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  • Articles: DFG German National Licenses  (15,816)
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  • Articles: DFG German National Licenses  (15,816)
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Years
  • 101
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 44 (1997), S. 320-324 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Wine analysis ; Pesticides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid method based on gas chromatography which determines parathion-methyl, fenitrothion, chlorpyrifos, dichlofluanid, vinclozolin, chlozolinate, procymidone and iprodione is described. It involves quantitative extraction with n-hexane and determination by capillary gas chromatography using an electron capture detector. Pesticides were satisfactorily separated in 15 min with a phenylmethylsilicone fused-silica capillary column under isothermal conditions. Quantitation was carried out using dieldrin as internal standard. The method seems appropriate for oenological laboratory work because of its simplicity and rapidity. It was successfully used to identify and quantify pesticides studied in musts and wines.
    Type of Medium: Electronic Resource
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  • 102
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Temazepam in plasma ; Pharmacokinetic studies ; Rats
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A sensitive method was developed for the determination of temazepam in plasma using capillary gas chromatography. After the extraction into dichloromethane-pentane (1∶1), temazepam was quantitated as its O-trimethylsilyl derivative on a capillary column with a63Ni electron capture detector using prazepam as internal standard. The detector response was found to be linear in the concentration range 0.031 to 8 μg mL−1. The detection limit was about 3.5 ng mL−1. The intraday and inter-day coefficients of variation were below 9%. The method was used to determine the pharmacokinetic profile of temazepam in rats after intravenous administration.
    Type of Medium: Electronic Resource
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  • 103
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Surface ionization detection (SID) ; Cocaine ; Cocaethylene ; Cocapropylene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Cocaethylene together with cocaine spiked in human whole blood has been found measurable at high sensitivities by capillary gas chromatography with surface ionization detection. The drugs could be rapidly extracted by Sep-Pak C18 cartridges with recovery of more than 60%. The calibration curves for both cocaethylene and cocaine using cocapropylene as internal standard were linear in the range 50–300 pmol mL−1 of whole blood. The detection limits of cocaethylene and cocaine were 5–10 pmol mL−1 (0.1–0.2 pmol on column if recovery is 100%). Cocaethylene could be determined for whole blood obtained from rats (ca. 200 g body wt.), which had received subcutaneous injection of 10 mg cocaine hydrochloride and 2.0 mL of 30% (v/v) ethanol 3 h before sampling; the mean levels of cocaethylene and cocaine were 101 and 1230 pmol mL−1, respectively.
    Type of Medium: Electronic Resource
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  • 104
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary phases ; Isomer separation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Heptakis(2,6-di-O-benzyl)-β-CD(I), heptakis(2,6-di-O-benzyl-3-O-pentyl)-β-CD(II), heptakis(2,6-di-O-benzyl-3-O-methyl)-β-CD(III) and heptakis(2,6-di-O-benzyl-3-O-acetyl)-β-CD(IV) derivatives were synthesized and identified. Their thermal stabilities were tested using PyGC. These CD derivatives are stable up to 300°C and suitable for use as gas chromatographic stationary phases. The fused silica capillary columns coated with heptakis(2,6-di-O-benzyl-3-O-methyl)-β-CD and heptakis(2,6-di-O-benzyl-3-O-pentyl)-β-CD showed excellent chromatographic properties in separating positional isomers.
    Type of Medium: Electronic Resource
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  • 105
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 10-16 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Purge and Trap ; Flavors ; Wine ; Polar analytes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (not readable) fully autimated purge and trap system has been developed for (not readable) detemination of volatile wine components. The proposed system consists of sampler, a purge and trap instrument, and a GC, (not readable) steps, from the uptake of the infiltrated wine from the sampler (not readable) to the printout of the intergrated chromatograms, proceed(not readable), Typical problems occurring when analyzing polar analytes by the classical purse and trap approach have been specifically addressed. The system has been desiggned to handle such difficult (not readable) analytes. Efforts have been made to improve the reproducibility and the carry-over of these analytes. The measures adopted include: thorough rinsing and subsequent conditioning of the P + T parger; elimination of matrix effects by dilution and high salt (not readable); tight specification of purge relevant parameters; split-inter-(not readable) to improve GC retention time reproducibility.
    Additional Material: 7 Ill.
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  • 106
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 471-481 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Carrier gas ; Gas viscosities ; Kinetic theory of gases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: After describing simplified equations exspressing the temparature dependency of the viscosity of carrier gases (helium, nitrogen and hydrogen ) relative to a base value, absolute relationships based on the kinetic theory of gases are discussed. Comparative data obtained using various calculation methods are given and are compared to measured values. Based on the kinetic relationshipsm, of viscosity. Finally, the influence of pressure on the viscosity is also briefly discussed. As a supplement, Viscosity data are tabulated for the three gases in the range of 0°C to 400°C in increments of 2 K, calculated using the kinetic relationships.
    Additional Material: 3 Ill.
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  • 107
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 605-610 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Retention index ; Homologous series ; Local cubic interpolation model ; Multiparametric least-squares adjustsment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The retention indices of three homologous series (2-alkanones, 1-alkanols, cycloalksanones) have been determined at high temperature by the application of two new adaptation methods: A multiparametric least-squares regressions iterative method based on the dertermination of the adjusted retention times and a cubic interpolation directly using the uncorrected retention times without dead time correction. The two methods were applied to two types of columns. The first group includes eight packed columns (seven OV polymethylphenylsiloxane and Apolane-87 stationary phases), while the second includes five glass capillary columns (four methyl-silicons with different film thicknesses and Apolane-87 stationary phases). The retention indices obtained with a multiparametric and a cubic interpolation methods were compared with each other and with those calculated by Grobler's, Guardino's, Kaiser's and Kovàts' methods. The influence of coating, film thickness, and temperature on them was investigated.
    Additional Material: 5 Tab.
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  • 108
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 697-700 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Mass spectrometry ; L-Phenylalanine mustard ; Melphalan ; 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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  • 109
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 50-51 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Kaurenic acids ; Espeletia schultzii ; Coespeletia moritziana ; 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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  • 110
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 20 (1997), S. 363-368 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Solid-phase extraction ; Automation ; Water samples ; Acetylation ; Chlorophenols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An automated system for derivaatization was coupled on-line with solid-phase extraction-gas-chromatography (SPE-GC). The system was optimized for the determination of phenol and chlorinated phenols in aqueous samples. The test analytes were acetylated with acetic anhydride; proper buffering of the sample was a critical factor. Next, the phenol acetates were enriched on a SPE cartridge and transferred to a GC; two appraoaches were studied. In the first approach, the derivatives were enriched on disposable C18 cartridges (ASPEC type) and desorbed with methylacetate. Aan aliquot of the final eluate was injected on-line the GC by means of a loop-type interface. In the second approach, trace enrichment was performed on 10 × 2 mm i.d. LC-type precolumn packed with polystyrenedivinylbenzene copolymer (PLRP-S) this precolumn was dried with a mitrogen purge and the phenol acetates were desorbed with ethyl acetate which was injectedon-line into the retention gap of the GC under partially concurrent solvent evaporation (PCSE) conditions. The Derivatization-SPE-GC system which was based on the loop-type interface has the advantage of simplicity and easy operation, the main drawback is the impossibility to determine phenol acetates which elute prior to trichlorophenol acetates. With the derivatization-SPE-GC approach using PCSE-based desorption, even the most volatile analyte of the test series, phenol acetate, can be determined successfully. The entire procedure, including the derivatization step, was fully automated and integrated in one set-up. The precision data for the integrated on-line derivatization-SP-FID system were fully satisfactory, with RSD values of 1-12 % at the 1 μg/1 level. When a sample volume of 2.2 ml was analyzed, The detection limits for the chlorinated phenol acetates were in the 0.1-0.3 μg/1 range.
    Additional Material: 4 Ill.
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  • 111
    ISSN: 0935-6304
    Keywords: Supercritical Fluid Extraction (SFE) ; Gas chromatography ; Dicofol ; Fish ; LC50 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Toxicity evaluation of Dicofol to Astyanax bimaculatus schubarti, a characteristic fish species living in tropical rivers and lakes was carried out through LC50 - 96 Hours. These experiments were performed under laboratory controlled conditions with atmospheric air flow and dilution water at 25°C in the static mode, supercritical fluid extraction (SFE) with pure CO2 and CO2 modified with hexane and methanol were used at 50, 70, 80, and 100°C and 300 atm. Several collection modes were studied to extract Dicofol from fish samples. The extraction efficiencies were directly comparedd with those obtained after 8 h of Soxhlet extraction using the same clean-up with Florisil and analysis by HRGC/ECD and HRGC/MS as a confirmatory analytical technique. The SFE recoveries at temperatures lower than 80°C were typically lower than soxhlet recoveries; however a temperature increase enhanced the efficiency of SFE. The results showed that under certain conditions, supercritical fluid gave higher extractio power (extracted 11 % more pesticide), shorter extraction time, and lower solvent consumption than Soxhlet, thus affording an excellent alternative to the conventional method for extracting Dicofol from fish sample.
