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  • Gas chromatography  (280)
  • Springer  (280)
  • Periodicals Archive Online (PAO)
  • 1985-1989  (172)
  • 1980-1984  (108)
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  • 1
    ISSN: 1432-1432
    Keywords: Primordial terrestrial atmospheres ; CH4, C2H2, CO2 ; Prebiotic synthesis ; High-frequency discharge ; Hydrocarbons ; Gas chromatography ; Mass Spectrometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Various hydrocarbons were synthesized by high-frequency discharge in a primordial terrestrial model atmosphere. The products were extracted by benzene or methanol and analyzed by GC-MS. The mean carbon chain length of the hydrocarbons formed by the discharge through pure CH4 gas was less than 6. Benzene was also obtained. Some isomers were obtained for each of the hydrocarbons containing a given number of carbons. When a small amount of C2H2 was added to the CH4, longer chain compounds were formed, as compared with discharge in CH4 only. However, when the amount of C2H2 was increased, unextractable high molecular weight compounds were produced. The amounts of products decreased as the mixing ratio of CO2 to CH4 increased. No hydrocarbons were detected when the ratio of CO2/CH4 exceeded 1.
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  • 2
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    Trees 1 (1987), S. 94-101 
    ISSN: 1432-2285
    Keywords: Monoterpenes ; Abies alba Mill ; Resin ; Seeds ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary Using gas-chromatographic methods, the variability of the contents of monoterpene hydrocarbons (α-pinene, β-pinene, Δ3carene and limonene) in the resin of silver fir seeds (Abies alba Mill.) was studied. Resin cavities were characterized according to their position on the seed surface. It was estabilished that the terpene content of the resin of cavities localized on the abaxialadaxial surfaces of the seed differs significantly, creating a gradient of resin composition around the circumference of the seed. The differences between various resin cavities of single seeds were greater than the differences between different seeds of a single cone and between seeds of various cones on a single tree. An accurate definition of the resin cavity location on the seeds appears to be a fundamental condition for the collection of a sample representing the resin composition of individual trees. Resin biosynthesis in the course of organogenesis and the control of terpene contents in the resin of various locations on the seed and the cone are discussed.
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  • 3
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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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  • 4
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    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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  • 5
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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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  • 6
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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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  • 7
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Crystal hydrates as stationary phases ; Mobile Phases containing water ; Selective retentions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The use of crystallohydrates, crystallohydrate solutions and melts as stationary phases in gas chromatography has been proposed. Crystallohydrates have been shown to display high selectivity in the separation of polar organic compounds when use is made of water vapours as the mobile phase. Some aspects of gas-liquid chromatography in water vapours and with the stationary phase comprising crystallohydrates have been studied, and the preliminary results obtained point to the desirability of further progress in this field.
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  • 8
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open-tubular (capillary) columns ; Immobilized liquid phases ; Thick-film columns ; GC-FTIR
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The performance of a column prepared with an immobilized (chemically bonded) methylsilicone phase having a film thickness of 5μm is investigated in detail. Due to their high sample capacity, such columns are particularly useful when directly coupling gas chromatography with spectroscopic techniques such as Fourier-transform infrared spectroscopy. Thick-film columns can even be used with thermal conductivity detectors.
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  • 9
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    Chromatographia 17 (1983), S. 241-243 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Detectors ; Flame ionization detector ; History of chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary On the occasion of the 25-year anniversary of its invention, this article summarizes the events which led to the development of the flame ionization detector.
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  • 10
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index ; Electric parameters ; Physico-chemical relationships ; Structure-retention study
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new equation is derived relating the retention index to the molecular polarizabilities, ionization potentials and permanent dipole moments of the stationary phase and the solute. Various implications of this equation to quantitative structure-retention relationships are discussed.
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  • 11
    ISSN: 1612-1112
    Keywords: Aldehydes and ketones ; 2,4-dinitrophenylhydrazine-coated silica gel ; Gas chromatography ; Column liquid chromatography ; Pollution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary After a brief review of several methods described in the literature this paper discusses air-sampling on 2,4-dinitrophenylhydrazine-coated silica gel and identification requirements for aldehydes and ketones most commonly found in industrial pollution. Quantitative analysis of formaldehyde and acetaldehyde either by GC or by HPLC techniques is established using a dynamic system producing test atmospheres and compared with the usual colorimetric determinations.
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  • 12
    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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  • 13
    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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  • 14
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    Chromatographia 17 (1983), S. 472-476 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid stationary phase ; Liquid phase bleeding
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The theory of the evaporation of the liquid stationary phase is elaborated and experimentally verified. On the basis of this theory the role played by the losses in the amount of liquid phase present is quantitatively determined. General techniques are examined which minimize the losses; these techniques are based on saturating the incoming carrier gas with liquid phase vapours and raising the pressure of the carrier gas in the column, e.g. by connecting a capillary to the column outlet in order to offer resistance to the gas flow. The application of these techniques ensures stable performance of the gas chromatographic columns using a volatile liquid phase.
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  • 15
    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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  • 16
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Step profile method ; Adsorption isotherm ; Water film pressure ; Surface free energy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Investigation of water adsorption by the step profile method (Glueckauf method) was carried out with the help of a modified gas chromatography equipped with thermal-conductivity detector. On the basis of the adsorption isotherm obtained, the water film pressure and the polar component of the surface free energy of quartz were calculated. The calculated value of the polar component of the surface free energy of quartz agrees with analogous values obtained by other methods.
