr/He consists principally of the resonance lines at 10.6 and 10.1 eV. These PDPIDs are used to analyze a 12 component mixture containing principally chloro alkane/alkene. The relative responses of the PDPID combined with the relative retention time can be used to qualitatively identify the chloro compounds.
    Additional Material: 5 Ill.
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  • 92
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 91-94 
    ISSN: 0935-6304
    Keywords: Chiral selector anchored to polysiloxane ; Chiral phase capillary GC ; Immobilization ; Thermal treatment ; High enantioselectivity ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The chiral selector L-t-leucine-t-butylamide has been anchored to a polysiloxane by nucleophilic displacement of 2,2,2-trifluoroethyl ester-functionalized block polysiloxanes with L-t-leucine-t-butylamide. Attempts were made to immobilize the chiral polysiloxanes inside the capillaries by thermal treatment at 300°C for 30-90 min. The polysiloxanes were found to be more resistant than Chirasil-Val to the racemization caused by such high temperature treatment. Capillary columns coated with this type of immobilized polysiloxane have shown very high enantioselectivity and thermal stability.
    Additional Material: 3 Ill.
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  • 93
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 99-104 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Micellear electrokinetic chromatography ; Organic modifiers ; Naphthalene sulfonates ; Surface water ; Thermostatting ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The production and use of naphthalene sulfonates can easily cause pollution of surface and other types of waters. In the present study, capillary electrophoresis in combination with UV absorption detection was used to separate 21 amino- and hydroxy-substituted naphthalene sulfonates which included multiple isomeric compounds. The influence of various parameters such as pH (which turned out to be extremely important), temperature of the surrounding air flow, and the use of buffer additives (micelles, cyclodextrins, organic modifiers) was studied. Complete separation of all analytes including the isomers, was achieved in two runs with a 50 mM boric acid/borate buffer, containing either 100 mM sodium dodecylsulfonate or 15% acetonitrile. The limits of detection obtained for the individual compounds typically were 20μgI-1. River water samples spiked at this concentration level could be analysed using a simple three-step sample clean-up procedure.
    Additional Material: 6 Ill.
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  • 94
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 511-514 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Enantiomer separation ; Amino acids ; N-Alkyloxycarbonyl alkylamide derivatives ; Nucleophilic substitution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The enantiomers of amino acids were first converted into N-alkyloxycarbonyl 2,2,2-trifluoroethyl esters, and then into N-alkyloxycarbonyl alkylamides by nucleophilic substitution of the ester group with amines. The first reaction proceeds instantaneously, while the second substitution occurs smoothly with n-propylamine and isobutylamine. The final derivatives were produced for separation on a capillary column coated with Chirasil-Val by GC. Pro, which is difficult to separate completely as its N-perfluoroacyl alkyl ester derivative, showed complete separation of the enantiomeric pair. All amino acids examined in this study showed an increased separation factor.
    Additional Material: 3 Ill.
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  • 95
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 520-520 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 96
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 217-223 
    ISSN: 0935-6304
    Keywords: High speed chromatography ; Sulfur compounds ; Photoionization detection ; Trace analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: There is a need for rapid, on-line, gas chromatographic analysis of trace levels of hydrogen sulfide and carbon oxysulfide in the oil-from-coal industry. In order to improve an existing method based on a polymer bed concentrator, a porous layer open tubular column, and a flame photometric detector, time-optimization of the various steps involved was attempted. Use of a redesigned concentrator, changed column operating conditions, and a photoionization detector reduced analysis times from 6.5 to 3 min and cycle times from 8 to 3 min. This could be achieved without compromising the 10 ppb detection limit required.
    Additional Material: 11 Ill.
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  • 97
    ISSN: 0935-6304
    Keywords: Chlorinated biphenyls ; Atroipisomer separation ; Multidimensional GC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A simple dual-column gas chromatographic system with a six-port switching valve has been used to separate the atropisomers of PCB congeners 84, 91, and 95 in technical PCB formulations and in extracts of soil and river sediment. A capillary column coated with a methylphenylsiloxane stationary phase (CP-Sil 8) was used as the first column, for retention window selection, and a permethylated β-cyclodextrin (ChirasilDex) capillary column as the main separation column. Because peak overlap could not be eliminated by optimization of column temperature, the enantiomeric ratios of PCB congeners could not be determined from the original chromatograms. The correct enantiomer ratio was determined from the peak areas obtained by deconvolution of the chromatograms. Whereas the PCB atropisomers considered were present in equal concentrations in the technical PCB formulations, analysis of a river sediment sample confirmed different residual concentrations of the atropisomers of congener 95.
    Additional Material: 6 Ill.
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  • 98
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 99
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 263-266 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Mass spectrometry ; Purge and trap ; Vegetable oil ; Soya oil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The analysis of volatile compounds, and particularly of certain hydrocarbons, e.g. pentane, and some aldehydes, e.g. hexanal, has been used to estimate the degree of oxidation of vegetable oil. We have tested a dynamic headspace technique without heating the sample during the purge time of the analysis. Some tests have been performed after heating the sample at 180°C for a specified time before the analysis, to compare the results of analysis with and without heating. The best results were obtained at room temperature.
    Additional Material: 3 Ill.
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  • 100
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 151-154 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Atomic emission spectroscopy ; Enantiomeric separation ; Cyclodextrins ; Chemical warfare agents ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of the organophosphorus nerve agents sarin, tabun, and cyclohexyl methylphosphonofluoridate (GF) produces a mixture of two stereoisomers except for soman where four stereoisomers are produced. Significant differences exist in the reported toxicity and AChE inhibition rates of the various stereoisomers. This makes the ability to distinguish between the different stereoisomers desirable. Five different derivatized cyclodextrin stationary phases developed for gas chromatography were tested for their ability to resolve the nerve agent stereoisomers using a gas chromatograph interfaced to an atomic emission detector. Of the five columns that we examined, only the 2,6-di-O-pentyl-3-O-trifluoroacetyl or 2,6-di-O-pentyl-3-O-butyryl γ-cyclodextrins were able to successfully resolve all four soman stereoisomers. The elution order for each column was determined using solutions of isolated soman stereoisomers. Enantiomers of sarin, tabun, and GF were resolved with varying degrees of success on the different cyclodextrin stationary phases. Only the butyryl γ-cyclodextrin was able to separate the enantiomers of all four of the nerve agents examined in this study. The capacity (k) and selectivity (α) factors were determined for each of the chemical warfare agents successfully separated. The TNO Prins Maurits Laboratory in the Netherlands has previously developed several different chromatographic methods to resolve the stereoisomers of soman, sarin, and tabun. The advantage of the method described here is that commercially available cyclodextrin gas chromatography columns were used to resolve the stereoisomers, thereby facilitating rapid and routine analysis of organophosphorus nerve agents.
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