    Additional Material: 5 Ill.
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  • 112
    ISSN: 1437-1596
    Keywords: Phencyclidine ; Pethidine ; Gas chromatography ; Surface ionization detection ; Sep-Pak C18 cartridges
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine , Law
    Notes: Abstract Phencyclidine (PCP) can be detected in body fluids with very high sensitivity by gas chromatography (GC) with surface ionization detection (SID) using pethidine as internal standard. PCP was extracted with Sep-Pak C18 cartridges from whole blood and urine samples, which gave clean extracts. The calibration curve for spiked whole blood was linear in the range 1.25–20 ng/ml. The detection limit of PCP was approximately 15 pg on-column (0.75 ng/ml sample), which was much lower than by GC-nitrogen phosphorus detection. The recovery of PCP and pethidine from spiked whole blood or urine samples was above 85%. This method seems very useful for the determination of PCP in forensic and clinical toxicology.
    Type of Medium: Electronic Resource
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  • 113
    Electronic Resource
    Electronic Resource
    Springer
    Journal of comparative physiology 179 (1996), S. 331-344 
    ISSN: 1432-1351
    Keywords: Hylobius abietis ; Olfaction ; Plant odours ; Receptor neuron responses ; Gas chromatography ; Electrophysiology
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Abstract Receptor neuron responses to plant volatiles, trapped by head-space procedures, were examined in the pine weevil Hylobius abietis, using gas chromatography linked with electrophysiological recordings from single neurons. Seventy-two receptor neurons were tested 173 times for various plant volatile mixtures, either via a polar or a non-polar column. 1) All responses appeared as increased firing rates which followed the concentration profiles of the GC-eluted compounds. 2) The neurons were classified separately for the two column types in 17 and 19 groups respectively, according to the compounds they responded to. It suggests that the plant odour information is encoded by a large, but limited number of receptor neuron types. 3) Most neurons responded to a limited number of compounds (1–5) and showed a marked best response to one of them, whereas additional responses to several other components which seems to be structurally similar, was recorded for some neurons. It suggests that the plant odour receptor neurons are rather narrowly than broadly tuned, and that each neuron is specialized for receiving information about one or a few related compounds. 4) Most neurons responded to monoterpenes, whereas the other neurons responded to compounds of other categories. 5) Both major and minor plant volatile components activated specifically receptor neurons.
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  • 114
    Electronic Resource
    Electronic Resource
    Springer
    International archives of occupational and environmental health 68 (1996), S. 262-267 
    ISSN: 1432-1246
    Keywords: Gas chromatography ; Mass spectrometry ; Benzene ; Air pollution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract There is no shortage of information about the average benzene concentrations in urban air, but there is very little about microenvironmental exposure, such as in-vehicle concentrations while driving in various traffic conditions, while refuelling, or while in a parking garage. The main reason for this lack of data is that no analytical instrumentation has been available to measure on-line trace amounts of benzene in such situations. We have recently proposed a highly accurate, high-speed cryofocusing gas chromatography/mass spectrometry (GC/MS) system for monitoring benzene concentrations in air. Accuracy of the analytical data is achieved by enrichment of the air sample before trapping, with a stable isotope permeation tube system. The same principles have been applied to a new instrument, specifically designed for operation on an electric vehicle (Ducato Elettra, Fiat). The zero emission vehicle and the fully transportable, battery-operated GC/MS system provide a unique possibility of monitoring benzene exposure in real everyday situations such as while driving, refuelling, or repairing a car. All power consumptions have been reduced so as to achieve a battery-operated GC/MS system. Liquid nitrogen cryofocusing has been replaced by a packed, inductively heated, graphitized charcoal microtrap. The instrument has been mounted on shock absorbers and installed in the van. The whole system has been tested in both fixed and mobile conditions. The maximum monitoring period without external power supply is 6 h. The full analytical cycle is 4 min, allowing close to real-time monitoring, and the minimum detectable level is 1 μg/m3 for benzene. In-vehicle monitoring showed that, when recirculation was off and ventilation on, i.e., air from outside the vehicle was blown inside, concentrations varied widely in different driving conditions: moving from a parking lot into normal traffic on an urban traffic condition roadway yielded an increase in benzene concentration from 17 to 62.3 μg/m3 even if the actual distance was small. A larger increase was observed when a car was left with the engine running at a distance 2 m from the zero emission vehicle: We measured an increment of benzene concentrations from 15.2 to 174.4 μg/m3 with a car equipped with a catalytic converter, and from 19.1 to 386.3 μg/m3 with a car without such a converter.
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  • 115
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Estuarine waters ; Solid-phase extraction ; Triazines, alachlor, metolachlor ; Nitrogen phosphorus detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The stability of atrazine, simazine, alachlor, metolachlor, and deethylatrazine on C18 Empore disks has been determined. Estuarine water (100 mL) spiked at 3 μg L−1 with the target pesticide mixture was preconcentrated on the disks; the disks were then stored at −20°C, 4°C, and at room temperature for periods up to three months and were analyzed by gas chromatography with nitrogen-phosphorus detection. Complete recovery was observed after storage at −20°C throughout the period of the study. Losses up to maximum of 10% were observed after storage at 4°C. Higher losses (up to 24% for alachlor) occurred only at room temperature; the coefficient of variation for these determinations (8–11%) was also higher than that for the others (3–5%). The stability of the pesticides was dependent on the water matrix, on storage temperature, and on properties such as vapor pressure and water solubility.
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  • 116
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 42 (1996), S. 660-664 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Unified retention data ; Alkanes, alkenes, naphthenes and aromatics ; Squalane
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic, unified retention data of 120 hydrocarbons including: alkanes, alkenes, alkynes, alkylcycloalkanes, alkylcycloalkenes, aromatics and dienes on squalane stacionary phases are given. These values agree well with the corresponding experimental values used in the statistical treatment of the experimental data.
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  • 117
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Dialkylhydrazones ; Kováts retention indices ; Structure-retention relationships
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary N,N-Dialkylhydrazones [DAHs; R1R2C=1N-2N(R3)2] were prepared and their Kováts retention indices determined on 100% dimethylpolysiloxane (HP-1) and 5% diphenyl and 95% dimethylpolysiloxane (HP-5) stationary phases. The physico-chemical and retention behaviour of the DAHs depend greatly on whether R2=H or an alkyl group. A similar difference is observed in the alkane and oxo homomorphic factors of DAHs formed from aldehydes or ketones. The difference is explained on the basis of NMR and quantum-chemical results by intramolecular interactions between R2 and the lone pair of the2N atom. A single linear equation is suitable for prediction of retention indices if parameters are introduced representing resonance structure (bond angle and electron density) besidesI oxo or the van der Waals' surface.
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  • 118
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 42 (1996), S. 462-464 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Alcohols ; Cellulose tribenzoate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Cellulose tribenzoate (CTB) has some desirable operational properties and special interactions with alcohols. When chromatographic separation is carried out at 150°C, the C1–C4 alcohols have enhanced retention and other alcohols are eluted rapidly. Some probe molecules were used to characterize the chromatographic behavior of CTB by calculating the adsorption enthalpy (−ΔHa) between the sample and stationary phase. Separation of aliphatic alcohols was successfully performed on a packed column with a support (GDX) coated with CTB and temperature programming improved the separation of these alcohols.
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  • 119
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Reversed-flow technique ; Rate constants ; Bimolecular gaseous reactions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Rate constants for bimolecular reactions in the gas phase, under diffusion controlled conditions, can easily be determined by the reversed-flow gas chromatography (RF-GC) technique. The analysis of the diffusion band by means of a simple PC programme gives directly an apparent, second-order rate constant for gaseous reactions. By varying the amounts of the reactants, one can calculate the true order of the reaction and the true non-first-order rate constant of gaseous reactions. The calibration problem of the analytical techniques in non-first-order reaction kinetics is absent as are other disadvantages connected with carrier gas flow, peak shape and their instrumental spreading. The method can be used for atmospheric reactions and was applied in the gaseous reaction systems: SO2+NO2, SO2+Br2, C6H6+NO2, C6H5CH3+NO2 and C3H6+NO2 with various concentrations of reactants in nitrogen. The effect of the NO2 concentration on the apparent second-order rate constant of C2H4+NO2 at 333.2 K was also studied. Finally, the effect of sun light pre-irradiation of C2H2+NO2 in nitrogen was investigated.
