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  • Gas chromatography  (272)
  • Springer  (272)
  • American Chemical Society
  • 2005-2009
  • 1990-1994  (164)
  • 1980-1984  (108)
  • 1925-1929
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  • 1
    ISSN: 1434-4475
    Keywords: Gas chromatography ; Polyphenyl ethers ; Lubricants, synthetic
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The described synthesis of synthetic lubricants based on polyphenyl ethers requires an analytical characterization of the isomerization step, which is important to the process optimization. The separation of the intermediates succeeds with gas chromatography; the isomers are determined using a retention index system. The obtained results are compared with the composition of the final product, which was investigated by HPLC analysis.
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  • 2
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    Entomologia experimentalis et applicata 34 (1983), S. 20-26 
    ISSN: 1570-7458
    Keywords: Dioryctria abietella ; Cone pyralid ; Lepidoptera ; Pyralidae ; Sex pheromone, (Z,E)-9,11-tetradecadienyl acetate ; Single sensillum recordings ; Electroantennography ; Gas chromatography ; Mass spectrometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Description / Table of Contents: Résumé L'analyse en chromatographie gazeuse associée à une détection électroantennographique a montré que l'acétate (Z,E)-9,11-tétradécadiényle (Z,E)-9,11–14:Ac est l'un des composants de la phéromone de Dioryctria abietella Schiff (Lepid.: Pyralidae). Couplage chromatographie en phase gazeuse spectrometrie de masse a montré la présence d'acétate tétradécadiényle avec un spectre de masse et un indice de rétention identiques au Z,E-9,11–14:Ac Un récepteur cellulaire sensible à la fois au Z,E-9,11–14:Ac et à un extrait de la femelle a été identifié sous l'antenne du mâle. Les analyses des antennogrammes et de la cellule isolée ont étayé la caractérisation du composant de la phéromone comme étant Z,E-9,11–14:Ac. Un récepteur cellulaire additionnel sensible à l'acétate (Z.)-9-tétradécadiényle et à l'acétate (Z.E.)-9,12-tétradécadiényle a été trouvé sur l'antenne du mâle, mais il n'était pas activé par l'extrait de la femelle. Sur le terrain Z,E-9,11–14:Ac, présenté seul, attirait des nombres importants de mâles de D. abietella. L'addition de l'acétate (Z)-9-tétradécényle a inhibé l'attraction des mâles par les pièges.
    Notes: Summary Gas chromatographic analyses coupled with electro-antennographic detection indicated that (Z,E)-9,11-tetradecadienyl acetate (Z,E-9, 11–14:Ac) is a pheromone component of the cone pyralid Dioryctria abietella. Gas chromatographic-mass spectrometric analyses confirmed the presence of a tetradecadienyl acetate with mass spectrum and retention index identical to Z,E-9,11–14:Ac. A receptor cell sensitive to both Z,E-9,11–14:Ac and the female extract was identified on the male antenna. An additional receptor cell sensitive to (Z)-9-tetradecenyl acetate and (Z,E)-9,12-tetradecadienyl acetate was found on the male antenna but was not activated by the female extract. In the field Z,E-9,11–14:Ac presented alone attracted significant numbers of male D. abietella. Addition of (Z)-9-tetradecenyl acetate inhibited the attraction of males to traps.
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  • 3
    ISSN: 1432-2285
    Keywords: Abies alba ; Abscisic acid ; Damage ; Gas chromatography ; Needles
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary The amount of abscisic acid (ABA) in needles of silver fir from a natural location was investigated with regard to position in the crown, damage, seasonal variation, and needle age. Because of problems of quantification of ABA in coniferous needles, which contain numerous secondary plant products, a method for reliable determination of both isomers cis-trans-ABA (c-ABA) and transtrans-ABA (t-ABA) was developed. By means of gas chromatography (GC) using an electron capture detector (BCD) and a programmed temperature vaporizer (PTV) injector complete separation of both compounds was achieved. Two different pairs of fir were investigated — in each case a damaged and a healthy tree. Needles from both trees from the first and the second pair collected in September contained 500–1100 ng c-ABA/g fresh weight (FW), and the concentrations of t-ABA varied from 400 to 700 ng/g FW. Investigations from the second pair show highest amounts of 2900 ng/g Fw c-ABA and 1800 ng/g FW of t-ABA in May and June. For the first pair a higher c-ABA content was found in needles from the top of the crown than in those from the middle and the base. This difference could not be confirmed in the analysis of the second pair. Because of the strong natural deviation no statistically significant difference between the healthy and the damaged tree was found. The first pair of firs examined showed a higher t-ABA concentration than the second one. In this case the highest amount was found in the top of the crown. Methodical mistakes during the clean-up procedure and in quantification by gas chromatography could be excluded. The presence of c- and t-ABA in the purified extract was corroborated by mass spectrometry. With regard to the seasonal variation both isomers of ABA show an unequivocal trend. The maximum concentration is achieved in May to June, whereas the content is minimal in August/September. In any case the level of t-ABA is lower than that of c-ABA. No correlation between the amount of ABA and the needle age could be established.
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  • 4
    ISSN: 1432-0878
    Keywords: Preputial glands ; Nude mice ; Ultrastructure ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary The preputial glands of male nude (nu/nu) mice were analyzed by a combination of electron microscopy and gas chromatography to determine whether or not they are affected, like developing hairs and nails, by the nu/nu genotype. Results of the analyses revealed no differences between the glands of nude and normal male mice in either their ultrastructural characteristics or lipid secretory products.
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  • 5
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    Chromatographia 13 (1980), S. 203-206 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carrier gas purity ; Sample stability
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The amount of oxygen which may be present in the gas volume corresponding to a peak is investigated and compared to the sample amounts. It is shown that even with high purity carrier gases one may have a significant excess of oxygen present at low sample amounts. Attention is drawn to the possibility of impurity build-up by diffusion e.g. through the septum.
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  • 6
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    Chromatographia 13 (1980), S. 263-270 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Metal complexes ; Enantiomers ; Isotopic composition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The high selectivity of complexation gas chromatography has been employed for enantiomer resolution and isotope separation. Thus, a chiral olefin, 3-methylcyclopentene, has been resolved analytically on optically active dicarbonyl-rhodium(I)-3-trifluoroacetyl-1R-camphorate in squalane. The deuterated ethylenes C2H4−nDn have been separated on the same rhodium(I)-containing stationary phase. The chiral aliphatic oxiranes epoxypropane andtrans-2,3-epoxybutane have been resolved on optically active nickel(II)-bis-3-trifluoroacetyl-1R-camphorate in squalane.
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  • 7
    ISSN: 1612-1112
    Keywords: Gas chromatography ; On-column abstraction ; Aliphatic aldehydes ; Amine antioxidants
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The selective on-column abstraction of aliphatic aldehydes by gas chromatographic stationary phases containing N-iso-propyl N′-phenyl-p-phenylenediamine is described.
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  • 8
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    Chromatographia 14 (1981), S. 19-22 
    ISSN: 1612-1112
    Keywords: Teflon columns ; Chemically modified teflon ; Gas chromatography ; Capillary columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Wall-coated open tubular columns prepared from chemically modified teflon tubing have been developed for gas chromatography. Chemical reaction of the inner walls of teflon tubing allows bonding of an adhesive layer on which a variety of stationary phaes can be coated. Test mixtures of alkanes and alcohols were used to investigate the chromatographic properties of these columns and the stability and mixing of the adhesive and stationary phae layers. the results in dicate that mixing of the layers is negligible and that the column is stable for a long period of time.
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  • 9
    ISSN: 1612-1112
    Keywords: Teflon capillary columns ; Chemically modified teflon ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of teflon capillary columns employing direct coating of the stationary phase to the chemically modified teflon surface and the role of the chemically modified teflon in the separation mechanism are described. Two types of contributions from the modified teflon have been observed: nonspecific adsorption of the carbon surface and specific interactions of polar groups in the carbon skeleton. The use of polar liquid phases can eliminate adsorption due to the presence of polar groups in the modified teflon.
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  • 10
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    Chromatographia 14 (1981), S. 55-66 
    ISSN: 1612-1112
    Keywords: Capillary columns, glass ; Gas chromatography ; Column preparation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Kapillar-Gas-Chromatographie ist heute das sich am stärksten entwickelnde Gebiet der Gas-Chromatographie. Es gibt viele komplexe, neue Fragestellungen in der Analytik, welche den Einsatz spezieller Kapillarsäulen erfordem. Glücklicherweise gibt es aber auch eine große Zahl von Herstellungsverfahren für Kapillarsäulen, welche — noch mehr als bei der Herstellung von gepackten Säulen — eine Anpassung an die gestellten Aufgaben ermöglichen. In diesem Artikel werden die Herstellungsverfahren für Kapillarsäulen zusammengestellt und Anregungen gegeben, wie aufgaben-orientierte Säulen erreicht werden.
