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  • Gas chromatography
  • Springer  (78)
  • American Meteorological Society
  • Institute of Physics
  • 1995-1999  (54)
  • 1990-1994  (24)
  • 1940-1944
  • 1996  (54)
  • 1990  (24)
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Publisher
  • Springer  (78)
  • American Meteorological Society
  • Institute of Physics
  • Wiley-Blackwell  (30)
Years
  • 1995-1999  (54)
  • 1990-1994  (24)
  • 1940-1944
Year
  • 1
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    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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  • 2
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    Chromatographia 29 (1990), S. 13-15 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Mass spectrometery ; Aerosol cans ; Chlorofluorocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic (GC) method for the routine analysis of fully halogenated chlorofluorocarbons (CFCs) in aerosol cans is described. The identification of CFCs by GC was found to be in full agreement with those by GC-mass-spectrometery. The method has been applied to the analysis of CFCs in 448 aerosol products. The most commonly used fully halogenated CFC propellants in aerosol cans were found to be CFC11, CFC12 and CFC114.
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  • 3
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    Chromatographia 29 (1990), S. 322-324 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; C6 epoxides ; Retention indices
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of C6 epoxides on a fused-silica capillary column coated with Permaphase DMS (dimethylsilicone) was investigated. Retention indices were determined at 50 and 60°C. We demonstrate that this stationary phase provides a better resolving power than OV-101.
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  • 4
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    Chromatographia 29 (1990), S. 385-388 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Split injector design ; Glass inserts
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In stop-flow split injection the careful choice of the experimental conditions is of great importance for accurate quantitation, the size of the gaseous sample plug and its position with respect to the column inlet and to the top of the insert during the evaporation period are critical to prohibit sample vapour overflow and aerosol splitting. The proper insert design is established. A sample volume of 0.5 μl is recommended in the practical application of the stop-flow method.
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  • 5
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Pesticide analysis ; Multiresidue methods ; Solvent extraction schemes ; Fruit samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A comparative study of different multiresidue methods for the determination of organochlorine and organophosphorus pesticides in fruit samples has been carried out. Recoveries for each pesticide added to a peach sample were obtained after applying different extraction systems. The study was performed with the following pesticides: dimethoate, chlorpyrifos, fenitrothion, lindane, malathion, methidathion, phentoate and tetradifon. Extraction systems induded: acetonitrile+anhydrous sodium sulphate, acetonitrile-water+Celite acetone and acetone-methanol. Determination of pesticides was performed by gas capillary chromatography with ECD and NPD. GC/FPD and GC/MS were also used for confirmation and identification purposes.
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  • 6
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Selective detection ; Oxygen flame ionization detector ; Camomilla oils
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The application of the Oxygenate Analyzer (O-FID) developed for the selective determination of oxygenated compounds has been studied for the quality control and classification of camomilla oils. In comparison to FID detection the O-FID results in a simpler chromatogram and a much higher sensitivity for the characteristic oxygenated compounds. On the basis of the O-FID chromatograms, by measuring the relative peak areas of the characteristic compounds, the camomilla oils can be classified and the oils of unacceptable quality unambigously distinguished.
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  • 7
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    Chromatographia 30 (1990), S. 630-634 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Poly(ethylene glycol) 20M ; Silanized supports ; Retention mechanisms
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The properties of poly(ethylene glycol) 20M (PEG 20M) on the silanized surface of Chromosorb W HMDS were investigated. It was found that the surface layer of PEG 20M is in a liquid form below its melting temperature. It the stationary phase loading ratio is above 0.105 the main retention mechanism is partition in both the liquid and solid forms of PEG 20M. The contribution of adsorption to the retention volume was also determined. It is suggested that in the case of methanol this contribution is caused by adsorption on the residual silanol groups present on the support surface whereas for n-octane this is rather adsorption on the gas-liquid interface.