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  • 120
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Molecular absorption spectrometry ; Gas phase detection ; Benzene derivatives
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple and inexpensive detection system for gas chromatography, based on gas-phase, molecular absorption measurements, is presented in which the chromatographic column is directly joined to the spectrophotometer flow cell, without heated transfer lines. A mixture of eight benzene compounds (including methyl, halogen and nitrogen derivatives) were separated and analyzed. Parameters affecting separation (temperature program and carrier gas flow) and measurement quality (wavelength and integration time) were studied and a measurement program designed to modify the wavelength during chromatography. The analytical characteristics of each compound were calculated, obtaining detection limits ranging from 0.5 to 9 μg mL−1. Finally, the method was applied to several synthetic mixtures, with good results.
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  • 121
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 42 (1996), S. 465-468 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Packed column separations ; Pyridine and alkylpyridines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The gas chromatography of the β-picolines in a lowboiling tar base fraction, is described. The methods developed employ packed columns with binary phases containing N,N,N′,N′-tetrakis(2-hydroxypropyl) ethylenediamine plus metal transition stearate, or with a ternary phase containing this mixture and o-hydroxyethylresorcinol
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  • 122
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 42 (1996), S. 547-550 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Supercritical Fluid Extraction ; Pesticides Residues ; Chlorothalonil ; Appels
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new method for the extraction of Chlorothalonil residues from apples using supercritical CO2 as the extracting fluid is described. The supercritical fluid extraction results were compared with those obtained by solid-liquid extraction. The results showed that SFE is faster and more selective with better recovery and higher selectivity.
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  • 123
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 42 (1996), S. 578-582 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; EDTA determination ; DTPA determination ; Water analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new analytical method and the method validation for the determination of ethylenediaminetetraacetic acid (EDTA) and diethylenetriaminepentaacetic acid (DTPA) in lake and sea water is presented. An aqueous sample, after evaporation to dryness, was treated with an esterification reagent. The resulting ethyl ester derivates were determined by capillary gas chromatography using a nitrogen phosphorus specific detector (GC-NPD). The response was linear up to 5 mg L−1. The recoveries from lake and sea waters were 59–105 % for EDTA and 86–112 % for DTPA. The run-to-run repeatabilities (R.S.D.) were 2–8 % for EDTA and 4–11 % for DTPA depending on concentration and the reproducibilities (R.S.D.) were 6–13 % and 3–11 %, respectively. The limits of detection for EDTA and DTPA were 3 and 12 μg L−1 in distilled water, respectively. The method is simple to use and reliable as shown by the analysis of samples of lake water that is influenced by pulp and paper industry.
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  • 124
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Electron capture detection ; Mass spectrometric detection ; Atomic emission detection ; PCBs in marine sediments
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Electron capture detection (ECD), low- and highresolution mass spectrometry (LR- and HRMS), and atomic emission detection (AED) were compared for the gas chromatographic (GC) detection of polychlorinated biphenyls (PCBs) present in highly contaminated marine sediments. With ECD, LRMS, and even HRMS, detection was seriously disturbed by the complex matrix of the sediments, whereas AED in the chlorine-selective mode provided excellent PCB profiles without interferences. In addition, GC-AED provided congener independent responses, which enabled accurate quantitation of all PCBs based on a single calibration curve. However, because GC-AED was less sensitive than the other techniques studied, preparation of relatively large amounts of sample (10–20 g dry sediment) was required for most analyses.
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  • 125
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 43 (1996), S. 73-75 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Spatial average gas velocity ; Temporal average gas velocity ; Column pressure drop
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary While the commonly known temporal average velocity of a carrier gas is approximately proportional to the pressure drop along a column, the spatial average velocity is exactly proportional to that pressure.
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  • 126
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Electron capture detection ; Solid phase extraction ; Chlorophenols ; Water analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A solid-phase extraction system coupled to a gas chromatograph fitted with an electron capture detector was developed for the determination of chlorophenols in waters. The continuous system consists of an XAD-2 adsorbent column where chlorinated phenols are preconcentrated and subsequently eluted with ethyl acetate. The sensitivity of the method is proportional to the number of chlorine substituents in the phenol; thus, the detection limit for monochlorophenols is ca. 10 μg L−1 and that for pentachlorophenol about 2 ng L−1. The method was used to determine chlorophenols in treated waters, with good precision; however, no mono or dichlorophenols were detected at the levels afforded by the proposed method.
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  • 127
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention indices ; Correlation equations ; n-Alkylcyclopentenes andn-alkylcyclohexenes ; n-Alkyl esters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Correlation equations have been derived which relate the Kováts retention indices ofn-alkylcyclopentenes,n-alkylcyclohexenes andn-alkyl esters of aliphatic acids on the stationary phases OV-101, OV-225 and PEG 20M to column temperature and carbon number in the alkyl chain. The universal equation: $$\begin{gathered} RI = A + B \cdot m + C \cdot \log (m)/m + \hfill \\ D/[(m - 2)^2 + 0.1] + Et \hfill \\ \end{gathered} $$ whereA, B, C, D andE are correlation coefficients,m is the number of carbon atoms in the side chain (forn-alkylcycloalkenes) or in the alcohol chain (for alkyl esters) andt is the column temperature, describes the retention indicesRI of these homologous series with high accuracy (SD〈1 index unit), beginning with the first members of the series.
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  • 128
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Solid phase extraction ; Nitrogen phosphorus detector ; SCH 44643 in rat plasma
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic (GC) assay for the determination of SCH 44643, an orally active antagonist of responses to both histamine and PAF, was developed and validated for rat plasma. The method involved organic solvent extraction followed by solid phase extraction on aminopropyl column. The separation was on a capillary column (DB-17) with quantitation by a nitrogen-phosphorus detection. The method was sensitive with a limit of quantitation of 5 ng mL−1. There was a good linear relationship between the peak height ratio (SCH 44643/internal standard) and SCH 44643 concentration in the range 5 to 200 ng mL−1. The method was precise with a coefficient of variation ranging from 1.8 to 3.0% and accurate with a bias ranging from 0 to 5.8%. Moreover, SCH 44643 was stable in rat plasma after being subjected to three freeze-thaw cycles. The assay was shown to be sensitive, specific, accurate and precise, and suitable for use in pharmacokinetic or toxicokinetic studies.
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  • 129
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Poly(L-glutamate) ; Cholesteric liquid crystal ; Properties as stationary phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Comparative gas chromatographic properties of two thermotropic Poly(L-glutamates) with long alkyl side chains (10 and 16 carbons called Poly 10 and Poly 16 respectively) are studied. Their thermal properties were established with differential scanning calorimetry (DSC) and gas chromatography. They present a cholesteric liquid crystal in a large temperature range. The chromatographic separation abilities of the two polymers in the liquid crystal state were studied using capillary glass columns. Interesting analytical performances were obtained in different fields: isomeric separation of alkanes, aromatics, polyaromatics, volatile aroma compounds and cis and trans isomers. Some differences were noticed in their behaviours; 2 and 3-methyloctane and xylene isomers are separated only on Poly 10 while limonene and eucalyptol are separated only on Poly 16.
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  • 130
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Aliphatic hydrocarbons ; Chlorinated aromatics ; Pork liver extracts
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A multicomponent extraction/concentration procedure has been developed for the enrichment of PCBs, PCTs and aliphatic hydrocarbons (pristane, C18, C19, C20, C22, C24, C28, C32 and C36) in pork liver. These components of the enriched extract were then simultaneously determined by gas chromatography. Mean recoveries ranged from 81.5% for pristane to 93% for PCBs;CV% (0.9–6.7) indicated the method to be both precise and reproducible.
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  • 131
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    Chromatographia 42 (1996), S. 77-82 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Modified alumina ; Coal mine air ; Alkenes, alkanes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method for the separation of alkanes and alkenes present in coal mine air has been developed using modified alumina columns. The separation was carried out using a GC equipped with a gas sampling valve, a FID and a surface modified alumina packed column with helium as carrier gas. An investigation was carried out into the effects of surface modifiers on alumina. The study examined the change in retention properties on alumina modified by alkali metal salts and the specific effects of the halide anions and metal cations. The paper describes the preparation of the alumina columns and the effects on selectivity of post heating the stationary phase. The study demonstrated that alumina modified with 2% sodium chloride and post heated to 150°C was the most appropriate stationary phase.