    Notes: Summary Glass capillary column chromatography is the most rapidly growing part of gas chromatography. There are many complex new analytical tasks and they require special capillary columns, Fortunately there is a wide range of column preparation methods available, and they make the preparation of glass capillary columns a more varied job than that of packed columns. In this paper these methods are reviewed and suggestions are given for making task-oriented columns.
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  • 11
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Urea herbicides ; Catalytic hydrolysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the rapid catalytic hydrolysis of phenylurea herbicides on silica gel at elevated temperatures. After derivatisation of the anilines produced with heptafluorobutyric acid anhydride final analysis is done on a gas chromatograph equipped with an electroncapture detector. Detection limits are in the 1–5 picogram range. The method has successfully been applied to residue analysis of water samples at the 1 ppb level. The determination of free anilines present in water samples and the potential of various techniques to be used to discriminate between free anilines and parent herbicides are also discussed.
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  • 12
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Graphitised carbon black ; Phenols ; Water pllutants
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The fractionation of eleven phenols which may be contaminants in drinking water has been accomplished by using acid-washed graphitised carbon black modified with trimesic acid and PEG 20 M.
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  • 13
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    Chromatographia 14 (1981), S. 447-451 
    ISSN: 1612-1112
    Keywords: Headspace analysis ; Gas chromatography ; Residual analysis of polyethylene terephthalate ; Acetylene reduction assay ; Ethylene evolution in germinating seed ; Acetaldehyde generation in polyester resin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary New application areas for headspace gas chromatography in agricultural and polymer degradation research are described. Specific examples are drawn from the various forms of headspace analysis with emphasis on the automated static equilibrium method.
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  • 14
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    Chromatographia 13 (1980), S. 35-39 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Nitromethane ; Nitroalkanes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Impurities in commercially available nitromethane have been determined by gas-liquid chromatography using six different column packings. Besides nitromethane, 1-nitropropane, 2-nitropropane, acetonitrile, methanol, small amounts of ethanol and acetaldehyde have been detected. The presence of formaldehyde, ethyl acetate and acetone is probable. Mixtures containing comparable amounts of the four nitroalkanes could be separated on all columns, but plots of logarithms of the retention times vs. carbon number or boiling points of the nitroalkanes or column temperatures were linear only in case of columns packed with Porapak R and Q.
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  • 15
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    Chromatographia 16 (1982), S. 60-62 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Amines ; Derivatization ; Chloroformate esters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The gas chromatographic analysis of amines after conversion to electron capture sensitive carbamates in two-phase systems has been studied. Hydrophilic compounds, for instance methylamine, are reacted with 2,2,2-trichloro-tert. butyl chloroformate. Quantitation below 10−7 M can be made by thermionic or electron capture detection. A hydrophobic amine, namely N,N-dimethyl-n-octylamine, was derivatized with 2,4,6-tribromophenyl chloroformate with addition of iodide ion to the aqueous phase. The favorable effect of iodide ion as well as the choice of pH and chloroformate ester is discussed.
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  • 16
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    Chromatographia 16 (1982), S. 98-102 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Rectangular channel ; Efficiency ; Capacity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic experiments have been performed in a truly rectangular channel with a 60∶1 cross-sectional aspect ratio, constructed according to the field-flow fractionation technology. It is shown that the peak broadening is controlled by the thickness of the channel while the maximum load is determined by the largest cross-sectional dimension. However, even with its elongated configuration, the side walls contribute significantly to the band broadening of solutes with a high diffusivity. Good agreement is found between the experimental plate height data and the recent theoretical calculations of Golay [13] taking into account the side-wall effect.
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  • 17
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    Chromatographia 17 (1983), S. 269-284 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid chromatography ; Phenols
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas and high-performance liquid chromatographic methods in the analysis of phenols are reviewed. Among the great number of phenolic compounds analyzed, alkylphenols, chlorophenols, dihydroxy- and trihydroxybenzenes and biphenols are chiefly considered. The advantages and drawbacks of the methods are discussed, quoting the most important work. Relationships between the structural characteristics of phenols, the stationary phase structure, the mobile phase composition and the retention data are treated. Typical examples of the conditions for GC and HPLC analysis are summarized in tables. The literature comprises over 270 references, most of them recent.
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  • 18
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Average molecular polarizability ; Retention index ; Polycyclic aromatic hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The Kováts retention indices of 10 polycyclic aromatic hydrocarbons were determined on SE-30, OV-101, SE-52, OV-7 and OV-17 stationary phases. A significant correlation has been found between the retention indices and the average molecular polarizabilities of the analyzed substances. Equations were derived for the direct determination of the average molecular polarizabilities from the retention index values. The influence of the temperature on this relationship is also indicated.
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  • 19
    ISSN: 1612-1112
    Keywords: Esterification in aqueous solution ; iso butyl esters of C1–C20 fatty acids ; Gas chromatography ; Fatty acid analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary C1–C20 carboxylic acids have been esterified in aqueous solutions with i-butanol. Gas chromatographic analyses have been performed from a single chromatogram. It has been established that esterification in the concentration range of [H2O]/[i-BuOH]=0.01–10.3 can be utilized for the quantitative determination of these carboxylic acids. The presence of water does not interfere in the range of [H2O]/[i-BuOH]=0.01–1.03. In the cases of [H2O]/[i-BuOH]〉1.03, anhydrous sodium sulfate has been used for binding the water, in an amount of [Na2SO4]anh./[H2O]≥0.2.
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  • 20
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Butyl esters of C2−C16 dicarboxylic acids ; Dicarboxylic acid analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary C2−C16 dicarboxylic acids were esterified in aqueous solution in the presence of sulfuric acid. Esterification in water/n-butanol mixtures with mole ratios between 0.02 and 2.53 can be utilized for the quantitative determination of the dicarboxylic acids by gas chromatography. The presence of water does not interfere at water/n-butanol mole ratios below 0.27. For mole ratios above 0.27 anhydrous sodium sulfate has been used for binding the water. The mole ratio range was 0.25–0.75 for anhydrous sodium sulfate/water, and 0.32–1.3 for sulfuric acid/anhydrous sodium sulfate.
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  • 21
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    Chromatographia 18 (1984), S. 663-667 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas solubilities ; Enthalpies of solution ; Polar solutions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The gas-liquid chromatographic method has been used to determine the solubilities and partial molar enthalpies of solution of the gases H2S, CO2 and COS in four polar solvents. The results agree well with literature values obtained using conventional techniques, with the one exception of H2S in N-methyl-2-pyrrolidinone. In this case there is some evidence for the occurrence of adsorption at the gas-liquid interface.
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  • 22
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Butyl esters of aromatic polycarboxylic acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The direct esterification and gas chromatographic analysis of aromatic carboxylic acids as n-butyl esters is described. Derivatization is performed in aqueous solution with n-butanol in the presence of sulfuric acid. The butyl esters of benzoic, phthalic, hemimellitic, trimellitic, trimesic and pyromellitic acids permit their gas chromatographic separation from each other and from fatty acids and alipatic dicarboxylic acids. At mole ratios of [H2O]/ [n-BuOH]≤0.04 the water present does not interfere with the esterification reaction. At mole ratios above 0.04 anhydrous sodium sulfate is used for binding the water, at mole ratios of [Na2SO4 anh.]/[H2O]=0.25–0.75.
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  • 23
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    Chromatographia 18 (1984), S. 202-204 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Polysiloxane stationary phases ; Heat of adsorption ; Heat of solution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The changes in the heat of solution of polar compounds and xylene isomers in methylsilicone fluid OV-101 deposited on Chromosorb W AW DMCS were studied. It was shown that the heat of solution increases with an increase of the percentage loading of the OV-101 up to 10%. Solution and adsorption thermodynamic characteristics of the studied system are briefly discussed.
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  • 24
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Metal complexes ; Chemically bonded phase
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Packings consisting of diphenylphosphine complexes with CoCl2 and CoBr2, chemically bonded to the silica surface, were synthesized and their retention parameters determined. The packings are capable of specifically interacting with electron-donating compounds by forming π-complexes. The interaction is considerably stronger in the case of CoBr2-containing packing than in the case of CoCl2-containing packing.
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  • 25
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    Chromatographia 18 (1984), S. 234-238 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open-tubular columns ; On-column injection ; Stopped-flow operation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple, inexpensive, on-column injector of the septum moving-needle kind is described for quantitative analysis using open-tubular columsn. when operated in the stopped-flow mode an improvement incolumn efficiency is observed combined wit a diminished tendency to produce split-top peaks, particularly for late eluting peaks. Using electronic integration a relative error of about 2.7% was observed for peaks spanning a wide range of sample concentrations and volatilities.
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  • 26
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    Chromatographia 18 (1984), S. 243-248 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carrier gas ; Viscosity ; Influence of temperature
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The vicosity-temperature relationship of the three gases (helium, nitrogen and hydrogen) most frequenly used as the carrier gas in gas chromatography is studied. Based on available data, equaitions are derived to describe this relationship. Using these equations viscosity data are tabulated for the chromatographically important temperature range.