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  • 8
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    Chromatographia 30 (1990), S. 493-499 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Chemical potential of solutes ; Ideal dilute solutions ; Effect of size of solvent molecule
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas-liquid chromatography allows the rapid experimental determination of the Henry coefficient of molecular probes if a number of precautions are taken. From a knowledge of the temperature dependence of the related standard chemical potential, the standard partial molar enthalpy, entropy and the mean heat capacity difference can be calculated. These functions determine the retention behaviour of the probe over a temperature range of more than 100 K with a precision better than 1%. They also give the necessary information to verify and to develop models for ideal dilute solutions and for the calculation of interaction forces. The choice of specific solvents is examined and justified and the experimental determination of retention data is discussed especially with reference to the precautions to observe in order to measure retention governed by gas-liquid partition only. Calculation of the standard chemical potential related to the molal Henry coefficient is advocated and the dependence of the standard chemical potential on size and shape of the solvent molecule based on data collected on paraffinic stationary phases is examined. This latter function is shown to depend linearly on the inverse of the molar mass of the solvent. Comparison with literature data demonstrates the general validity of this finding and that the shape of the solvent molecule is of less importance.
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  • 9
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    Chromatographia 30 (1990), S. 421-423 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column liquid chromatography ; Carbofuran ; Hydroponics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two analytical methods using GC/NPD and HPLC to analyse carbofuran in a nutrient solution used in hydroponic culture are described. Both methods show a high recovery, (greater than 90%), and their limits of detection are low.
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  • 10
    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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  • 11
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    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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  • 12
    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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  • 13
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    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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  • 14
    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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  • 15
    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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  • 16
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    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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  • 17
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    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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  • 18
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    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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  • 19
    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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  • 20
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    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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  • 21
    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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  • 22
    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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  • 23
    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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  • 24
    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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  • 25
    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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  • 26
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    Chromatographia 29 (1990), S. 544-546 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace sampling ; Fluoride in milk ; Trifluorosilane derivative
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new method was developed for the determination of fluoride in fluorinated milk on the basis of headspace gas chromatography utilizing, the reaction between trimethylchlorosilane and ion-bound fluorine in highly acidic media. The obtained trifluorosilane has a high volatility and can be easily determined by headspace gas chromatography.
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  • 27
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Leaded fuels ; Unleaded fuels ; Gasohol ; Straight-hydrocarbon fuels
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary It has been theorized that the removal of lead in fuels may result in an increase of fuel volatility. In addition, alcohols added to fuels (“gasohols”) increase volatility. Consequently, benzene emissions in unleaded and gasohol vapors may be increasing. Flame ionization detection gas chromatography was used to analyze benzene concentrations in fuel vapors. Results indicated that leaded fuels emitted more benzene than unleaded fuels. Though benzene concentrations varied for unleaded vapors, leaded gasohol fuels had higher benzene levels than their straight-hydrocarbon counterparts. These higher benzene emission levels may be an indication that volatility increases in leaded and some gasohol brands.
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  • 28
    ISSN: 1612-1112
    Keywords: Gas chromatography ; FPD-Detection ; Sulfur compounds ; Quenching effects ; Series-coupled columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In a series-coupled system of two capillary columns with different polarity, a controlled overlapping of sulphur-containing and sulphur-free compounds can be achieved by means of different mid-point pressure settings. By means of this selectivity tuning it is possible to measure exactly the quenching of the flame photometric detector signal for a sulphur compound coeluted with an excess of a sulphur-free compound. With the example of a complex sample it is shown that, with a suitable system of columns, selectivity tuning can give quench-free FPD chromatograms or chromatograms with quench-free regions.
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  • 29
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    Chromatographia 30 (1990), S. 635-638 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention values ; Adsorption ; Glass capillary columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Effect of adsorption on the retention values for some n-alkanes, n-alcohols and esters in glass capillary columns coated with PEG-20M was studied. Adsorption parameters for the used solutes were evaluated from the retention data.
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  • 30
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    Chromatographia 30 (1990), S. 144-148 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index calculation ; Alkylbenzenes ; Structure-retention relationships
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The correlation between retention data of alkylbenzenes in GLC (measured on the stationary phase OV-101) and contribution of the Gibbs solvation energy are investigated in order to determine the dominant factor controlling retention. The retention in GLC can be predicted with help of our thermodynamic retention model.