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  • 17
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    Chromatographia 20 (1985), S. 371-375 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Flame photometric detector ; Sulphur
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The effect of experimental conditions such as gas flow rates, detector and column temperatures on sulphur response are discussed. It is concluded that the response of the flame photometric detector is affected by the O/H ratio and the total gas flow. Column temperature has an important influence upon S2 emission. It is shown that the sulphur response of the FPD is dependent on the compound containing the sulphur.
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  • 18
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Linear temperature programming ; Thermodynamic chracteristics ; Calculation of k PT ′ for LPTGC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple method has been elaborated to calculate capacity ratios under programmed-temperature conditions (k PT ′ ) from the thermodynamic characteristics determined for the given column under isothermal conditions and the parameters of programmed-temperature operations.
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  • 19
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    Chromatographia 21 (1986), S. 157-160 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Alkylation ; Carboxylic acids ; Urine analysis ; Micelles
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Carboxylic acids can be converted to their methyl esters in an aqueous sample which contains no organic solvent. The reaction appears to be assisted by the presence of a quaternary ammonium salt surfactant. The procedure is best described as a pseudo-organic phase, or micelle-like, reaction. The important experimental variables have been optimized by Simplex procedures. The reaction proceeds in 80–100% yield, for common carboxylic acids, at room temperature in less than one hour. This reaction is superior to existing two-phase extractive alkylation procedures.
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  • 20
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Ethylene oxide ; HBr-treated charcoal tubes ; Pollution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Air sampling of ethylene oxide on HBr-treated charcoal tubes followed by capillary GC analysis of the 2-bromoethanol produced allows pollution control evaluation for concentrations ranging from 0.2 to 20 mgm−3. The adequacy of the method is assessed taking into account ambient temperature and relative humidity.
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  • 21
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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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  • 22
    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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  • 23
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Polycyclic aromatic hydrocarbons ; Retention index ; Average molecular polarizabilities
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A significant correlation has been found between the retention indices of polycyclic aromatic hydrocarbons on non-polar stationary phases and the average molecular polarizabilities of the molecules separated on these phases. Equations have been derived for the determination of the average molecular polarizabilities, directly from the retention indices.
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  • 24
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Kováts retention indices ; Propellants ; Solvents ; Aerosol packs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary A gas chromatographic method is described by which a nearly complete separation of all commonly used propellants and solvents and their identification and determination can be achieved in one step. The separation is by simple adsorption chromatography on columns packed with Porapak-T with a temperature program 100–180°C at 10°C/min. Kováts' retention indices have been calculated for isothermal conditions at 150°C respectively 100°C for the propellants, at 180°C for the solvents. An exact identification of the propellants and solvents by means of the Kováts' indices is practicable even in complex mixtures.
    Notes: Zusammenfassung Es wird eine gas-chromatographische Methode angegeben, welche eine fast vollständige Auftrennung aller handelsüblichen Aerosol-Treibgase und Lösungsmittel und ihre Identifizierung und Bestimmung in einem Schritt gestatet. Die Trennung erfolgt durch reine Adsorptions-Chromatographie and Porapak T-Säulen bei 100–180°C mit einer Temperaturate von 10°C/min. Zur Bestimmung der Retentionsindices nach Kovats wurden die Treibgase isotherm bei 150°C bzw. 100°C, die Lösungsmittel bei 180°C aufgetrennt. Anhand der Kovats-Indices ist eine eindeutige Identifizierung der Treibgase und Lösungsmittel selbst in vielfältigen Gemischen möglich.
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  • 25
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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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  • 26
    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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  • 27
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Glass capillary column ; Retention indices ; Alkylcyclopentane and Alkenylcyclopentane ; Alkylcyclohexane and Alkenylcyclohexane
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Reaction products of the pyrolysis of n-dodecylpentane and n-hexylcyclohexane had been separated and identified on a glass capillary column coated with Polydimethylsiloxane OV-1. The identification of the components in the pyrolysis products and of the corresponding hydrogenated samples was performed from structure retention correlations, especially retention index increments (1CH2), homomorphy values (HOV-1) and the temperature coefficients of retention indices (δI/δT). Hence the presence of homologous 1-alkenes and of monoalkenylcycloalkanes could be confirmed. Based on the addition principle of index increments the determination of the side chain structure of alkenylcycloalkanes (straight chain) and the position of the double bond was ascertained. The calculation of the retention indices of these compounds was performed with high accuracy (deviation 〈1 index unit). Retention indices of 10 1-alkenes, 11 monoalkenyl-cyclopentanes, 11 monoalkylcyclopentanes, 5 monoalkenylcyclohexanes and 5 monoalkylcyclohexanes were determined on the liquid phase Polydimethylsiloxane OV-1.
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  • 28
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    Chromatographia 23 (1987), S. 722-726 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Adsorbents for gas chromatography ; Strong adsorption sites ; Heterogeneity of silica surface
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple gas chromatographic method is presented for the determination of the quantity of the strongest adsorption sites on an adsorbent's surface. The method consists of the blockage of the sites with quasi-irreversibly adsorbed, known amount of a strongly interacting compound and subsequent measuring of the retention of a hydrocarbon during the presence of the blocking compound in the column. Heterogeneity of chromatographic grade silicas is investigated with this method.
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  • 29
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    Chromatographia 15 (1982), S. 245-248 
    ISSN: 1612-1112
    Keywords: Chromatoscopy ; Gas chromatography ; Graphitized carbon black ; Molecular structure and retention ; Aromatic hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A molecular-statistical calculation of the retention volumes at zero sample size on graphitized thermal carbon black is carried out for quasi-rigid molecules of fluorene, indene, 1-methylindene, 2-methylindene and three dimethylindenes. A reasonable agreement is observed between the calculated and the available experimental gas chromatographic data. The potential barrier to internal rotation and the torsional angle in styrene molecules are estimated by comparing theoretically calculated and measured retention volumes.