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  • 132
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace sampling ; Solid-phase microextraction (SPME) ; Nitrogen-phosphorus detection (NPD) ; Organophosphate pesticides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Organosphosphate pesticides have been found extractable by headspace solid-phase microextraction (SPME), and the best conditions of their extraction from human whole blood and urine samples have been investigated. The body fluid samples containing nine pesticides (IBP, methyl parathion, fenitrothion, malathion, fenthion, isoxathion, ethion, EPN and phosalone) were heated at 100°C in a septum-capped vial in the presence of various combinations of acid and salts, and SPME fiber was exposed to the headspace of the vial to allow adsorption of the pesticides before capillary gas chromatography (GC) with nitrogen-phosphorus detection. The heating with distilled water/HCl/(NH4)2SO4/NaCl and with distilled water/HCl gave the best results for urine and whole blood, respectively. Recoveries of the nine pesticides were 0.8–10.6% except for phosalone (0.03%) for whole blood, and 3.8–40.2% for urine. The calibration curves for the pesticides showed linearity in the range of 50–400 ng/0.5 mL for whole blood except for malathion (100–400 ng/0.5 mL whole blood) and 7.5–120 ng/0.5 mL for urine except for phosalone (15–120 ng/0.5 mL urine) with detection limits of 2.2–40 ng/0.5 mL for whole blood and 0.8–12 ng/0.5 mL for urine.
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  • 133
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    Chromatographia 42 (1996), S. 309-312 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Graphite coated capillary columns ; Ephedrines separation ; Drug analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of graphite-layer capillary column is described together with their application to the analysis of aliphatic and aromatic amines. Attention is mainly focused on the separation of ephedrines which, being sympathomimetic amines, are often present in pharmaceutical preparations, but are also illegally used by athletes as stimulants. Complete separation of these compounds, using direct GC-NPD analysis of human urine extract, without derivatisation, has been obtained.
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  • 134
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column liquid chromatography ; Pesticide residues ; Surface water analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A monitoring programme based on gas chromatography (NPD, ECD) using MSD for confirmatory purposes and coupled-column liquid chromatography was applied to the analysis of pesticide residues in surface water from a predominantly agricultural area of Spain (Comunidad Valenciana). Samples analysed by means of enzyme-linked immunosorbent assay gave similar results to those obtained by GC (MSD) for the determination of total triazines. The test employed had the advantages of a simple test procedure, short analysis time and high confirmatory value. Nevertheless, the multiresidue character, accuracy and unequivocal identification of individual pesticide residues of GC (MSD) make this technique the most appropriate for environmental monitoring programmes. In this monitoring programme about 200 samples were analysed between 1993–1994. 27 different pesticides were detected in 91 of these samples. The pesticides more frequently detected were dimethoate, methidathion, endosulfan A and B, endosulfan sulphate and pirimicarb. The highest concentrations found were 39.9 μg L−1 of dimethoate, 10.6 of pirimicarb and 10.6 of methidathion.
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  • 135
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Supercritical fluid extraction ; Pesticide residues ; Norflurazon residues ; Oxadixyl residues ; Food crops
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Norflurazon and Oxadixyl residues have been analysed by HRGC-ECD after extraction from field-treated sugar cane and grapes using classical solid-liquid extraction or supercritical fluid extraction. The extraction techniques were compared; the results indicate the advantages of SFE as an alternative method for analysis of pesticides in these samples.
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  • 136
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Microwave extraction ; Sample clean-up ; Organochlorine compounds ; Blubber of marine mammals
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid and effective method is described for the extraction of organochlorine compounds (PCB 153, PCB 138, PCB 180, p,p′-DDE, α-HCH, γ-HCH, ε-HCH and HCB) from seal blubber and pork fat withn-hexane using a microwave technique. Heating of the non-polarn-hexane was achieved using a microwave transformer. The lipid content of the samples obtained by this extraction was identical to that by Soxhlet extraction. After separation of sample matrix and organochlorines on a silica gel column the organochlorine compounds were determined by GC-ECD. The efficiency of the method was tested with 500 mg spiked fat, extracted using various numbers of extraction cycles. Recoveries of organochlorine compounds in grey seal blubber and spiked pork fat generally exceeded 90 %.
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  • 137
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Solid phase micro extraction ; Chloroethenes ; Reductive dechlorination
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An analytical method has been developed to determine the chloroethene series, tetrachloroethene (PCE), trichloroethene (TCE),cisdichloroethene (cis-DCE) andtransdichloroethene (trans-DCE) in environmental biotreatment studies using gas chromatography coupled with a solid phase micro extraction (SPME) technique. The volatile chlorinated compounds in aqueous solution can be analyzed directly without solvent extraction, purge and trap, or thermal heating. The calibration curves have demonstrated good linear relationships within 50.0 to 3000.0 μg L−1 concentration range. Detection limits are 18.0, 5.0, 25.0, and 42.0 μg L−1, for PCE, TCE,cis-DCE andtrans-DCE, respectively. Factors which affect the SPME process, such as sample adsorption time, thermal desorption time, and concentration of salt in the matrix, have also been evaluated.
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  • 138
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Local anaesthetics ; Solid phase micro extraction (SPME) ; Direct immersion
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Local anaesthetics have been shown to be extractable from human whole blood samples by direct immersion (DI)-solid phase micro extraction (SPME). After deproteinization with perchloric acid, the pH of the clear supernatants of human whole blood samples containing the drugs were adjusted to about 7 with 10 M NaOH in the presence of NaCl; a polydimethylsiloxanecoated SPME fiber was then immersed directly into the sample solution to allow adsorption of the drugs before capillary gas chromatography (GC) with flame ionization detection. The DI-SPME for 1-mL whole blood gave peaks for all the drugs; only a small amount of background noise appeared and this gave no problems in the detection of the drugs. Recoveries of the ten drugs from human whole blood was 0.74–19.7 %. The calibration curves for seven drugs showed linearity in the range of 0.25–12 μg mL−1 whole blood, with detection limits of 54–158 ng mL−1.
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  • 139
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary phase ; β-Cyclodextrin ; Separation mechanism
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Three peralkylated β-cyclodextrins (CD), perethylated β-CD, perbutylated β-CD and peroctylated β-CD have been coated on to untreated fused-silica capillary tubing and used to separate some achiral and chiral compounds. The separation mechanism is discussed in the paper.
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  • 140
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Dicofol ; Fish ; Lethal concentration ; Bioconcentration factor
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Evaluation of the toxicity of Dicofol was carried out onAstyanax bimaculatus schubarti, a characteristic fish species living in tropical rivers and lakes. Experiments were under laboratory controlled conditions with atmospheric air flow and dilution water at 25°C in the static mode. Fish samples were collected and submitted to appropriate analytical procedure: Soxhlet extraction, clean-up by Florisil adsorbent and finally quantification by GC-ECD. The results showed good recoveries (〉 89%) for the developed method both in water and fish samples. The lethal concentration, LC50, and the bioconcentration factor, BCF, were 18.13 mg L−1 and 241.70, respectively forAstyanax bimaculatus schubarti demonstrating the lipophilic nature of the studied compound.
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  • 141
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Electronic pressure control ; Mass selective detector ; Pesticide residues ; Cereals
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An analytical method for the confirmation of 30 pesticide residues in cereals and related products has been developed. Splitless injection with electronic pressure control using constant carrier gas flow gives higher sensitivity and better resolution than electronic pressure control and isobaric analysis. The use of electronic pressure control assures consistent retention times enabling selected ions to be collected in short time windows. Mass spectrometric detection in the selected ion monitoring mode using three ions for each pesticide ensured good sensitivity and accurate pesticide confirmation.
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  • 142
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    Chromatographia 43 (1996), S. 208-210 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Epoxystyrenes ; Retention index
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of some epoxystyrenes on fused silica capillary columns coated with poly(ethylene glycol) was investigated, Retention indices were determined at two temperatures to interpret chromatographic behaviour, The standard deviation was 0.3 index units.
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  • 143
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Microwave-assistend solvent extraction (MASE) ; Pesticide residue analysis ; Triazine herbicides ; Soil samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The use of microwave-assisted solvent extraction (MASE) as an alternative for conventional solvent extraction procedures for the determination of some triazine herbicides in soil samples has been investigated. In this study MASE method development was focused on the selection of a suitable extraction solvent prior to the instrumental analysis of uncleaned extracts with gas chromatography and nitrogen-specific detection. A mixture of dichloromethane-methanol (90∶10, v/v) yielded recoveries ranging from 89 to 103 (spiked level 200 μg/kg) with RSDs ranging from 2.1 to 5.3%. This solvent mixture is also very convenient for further procedure. The selected MASE procedure was tested by analyzing freshly spiked soil samples and samples with aged residues of atrazine, desethylatrazine, desisopropylatrazine and simazine. The results were compared with those obtained by a conventional liquid extraction method. The comparative study indicated that MASE yields recoveries at least as good as those obtained by the conventional method. Moreover, the MASE procedure provides low solvent consumption in combination with a high sample throughput.