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  • 27
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    Chromatographia 18 (1984), S. 260-264 
    ISSN: 1612-1112
    Keywords: Parabens and their dissolution ; Pharmaceutical dosage forms ; Derivatization ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A specific, sensitive and general applicabla gas chromatographic method is described for the determination of parabens in various liquid pharmaceutical preparations: propylparaben and butylparaben in a liquid antacid dosage form (I); methylparaben, ethylparaben and propylparaben in a syrup (II); methylparaben and propylparaben in a solution for injection (III). Each time one of the parabens is used as internal standard. The parabens are extracted with diethylether and derivatized by silylation. Different columns are used for the analysis of the parabens: 3% SE-30 column, a 3% QF-1 column for different selectivity, a 2% OV-1 column for isothermal operation. Special attention is attributed to the standard: the parabens are dissolved in a minimal amount of 0.1 M sodium hydroxide and extracted in the same way as the pharmaceutical dosage form.
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  • 28
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Configuration ; Resolution ; Alcohols
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The study of the resolution of sixteen secondary aliphatic alcohols by gas chromatography on (+)-dodecyl (2R, 3R)-tartrate, trapping the ascending part of the peak from a conventional filled column, has allowed the determination in a single operation of the sign and order of emergence of enantiomers. A correlation between the configuration of these secondary alcohols and their order of emergence has been established.
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  • 29
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    Chromatographia 18 (1984), S. 309-312 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carboxylic acids ; Acetonyl derivatives
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of the acetonyl esters of nine aliphatic carboxylic acids is described, the general formula of the derivatives being RCOOCH2COCH3 where R=alkyl or H. The derivatives show good chromatographic properties on both packed and capillary columns. The electron impact and chemical ionisation mass spectra of the derivatives are discussed.
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  • 30
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Thermodynamic relationships ; Retention index ; Peak identification
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A thermodynamic criterion, ΔQ, is suggested which permits to estimate the difference in the functional group energy of interactions for two different stationary phases. The linear dependence of ΔQ on the homolog number m of any series Rm X can be used as the thermodynamic criterion for the identification of substances by GC analysis.
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  • 31
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    Chromatographia 18 (1984), S. 477-488 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open tubular (capillary) columns ; Sample capacity ; Column comparison ; Film thickness ; Column diameter
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Wall-coated, open-tubular (capillary) columns prepared from different diameter tubing, with different liquid phase film thickness, are compared with each other and with packed and support-coated open-tubular columns. The comparison is based on the variation of the phase ratio and the capacity factor, and includes column efficiency (HETP, theoretical plate number), resolution, retention time, and sample capacity. Problems associated with the evaluation of the sample capacity are outlined. The influence of temperature on column performance is discussed in detail. Finally, the possibilities of short, wide-bore open-tubular columns prepared with a thick liquid-phase film are demonstrated.
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  • 32
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    Chromatographia 35 (1993), S. 649-652 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Triglycerides in cheese ; Programme temperature (PTV) injection ; Silica capillary columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid gas chromatographic method for the analysis of triglycerides in cheese on a capillary column with a programmed temperature vaporizer has been developed. Fat were extracted with hexane to dryness. The reproducibility of the method was assessed and the coefficient of variation for the total triglycerides was 2.50%. Recovery of individual triglycerides ranged between 87 to 105%.
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  • 33
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Curie-point pyrolysis ; Multivariate analysis ; Sodium dodecylbenzene sulfonate
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    Topics: Chemistry and Pharmacology
    Notes: Summary Multivariate analysis can be applied to quantitative analysis of sodium dodecylbenzene sulfonate (DBS) by pyrolysis gas chromatography. The pyrograms obtained from mixtures of DBS and polyoxyethylene lauryl ether (PEG) were normalized for the peak heights and areas of several internal standards which appeared in every pyrogram, against the characteristics peaks for DBS and PEG. This normalization method gave smaller experimental errors than when using one internal standard. The normalization values were used for cluster analysis unchanged. The values were calculated correlation coefficients and principal component analysis was performed using 11 data base and a set of sample data simultaneously. One calibration curve was calculated from the principal component scores. The DBS content of a sample was obtained from the calibration curve. Calculated values were in fair agreement with theoretical values.
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  • 34
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    Chromatographia 36 (1993), S. 187-190 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Solid-phase extraction disks ; Pesticides ; Soil analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A systematic study comparing the methodology and analytical results obtained in an investigation of seven pesticide residues (Molinate, Atrazine, Carbofuran, Pirimicarb, Prometryn, Malathion and Tetrachlorvinphos) in soil samples is reported. Solid-phase extraction (SPE) using glass columns and 47 mm disks of octyl and octadecyl-bonded silica was used in the pesticide analysis. The best extraction efficiency and clearest extracts are obtained with C8 disks. The analyses were carried out by capillary gas chromatography with nitrogen and phosphorus detection. Recovery experiments were performed at ppb levels in spiked soil samples. The average recoveries of the compounds were 53–77%. Detection limits are between 5 and 30 ng g−1 based on 5 g moist soil sample. The method was validated by comparing it with conventional liquid-liquid extraction.
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  • 35
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Activity coefficients ; 18-Crown-6-ether and tetraethyleneglycol dimethyl ether ; Thermodynamic properties
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    Topics: Chemistry and Pharmacology
    Notes: Summary The thermodynamic properties of different solutes at infinite dilution have been determined at 323.15 K. Deviations from ideality are discussed in terms of different contributions. The activity coefficients are compared with the calculated values by the one group contribution method.
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  • 36
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fatty acid methyl esters ; Diesel fuel substitute ; Glycerol
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    Topics: Chemistry and Pharmacology
    Notes: Summary A GC method for the determination of free glycerol in vegetable oil methyl esters used as diesel fuel is described. The sample preparation includes dissolving in dimethylformamide, silylation with bistrimethylsilyltrifluoroacetamide (BSTFA) and separation on a methyl silicone capillary column using either FID or MS detection. The recovery was tested using standard samples containing known amounts of glycerol. The results of the analysis of different samples were compared with those obtained by enzymatic determination. The method described offers a far more sensitive and quick determination of free glycerol compared to other methods.
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  • 37
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Electron capture detection ; Trichothecenes ; Cereal grain
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Various analytical methods developed for trichothecene determination, including TLC, HPLC, GC, supercritical fluid chromatography (SFC) and enzyme immuno assay (EIA) are reviewed. In addition a new method is described for the simultaneous determination of the trichothecene mycotoxins deoxynivalenol (DON), nivalenol (NIV), 3-acetyldeoxynivalenol (3-ADON), diacetoxyscirpenol (DAS), T-2 toxin (T-2), HT-2 toxin (HT-2) and T-2 triol (TRIOL), in Austrian wheat and corn samples by GC-ECD. A clean-up procedure has been developed using a combination of liquid-liquid and liquid-solid extraction. Trichothecenes were detected as their heptafluorobuturyl esters or alternatively as trimethylsilyl ethers (only sensitive for deoxynivalenol and nivalenol) using nandrolone or chloramphenicol as internal standard. Four derivatization techniques using HFBI, HFBA+DMAP on polystyrene, TMSI and TMSI+BSA+TMCS have been studied and the advantages and disadvantages of each are discussed. Quantification of trichothecenes from 10 to 1000 ppb in cereals could be accomplished routinely.
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  • 38
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    Chromatographia 37 (1993), S. 215-217 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Unified retention indices ; Dimethylsiloxane stationary phases
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    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic, unified retention-indices of 56 alkylbenzenes up to C15 on dimethylsiloxane OV-101 and SE-30 stationary 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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  • 39
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    Chromatographia 37 (1993), S. 259-263 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Quantitative analysis ; Ethylene oligomer by-products ; n-Alkanes, n-alkenes and 2-alkyl-1-alkenes
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    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method using temperature-programmed poly-dimethylsiloxane OV-101 and poly(pheny ether) (5 rings) capillary columns was developed to separate and quantify the reaction by-products in ethylene oligomers. It was found that the content of 2-alkyl-1-alkenes, 2-alkenes and n-alkanes in the C8−C18 α-olefin fractions amounts to 29, 10 and 2.6% respectively.
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  • 40
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    Chromatographia 37 (1993), S. 211-214 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Organic solvents ; Routine analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method for the analysis of organic solvents in chemical products is described. The analysis is performed by the use of a polar column, Supelcowax 10, and a non-polar column CP-Sil-5CB. Samples containing a non-volatile matrix or water were analysed by headspace analysis. The identification of the solvents in a sample, based on GC retention times on one column, is confirmed by GC of the sample on the second column. The method has been found to be suitable for the routine analysis of solvent mixtures.