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  • 30
    ISSN: 1612-1112
    Keywords: Phthalides ; Gas chromatography ; Chromosorb W ; Isomerization ; Ligustilide
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary During GLC of naturally occurring mixtures of phthalides on packed columns an artefact was sometimes detected that originated from Z-ligustilide. Active sites of Chromosorb W were responsible for the formation of the artefact, that was assumed to be E-ligustilide as GC-MS revealed that its mass spectrum was identical with that of Z-ligustilide. No isomerization was observed when freshly coated Chromosorb W was used or the support was deactivated by benzoyl chloride or melamine. The identity of the artefact was confirmed by UV irradiation experiments.
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  • 31
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Multi-chromatography ; Selectivity tuning ; Column combination ; Theory
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The evolution of the use of mixed phases or serial column combinations is outlined, leading to systems with fixed-length columns to be used in selectivity tuning (“multi-chromatography”). The difference between multi-chromatography and multi-dimensional gas chromatography is outlined. After discussing the system used in subsequent work, the fundamental relationships of multi-chromatography are detailed. Among the basic relationships the additivity of retention data, the relationship between the individual and composite capacity factors and the relative retentivity serving as the fundamental parameter of a multi-chromatography system are discussed. The relative retentivity is derived as a function of gas holdup times, pressures, and average velocities or flow rates. Finally, the relationships between individual vs. composite relative retention, efficiency, and resolution values are deduced.
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  • 32
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    Chromatographia 23 (1987), S. 132-136 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column liquid chromatography ; Thin-layer chromatography ; Analysis of lactulose in carbohydrate mixtures
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Lactulose is a disaccharide with important implications in medicine, nutrition and dairy technology. It has to be determined usually as a minor component in complex matrices containing many other sugars. This paper describes the different chromatographic techniques (planar, liquid and gas chromatography) which have been proposed for the separation and quantification of lactulose in mixtures with other carbohydrates; the advantages of each technique are compared and some features where more research is necessary are outlined.
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  • 33
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    Chromatographia 15 (1982), S. 521-524 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index ; Connectivity index ; Van der Waals' volume ; Alkanes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The relationships between retention index and Van der Waals' volume and between retention index and connectivity index have been studied for 58 different alkanes (C1−C9) on squalane. The correlation coefficient for the former is higher than for the latter. From these equations a linear relationship between Van der Waals' volume and connectivity index is obtained which indicates that the two parameters are equivalent. A simple method for calculating the Van der Waals' volume of alkanes is proposed.
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    Chromatographia 23 (1987), S. 215-219 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid chromatography ; Thermodynamic equilibria ; Solution and adsorption thermodynamics ; Gas adsorption isotherms
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    Topics: Chemistry and Pharmacology
    Notes: Summary After a brief recall of the chromatographic principles, the different applications of gas chromatographic measurements of thermodynamic equilibria were reviewed. Gas and liquid chromatographies are now well known and elegant methods for measuring the physicochemical properties and phase equilibrium thermodynamic constants. Although fundamentally a dynamical method and mostly known as a powerful separation technique, chromatography can be schematized by a sucession of equilbria of a chemical species partitioning between a mobile phase and a fixed liquid or solid stationary phase. It can be operated in either infinite dilution or finite concentration conditions and permits to collect a large number of data for calculating molecular interactions for solutes which are either rare or available at the trace level. Gas chromatography permits the measurement of gas adsorption isotherm, gas-liquid equilibria, molecular diffusion and interaction virials. The modelization of successive partition equuilibria occuring in the chromatographic column leads to rather simple expression of differential enthalpy, entropy, free energy of adsorption or solution, variation of heat capacity, complexation constant, second virial coefficients, gas-solid and gasliquid isotherm and also binary or ternary equilibria. The possibilities of High Performance-Liquid Chromatography to investigate adsorption from solutions and chemical equilibria are also discussed.
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  • 35
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Ethylene oxide ; Active charcoal tubes ; Pollution
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    Topics: Chemistry and Pharmacology
    Notes: Summary Air sampling of ethylene oxide on active charcoal tubes followed by GC analysis is a frequently proposed method. This paper studies just to what extent it can be used, defining its limitations (concentration range, influence of ambient temperature and relative humidity), which are seldom taken seriously into account. This method proves inadequate to determine low pollution levels, i.e. around 2 mg m−3.
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  • 36
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    Chromatographia 23 (1987), S. 423-426 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Complexation ; Mercaptosilane chemically bonded phase ; Transition metal complexes ; Olefinic π-complexes
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    Topics: Chemistry and Pharmacology
    Notes: Summary A column packing containing thiol groups chemically bonded to the silica surface was synthesized. The thiol functional groups were used as ligands capable of forming stable complexes with Cu(II). The prepared material was characterized by gas chromatography using unsaturated linear and branched hydrocarbons as well as cyclic and aromatic hydrocarbons. The occurrence of specific metal—olefin interactions resulting from the formation of π-complexes during the chromatographic process was observed.
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  • 37
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    Chromatographia 17 (1983), S. 33-36 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Preparative scale chromatography ; Capacity ; Dual-step separation
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    Topics: Chemistry and Pharmacology
    Notes: Summary The capacity of dual-step preparative chromatographic separation systems is considered. It is shown that dualstep separation makes it possible to enhance the capacity of preparative installations as compared with single- and dual-stage purification of the compounds.