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  • 144
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fosfomycin in urine ; Pharmacokinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A capillary gas chromatographic method for the determination of fosfomycin in human urine is described. After dilution of the sample and derivatization, analysis was on a HP-1 capillary column and a flame ionization detector was used to determine the bistrimethylsilyl derivative of fosfomycin. Response was linear in the range 50–5000 μg mL−1. The detection limit was about 10 μg mL−1. The within and between day coefficients of variation did not exceed 6%. The method was applied to the determination of fosfomycin in urine samples collected during clinical pharmacokinetic studies.
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  • 145
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Sulfur chemiluminescence detector ; Flame ionisation ; Dual-channel detection ; Optimization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The dual-channel detection of samples with detectors coupled in series is possible only when the first detector is a non-destructive one. However, the configuration where a destructive detector, such as the flame ionization detector (FID), is followed by the flameless, sulfur chemiluminescence detector (flameless SCD) can be used to detect simultaneously carbon and sulfur. In this work, the FID and flameless SCD are coupled in series for dual-channel detection of sulfur compounds in three gasoline samples. Optimum conditions for flameless SCD were evaluated by altering the flow rates of hydrogen and air and the oxygen pressure to the ozone generator. Samples are identified by retention indices where the homologous n-alkylthiols are used as standards. The increment in retention index per carbon number of the n-alkylthiols is 105.54 in the Quadrex 007 series, 0.32 mm i.d., 4 μm film, column.
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  • 146
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary phase ; Polysiloxane matrices ; β-Cyclodextrin ; Crown ether ; Liquid crystal ; Coordination effect
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This paper investigates the possibility of using a sidechain crown ether polysiloxane (PDB-14-C4) and a side-chain liquid-crystalline polysiloxane-containing crown ether (PSC-3) as matrices for peralkylated β-CD employed as stationary phases. Three columns, coated with PSC-3 + permethylated β-CD, PDB-14-C4 + permethylated β-CD and PDB-14-C4 + perethylated β-CD were characterized by gas chromatography. The column efficiencies, phase transitions, and selectivities were measured and compared.
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  • 147
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    Chromatographia 42 (1996), S. 63-71 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; High efficiency open tubular columns ; Columns connected in series ; Gasoline analysis ; Detailed hydrocarbon analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary More than 1.3 million effective plates were produced by a column 450 meters long, 200 μm inner diameter. The column was built up by connecting nine 50 meter columns in series. The sum of the efficiencies of the individual pieces equalled the efficiency of the combined column. Up to 970 components were differentiated in a gasoline standard.
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  • 148
    ISSN: 1612-1112
    Keywords: Gas chromatography ; flame photometric detector ; Sulfur in diesel fuel
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new method is proposed for the computerized determination of sulfur in diesel fuel by capillary gas chromatography with a flame photometric detector (FPD). The diesel fuel is injected in the gas chromatograph after dilution with n-hexane. After recording the chromatogram, the sulfur content in the diesel fuel (mg L−1 or w/w) is given directly by an integrator provided with a Basic card or by a personal computer in which the algorithm of the calibration curve has been entered. Use of a calibration curve does not require the identification of the numerous sulfur compounds present in diesel fuel. The calibration curve was corrected for the quenching effect that the hydrocarbon components of the diesel fuel produce on the detector response. The method was tested using diesel fuel with a known sulfur concentration and was found to be very accurate; it is reproducible, fast and may be automated.
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  • 149
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Semivolatile flavor compounds ; Cinnamon ; Solid-phase microextraction ; Chemometric classification
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The conditions which affect the reproducibility of characteristic chromatographic profiles of semivolatile compounds from true cinnamon and cassia by headspace solid-phase microextraction are determined. Optimum conditions for sample amount, vial size, temperature, sampling time, and fiber type for steady state sampling conditions are identified. Vial size was an unexpected critical parameter possibly related to the build up of internal ternal pressure during sample heating followed by expulsion of a portion of the vapor phase through the septum as it was punctured by the syringe. Gas chromatography with ion trap mass spectrometry was used to identify the major volatile compounds in cassia and true cinnamon. Reasonable semi-quantitative agreement (r 2〉0.87 and generally greater than 0.93) was observed for the major semivolatile compounds isolated by headspace solid-phase microextraction and solvent-assisted supercritical fluid extraction. The extracts isolated by solid-phase microextraction contained relatively high concentrations of terpene-type compounds in low abundance in the solvent-assisted supercritical fluid extracts, but these compounds were of little value in distinguishing the botanical origin of authentic cinnamon and cassia samples. The latter were easily distinguished by the presence of eugenol and benzyl benzoate in true cinnamon, that was absent in cassia, and the presence of coumarin and δ-cadinene, in cassia, that was either absent or in low concentration in true cinnamon. Headspace solid-phase microextraction provides a rapid and simple method for establishing the botanical origin of the principal cinnamons of commerce.
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  • 150
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Atomic emission, electron capture ; and nitrogen phosphorus detection ; Honey ; Acaricides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The performance of a gas chromatographic system coupled to an atomic emission detector (GC/AED) is tested by comparison with a two-dimensional gas chromatographic system equipped with capillary columns of different polarity and simultaneous electron capture and nitrogen-phosphorus detection (ECD/NPD), for the determination of the acaricides chlordimeform, bromopropylate, amitraz and coumaphos on spiked honey samples. The acaricides were extracted with ann-hexane/acetone mixture (80∶20, v/v) with a further clean-up step on an octadecylsilane cartridge. The 193 nm carbon emission line is the best choice in terms of sensitivity whereas the ECD/NPD system gives better selectivity.
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  • 151
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Low-molecular-weight hydrocarbons ; Extraterrestrial atmospheres ; Chemically bonded squalene(ane) phase ; 13C and29Si CP-MAS NMR
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Chemically bonded squalene(ene) phases have been synthesized via a hydride modified silanization process using dimethylchlorosilane, triethoxysilane and trichlorosilane. The surface structure of the bonded phases were characterized with DRIFT and solid state NMR studies. The results of the latter indicate successful bonding of a non-terminal olefin to the silica surface and that bonding of individual squalene molecules appeared not to occur at the same site(s) presumably due to steric hindrance. Among the phases examined, the trichlorosilane-based material exhibits better chromatographic properties probably due to greater surface coverage and hence effective non-polar interaction between the solutes and the bonded ligands. Under isothermal conditions, the present packings produced fast and efficient separation of C1–C4 saturated hydrocarbons on shorter columns than similar columns containing alkyl- or bidentate alkyl-modified silica packings at low column head pressure and are thermally stable at temperatures up to 250°C or higher.
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  • 152
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    Chromatographia 42 (1996), S. 431-434 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fatty acid methyl esters ; Biodiesel ; Methanol ; Glycerol
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The methanol and free glycerol content of vegetable oil methyl esters used as diesel fuel (biodiesel) is very important in describing the quality of this fuel and is therefore limited by specifications. A previously described GLC method for the determination of free glycerol in biodiesel has been further developed and also allows the simultaneous determination of methanol. Sample preparation includes dissolving in dimethylformamide, silylation with bis-trimethylsilyltrifluoracetamide (BSTFA) and separation on a methylsilicone fluid, coated-capillary column using either FID or MS-detection. Ethanol and 1,4-butanediol were used as internal standards. Both detection systems show sufficient sensitivity for concentrations relevant to biodiesel samples. The recovery was tested using a RME-sample containing known amounts of methanol and glycerol.
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  • 153
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Bonded silicas ; Phase transitions ; Differential scanning calorimetry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In order to give a molecular interpretation to the phase transition observed with densely bonded octadecyl-silicas in reversed phase liquid chromatography (RPLC) as well as in gas chromatography (GC), nine new bonded silicas were prepared including grafts with polar groups at the extremities of long spacers (18 carbon atoms). The interpretation is simplified by using large-pore macroporous substrates and inverse GC in conjunction with differential scanning calorimetry (DSC) as the test method. A phase transition is observed in almost all cases, but the temperature range is lower and more extended in comparison to the dimethyloctadecyl reference silica. An interpretation of the phase transition is given, based on the folding of the chains and the resulting “autodensification” of the layer.
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  • 154
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    Chromatographia 42 (1996), S. 593-594 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Double-base propellants ; Nitroglycerin ; Centralite I ; Dibutyl phthalate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The separation and quantitative determination of propellant constituents on short, wide-bore fused-silica capillary columns, coated with crosslinked methylsilicone phase was investigated. The analytical results were quite satisfactory.