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  • 41
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    Chromatographia 37 (1993), S. 264-270 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Temperature programmed ; Peak widths ; Polynomial interpolation
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    Topics: Chemistry and Pharmacology
    Notes: Summary Isothermal chromatographic measurements lead directly to ΔH v o and A (entropy term) of solutes, and three constants of an empirical relationship between peak width and column temperature. From the thermodynamic parameters ΔH v o and A retention temperatures have been computed by means of a theoretical model including temperature dependence of carrier gas viscosity, and subsequently retention times; programmed retention indices have been determined by linear and polynomial interpolations. By substituting the value of the calculated retention temperature in the above-mentioned relationship, peak width at half-height for a linear temperature may be estimated. Predicted retentions correlate with observed data, with a P-value ≤0.01; simulation accuracy is generally 6–10% for peak widths. Retention indices of some organochlorine species, separated on an OV-101 capillary column, may differ by as much as 26 units depending on the method of calculation. Polynomial-calculated indices are more consistent with the retention index scheme, and have smaller standard deviations and better constancy at different heating rates.
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  • 42
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Inverse gas chromatography ; Poly(ethylene glycol) 20M ; Retention mechanisms
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    Topics: Chemistry and Pharmacology
    Notes: Summary The properties of poly(ethylene glycol) 20M (PEG 20M) coated on the hydroxylated surface of Chromaton N AW were investigated by inverse gas chromatography. It was found that the solid form of PEG 20M exhibits partition as the retention mechanism even below its melting range. The contribution of adsorption to the specific retention volume was also determined. It was demonstrated that inverse gas chromatography establishes the existence of a polymer surface layer but precise determination of its thickness is difficult. The limitation of the applicability of inverse gas chromatography results from the structure of the investigated surface layer which is thin and not coherent so that solute molecules can penetrate it.
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  • 43
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    Chromatographia 33 (1992), S. 103-112 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography ; Chiral separations ; Allethrin ; Cypermethrin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Liquid and gas chromatographic separations of the pyrethroid insecticides allethrin and cypermethrin have been investigated with various achiral and chiral stationary phases. Diastercomeric and enantiomeric selectivity was observed for cypermethrin on a Pirkle-type chiral LC stationary phase, but very strong interactions and therefore long retention times prevented the separation of allethrin on this phase. Trans-allethrin isomers were separated on a chiral β-cyclodextrin RP-HPLC column while cypermethrin showed some difficulties on this phase due to isomerization. Diastereomeric but no enantiomeric selectivity by GC was achieved for cypermethrin with an apolar DB 5 capillary. GC separation of the diastereomers was used to study the selective photodegradation of cypermethrin isomers after forestry applications. Chiral β-cyclodextrin-based GC phases showed some enantioselectivity for cis- and trans-allethrin isomers. A separation of the eight isomers into six partially resolved peaks was achieved by GC with a coupled column consisting of chiral permethylated β-cyclodextrin and DB 1701 as stationary phases. This combination was used to characterize allethrin formulations intended for indoor use and to investigate allethrin products formed by ozonolysis of thin films of the insecticide.
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  • 44
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    Chromatographia 38 (1994), S. 22-28 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Chiral separation ; Capillary column ; 2,6-Di-O-pentyl-3-O-propionyl-γ-cyclodextrin
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    Topics: Chemistry and Pharmacology
    Notes: Summary 2,6-Di-O-pentyl-3-O-propionyl-γ-cyclodextrin has been synthesized and used for enantiomer separation in capillary gas chromatography. Experimental results showed that the stationary phase has good enantiomer selectivity toward amino acids, amines, alcohols, diols, epoxides, and lactones,etc. 2,6-Di-O-pentyl-3-O-propionyl-γ-cyclodextrin has good thermal stability: the highest recommended temperature isca 170°C.
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  • 45
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Pentachlorophenol residues ; Off-flavours ; Wines and corks ; Electrolytic conductivity detector/mass spectrometry ; detectors
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    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic methodology with selective detection is presented for the analysis in wines and corks of pentachlorophenol residues, which are suspected to be the most likely precursors of some off-flavours described in several wine samples. After derivatisation, pentachlorophenol acetate residues were monitored by electrolytic conductivity detection and/or mass spectrometric detection in the selective ion mode at m/z 264 and 266. Recoveries varied from 80 to 96% for wine samples fortified with 5 to 100 μg l−1 and from 83 to 91% for corks (fortified at 25 to 100 μg kg−1). The proposed methodology allowed for a determination limit of μg l−1 for wine and 10 μg kg−1 for corks.
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  • 46
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    Chromatographia 38 (1994), S. 475-478 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Phenolic acids ; Olive and elm tree tissues ; Soil phenolics
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method for the separation of phenolic acids along with shikimic and quinic acids by means of capillary gas chromatography is described and discussed. The method involves the previous derivatization of the acids to trimethylsilyl derivatives and it has been applied to the separation of acids extracted from olive leaves and roots, elm leaves and a soil A horizon. Quite good results were achieved both from qualitative and quantitative points of view. Qualitative differences have been pointed out in the phenolic acid composition of two olive cultivars and between leaves and roots of the same cultivar; also two elm species can be discriminated on the basis of the phenolic acid content.
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  • 47
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Porous polymer stationary phase ; Selectivity studies
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    Topics: Chemistry and Pharmacology
    Notes: Summary The behaviour of GC columns packed with the copolymer of methacrylic ester of p,p'-dihydroxydiphenylpropane diglicydyl ether and divinylbenzene was studied. Selectivity studies were made for three polymer samples of different molar ratio of monomers. To determine the selectivities of these copolymers retention indices for seven test compounds in comparison to those obtained on Porapak Q are calculated. Additionally, the efficiency of porous polymer purification was studied by a SFE-GC-MS technique.
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  • 48
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    Chromatographia 38 (1994), S. 595-598 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Chiral / enantiomeric separation ; Amphetamine ; Methamphetamine ; Cyclodextrin-derivatized phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Enantiomeric separation of amphetamine and methamphetamine as achiral derivatives on 2,6-di-O-pentyl-3-O-trifluoroacetyl-β-cyclodextrin, 2,6-di-O-pentyl-3-O-trifluoroacetyl-γ-cyclodextrin and 2,6-di-O-pentyl-3-O-propionyl-γ-cyclodextrin stationary phase in capillary gas chromatography is described. Trifluoroacetic anhydride and acetic anhydride were used as derivatizing reagents. Excellent precision was obtained for concentrations down to 0.1% / e.e. On 2,6-di-O-pentyl-3-O-propionyl-γ-cyclodextrin the elution order of R,S-amphetamine was reversed when the derivatizing reagent was changed but could not be reversed on any of the other phase types.
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  • 49
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Nitrogen phosphorus detection ; Atrazine and simazine ; Freeze-dried water analysis ; ELISA
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    Topics: Chemistry and Pharmacology
    Notes: Summary The determination of atrazine in freeze-dried water samples containing simazine, 0.6% glycine as stabilizer and other pesticides has been compared using three different techniques: (i) direct rapid-magnetic particlebased ELISA, (ii) dichloromethane liquid-liquid extraction (LLE) and Florisil column clean-up prior to ELISA determination and (iii) LLE, Florisil column clean-up and gas chroamtography with nitrogen phosphorus detection (GC-NPD). The methodology developed in this paper has shown the advantages of the introduction of a clean-up step prior to ELISA determination and its correlation with GC-NPD determinations. Atrazine could be determined at levels between 0.1 to 5 μg l−1 in water smaples using the different methods described in this paper. The crossreactivity problems found in the ELISA test associated with the presence of simazine are also discussed.
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  • 50
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    Chromatographia 39 (1994), S. 71-73 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Spectinomycin ; Silylation
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    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic assay for spectinomycin hydrochloride is described. The method is based on that prescribed by the United States Pharmacopeia (USP XXII). The method involves silylation of spectinomycin hydrochloride; phenazone is used as an internal standard. Spectinomycin and phenazone have adequate stability under the prescribed conditions. The stationary phase is 3% OV-17 on Gaschrom Q 100–120 mesh. The selectivity of the proposed method is better than that of the GLC method described in the USP XXII.
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  • 51
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Free fatty acids ; Cheese ; Programmed temperature vaporizer
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    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method with a capillary column and a programmed temperature vaporizer injector has been used to analyze the individual free fatty acids in cheese. The lipids were extracted from an acidified cheese slurry with diethyl ether and treated with tetramethylamonium hydroxide (TMAH) to convert the free fatty acids to tetramethylammonium soaps (TMA-soaps), which were subsequently pyrolyzed to methyl esters in the injector. Carrying out injection at the initial column temperature resulted in lower dispersion of the results, but the solvent front prevented quantitative determination of butyric and caproic acids, and an injector temperature of 300°C was therefore employed. Under the conditions tested, trimethylamine (tma) flash-off did not affect the determinations. The accuracy of the method improved at higher free fatty acid contents (coefficient of variation of 0.53% for a total free fatty acid content of 9000 mg/kg as opposed to 7.0% for a total free fatty acid content of 1400 mg/kg). The recovery rate for individual free fatty acids ranged between 91 and 103%.