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  • 38
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Preparative scale separations ; Plate model
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    Topics: Chemistry and Pharmacology
    Notes: Summary Two close-boiling materials, diethyl ether (DEE) and dichloromethane (DCM), were separated to investigate the effects of the pure components and the mixture on elution in preparative gas-liquid chromatography. Nitrogen was used as the carrier gas, and the chromatographic column (1 cm I.D. and 0.75m length) was packed with Chromosorb A with different quantities of dinonyl phthalate stationary phase and particle sizes. Below ca. 7% (by wt.) of feed concentration, the experimental elution curves of pure DEE and DCM were almost the same as those of the mixture, and the theoretical plate model can be used successfully to predict the elution curves.
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  • 39
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    Chromatographia 25 (1988), S. 993-998 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; HPLC system ; Micropacked column ; Organic mobile phase ; UV detection
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    Topics: Chemistry and Pharmacology
    Notes: Summary Retention behaviours of aromatic hydrocarbons were examined by using the vapour of an organic substance as the mobile phase and silica gel as the stationary phase. Gas chromatographic separation of aromatic hydrocarbons was demonstrated by using a system comprising a liquid chromatographic (LC) pump, a micropacked column for LC, a column oven and a UV detector.
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  • 40
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Micropacked columns ; Quantitation ; Fermentation products
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    Topics: Chemistry and Pharmacology
    Notes: Summary A new method is proposed for the analysis by gas chromatography of volatile compounds found in alcoholic and acetic fermentation samples. The method represents a suitable choice for the accurate and precise determination of 19 compounds (including Methanol) by direct injection onto a single column. Chromatograms of synthetic mixtures as well as actual samples show the capabilities of the micropacked column used.
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  • 41
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    Chromatographia 23 (1987), S. 50-52 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention indices ; C6 alkanols ; OV-101 ; Carbowax 20M
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    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic retention indices for 16 C6 alkanols measured on capillary columns coated with OV-101 methylsilicone and Carbowax 20M propylethyleneglycol liquid phases at 80° and 90°C were determined. The respective standard deviation values were 0.5 and 0.8 i.u. The correlation between the retention indices measured on non-polar and polar stationary phases and the boiling points of the alkanols was studied.
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  • 42
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Propyl esters of aliphatic hydroxy acids
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    Topics: Chemistry and Pharmacology
    Notes: Summary Aliphatic hydroxy acids were esterified in aqueous solution in the presence of different amounts of sulfuric acid. Esterification of lactic, tartronic, malic and citric acids in water/n-propanol mixtures with mole ratios between 0.03 and 2.15 can be utilized for the determination of these acids by gas chromatography. Water does not interfere at water/n-propanol mole ratios below 0.03. For mole ratios above 0.03 anhydrous sodium sulfate is used for the binding of water. The mole ratio range was 0.24–2.13 for anhydrous sodium sulfate/water, and 0.16–1.28 for sulfuric acid/anhydrous sodium sulfate.
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    Chromatographia 23 (1987), S. 850-855 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Bacterial cellular fatty acids ; Stationary phase selectivity ; Solid phase preseparation
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    Topics: Chemistry and Pharmacology
    Notes: Summary The importance of selectivity in the capillary gas chromatographic analysis of the cellular fatty acids of micro-organisms is underestimated. The analysis on apolar silicone phases can lead to erratic elucidation of the fatty acid structure. Qualitative errors have been detected in commercially available standards on which computer matching identification techniques are based. Using highly polar capillary columns of the cyanopropyl silicone type, the errors could be elucidated. The exact identification of the hydrolysis products of bacteria is a must for chemotaxonomic studies applying chromatographic techniques. The fatty acid methyl ester profiles can also contain other chemical components which are very important taxonomic markers. Fatty aldehydes, for example, are main components in someClostridium species. Fractionation techniques are described for selective enrichment of fatty aldehydes and hydroxy fatty acids.
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  • 44
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    Chromatographia 25 (1988), S. 547-559 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid column chromatography ; Process scale separations ; Review
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    Topics: Chemistry and Pharmacology
    Notes: Summary The relative merits of large scale gas chromatography (GC) and high performance liquid chromatography (HPLC) have not been reviewed for some considerable time. Although methodologies capable of manufacturing high efficiency (and hence cost effective) plant have existed for over a decade, commercial introduction has been remarkably slow. This has primarily been caused by confidentiality restrictions placed on equipment manufacturers, in turn severely limiting wide ranging applications data. These are necessary to raise potential end users confidence that both techniques offer viable large scale routes to separation and purification of mixtures as analysed by laboratory chromatographic methods. Considerable recent progress has been made with large scale HPLC plant, which has led to sufficient published data to make both technical and economic comparisons against GC possible.
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    Chromatographia 25 (1988), S. 598-602 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Steroid profiles
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    Topics: Chemistry and Pharmacology
    Notes: Summary Steroid conjugates are hydrolysed enzymatically using β-glucuronidase after extraction from urine using a solid phase extraction cartridge. After hydrolysis the free steroids are removed from the matrix, again utilising solid phase extraction. Derivatisation of the free hydroxyl groups using Hydrox-Sil AQ produces the respective TMS ethers which are extracted into hexane, in which solvent they are stable for many days. Capillary GC analysis with flame ionisation detection produces a profile of the steroids present in the sample. This technique is suitable for following changes in the urinary excretion profiles of patients undergoing investigation for a variety of steroid production-related diseases.