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  • 155
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Partition coefficients ; Henry's constants ; High density polyethylene ; Polymer drying
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas-solid partition coefficients (K) for n-hexane in high density polyethylene (HDPE) have been measured at conditions applicable to large-scale drying utilizing a novel headspace method. The method features considerable versability and simplicity due to the control of experimental conditions designed to favor full extraction of the analyte into the headspace. By combining this full extraction technique with a traditional static headspace experimental scheme, a method which measuresK and residual concentration is achieved. The results show that partition coefficients differ significantly between HDPE in its virgin powder and pellet forms, as well as among various HDPE grades. The differences are shown to be attributable to differences in % crystallinity of the specific polymer. Data collected over a wide range of hexane concentrations reveals saturation levels (solubilities) which correspond to crossover from evaporative to diffusion-controlled drying.
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  • 156
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    Chromatographia 43 (1996), S. 625-627 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace sampling ; Formaldehyde ; Plastics ; Foods ; Biological samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A modified headspace gas chromatographic method, based on polycondensation with formaldehyde, has been developed for derivatization with formaldehyde in foods, biological media and other products. The method provides the possibility of obtaining results within three minutes, which is of significant importance for the control of food and cosmetics production and the quality of polymer products based on formaldehyde, as well as for biological monitoring.
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  • 157
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    Chromatographia 43 (1996), S. 159-162 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas pressures ; Gas compressibility ; Retention volumes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The true meanings of the so-called corrected retention volume and the specific retention volume are explained in the light of the recent paper by Davankov.
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  • 158
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    Chromatographia 43 (1996), S. 163-176 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index estimation ; Aromatic compounds ; Incremental models
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Pure topologically based incremental models have been developed in order to estimate the retention indexes of aromatic compounds substituted with groups containing the hetero atoms nitrogen, oxygen and halogens. The bond-types of the compounds are counted and used as molecular descriptors. The observed estimation errors are about 1 % for compounds containing no hetero atoms and for those containing halogenated substituents; the errors are approximately 2 % for aromatic compounds with nitrogen- and oxygen-containing substituents. The method is validated by prediction of the retention indexes for an additional group of aromatic compounds (the validation data set).
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  • 159
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Molecular modelling ; Molecular mechanics calculations ; Permethylated α-, β- and γ-cyclodextrins ; Interaction mechanism
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The capillary gas chromatographic retention behavior of α-pinene and tricyclene has been investigated on stationary phases of different polarities. On all but one of the columns employed, tricyclene eluted before α-pinene; only permethylated β-cyclodextrins dissolved in moderately polar polisiloxanes gave a reversed elution order. The intermolecular interactions which caused the unexpected retention behavior were investigated in detail, applying methods of computer simulation. To achieve this, we have developed a calculation algorithm on the basis of molecular mechanical optimizations and programmed it in a macro. This makes it possible to systematically investigate a given configuration space in which all the possible interactions can take place. It was shown that permethylated β-cyclodextrin as host molecule for both guest molecules offers an optimum cavity size. As a result the number of energetically favorable contacts between host and guest molecules as well as the strength of the interactions in this stationary phase were larger. As a consequence the elution order, normally only influenced by the vapor pressure of the compounds at a given temperature, was changed. Nonspecific interactions played an especially important role for these kinds of substances.
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  • 160
    ISSN: 1612-1112
    Keywords: Column liquid chromatography-gas chromatography ; Gas chromatography ; 3,5-Stigmastadiene ; Cold pressed olive oil
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The quantitation of 3,5-stigmastadiene and other steroidal hydrocarbons, commonly known as steradienes, is a valid tool for the recognition of refining (in particular bleaching) of edible oils; the evidence of this process is nowadays of a great interest due to growing market for “virgin”, cold-pressed, “natural” oils. Due to the long time required (about 4 hours) and the amount of solvents employed (about 650 mL) to perform the official analysis, other methods have been recently proposed, the most important of which involves high performance liquid chromatography coupled with capillary gas chromatography (HPLC-GC). In this study the results of ten oil samples, analysed by both the official method and HPLC-GC, are reported and the two methods compared and discussed, for routine use, in terms of sample preparation, time of analysis and setting up, difficulty and reproducibility.
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  • 161
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Zeolite membrane PLOT columns ; In-situ synthesis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of a zeolite membrane PLOT column by in-situ synthesis is described. The advantages of this new column are discussed. Some analytical applications to alkanes, arenes, esters, alkyl halides and ethers on the zeolite membrane PLOT column compared with those on a coated zeolite PLOT column are reported.
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  • 162
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column liquid chromatography ; ECD, UV and MS detection ; EPA Method 515.1 ; Chlorinated acidic pesticides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A comparison of the official EPA method 515.1 for determination of chlorinated acidic pesticides and a modification of it is illustrated. Extraction of the analytes from water and their determination and quantitation is by gas chromatography-electron capture detection (GC-ECD), liquid chromatography-UV detection and liquid chromatography-particle beam mass spectrometry. Although HPLC-PBMS was found to be less sensitive than the GC-ECD method, it was, nevertheless, more sensitive than HPLC-UV. The modified method is simpler, quicker and allows more accurate determination of pesticides in aqueous samples.
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  • 163
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    Chromatographia 43 (1996), S. 296-300 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Thermal desorption ; Ion-pair column liquid chromatography ; Nicotine, 3-ethenylpyridine ; Environmental tobacco smoke
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Different sampling and analysis techniques for the determination of gas-phase nicotine and 3-ethenylpyridine in environmental tobacco smoke are reported. Graphitized carbon traps, annular diffusion denuders, and nebulizer collectors have been used as sampling devices in combination with either thermal desorption or with water extraction. Capillary gas chromatography and ion-pair reversed-phase chromatography were applied to desorbed and liquid samples obtained in an intercomparison indoor study. The methods developed here show some advantages over existing methods in terms of analysis time, sensitivity and loading capacity.
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  • 164
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Electron-capture detector ; Photoionization detector ; Pulsed discharge detector
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Since the electron-capture detector (ECD) is highly selective, it is imperative to use a more universal ionization detector in conjunction with the ECD in order to detect non-capturing or weakly capturing compounds. Also in an EC study of weakly or moderately strong electron-capturing compounds, it is necessary to identify the EC peak of the compound by identifying the major component with an ionization detector. In this paper we have shown that the pulsed discharge detector can be interchanged between the EC and the helium ionization modes within 4–6 s. The application of this procedure has been illustrated with a mixture of alkane/alkene chlorocompounds. The interchange between EC and argon photoionization modes has also been investigated. The change from EC to argon photoionization also occurs in 4–6 s but the reverse process requires ∼9 s.
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  • 165
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Solid-phase micro extraction (SPME) ; Headspace sampling ; Ethanol ; Alcohol
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Ethanol has been found extractable from human whole blood and urine samples by headspace solid-phase micro extraction (SPME) with a Carbowax/divinylbenzene-coated fiber. After heating a vial containing the body fluid sample with ethanol, and isobutanol as internal standard (IS) at 70°C in the presence of (NH4)2SO4, a Carbowax/divinylbenzene-coated SPME fiber was exposed in the headspace of the vial to allow adsorption of the compounds. The fiber needle was then injected into a middle-bore capillary gas chromatography (GC) port. The headspace SPME-GC gave intense peaks for both compounds; a small amount of background noises appeared, but did not interfere with the detection of the compounds. Recoveries of ethanol and IS were 0.049 and 0.026% for whole blood, respectively, and 0.054 and 0.085% for urine, respectively. The calibration curves for ethanol showed excellent linearity in the range of 80–5000 mg L−1 for whole blood and 40–5000 mg L−1 for urine; the detection limits for both samples were 20 and 10 mg L−1, respectively. The data on actual determination of ethanol after the drinking of beer are also presented for two subjects.
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  • 166
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    Chromatographia 43 (1996), S. 444-446 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; History of chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In November 1995, theDeutsches Museum, the world's largest technical museum, opened a new branch in Bonn, devoted to achievements after 1945. There, the first gas chromatographic system used by Erika Cremer and Fritz Prior, in 1945–47, in Innsbruck, is exhibited. The new display is described and the early activities of Erika Cremer and her students are summarized.