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  • 52
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Enantiomer separation ; Permethylated cyclodextrin stationary phases ; Side-chain fluorinated alkylbenzenes ; Thermodynamic data
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    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of racemic side-chain fluorinated alkylbenzenes and bromofluorinated analogues by capillary gas chromatography using permethylated α, β and γ-cyclodextrins dissolved in polysiloxanes of different polarity as stationary phases is described. The influence of the achiral polysiloxane matrices on the separation of enantiomers is discussed in the light of the results obtained with the different phases. For a part of the tested compounds thermodynamic data are determined which describe the interaction of enantiomers with the stationary phase. The mechanism of separation is discussed on this basis and by comparison with data for structurally similar compounds.
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  • 53
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Method validation ; Reggedness test ; Residual solvents
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    Topics: Chemistry and Pharmacology
    Notes: Summary Ruggedness testing is performed on a gas chromatographic method for the quantitative determination of residual solvents in steroids. Eight experimental variables or factors which were expected to influence the quantitative results were selected. These factors were divided into two independent groups, i.e. four factors related to the injection process and four factors related to separation and detection. In order to determine interaction between factors and quadratic effects, a central composite design was selected for the set-up of the experiments. Because in the method an internal standard is used, relative peak area was used as response. A deviation of up to 2.5% per factor for the quantitative results was regarded as acceptable. Other responses studied are related to the system suitability. Observed main, quadratic and interaction effects were translated into rugged intervals of the experimental variables by graphical presentation. It was found that besides main effects significant interaction effects were present, for example between the temperature of the injector and the split-flow. Interaction effects can easily result in the reduction of the rugged intervals by a factor of 2. The calculated rugged intervals were compared with the precision of the instrument or factor settings in order to estimate the ruggedness of the factors. Eventually, the maximum effect of the variation in the instrument settings on the quantitative results regarding the precision of the factor settings was found to be only 2.2%. Overall, the method proved to be rugged for most factors, except for the split-flow of the injector for which the method was only rugged to a limited extent.
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  • 54
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention/structure and retention/temperature ; relationships ; Experimental design ; Enthalpy-entropy compensation ; para-Hydroxy benzoic esters
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    Topics: Chemistry and Pharmacology
    Notes: Summary An experimental design has been used to study the effect of column temperature on the gas chromatographic retention of eightpara-hydroxy benzoic esters. A rapid procedure has been developed to reduce the number of experiments compared with traditional methods. Capacity factors were determined and the enthalpy and entropy of transfer from the mobile phase to the stationary phase, ΔHo and ΔSo, respectively, were calculated using the linear Van't Hoff equation (dependence of ln k′ on 1/T). A retention prediction system (RPS) for these compounds in GC was investigated. The molecular connectivity index was used to describe the quantitative structure relationships. Enthalpy — entropy compensation revealed that the mechanism was similar for all the compounds studied.
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  • 55
    ISSN: 1612-1112
    Keywords: Gas chromatography ; coupling capillary columns ; Selectivity optimization ; Dual oven tuning
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    Topics: Chemistry and Pharmacology
    Notes: Summary A computer-assisted procedure is presented for optimization of selectivity of tandem capillary columns with the same apolar (SE-54) stationary phase by varying column temperatures. The procedure is based on a threshold criterion calculated from the required resolution factor in which the separating power of the columns as a function of temperature is incorporated. The validity of the procedure has been verified by the analysis of a sample containing 33 hydrocarbons on two 31 m×0.3 mm i.d. SE-54 capillary columns coupled in series and by varying the temperatures of both columns in the range 60–100°C. At the optimum temperatures (70°C for the first and 92°C for the second column) 26 compounds were resolved equal to or better than Rji=1.00 in 22.8 min.
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  • 56
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carbon adsorbents ; Methyliodide ; Effect of KI on adsorption ; Thermodynamics of adsorption
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    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatography has been used to measure the adsorption at zero surface coverage of methyl iodide on different types of carbon. The effect on the adsorption of methyl iodide of adding potassium iodide to the carbon samples was also studied. The differences observed in the behaviour of these samples for the adsorption of methyl iodide are explained on the basis of the textural characteristics of the samples. Thermodynamic functions of adsorption of methyl iodide at zero surface coverage are obtained.
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  • 57
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Partition coefficients ; Olive oil-nitrogen partition ; QSAR
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    Topics: Chemistry and Pharmacology
    Notes: Summary A gas-liquid chromatographic method has been used for direct determination of the partition coefficients (KD) of alcohols, ethers and ketones between olive oil and nitrogen. Olive oil was characterised as a stationary phase for gas chromatography. The differential molar enthalpies of solution were also calculated from retention data. Correlations between log KD for olive oil — nitrogen and molecular connectivity indices, differential molar enthalpies of solution, biological activity and partition coefficients for blood-air were obtained.
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  • 58
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    Chromatographia 34 (1992), S. 621-626 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Methyl and ethyl chloroformate ; Derivatization in the presence of water ; Alkyl and alkoxycarbonyl esters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Phenolic acids, i.e. benzoic, phenylacetic, phenylpropenoic (cinnamic), phenylglycolic (mandelic), phenylpropionic and their variously substituted forms can be converted almost instantly to derivatives amenable to GC by treatment with methyl or ethyl chloroformate. The reaction, catalyzed by pyridine, proceeds even in the presence of water. The carboxylic group is esterified to the corresponding alkyl ester but even the alkoxycarbonyl ester (mixed anhydride) can be produced by altering the reaction conditions. Hydroxyl groups on the benzene ring or adjacent to the carboxylic group are converted to the alkoxycarbonyl ethers. Benzoic acid and some of its substitutents, unlike the other aromatic acids, shows a tendency to mixed anhydride formation even under conditions used for alkyl esters. A well deactivated capillary column with a thin film of stationary phase of low polarity enables even the mixed anhydrides to be analyzed successfully.
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  • 59
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    Chromatographia 34 (1992), S. 163-165 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Cyclodextrins ; Crown ethers ; Dimethylnaphthalene isomer
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    Topics: Chemistry and Pharmacology
    Notes: Summary The twelve structural C2 isomers of naphthalene are resolved on a single capillary column using α, β, or γ cyclodextrin as the stationary phase. A change in elution order is seen upon going from α to β and then γ cyclodextrin which can be related to the size of the cyclodextrin cavity and the stereochemical fit of the isomer. A crown-ether column and a liquid-crystal column were found to be unable to separate all of the isomers.
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  • 60
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace sampling ; Partition coefficients ; Multiple headspace extraction
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    Topics: Chemistry and Pharmacology
    Notes: Summary Equilibrium headspace gas chromatography has been applied to the determination of the partition coefficients of volatile compounds in water-air systems. Only techniques that are suited to a fully automatic headspace procedure using the pneumatic headspace sampling-technique have been considered. Particularly simple is the technique of “vapor phase calibration —VPC” where an external vapor standard is used to calibrate the concentration of the volatile analyte in the headspace, while the concentration in the sample is found from the difference in the total amount in the vial. This technique is described in detail for 2-butanone in water. Finally, the water-air partition coefficients of several selected volatile compounds at different temperatures are listed together with their temperature functions.
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  • 61
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    Chromatographia 34 (1992), S. 241-248 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Natural insecticides ; Marigolds ; Isolation of volatiles
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The results of optimizing Soxhlet and Simultaneous Distillation-Extraction (SSDE) procedures for the isolation of natural insecticides fromTagetes erecta, Tagetes patula, andTagetes minuta, members of theCompositae family, are presented. Extraction procedures were developed and validated that produced the extract with the highest degree of biocidal activity. The highest activity was obtained with extracts isolated by SSDE using methylene chloride. Initial work was carried out on a micro-SSDE. Preparative SSDE was used to provide large quantities of extracts for bioassays. Bioassays were used to govern optimization procedures usingAedes aegypti andAnopheles stephensi adults and larvae as target organisms.Tagetes minuta was determined to be the most active of the three species studied. Evaluation of activity and recovery versus extraction time was investigated. It was determined that an extraction time of ten hours resulted in the highest activity and over 90% recovery of the oils. Finally, supercritical fluid extraction of the flowers with CO2 was compared to SSDE.
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  • 62
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Sociation constants ; Hydrogen bonding solutes ; Nearly ideal binary solvent theory ; Isosteric solvents
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    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic data measured on mixtures of 19,24-dioctadecyldotetracontane, A≡C78, and 18,23-dioctadecyl-1-hentetracontanol, POH, allow the determination of the standard chemical potential of a solute on an ideal stationary phase with primary alcohol groups at ideal dilution. The Nearly Ideal Binary Solvent Theory provides the link between these data and the sociation constant of the solute with the primary alcohol. The method was applied to calculate sociation constants of a series of hydrogen bonding solutes. Results are compared with those determined by spectroscopy and calorimetry.