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    Chromatographia 25 (1988), S. 655-658 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Structure-retention relationships ; Connectivity indices, topological indices ; Alkenes
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    Topics: Chemistry and Pharmacology
    Notes: Summary Retention indices of different alkenes are correlated with connectivity and topological parameters. The appropriate statistically valid relations hips are derived and discussed.
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    Chromatographia 23 (1987), S. 240-242 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stillingia oil ; Quantitative lipid analysis ; Chinese tallow,Sapium sebiferum
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    Topics: Chemistry and Pharmacology
    Notes: Summary Contemporary stillingia oil from China is qualitatively similar to the oil described earlier, but it exhibits significant quantitative differences reflecting a degree of autoxidation of the unsaturated fatty acids either before or after crushing of the seeds.
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  • 48
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fourier transform IR detection ; Headspace sampling ; Solvents of abuse
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    Topics: Chemistry and Pharmacology
    Notes: Summary After experimental intoxication of rats, gas chromatography — Fourier transform infrared spectrometry with headspace sampling (HS/GC/FT-IR) was used to identify solvents of abuse in biological material (blood, liver, lungs and brain). Limits of detection were measured for acetone, 2-butanone, ether, toluene and trichlorethylene with standard solutions. All the solvents have been identified in the organs of the intoxicated rats. For blood samples a salting-out effect was obtained with potassium carbonate. HS/GC/FT-IR allowed the identification of metabolites of acetone (isopropanol) and of 2-butanone (2-butanol) in blood and organs.
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  • 49
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    Chromatographia 26 (1988), S. 125-132 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Non-equilibrium frontal chromatography ; Nonlinear isotherms ; Variable velocity ; Multicomponent mixtures
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    Topics: Chemistry and Pharmacology
    Notes: Summary The paper presents a classification of various theoretical models for multicomponent gas chromatography at u=var for high concentrations of the mixture components with consideration of the major distinctive features of the interphase mass exchange inside the porous grains of the adsorbent and outside them within the porous medium of the chromatographic column. It has been shown that the conditions determining a given front behaviour of multicomponent gas mixture at u=var depend on: theoretical models for the kinetics and dynamics of adsorption; the values of mass exchange parameters inside the porous grains and in the porous medium. Formulae have been derived for calculating the values of the quantities characterising the frontal behaviour in the stage of adsorption and desorption of multicomponent mixture at u=var.
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    Chromatographia 27 (1989), S. 60-66 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Mass loadability ; Stationary phase capacity ; Capillary columns
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    Topics: Chemistry and Pharmacology
    Notes: Summary In GLC the mass load can be normalized with respect to the amount of stationary phase in one plate. This quantity can be used for a specified solute-liquid phase combination in any capillary or packed column, irrespective of the column dimensions or the number of plates. For each individual solute in a given stationary phase a unique factor β″ can be found, which accounts for the specific shape of the isotherm of this particular combination. this factor β″ corresponds well with the activity coefficients of the solutes in the stationary phase, by which a fairly good approximation of the mass loadability of the column at hand can be made without need for experiment.
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    Chromatographia 25 (1988), S. 134-138 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Sulfur ; n-Octane adsorption
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    Topics: Chemistry and Pharmacology
    Notes: Summary From the adsorption isotherms of n-octane on the surface of sulfur at 29.8°C and 40.6°C some thermodynamic functions were determined. On the basis of these data the structure of the adsorbed layer of n-octane is postulated. The molecular interactions and adsorption mechanism are also discussed. It is stated that both quasi-liquid and quasi-sold layers may be formed on the surface of sulfur depending on the surface coverage with n-octane.
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    Chromatographia 27 (1989), S. 333-339 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Catalytic reactions ; Adsorption and desorption rate constants ; Reversed-flow techniques
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    Topics: Chemistry and Pharmacology
    Notes: Summary A small volume of reactant, 1-butene, is injected onto a catalytic bed and is allowed to diffuse away from it together with the product butane, along a narrow empty chromatographic tube; the latter is connected perpendicularly to the middle point of another similar tube through which hydrogen flows as reactant and carrier gas, transferring both 1-butene and butane to the detector through an analytical column. By using the reversed-flow GC technique, extra peaks are obtained in the chromatographic trace, sampling the concentration of both the readtant and product at the junction of the two tubes as a function of time. These concentrations are the result of the diffusion of the substances along the narrow empty tube, modified by the adsorption-desorption rates and the rate of the catalytic reaction. From the extra peaks of the reactant and product, a number of physicochemical quantities pertaining to the catalytic reaction can be calculated simultaneously, using appropriate mathematical analysis. These include adsorption rate constants, reaction rate constants, desorption rate constants, partition coefficients, and the overall mass transfer coefficients of the reactant across the gas-solid boundary of the catalytic bed.
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  • 53
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Coke oven gas evolution ; On-line gas analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatograph will thermal conductivity detector (TCD) connected on line via a cleaning train to the semi-industrial scale Coke Oven Text Plant of the Spanish National Coal Institute (INCAR), has been used to control the evolution of the permanent gases during the coking process. The undesirable presence of oxygen in the coke oven gas can be detected with this system that will be applied to determine the end of the coking process by quantitative analysis of the gas evolved.
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  • 54
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Adsorption studies ; Clinoptilolite ; Zeolite
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    Topics: Chemistry and Pharmacology
    Notes: Summary Adsorption properties of NH4-clinoptilolite, thermally treated at 400, 550 and 650°C, were investigated by gas-solid chromatography. Adsorption of ten hydrocarbons, including aliphatic, alicyclic, chlorinated and aromatic compounds is discussed in the light of adsorbate-adsorbent interactions. The imporatant thermodynamic parameters of adsorption are determined. A detailed discussion is presented on the alteration of the surface properties of NH4-clinoptilolite caused by thermal treatment. Experimental data obtained show that NH4-clinoptilolite treated at 650°C can be successfully employed as a column packing in analytical gassolid chromatography.