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  • 31
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Chemiluminescence detection ; Se, Te and S compounds ; Speciation of elements ; Headspace analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The sensitive detection of volatile, methylated selenium and tellurium compounds based on capillary gas chromatography coupled to fluorine-induced chemiluminescence detection is described. The method requires no sample derivatization, and the detection limits for selenides and tellurides (low pg range) are the lowest reported to date. This technique can resolve and speciate complex mixtures of methylated tellurium, selenium, and sulfur gases and is useful for analysis of selenium and tellurium gases in environmental samples that also contain usually interfering reduced sulfur gases. Applications of the technique for analysis of bacterial and fungal headspace samples are presented.
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  • 32
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    Chromatographia 30 (1990), S. 489-492 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Trace enrichment in gases ; Adsorption effects
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
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  • 33
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index reproducibility ; Alkylbenzenes ; HP PONA columns ; OV-101 glass capillary columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Reproducibility of the Kovats retention indices of alkylbenzenes was studied on conventional “PONA” fused-silica capillary columns coated with crosslinked dimethyl silicone phase, with a film thickness of 0.5 μm. The data were compared with those obtained on conventional OV-101 columns. The tested PONA columns showed reproducible chromatographic properties, capacity ratios and high efficiencies. Having a standard deviation of s=0.03 i.u. of the retention indices on a single column, the column-to-columns differences were found to be up to 0.3 i.u. Higher indices were determined for crosslinked columns, the difference being in most cases about one i.u.
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  • 34
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    Chromatographia 42 (1996), S. 77-82 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Modified alumina ; Coal mine air ; Alkenes, alkanes
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    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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  • 35
    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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  • 36
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    Chromatographia 42 (1996), S. 309-312 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Graphite coated capillary columns ; Ephedrines separation ; Drug analysis
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    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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  • 37
    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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  • 38
    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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  • 39
    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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  • 40
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Solid phase micro extraction ; Chloroethenes ; Reductive dechlorination
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    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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  • 41
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Local anaesthetics ; Solid phase micro extraction (SPME) ; Direct immersion
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    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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  • 42
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary phase ; β-Cyclodextrin ; Separation mechanism
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    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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  • 43
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Dicofol ; Fish ; Lethal concentration ; Bioconcentration factor
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    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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  • 44
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Electronic pressure control ; Mass selective detector ; Pesticide residues ; Cereals
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    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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  • 45
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    Chromatographia 43 (1996), S. 208-210 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Epoxystyrenes ; Retention index
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    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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  • 46
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Microwave-assistend solvent extraction (MASE) ; Pesticide residue analysis ; Triazine herbicides ; Soil samples
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    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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  • 47
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fosfomycin in urine ; Pharmacokinetics
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    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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  • 48
    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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  • 49
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary phase ; Polysiloxane matrices ; β-Cyclodextrin ; Crown ether ; Liquid crystal ; Coordination effect
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    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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  • 50
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    Chromatographia 29 (1990), S. 571-574 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Micro-trap ; Trace analysis ; Airborne halocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary For routine analyses involving numerous samples or for field operation of on-site instruments, cryogenic traps are inconvenient: their operation is timeconsuming and automation is technically demanding. complete trapping and efficient band-focussing may be achieved at ambient temperature with micro-traps packed with suitable sorbents. Two approaches have been evaluated: if the boiling points of the analytes are within a range of about 100°C, a single-sorbent trap and direct coupling to the column are recommended; for samples containing components wih widely different volatilities, a trap composed of two or more segments with complementary affinties and coupling to the chromatographic column under carrier-gas flow-reversion is preferable. The procedure has been evaluated for airborne C1 and C2-halocarbons; it is also applicable to trace analysis of other volatile organic air pollutants.
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  • 51
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    Chromatographia 29 (1990), S. 575-578 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention values ; Adorption effects ; Glass capillary columns
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    Topics: Chemistry and Pharmacology
    Notes: Summary Effect of adsorption on the retention values for C5−C10 alkanes and C1−C8 n-alcohols in glass capillary columns coated with OV-101 is investigated. Adsorption parameters are evaluated from the retention data
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  • 52
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    Chromatographia 29 (1990), S. 347-350 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Quantitative determination of carbon monoxide ; In-situ generation of standards
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    Topics: Chemistry and Pharmacology
    Notes: Summary Carbon monoxide, produced from the dehydration of formic acid in the presence of sulfuric acid is proposed for the quantitative determination of the gas in the parts-per-million range. In this method the standard solution of formic acid in acidified water is introduced with a total-volume syringe from the injector and passes through a precolumn packed with sulfuric acid on diatomite support. The produced carbon monoxide is converted to methane over nickel and determined with a flame-ionization detector. The accuracy of this method is about 5% in the experimental range.