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    Chromatographia 34 (1992), S. 398-410 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Reversed-flow technique ; Catalysis ; Hydrodenitrogenation
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    Topics: Chemistry and Pharmacology
    Notes: Summary Many important parameters of surface catalysed reactions can be determined simultaneously, under nonsteady state conditions using Reversed-Flow Gas Chromatography. A simple, slightly modified gas chromatograph is required. The distorted diffusion bands, obtained experimentally for reactant and product(s), can be analysed mathematically, using simple PC programs, to give the pre-exponential factors and the exponential coefficients of a function consisting of the sum of two-four exponential functions of time. From these, and some geometrical and diffusional characteristics of the reaction cell, the values of adsorption, desorption and reaction rate constants, the overall mass transfer coefficients in the gas and in the solid catalyst, and the adsorption equilibrium constant, for both reactant and product(s) can be calculated. The above parameters were determined at various temperatures and over three catalysts for the hydrodenitrogenation of piperidine ton-pentane, an industrially important hydrotreating process. The results obtained can help to understand the mechanism of reactions on solid surfaces and to confirm experimentally theoretical calculations on adsorption and surface reactions.
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  • 64
    ISSN: 1612-1112
    Keywords: Gas chromatography ; High-pressure Soxhlet extraction ; Organochlorine residue analysis ; Supercritical fluid extraction
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    Topics: Chemistry and Pharmacology
    Notes: Summary The operational conditions of a high-pressure Soxhlet extractor (pressure, temperature, time and amount of sample) have been optimized, using carbon dioxide as extractant for the determination of organochlorine pesticides and polychlorinated biphenyls (PCBs) in certified potato, carrot, olive oil and lyophilized fish tissue samples. Good recoveries were obtained.
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  • 65
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    Chromatographia 34 (1992), S. 475-478 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Telomeric fluoroalkanols ; Retention index ; Regression equation
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    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of fluoroalkanols with the general formula H(CF2CF2)nCH2OH (n=1–8) on fused-silica capillary columns coated with dimethylsilicone and cyanopropylmethylsilicone stationary phases was investigated. Retention indices were determined at three temperatures. A correlation between the retention index values, the molecular weights and the number of C and F atoms in the solute molecules was found.
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  • 66
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    Chromatographia 34 (1992), S. 461-467 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Allyl thiocyanate and isothiocyanate ; Plant extract ; Analytical artifacts ; Isomerization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Allyl thiocyanate and isothiocyanate were synthesized and could be analysed by gas chromatography without isomerization by keeping the injector at, or below, 50°C. Synthetic allyl isothiocyanate contained none of the isomeric thiocyanate but allyl thiocyanate contained 0.5% of isothiocyanate. The NMR spectra indicated both compounds to be free of the corresponding isomer. Analysis of extracts of stinkweed, mustard and horseradish by GC using non-isomerizing conditions showed that only the stinkweed extract contained allyl thiocyanate. Mustard and horseradish extracts contained allyl, and other, isothiocyanates but no allyl thiocyanate. Allyl thiocyanate previously reported in extracts of mustard and horseradish was most likely an artifact caused by partial isomerization of allyl isothiocyanate under the conditions of isolation and/or analysis.
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  • 67
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    Chromatographia 34 (1992), S. 513-528 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open-tubular (capillary) columns ; History of chromatography
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  • 68
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    Chromatographia 35 (1993), S. 33-37 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Crown ether polysiloxane phases ; Selectivity mechanisms
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    Topics: Chemistry and Pharmacology
    Notes: Summary The phase recognition mechanism of nine groups of position isomers on four crown ether polysiloxanes, OV-1701 and PEG 20M has been investigsated by measuring various thermodynamic parameters. The high selectivity of crown ether polysiloxane phases is due to hydrogen bonding and the extent of fitting between the analytes and the crown ethe cavity. The effects on selectivity of cavity size, heteroatoms and substituent groups on the crown ether are discussed.
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  • 69
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Equilibrium headspace sampling ; Partition coefficient determination ; Theory of chromatography
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    Topics: Chemistry and Pharmacology
    Notes: Summary The new phase ratio variation method is described which represents a convenient way for the determination of gas-liquid partition coefficients for practical purposes, utilizing equilibrium headspace-gas chromatography (EHS-GC). This method is based on the relationship between reciprocal peak area and the phase ratio in the vial containing the sample solution; it involves regression analysis of the EHS-GC measurements of a number of sample vials containing the same sample solution but with a wide variation of phase ratios. Examples are given for both aqueous systems and systems consisting of a stationary (liquid) phase used as the solvent; comparison of the measured values with results obtained by other methods shows satisfactory agreement. A critical discussion of the conditions influencing the accuracy of the analytical results is given.
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  • 70
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    Chromatographia 35 (1993), S. 109-110 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Unified retention index ; Correlation of data ; Hydrocarbons
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    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic unified retention indices for 43 hydrocarbons (alkanes and cycloalkanes) are given for squalane and OV-101. Comparison of these values and unified retention index increments are presented as linear regression equations with high correlation coefficients and acceptable standard deviations.
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  • 71
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    Chromatographia 35 (1993), S. 160-166 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Neural networks ; Classification ; Pattern recognition
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    Topics: Chemistry and Pharmacology
    Notes: Summary Artificial Neural Networks are proposed for the classification of vegetable oils submitted to gas chromatography analysis through their FAME profiles. Three important neural networks are evaluated here: the Hopfield model as a content-addressable memory (CAM), the Hamming model and the multi-layer perceptron. A brief description of these nets is first presented and further implemented for the classification of known vegetable oils. After the learning step, unknown samples are presented to the nets and the identification step performed. The performances of these nets are compared for the recognition of popular vegetable oils, including several edible oils.
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  • 72
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Mass spectrometry ; Atomic emission spectroscopy ; Pulp mill effluents
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    Topics: Chemistry and Pharmacology
    Notes: Summary Three chlorinated dimethyl sulfones and five chlorinated thiophenes have been identified in the alkaline extraction liquor from a bleach plant by gas chromatography with atomic emission detection (GC-AED) and with mass spectrometry (GC-MS). The information on elemental content obtained by GC-AED enabled a rapid screening of the sulfur compounds and provided important structural information complementary to the mass spectral data. Quantitation was accomplished by GC-AED based on universal calibration.
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  • 73
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    Chromatographia 35 (1993), S. 209-215 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas chromatography-mass spectrometry ; Tagetes ; Plant volatiles ; Extractions ; Natural insecticides ; Mosquitos
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    Topics: Chemistry and Pharmacology
    Notes: Summary Volatiles from three species of the genustagetes, commonly called marigold have been isolated and characterized. Simultaneous steam distillation extractions (SSDE) produced consistently extracts of higher insecticidal activity than Soxhlet extractions. Methylene chloride was the best solvent. Volatiles isolated from theminutae species showed higher activity than those frompatula anderecta. Comparison of extracts from the flower, foliage and roots of the plant showed that most of the activity is located in the flower. The volatiles are highly effective toward both larvae and adult mosquitoes.
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  • 74
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    Chromatographia 35 (1993), S. 237-240 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Enantioselectivity ; Polysaccharide chiral stationary phase ; Amylose tris(n-butylcarbamate) ; Grob test
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    Topics: Chemistry and Pharmacology
    Notes: Summary Seven aromatic and alkyl amylose and cellulose carbamates have been tested as chiral stationary phases in gas chromatography. One of them, amylose tris(n-butylcarbamate) can be used for enantiomer separation.
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  • 75
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    Chromatographia 35 (1993), S. 290-294 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Solid phase extraction ; Organochloride pesticides ; Water analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatography of chlorinated pesticides in water is carried out after adsorption of a 50 mL sample using a cartridge containing 100 mg CN-bonded porous silica and extraction with 500 μL pentane. The average recovery for eight organochloride pesticides at 1 ppb was 〉95%. The procedure described is simple, selective and reproducible.
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  • 76
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    Chromatographia 35 (1993), S. 339-343 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Preconcentration techniques ; Trace gas analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary The blanks in preconcentration methods for determining trace amounts of impurities in ultra-pure gases, which include the preconcentration volume of sample gases, carrier gas impurities and atmospheric contamination are discussed and three concentration methods for eliminating blank errors are proposed. These are, the differential volume method by concentrating at the same flow-rate but different times (DVMSF), the differential time method by concentrating the same volumes at different flow-rates (DTMSV) and the differential volume method by concentrating for the same times but different flow-rates (DVMST). DVMST is proposed as the best method for its ability to eliminate all blank errors described. The methods are used to determine trace amounts of Ar+O2 and N2 in ultra-pure hydrogen. Calculations demonstrate that the methods can effectively improve analytical accuracy.
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  • 77
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Micropacked columns ; Retention behavior ; LC silica packing materials ; Silanol groups
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    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic retention of cyclohexane and benzene on microcolumns packed with silica-based materials for liquid chromatography has been investigated to elucidate the relationship with the surface properties of the packing materials. Differences in capacity factors (Δk′) for these two hydrocarbons were related to the surface area of the packing materials. For untreated silica gels, the Δk′ value increased with increasing total surface area of the column employed and measurement of Δk′ for chemically-bonded stationary phases allowed estimation of accessible residual silanol groups.