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  • 55
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Perhalogenated compounds ; Relative retentions ; Identification by interpolation
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    Topics: Chemistry and Pharmacology
    Notes: Summary Separation of perhalogenated compounds resulting from thermolysis, photolysis or radiolysis of mixtures of halogens in carbon tetrachloride was carried out by programmed temperature gas chromatography. Plots of relative retentions (to CBr4) vs the number of bromine atoms present for known compounds of the general formula CxBryClz (x=1 and 2; y+z=4 or 6) gave three linear correlations (all with r〉0.99). These correlations permitted projections of the identities of reaction products for which no standards were available. These projections were later confirmed by CG-MS. *** DIRECT SUPPORT *** A0732166 00010
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    Chromatographia 27 (1989), S. 631-632 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Wide-bore glass capillary columns ; End-sealing ; Static coating
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    Topics: Chemistry and Pharmacology
    Notes: Summary An end-sealing method to be used for static coating of wide-bore glass capillaries is described. After the capillary was completely filled with the coating solution, one end is connected to a gas-tight syringe (10-ml volume) via silicone tubing and the other end is fixed with shortcutted silicone tubing for sealing with a plug. The method is highly successful.
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  • 57
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Ethyl carbamate ; Direct injection quantification ; Cold injection system ; Optimised SIM
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    Topics: Chemistry and Pharmacology
    Notes: Summary An integrated procedure is described which allows direct injection quantitative screening to single figure parts per billion (μg/L) levels of ethyl carbamate in the natural matrix of distilled alcoholic beverage. Injection and detection performance was studied and optimized to allow this routine, reproducible, trace analysis without any sample pre-treatment. All aspects of the analysis including autosampler run sequences and automated internal standard report generation are initiated and controlled from a single GC/MS workstation.
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    Chromatographia 28 (1989), S. 237-240 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Slope of log plot ; Homologous series ; Retention index ; Retention time ; Uncertainty ; Free energy
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    Topics: Chemistry and Pharmacology
    Notes: Summary The free energy of partition of a methylene group $$\Delta G_{CH_2 }^ \circ $$ is constant within a homologous series down to C5 and nearly constant to C3, contrary to the finding of Golovnya and Grigoryeva [5]. Retention indices are linear with carbon number: values may be extrapolated from higher carbon numbers to C5 within experimental uncertainty, to C4 with error no greater than 5 units and to C3 with error no greater than 10 units. Error in extrapolating the logarithm of the adjusted retention time, log t′R, to C5 is thus negligible, to C4 has possible error up to 5b/100 and to C3 up to 10b/100, whereb is the slope of the plot of log t′R against carbon number.
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  • 59
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    Keywords: Gas chromatography ; Optimization of gas-solid separations ; Plate height equation ; Computer mapping procedure
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    Topics: Chemistry and Pharmacology
    Notes: Summary This paper proposes an optimization model for gas-solid chromatographic separations in a non-linear programming form and an approximate equation of the plate height for the model. A computer-modified mapping procedure is also described for searching the optimum separation conditions. Just five experiments and about 20 minutes of the computer time are needed to establish the optima of column temperature and of the carrier gas linear velocity. The relative deviation between the predicted and the experimental values was found to be within 20% for the plate heights, and within 1.5% for the retention times.
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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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  • 61
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    Keywords: Configuration ; Chiral phases ; Gas chromatography ; Isovaline
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    Topics: Chemistry and Pharmacology
    Notes: Summary The D-(resp. R) configuration of isovaline (=2-ethylalanine) was proved for the peptide antibiotics antiamoebin, Tü 165 (CBS 382.62), stilbellin, samarosporin (=emerimicin IV), suzukacillin B (A), trichotoxin A-40 and A-50. This contradicts the previously reported L-configuration for isovaline in antiamoebin and emerimicin IV. The configuration was determined by GC of the N-trifluoroacetyl-isovaline n-propyl ester on glass capillary columns coated with the chiral stationary phase N-propionyl-L-valine tert.-butylamide polysiloxane (Chirasil Val). The D-configuration of the isovaline from trichotoxin A-40 was also established independently using GC of N-pentafluoro-propionyl-isovaline (+)-3-methyl-2-butyl esters on glass capillary columns coated with OV 17.
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    Chromatographia 14 (1981), S. 143-147 
    ISSN: 1612-1112
    Keywords: Capillary columns ; Gas chromatography ; Retention index ; Structure
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    Topics: Chemistry and Pharmacology
    Notes: Summary The retention index of twenty different homologous series of esters have been determined experimentally on polar (Carbowax 1540) and non-polar (squalane) columns. General equations to calculate retention index have been established by statistical methods. The influence of the length and inductive effect of acid and alcohol chains and the relative position of the carboxylic group are discussed.
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    Chromatographia 14 (1981), S. 203-211 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Quantitative analysis ; Copper oxide converter ; Inorganic gas analysis ; Determination of fluorine and oxygen ; Hydrocarbon analysis ; Wine analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary A review of past activities concerning selected industrial analytical problems is given. This includes the following question: preparation of pure gas mixtures to be used for calibration, catalytic conversion of ester and pyridin samples to carbon dioxide and a one-point calibration method using peak heights, both for quantitative analysis, analysis of gas mixtures containing fluorine and inorganic fluorine compounds and the determination of the oxygen and fluorine content of the sample, separation and identification of hydrocarbons in shale oil and petroleum fraction samples, and analysis of wine.