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  • 53
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    Chromatographia 30 (1990), S. 255-262 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; FTIR ; γ-Irradiation sterilization ; Medazepam ; 1,4-Benzodiazepines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A methanolic solution of 2% medazepam was irradiated with a dose of 50 kGy. A capillary gas chromatograph with a Fourier Transformation Infrared Spectrophotometer (FTIR) was used to investigate the radiolysis products in the solution. The changed products found earlier were confirmed and new ones identified. The radiolytic scheme can be improved and enlarged.
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  • 54
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    Chromatographia 30 (1990), S. 267-270 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Split injection ; Insert packing material ; Melissyl alcohol
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    Topics: Chemistry and Pharmacology
    Notes: Summary For accurate determination of polar, high-boiling melissyl alcohol in mixtures containing also low-boiling components by capillary column gas chromatography with hot split injection, all experimental paramenters, such as the injection procedure, insert size and design, injector temperature, sample size, solvent and carrier gas nature, etc. must be optimized. Of the factors affecting the quantitation the nature of the insert packing material is of the greatest importance. With the commonly used packing material, quartz wool, in the insert, a much lower than true melissyl alcohol concentration was obtained. Accurate quantitation was only possible when stop-flow injection, together with an insert packed with glass beads was used.
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  • 55
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    Chromatographia 30 (1990), S. 163-170 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Universal retention index ; Classification of stationary phases ; Identification
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    Topics: Chemistry and Pharmacology
    Notes: Summary The universal retention index has been developed on the basis of a critical analysis of the forms of chromatographic retention data presentation. Methods are presented for the determination of the universal retention index. The advantages of the universal retention index system in the evaluation of the selectivity and classification of stationary phases and in the determination of the composition of binary and polynary stationary phases are discussed. The thermodynamic aspect of the suggested system of chromatographic retention data presentation is also considered.
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  • 56
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    Chromatographia 30 (1990), S. 211-214 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Determination of adduction contant ; Enthalpies and entropies
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    Topics: Chemistry and Pharmacology
    Notes: Summary The adduction constants for the following eight binary systems were measured by gas liquid chromatography, at different temperatures: tetrachloromethane/p-xylene, tetrachloromethane/pseudocumene, chloroform/p-xylene, chloroform/pseudocumene, chloroform/aniline, m-methylphenol/aniline, o-methylphenol/aniline, and o-chlorophenol/aniline. The relationships between the adduction constant and temperature were used to fit the enthalpies and entropies of adduct formation.
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  • 57
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Trimethylsulfonium hydroxide (TMSH) ; FAME analysis ; Bacteria ; Blood serum
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Trimethylsulfonium hydroxide (TMSH) can convert fatty acids into the corresponding fatty acid methyl esters (FAMEs) in a single step. These fatty acids may also be bound in biomolecules such as phospholipids and/or glycerides. Complex mixtures of saturated and unsaturated FAMEs which may contain hydroxy and cylopropyl groups are obtained by trans-esterification; they can easily be separated in most cases by capillary GC. When FAMEs are generated from different microorganisms e.g. bacteria the patterns of the chromatograms are characteristic. Examples of characteristic patterns of bacteria with different cell wall structures are shown. The described method of transesterification can also be applied directly to blood serum without sophisticated sample pretreatment. The profiles of the chromatograms match well those described in the literature obtained by other methods of trans-esterification or sample preparation.
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  • 58
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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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  • 59
    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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  • 60
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Semivolatile flavor compounds ; Cinnamon ; Solid-phase microextraction ; Chemometric classification
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    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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  • 61
    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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  • 62
    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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  • 63
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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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  • 64
    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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  • 65
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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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  • 66
    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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  • 67
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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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  • 68
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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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  • 69
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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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  • 70
    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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  • 71
    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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  • 72
    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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  • 73
    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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  • 74
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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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  • 75
    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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  • 76
    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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  • 77
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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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  • 78
    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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