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  • 78
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Pesticides in groundwater ; Solvent extraction ; Multiresidue analysis ; Selective detection
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    Topics: Chemistry and Pharmacology
    Notes: Summary A simple multi-residue procedure has been developed and applied to the analysis of pesticides in groundwater samples from the Comunidad Valenciana, a predominantly agricultural area on the Mediterranean coast of Spain. The procedure includes a liquid-liquid extraction, after addition of NaCl on the samples, and a subsequent analysis by capillary gas chromatography using a dual detection system with electron capture and nitrogen-phosphorous detectors. This allows the determination of more than 30 compounds (organophosphorous, organochlorine and pyrethroid pesticides) at the low ppb (μg l−1) levels. Detection limits obtained varied between 0.01 μg l−1 (lindane, fonofos) and 0.5 μg l−1 (cypermethrin). An additional injection of the sample extracts into a gas chromatograph equipped with a column of different polarity and electron capture detector is used for the confirmation of chromatographic peaks. The recommended procedure has been applied to 66 ground water samples. Pesticides, including organophosphorus and organochlorine compounds were detected in 31 of them, in levels ranging from 0.02 to 0.7 μg l−1.
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  • 79
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace sampling ; PTV-System ; Ethephon in drinking water
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    Topics: Chemistry and Pharmacology
    Notes: Summary An indirect GC method is described for the determination of Ethephon in drinking water on the basis of the headspace analysis of the ethylene formed from Ethephon. In order to reach the necessary detection limit, the entire volume of the static headspace distribution is transferred into a cold injection system (CIS). There, the ethylene is adsorbed on Carbosieve SIII at 10°C and, subsequently, desorbed at 300 °C. The water vapour included in the headspace is completely eliminated through the splitting system. By means of this technique, a detection limit of 0.05 μg/l water was reached.
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  • 80
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    Chromatographia 37 (1993), S. 399-401 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Viscosity ; Carrier gases
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    Topics: Chemistry and Pharmacology
    Notes: Summary Equations are derived for viscosities of H2, He, N2 and Ar for use at chromatographic temperatures which are accurate to within 0.3% for H2, and 0.1% for the other gases. The effect of pressure is usually negligible but may increase the viscosity of N2 or Ar by as much as 0.5% at 25°C or lower and 5 atm or higher.
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  • 81
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Priority pollutants ; EPA methods ; Unleaded gasoline ; Volatile organochlorine compounds
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    Topics: Chemistry and Pharmacology
    Notes: Summary The complete separation of the sixty volatile organochlorine (VOC) priority pollutants has been achieved by coupling two different liquid-modified adsorption chromatography columns. Two temperature programs were used to obtain the complete separation in a relatively short analysis time. Detection was by FID alone
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  • 82
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    Chromatographia 38 (1994), S. 93-97 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index ; Adsorption effects ; Terpene alcohols ; Fused-silica capillary columns
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    Topics: Chemistry and Pharmacology
    Notes: Summary Retention indices of 6 selected hydroxy compounds (aliphatic and bicyclic alcohols, phenols) were determined on 2 HP-5 fused-silica, capillary columns with different film thicknesses (0.11 μm and 0.33 μm) at 8 different oven temperatures between 80 and 150°C. For some substances the I-T plot was found to show a minimum which cannot be explained by the common retention-index temperature-dependence in gas-liquid chromatography. This result is discussed in terms of adsorption at the liquid-solid interface of the capillary column.
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  • 83
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary Phase and solute polarity ; Molecular structural coefficients ; Retention index ; Takács equation
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    Topics: Chemistry and Pharmacology
    Notes: Summary Molecular structural coefficients, Sc, for one hundred solutes have been calculated by means of the Takács equation using retention data obtained with over fifty stationary phases, SP. Employing data of seven SP's (characterized in our laboratories) it was found that the variation of Sc with column temperature was linear for most solutes. With data of n-decane and the ten McReynolds probes on up to fifty SP's of polarity less than RP=72, at 120°C, it was found that the Sc of n-decane and cis-hydrindane decreased slightly with increasing SP polarity, while the Sc of non-alkanes remained constant or increased very little as the SP polarity increased. The points for n-decane fit well to a second order polynomial. Again using a temperature of 120°C, the increments of Sc for solutes belonging to an homologous series were correlated with the polarity of SP's. Reasonably straight lines were obtained for all the chemical functions studied, Sc increasing with increasing SP polarity.
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  • 84
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary phase characterization ; Principal component analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary In this study, several new stationary phases were characterized by principal component analysis. Fourteen new stationary phases, including substituted phenyl and oligoethyleneoxide functionalities on polysiloxane polymers, were tested and compared to three well known stationary phases. The main features of these phases were studied using a series of test solutes of varying chemical characteristics representing the data set for principal component analysis. Two principal compounds were found to account for 99.20% of the variance (the first accounted for 94.96% and the second for 4.24%). The data were represented as a two-dimensional map for visual representation of the characteristics of these stationary phases. The first principal component represented a selectivity based on polarity (r2=0.998), while the second showed Lewis acid-base characteristics of the phases. Polarizable and amphoteric characteristics of these phases also became evident using this evaluation method.
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  • 85
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid-liquid extraction ; Supercritical fluid extraction ; Pesticides ; Freeze-dried water
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    Topics: Chemistry and Pharmacology
    Notes: Summary The stability of freeze-dried water samples spiked with eight agrochemicals (atrazine, simazine, linuron, carbaryl, propanil, fenitrothion, parathion and fenamiphos) were examined to evaluate their suitability as candidate reference materials for their determination in water samples. In addition, two different extraction procedures, liquid-liquid and supercritical fluid extraction, were compared for the isolation and trace enrichment of target analytes from freeze-dried water samples. Final analytical determinations were by gas chromatography-nitrogen phosphorus detection and electronic impact mass spectrometry, and by liquid chromatography-diode array detection. The whole methodology developed in this paper permitted the determination of pesticides spiked in water at levels varying from 0.03 to 6.9 μg L−1.
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  • 86
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    Chromatographia 38 (1994), S. 624-628 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Ion-trap detection ; Nitriles ; Cerelas ; Perfluoroacylation
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    Topics: Chemistry and Pharmacology
    Notes: Summary Bromoxynil and ioxynil have been determined inplants and soil by gas chromatography. These herbicides are extracted from soil samples with methylene chloride at acidic pH. Plant samples are extracted with a basic acqueous solution and extracts purified by solvent partitioning. Herbicide residues are submitted to perfluoroacylation prior to GC separation. These compoiunds are determined by ion-trap detection with single ion monitoring; N-(3-chloro-4 methyl-phenyl_ perfluoropropyl amide is used as internal standard. The detection limit of the method is near 0.001 μg g−1 for the samples studied. The proposed methods are sensitive and reproducible enough to allow determination of these herbicides at residue levels in plants and soil.
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    Chromatographia 39 (1994), S. 11-14 
    ISSN: 1612-1112
    Keywords: Supercritical fluid extraction (SFE) ; Gas chromatography ; Pesticide residues ; Oxadixyl
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    Topics: Chemistry and Pharmacology
    Notes: Summary This work describes the study of a degradation curve of Oxadixyl in field-treated potato and tomato samples. The residues were extracted using classical and supercritical fluid (SFE) extraction methods and analyzed by HRGC/ECD. The extraction techniques were compared and the results indicate the advantages of using SFE as an alternative method for pesticide analyses in these samples.
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  • 88
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    Chromatographia 39 (1994), S. 706-712 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Short chain fatty acids ; Intestinal fluids
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    Topics: Chemistry and Pharmacology
    Notes: Summary The quantification of short chain fatty acids in their free form, by gas chromatography, is the method of choice provided that the underivatized acids elute with good peak shape and reproducibility. In biological samples not only the highly polar acids themselves but also deposits of nonvolatile sample components may interact with the column or the packing material. As a result, the peak symmetry of the fatty acids and their reproducibility can become increasingly poor. Reduction of the nonvolatile matrix components by filtration of the sample has been examined in order to achieve direct analysis of the short chain fatty acids in intestinal samples by packed column GC. Membrane filter units (0.8 μm) allow a quick and simple filtration of the samples. This pretreatment reduces the peak tailing and the broadening of the peaks. The method, when applied to different intestinal samples, allowed the quantification of short chain fatty acids in hundreds of samples without derivatization. Good results are obtained at sample concentrations higher than 0.2 mmol l−1 for each acid.
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    Chromatographia 39 (1994), S. 224-227 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; C1−C4 alkyl tert-butyl ethers ; Retention index
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    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of C1−C4 alkyl tert-butyl ethers with the general formula (CH3)3C−O−R (R-alkyl substituent) on fused-silica capillary columns coated with dimethylsilicone and cyanopropylmethylsilicone stationary phases was investigated. Retention indices were determined at two temperatures in order to understand their chromatographic behaviour. The respective standard deviations were 0.3 and 0.5 i.u.