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    Chromatographia 14 (1981), S. 19-22 
    ISSN: 1612-1112
    Keywords: Teflon columns ; Chemically modified teflon ; Gas chromatography ; Capillary columns
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    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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    Chromatographia 14 (1981), S. 576-578 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Tortuosity factor
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    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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    Chromatographia 14 (1981), S. 601-602 
    ISSN: 1612-1112
    Keywords: Ethanolamines ; Ethylene glycols ; Direct separation ; Gas chromatography ; Short glass capillaries
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    Topics: Chemistry and Pharmacology
    Notes: Summary An effective and rapid GC separation of ethanolamines, even in the presence of ethylene glycols, using short glass capillary columns is developed. No preliminary derivatisation of the sample is necessary. The separation is completed in 6 minutes.
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    Chromatographia 14 (1981), S. 648-652 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas-liquid adsorption ; Bulk solution ; Mixed stationary phases
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    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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  • 68
    ISSN: 1612-1112
    Keywords: Gas chromatography ; C1−C5 Hydrocarbons ; Dimethyl ether
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    Topics: Chemistry and Pharmacology
    Notes: Summary An analytical GC method was developed which uses a single packed column consisting of three packings in series prepared with the following liquid phases: dimethyl sulfolane, propylene carbonate, and silver nitrate. This system provides satisfactory resolution of mixtures of C1−C5 hydrocarbons and dimethyl ether obtained when converting methanol to gasoline. Due to the high capacity of the column it is possible to inject larger sample amounts permitting trace analysis.
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  • 69
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    Chromatographia 15 (1982), S. 117-124 
    ISSN: 1612-1112
    Keywords: Various packed GC column ; Gas chromatography ; Porous layer beads ; GC/MS analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary Theoretical comparisons of various packed GC column types are presented with respect to analysis time, efficiency, sample dilution, and sample capacity for a given maximum inlet pressure. In particular, totally porous particles, porous layer beads, and glass beads are compared with one another. It is shown that 30 μm porous layer beads offer a useful compromise between analysis time and plate count with relatively good sample capacity. Moreover, when using 1 mm i.d. columns (microbore), outlet flow rates that are reasonable for direct coupling to magnetic sector mass spectrometers are achieved making these columns suitable for GC/MS. Using 30 μm Zipax porous layer beads, columns yielding 8,000 to 10,000 plates/meter have been produced with inlet pressures of 13 to 26 atm. A simple modification of the injection port converts the maximum inlet pressure of a commercial gas chromatograph to 26 atm. With such pressures, columns in excess of 20,000 plates can be achieved. Chromatograms are presented illustrating the promise of these microbore columns for GC and GC/MS analysis.
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  • 70
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    Chromatographia 14 (1981), S. 507-509 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace ; Phenol ; Urine ; Enzymatic hydrolysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary A new method has been developed for the determination of phenol in urine in which the phenol conjugates are hydrolysed enzymatically and the liberated phenol is analysed by headspace chromatography. The results compare favourably with those obtained by the method of van Haaften and Sie in which acid hydrolysis is carried out in a heated GC precolumn. The enzymatic hydrolysis headspace technique appears to be very reliable and does not suffer from the disadvantages of precolumn acid hydrolysis.
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  • 71
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    Chromatographia 15 (1982), S. 351-354 
    ISSN: 1612-1112
    Keywords: Supported catalysts ; Reserved-flow GC ; Drying step ; Gas chromatography
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    Topics: Chemistry and Pharmacology
    Notes: Summary Application of reversed-flow gas chromatography to study the drying step in the preparation of supported catalysts is proposed. It is demonstrated that this technique can be applied to investigate the kinetic law followed, as well as to obtain kinetic parameters of drying (rate constants, activation energies and frequency factors). Amaterial illustrating this application is γ-Al2O3 impregnated with usual organic solvents (n-C5H12,n-C6H14,n-C7H16, CH3COCH3 and CH3CH2OH). It was found that in all cases above a simple first-order law based onone kind of active site is followed. Moreover, it was observed that the activation energyE a of the drying process increases almost linearly with the relative molecular mass of the solvent, whereas for the same solventE a increases with the amount used. The operation of a kinetic compensation effect suggests “similar” activated complexes of the various solvents used.
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  • 72
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    Chromatographia 15 (1982), S. 546-558 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Quantitative analysis ; Sample inlet systems ; High-speed analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary The attainment of precise quatitative analytical data using open-tubular (capillary) columns in standard, commercially available gas chromatographic instrumentation is demonstrated. Key elements in the design and proper utilization of the instrumentation are discussed. The function of the various sample introduction systems is elaborated and their quantitative performance demonstrated. The extra-column contribution to band-spreading is determined and the resultant data is used assessing the suitability of commercial instrumentation for highspeed capillary gas chromatography. The quantitative analysis of a sample containing some eleven components in less than thirty seconds is shown.
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  • 73
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    Chromatographia 15 (1982), S. 312-314 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Injection-port modification ; Oxygen and nitrogen traces
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    Topics: Chemistry and Pharmacology
    Notes: Summary The paper presents a new device modifying normal injection port of a gas chromatograph for eliminating air contamination thus enabling determination of traces of oxygen or nitrogen. Further modification is also proposed which enables the analysis to be carried out with a limited quantity of sample gas. Potential application of this device in the analysis of reactive gases like florine has been indicated.