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  • 167
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Solid-phase microextraction ; Headspace sampling ; Phencyclidine (PCP) ; Surface ionization detection (SID)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Phencyclidine (PCP) was found to be extractable by headspace solid-phase microextraction (SPME) from human whole blood and urine. Sample solutions were heated at 90°C in the presence of NaOH and K2CO3, and an SPME fiber was exposed in the headspace of a vial for 30 min. Immediately after withdrawal of the fiber, it was analyzed by gas chromatography with surface ionization detection (GC-SID). Recoveries of PCP were approximately 9.3–10.8% and 39.8–47.8% for whole blood and urine samples, respectively. The calibration curve for PCP showed good linearity in the range 2.5–100 ng mL−1 whole blood and 0.5–100 ng mL−1 urine. The detection limits were approximately 1.0 ng mL−1 for whole blood and 0.25 ng mL−1 for urine.
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  • 168
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    Communications in Numerical Methods in Engineering 12 (1996), S. 13-20 
    ISSN: 1069-8299
    Keywords: open channel flows ; Riemann solver ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: An efficient numerical method is developed for the one-dimensional open channel flow equations. The scheme is a modification of one presented recently, but with an improvement in the efficiency made through the use of the arithmetic mean as an average of flow variables across the interface between adjacent states. Numerical results are shown for two problems, and an indication of the efficiency gained is given.
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  • 169
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    Communications in Numerical Methods in Engineering 12 (1996), S. 21-29 
    ISSN: 1069-8299
    Keywords: finite element systems ; elliptic partial differential equations ; approximate LU factorization ; explicit matrix inversion ; preconditioning ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: A new class of explicit generalized approximate inverse finite element matrix algorithmic methods, based on the concept of LU-sparse factorization procedures, without inverting the decomposition factors, has recently been introduced. The large sparse unsymmetric coefficient matrix of irregular structure is factorized approximately and, in conjunction with approximate inverse matrix techniques, yields explicit preconditioned methods for the finite element (FE) and finite difference (FD) method. The numerical implementation of these algorithms is presented and Fortran subroutines for the efficient solution of the sparse unsymmetric linear systems are given.
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    Communications in Numerical Methods in Engineering 12 (1996), S. 147-148 
    ISSN: 1069-8299
    Keywords: Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
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  • 171
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    Communications in Numerical Methods in Engineering 12 (1996), S. 149-150 
    ISSN: 1069-8299
    Keywords: Engineering ; Engineering General
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  • 172
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    Communications in Numerical Methods in Engineering 12 (1996), S. 63-73 
    ISSN: 1069-8299
    Keywords: asymptotic solution ; natural frequencies ; membrane vibrations ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: In the paper an asymptotic formula has been developed to correct the discretization error for the finite element predicted natural frequencies of membrane transverse vibration problems. The general idea behind deriving this asymptotic formula is that, when the finite element size approaches zero, a discretized finite element system approaches a continuous system and the predicted natural frequencies of the system from the finite element analysis therefore approach the exact solutions of the system. Without losing generality, several different finite element mesh patterns have been considered and the same asymptotic formula for correcting the finite element predicted natural frequency has been obtained for all the different mesh patterns because of the uniqueness of the exact solution to the natural frequency of a real structure. The usefulness, effectiveness and efficiency of the present asymptotic formula have been assessed by a simple but critical problem, for which the exact solution is available for comparison. In order to investigate the applicability of the asymptotic formula to practical engineering problems, two challenging membrane vibration problems of irregular shapes, an L-shape and a tapered shape with a circular hole in the centre, have also been analysed. The related numerical results have demonstrated that the asymptotic formula provides a very useful post-processing error corrector for the finite element predicted natural frequencies of membrane transverse vibration problems, even though the problem domains are of irregular shape. The greatest advantage in using the present asymptotic formula is that it yields a solution of higher accuracy, by simply using the formula to correct the rough solution obtained from a much coarser finite element mesh with fewer degrees of freedom, without any further finite element calculation.
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  • 173
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    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.
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  • 174
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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.
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  • 175
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    Journal of High Resolution Chromatography 19 (1996), S. 359-361 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Atomic emission detection ; Triclosan ; Dental plaque ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A validated gas chromatographic method for the determination of triclosan in human dental plaque is described. Based on plaque sample weights of 10 mg, the limit of detection (2 × S/N) is 0.5 μg/g. The method is linear (r = 0.9986) from the limit of detection to 50 μg/g. Recoveries from placebos spiked with 2.0, 25, and 50 μg/g of triclosan were 105.6%±7.5%, 107.2%±3.1%, and 99.1%±1.1%, respectively (n = 3 at each level). Twenty replicate preparations and analyses of a homogenized sample, conducted by two operators over the course of 4 days, showed agreement to within 9% RSD. Analyses of dental plaque collected from patients after brushing with dental cream containing triclosan, shows triclosan to be retained in dental plaque at concentrations above the minimum inhibitory concentration (1 μg/g) after 12 h.
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  • 176
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    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.
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  • 177
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    Journal of High Resolution Chromatography 19 (1996), S. 543-548 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; High temperature ; Dead time ; Constants of the n-alkane retention time curve ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In gas liquid chromatography, the column dead time and the constants of the n-alkane retention time curve are calculated by the multiparametric least-squares regression iterative method at high temperature between 180 and 270°C. The method was applied to two types of columns. The first group includes eight packed columns (seven OV polymethylphenylsiloxane and Apolane-87), while the second includes five glass capillary columns (four methylsilicone with different film thicknesses and Apolane-87). The calculated tM and b values were compared with those obtained by Guardino's, Grobler's, and Kaiser's methods. The influences of coating thickness and temperature thereon were investigated.
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  • 178
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    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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  • 179
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    Communications in Numerical Methods in Engineering 12 (1996), S. 107-114 
    ISSN: 1069-8299
    Keywords: beam ; vibration ; trial functions ; Ritz method ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: Free vibration of beams with intermediate point supports is studied by the classical Ritz method within the context of Euler beam theory. For the Ritz method, the displacement of a beam is approximated by a set of admissible trial functions which must satisfy the kinematic conditions at the ends and intermediate supports of the beam. To this end, a polynomial is superimposed on the conventional single-span beam vibration functions to form continuous-span or modified beam vibration functions. These modified beam functions are taken as the admissible trial functions for subsequent formulation. Stiffness and mass matrices are formulated using the conventional procedure and the resulting linear eigen-equation can be solved easily. A number of numerical examples are given to demonstrate the accuracy and efficiency of the present method.
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  • 180
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    Communications in Numerical Methods in Engineering 12 (1996), S. 141-145 
    ISSN: 1069-8299
    Keywords: numerical integration ; Gauss quadrature rules ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: The advance of powerful software for symbolic and numerical computations such as Mathematica sheds a new light on a paper by Golub and Welsch from 1969. Based on this paper the author describes a Mathematica procedure for determining the weights and abscissae of a Gauss quadrature rule with a user-defined weight function. After a brief description of the algorithm and its implementation examples demonstrate the usefulness of the procedure. The procedure is extremely useful if one has to compute many integrals with the same, possibly weakly singular, weight function. This might happen, for example, in the boundary element method.
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  • 181
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    Communications in Numerical Methods in Engineering 12 (1996), S. 127-134 
    ISSN: 1069-8299
    Keywords: Laplace equation ; singularities ; boundary integral method ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: The authors present a new singular function boundary integral method for the numerical solution of problems with singularities which is based on approximation of the solution by the leading terms of the local asymptotic expansion. The essential boundary conditions are weakly enforced by means of appropriate Lagrange multipliers. The method is applied to a benchmark Laplace-equation problem, the Motz problem, giving extremely accurate estimates for the leading singular coefficients. The method converges exponentially with the number of singular functions and requires a low computational cost. Comparisons are made to the analytical solution and other numerical methods.
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    Communications in Numerical Methods in Engineering 12 (1996), S. 115-125 
    ISSN: 1069-8299
    Keywords: experimental measurements ; filtering ; dynamics ; structures ; models ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: The paper presents a filtering algorithm which corrects the results of measurements of certain physical quantities if some information about the model of the system is known. The results of measurements are not only obtained in an explicit form for the considered variable but also in a form of dependent variables which are related to the measured quantity by certain mathematical relations. Combining the information obtained from different measurements, much better accuracy can be reached. It is proved that the proposed algorithm is able not only to enhance the measured data but also to detect the errors of the instruments.
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  • 183
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    Communications in Numerical Methods in Engineering 12 (1996) 
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    Keywords: Engineering ; Engineering General
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  • 184
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    Communications in Numerical Methods in Engineering 12 (1996), S. 221-222 
    ISSN: 1069-8299
    Keywords: Engineering ; Engineering General
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  • 185
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    Communications in Numerical Methods in Engineering 12 (1996), S. 151-159 
    ISSN: 1069-8299
    Keywords: response reanalysis ; structural modifications ; matrix partitioning ; Sherman-Morrison formula ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: The paper lays out an exact method, using the receptance strategy, to calculate the frequency response of a modified structure. A direct inversion of the modified impedance matrix is proposed, which reduces the computation time for successive calculations of an evolving design of the structure.