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  • 90
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Organonitrogen pesticides ; Organophosphorus pesticides ; Apples ; Solvent extraction
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    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method employing a capillary column and a selective nitrogen/phosphorus detector (NPD) has been developed for the determination of organophosphorus (OP) and organonitrogen (NP) pesticides in horticultural samples (apples). The separation of sixteen pesticides and the internal standard was performed in thirteen minutes. The analytical characteristics of the method, including linear response ranges, detection limits, and reproducibility, have been studied using a 1∶1 mixture of ethyl acetate and xylene as extraction solvent. The possibility of mutual interference between pesticides has also been studied. A procedure for the quantitative extraction of the sixteen pesticides from apple samples has also been developed; for fifteen of the pesticides recoveries 〉85% were obtained after 90 minutes extraction. The effect of different solvents both on recovery and on the sensitivity of the subsequent chromatography were also investigated. It was found that the sensitivity required must be considered when the solvent for sample treatment is selected.
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    Chromatographia 39 (1994), S. 419-426 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography ; Chirasil-Val ; Amino acid enantiomers ; N-Isobutyryl-cysteine
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    Topics: Chemistry and Pharmacology
    Notes: Summary Free D-amino acids (D-AA) were detected as native constituents in juices of vegetables (cultivars of cabbage, tomato, carrot, garlic) and fruits (organes, clementine, grapefruit, lemon, apples, pear, grapes) using gas chromatography (GC) or high-performance liquid chromatography (LC). For investigation by GC, AA enantiomers were converted into theirN(O)-pentafluoropropionyl 2-propyl esters and resolved on a Chirasil-L-Val capillary column. For determination by LC, precolumn derivatization of AA enantiomers usingo-phthaldialdehyde together with the chiral thiolsN-isobutyryl-L-cysteine orN-isobutyryl-D-cysteine and fluorescence detection of the diastereomeric isoindole derivatives, resolvable on an octadecylsilyl stationary phase, were used. D-Ala (0.6–3.8%) was detected in all freshly pressed plant juices usually in the highest relative amounts. Other D-AA detected were D-Asx (0.1–1.9%), D-Glx (0–1.3%), D-Ser (0–1.7%), D-Arg (0.4–1.2%, in grapes, orange, grapefruit, and clementine) and D-Leu and D-Val (1% in cabbage). Absolute amounts of native D-AA were totally 28–57 μmol L−1 in fruit juices, 14.5 μmol L−1 in a tomato juice and 8.5 μmol L−1 in a carrot juice.
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  • 92
    ISSN: 1573-5133
    Keywords: Polychlorinated biphenyl ; DDT ; Gas chromatography ; Mass spectrometry ; Crossopterygii
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    Topics: Biology
    Notes: Synopsis Gas chromatography coupled with electrolytic conductivity detection and electron capture negative chemical ionization mass spectrometry have been used to identify and quantify organochlorine xenobiotics in tissues from two specimens of the living coelacanth Latimeria chalumnae. Compounds identified include polychlorinated biphenyls (PCB), 4,4′-DDT and its metabolites 4,4′-DDD and 4,4′-DDE. Levels of these compounds in the specimens were observed to be generally related to tissue lipid content. Highest concentrations of the xenobiotics were present in the lipid-rich swim bladder, followed by adipose tissue and liver. Levels ranged from 89 to 510 μg kg−1 for PCB and 210 to 840 μg kg−1 for Σ-DDT (including DDD and DDE) on a wet-weight basis. Organochlorine concentrations in relatively lipid-poor tissues, i.e. muscle and kidney, were lower. Parent DDT contributed significantly to the Σ-DDT burden. PCB congeners containing five to seven chlorines were most prevalent. Component distributions did not match those present in common commercial PCB formulations. However, major congeners observed were similar to those reported for other fishes.
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    Chromatographia 13 (1980), S. 686-692 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Micropacked columns in GC ; Microparticles
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    Topics: Chemistry and Pharmacology
    Notes: Summary Porous silica microparticles designed for modern liquid chromatography have proven effective in gas chromatography. Columns of 35–50 cm gave plate heights as low as 3.3 particle diameters and speeds of 2400 theoretical plates per second or 500 effective theoretical plates per second. Inlet pressures up to 70 atmospheres were required using hydrogen as carrier gas. The particles as received were too retentive for fast chromatography and gave asymmetric peaks. A coating of fluorosilicone oil overcame both problems. Other coatings were less effective. Bonded phases proved less satisfactory on both counts and also gave substantially less efficient columns and greater flow resistance. Column efficiency and flow resistance were sharply dependent on physical properties of the particles. The most efficient packing was clearly spherical particles of 5–10 μm diameter with narrow size distribution, pore diamters about 50 nm, BET surface areas of 25–50 m2/g and surfaces modified with trifluoropropyl silicone. A six-component hydrocarbon sample was separated in 33 s with a resolution of 4 for the most difficult pair and in 2.6 s with a minimal resolution. Performance was limited by end effects and by available pressure so that much better performance can be expected from longer columns and higher pressures.
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    Chromatographia 13 (1980), S. 752-754 
    ISSN: 1612-1112
    Keywords: Xylenol isomers ; Gas chromatography ; Polyols and polyethers as stationary phase ; Hydrogen bonding
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    Topics: Chemistry and Pharmacology
    Notes: Summary Xylenol isomers can be resolved on most polyols (sugars or sugar alcohols) and polyethers (polyethylene glycol or polypropylene glycol) with hydrogen-bonding interaction. They are separated on vinical polyols which have more hydroxy hydrogen than tetrol, and even on vicinal triol when its hydroxy hydrogen is acidic (stronger proton donor). The stronger is the hydrogen bonding interaction between xylenols and the liquid phase, the better is the separation of 2,4- and 2,5-xylenol, and the poorer the separation of 2,4-and 2,3-xylenol.
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    Chromatographia 13 (1980), S. 651-660 
    ISSN: 1612-1112
    Keywords: Capillary columns, glass ; Gas chromatography ; Column preparation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Glass capillary column chromatography is the most rapidly growing part of gas chromatography. There are many complex new analytical tasks and they require special capillary columns. Fortunately there is a wide range of column preparation methods available, and they make the preparation of glass capillary columns a more varied job than that of packed columns. In this paper these methods are reviewed and suggestions are given for making task-oriented columns.
    Type of Medium: Electronic Resource
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  • 96
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    Electronic Resource
    Springer
    Chromatographia 13 (1980), S. 73-84 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas hold-up time ; Dead time
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The two approaches used for the calculation of the gas hold-up time and thus, the adjusted retention time are outlined, first for the restricted case when the carbon numbers of the three homologues used for the calculation are evenly spaced (c3−c2=c2−c1) and then, for the general case when (c3−c2) differs from (c2−c1). The basic difference in the philosophy of the two approaches is shown.
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  • 97
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    Chromatographia 14 (1981), S. 576-578 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Tortuosity factor
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The relationship between the obstructive factor γ and velocity was restudied. The dependence of the obstructive factor on velocity was verified. The effects of diffusion coefficient and particle-to-column diameter ratio on the obstructive factor-velocity relationship were investigated. The results are consistent with Hawkes' hypothesis that values of γ at low velocities are averages over tightly packed and loosely packed domains while at high velocities they are weighted in favour of the loosely packed domains where there is more flow.
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  • 98
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    Chromatographia 14 (1981), S. 648-652 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas-liquid adsorption ; Bulk solution ; Mixed stationary phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary It is shown that the blending of some retention effects can make the resolution of complex mixtures on short classical columns as effective as on capillary columns.
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  • 99
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    Electronic Resource
    Springer
    Chromatographia 14 (1981), S. 699-703 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace analysis ; Aromatic hydrocarbons ; Water analyses
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The possibilities of using headspace analysis of aromatic hydrocarbon traces in aqueous solutions with changing values of the partition coefficients are discussed. A variant of headspace analysis of the simplest aromatic hydrocarbon in natural and waste water is described. It involves two-step gaseous extraction of a sample in vessels of varying volume before and after the equilibrium phase is replaced with a pure gas (air or nitrogen). This method permits to analyse 5–50 ml water samples with benzene and toluene contents varying from the ppb to the ppm range within an error not exceeding 155. The analysis time is about 1.5 h. The presence of non-volatile organic or mineral substances does not influence the determination. This method is unsuitable to heterogeneous systems (aqueous oil emulsions): before carrying out the analysis for the hydrocarbon content these systems have to be homogenized first.
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  • 100
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open tubular (capillary) columns ; Glass columns ; Fused-silica columns ; Column testing
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Column characteristics affecting the chromatographic behavior of glass and siliceous glass (“fused silica”) capillary columns include the dimensional uniformity of the column, the physical and chemical characteristics of the column wall and the characteristics of the liquid phase. In the case of the coated column the uniformity and thickness of the liquid phase film are the most important criteria affecting column reproducibility. The paper discusses these factors and their influence on column performance.
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