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  • 186
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    Communications in Numerical Methods in Engineering 12 (1996), S. 175-180 
    ISSN: 1069-8299
    Keywords: permanent capillar-heavy waves ; conformal mapping ; circular shaped channels ; Zeidler's method ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: E. Zeidler gave an existence and uniqueness proof for permanent heavy and capillar-heavy waves in circular shaped channels. Based on this proof and on a general computational method for constructing the solutions numerically given by the author (1991), the case of permanent heavy waves in circular shaped channels was recently computed by the author. In this work the case of permanent capillar-heavy waves in circular shaped channels is considered.
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  • 187
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    Communications in Numerical Methods in Engineering 12 (1996), S. 161-173 
    ISSN: 1069-8299
    Keywords: inverse identification ; non-linear behaviour ; material parameters ; sensitivity analysis ; finite elements ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: The identification of materials rheological behaviour in the non-linear range is based on experimental tests. When using direct identification methods, one faces the problem of the interpretation of the experimental tests, which requires the assumption of deformation homogeneity and therefore the use of approximation methods. Since this assumption is often not satisfied in the case of non-linear behaviour, material parameters are not assessed precisely. In the paper, an inverse identification method is proposed to avoid the problems raised by interpretation of the experimental tests and to determine material parameters more accurately. The algorithm developed consists of both an optimization method and a finite element method. This method is applied to the inverse identification of viscoplastic parameters of an aluminium alloy, with an investigation on the effect of the initial guess and errors in experimental data on the identified values.
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    Communications in Numerical Methods in Engineering 12 (1996), S. 181-184 
    ISSN: 1069-8299
    Keywords: finite elements ; infinite elements ; mapping functions ; unbounded domains ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: A few of the published three-dimensional Serendipity infinite element mapping functions have been discovered to be in error. The paper gives corrected versions of the defective mapping functions. The problems only relate to three-dimensional elements of the Serendipity type, when they extend to infinity in two or more directions. The new version of the mapping functions have been tested and appear to be robust.
    Additional Material: 3 Tab.
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  • 189
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    Communications in Numerical Methods in Engineering 12 (1996), S. 185-196 
    ISSN: 1069-8299
    Keywords: homogenization ; boundary conditions ; periodicity ; finite element ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: The numerical solution of homogenization equations by the finite element (FE) method is explained briefly. The issue of extracting boundary conditions from the periodicity assumption is addressed and a direct method utilizing symmetry is presented. Using this method, the computation of the elements of the constitutive matrix of a composite material is reduced to a very conventional boundary value problem with known forces and boundary conditions which can be carried out with any FE code. Two examples are presented.
    Additional Material: 15 Ill.
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  • 190
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    Communications in Numerical Methods in Engineering 12 (1996) 
    ISSN: 1069-8299
    Keywords: Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Type of Medium: Electronic Resource
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  • 191
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    Communications in Numerical Methods in Engineering 12 (1996), S. 269-270 
    ISSN: 1069-8299
    Keywords: Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Type of Medium: Electronic Resource
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  • 192
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    Communications in Numerical Methods in Engineering 12 (1996), S. 209-220 
    ISSN: 1069-8299
    Keywords: boundary element method ; dual reciprocity ; radial basis functions ; augmented thin plate splines ; body forces ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: This paper presents a novel dual reciprocity formulation for elasticity problems with body forces in which the approximating functions are given in terms of augmented thin plate splines (ATPS). It is shown that the ATPS approximation is capable of correctly representing gravitational and centrifugal body forces, and provides superior accuracy for general load cases.
    Additional Material: 6 Ill.
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  • 193
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    Communications in Numerical Methods in Engineering 12 (1996), S. 197-208 
    ISSN: 1069-8299
    Keywords: curved surface ; triangular mesh ; automatic generation ; Bézier patches ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: The paper deals with the discretization of any given multi-connected curved surface into triangular elements with straight sides. The method evolves from an initial rough triangular mesh generated from a set of input points which describe the geometry of the problem domain. Interior nodes are distributed according to user-established node-spacing functions of pre-specified spacing control parameters, and they are linked using the advancing front technique. Particular attention is paid to obtaining good distribution of interior nodes in the vicinity of the domain limits. Surface geometry representation is established using triangular Bézier patches with G1 continuity. This approach ensures a geometrically well-defined working platform for the subsequent discretization of the problem domain. The proposed method requires minimum input from the user and allows mesh gradation and remeshing to be carried out in a straightforward manner. Furthermore, problems associated with variations in the domain geometry as a result of local remeshing are eliminated with the aid of the geometrically pre-defined discretization platform. Results are presented for a range of both curved and planar surfaces, typical of those which might be encountered in hydrodynamics modelling involving flows with a free surface. The presented results demonstrate the flexibility and power of the technique.
    Additional Material: 11 Ill.
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  • 194
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    Communications in Numerical Methods in Engineering 12 (1996), S. 229-234 
    ISSN: 1069-8299
    Keywords: higher-order beam element ; best-fit stress prediction ; a priori error analysis ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: It is known that finite elements try to capture stresses within each discretized local region in a ‘best-fit’ sense. In the paper we examine the performance of a beam element based on a higher-order shear deformation theory and show that the best-fit paradigm accounts for the manner in which through-the-thickness displacement and stresses are modelled. An a priori prediction derived from the paradigm is confirmed by a carefully chosen numerical experiment. This provides a measure of the quality of approximation as well as another ‘falsification’ of the best-fit paradigm.
    Additional Material: 1 Ill.
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  • 195
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    Communications in Numerical Methods in Engineering 12 (1996), S. 223-228 
    ISSN: 1069-8299
    Keywords: Discretization ; heat conduction ; simulation ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: A different approach to discretization is described with which complicated three-dimensional heat transfer problems can be solved with a finite volume approach on a general curvilinear grid. It represents an improvement on the existing methods in that it can easily be expanded to three-dimensional problems. A concise explanation of the transformation process is given, together with a discussion of the discretization procedure. The method is evaluated by solving two simple test problems and comparing the results with those of existing methods and the analytical solution. In conclusion it is found that this method yields equally or more accurate results than the existing methods, with the additional advantage of being easily expandable to three-dimensional problems.
    Additional Material: 5 Ill.
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  • 196
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    Communications in Numerical Methods in Engineering 12 (1996), S. 243-248 
    ISSN: 1069-8299
    Keywords: finite elements ; automatic generation ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: Finite element generation methods, such as Delaunay, allow the meshing of shapes from a set of nodes. These nodes must previously exist. The authors present a simple, fast and reliable method to generate them in an unstructured way in N-dimensional space. Its main characteristic is to easily allow variation of the node density by introducing a density function, either analytical or discretized. This function can also be anisotropic. Some nodes can have a pre-fixed position. Inner lines and holes can also be specified in the domain to be meshed. Generated nodes are to be connected according to triangles in 2D and tetrahedrals in 3D.
    Additional Material: 6 Ill.
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  • 197
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    Communications in Numerical Methods in Engineering 12 (1996), S. 235-242 
    ISSN: 1069-8299
    Keywords: finite member element ; modified theory ; geometrical non-linearity ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: In the paper a modified non-linear member element is derived which can lead to satisfactory computed results even for large loading and displacement increments from pre-instability to post-instability of structures. The high accuracy of this element is proved by numerical examples.
    Additional Material: 4 Ill.
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  • 198
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    Chichester : Wiley-Blackwell
    Communications in Numerical Methods in Engineering 12 (1996) 
    ISSN: 1069-8299
    Keywords: Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Type of Medium: Electronic Resource
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  • 199
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    Communications in Numerical Methods in Engineering 12 (1996), S. 249-256 
    ISSN: 1069-8299
    Keywords: obstacle problems ; quadratic programming ; finite element ; Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Notes: The numerical solution of problems involving frictionless contact between an elastic body and a rigid obstacle is considered. The elastic body may undergo small or large deformation. Finite element discretization and repetitive linearization lead to a sequence of quadratic programming (QP) problems for incremental displacement. The performances of several QP algorithms, including two new versions of a modified steepest descent algorithm, are compared in this context. Numerical examples include a string, a membrane and an Euler-Bernoulli beam, in contact with flat and non-flat rigid obstacles.
    Additional Material: 2 Ill.
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  • 200
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    Communications in Numerical Methods in Engineering 12 (1996), S. 317-319 
    ISSN: 1069-8299
    Keywords: Engineering ; Engineering General
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mathematics , Technology
    Type of Medium: Electronic Resource
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