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  • 74
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Butyl esters of aromatic polycarboxylic acids
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    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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  • 75
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    Chromatographia 17 (1983), S. 418-420 
    ISSN: 1612-1112
    Keywords: Separation of metal chelates ; Gas chromatography
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    Topics: Chemistry and Pharmacology
    Notes: Summary A very good separation of the acetylacetonate of AL-(III), Cr(III) and Co(III) has been obtained by gas chromatography, on a column containing OV-17 silicone oil as the stationary phase.
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  • 76
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    Chromatographia 17 (1983), S. 421-425 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Purge and trap sampling ; Cryogenic focussing ; Water analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary The most important operating parameters of a commercial purge and trap GC apparatus have been investigated. Band broadening problems arising from the slow desorption of compounds from the Tenax trap have been overcome by cryogenic focussing at the beginning of the column. Good results have been obtained with both packed and capillary columns. The sensitivity of the technique is sufficient to detect benzene in water at concentrations below 1μg kg−1 (1 ppb).
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  • 77
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Cross-linked Stationary phase ; Immobilized Stationary phase ; Packed columns ; Trapping
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    Topics: Chemistry and Pharmacology
    Notes: Summary A coating of silicone SE-54 on Chromosorb W has been converted to an analytically stable, immobilized stationary phase layer by cross-linking with an organic peroxide. Up to 10% by weight has been applied in this manner. Excellent high temperature qualities are exhibited, such as low bleeding and good base line stability, during typical analyses. Poly (2,6-dimethyl-p-phenylene oxide) has also been crosslinked as a surface coating on Chromosorb W with an organic peroxide. From 3 to 4% by weight has been immobilized in this way. The resultant packing material, following high temperature conditioning, has been examined for use as an adsorbent of trace substances, similar to the applications to which such adsorbents as Tenax GC have commonly been applied, e.g. trace analysis of air. It appears to exhibit satisfactory properties for this analytical purpose.
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  • 78
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    Chromatographia 18 (1984), S. 556-559 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid chromatography ; Tetramethrin ; Residues
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the analysis of tetramethrin aqueous formulation and residues of tetramethrin on woolen cloth. The samples were extracted with acetonitrile and partitioned with benzene. Interferences were removed by liquid column chromatography with acid alumina and eluted with 10% ethyl acetate-hexane. Analysis was by gas chromatography with a 10% UCW98 (methylsilicone) column. Detection was made with the flame ionization detector to avoid the repeated dilutions necessary with use of the electron capture detector.
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  • 79
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    Chromatographia 18 (1984), S. 663-667 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas solubilities ; Enthalpies of solution ; Polar solutions
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    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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  • 80
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid crystal ; Capillary columns ; Retention data ; Stationary phase film thickness ; Column surface quality
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    Topics: Chemistry and Pharmacology
    Notes: Summary Glass capillary columns were prepared from non-deactivated and deactivated glass and coated with (2-methyl-4-[trans-4-n-propyl-cyclohexylcarbonyloxy]-benzoic acid-[4-n-heptyloxy-phenylester]) as the liqud phase, in different film thicknesses. The columns were tested using substances of different structures and polarities. It was verified that the capacity factors, retention indices and selectivity significantly depend on the thickness of the liquid crystalline stationary phase film and the quality of the tube, particularly in the case of columns with thin films. Trasition temperatures (melting and clearing point) of the liquid crystal are also dependent on these two factors.
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  • 81
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    Chromatographia 18 (1984), S. 243-248 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carrier gas ; Viscosity ; Influence of temperature
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    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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  • 82
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Nitrogen dioxide ; Diethyl ether ; Photo-induced reaction
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    Topics: Chemistry and Pharmacology
    Notes: Summary When dissolved in diethyl ether, nitrogen dioxide reacts with the solvent, slowly at room temperature, more rapidly on heating of UV irradiation. A complex mixture of products is formed in which further changes are observed after prolonged storge: these are less pronounced if the unreacted nitrogen oxides are removed. A gas chromatographic method was applied for the identification of the majority of products. Irradiation does not change significantly the qualitative and quantitative composition of the reaction products. The reaction is thus the so-called photo-induced process [ΔG〈0]. Preliminary suggestions are made concerning the reaction mechanism.
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  • 83
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    Chromatographia 20 (1985), S. 403-406 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Separation of sugars ; Oxime formation ; Silylation
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    Topics: Chemistry and Pharmacology
    Notes: Summary The procedure involving oxime formation followed by silylation for the analysis of standard hexoses by GC resulted in unseparated peaks for D-glucose, D-mannose and D-galactose. This procedure was therefore modified to obtain clear separation of hexoses. STOX (hydroxylamine containing phenyl-β-D-glucopyranoside as the internal standard) was mixed with trimethylsilylimidazol or hexamethyldisilazane, and then added to a standard sugar mixture containing D-glucose, D-galactose and D-mannose. The mixture was analyzed by gas chromatography with OV-17/OV-22 as the stationary phase, resulting in three distinct peaks.
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  • 84
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Macroporous silica ; Silica-adsorbent modification ; Low boiling halocarbons ; Analysis of water pollutants
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    Topics: Chemistry and Pharmacology
    Notes: Summary The use of the silica adsorbent Silochrom C-80 modified by a thin liquid stationary phase film is proposed for the gas chromatographic analysis of low molecular weight halocarbons. Such modified adsorbents are characterized by good retention of the volatile halocarbons and high selectivity with respect to halocarbons. The thermodynamic sorption characteristics of alkanes, chloroalkanes and chloromethanes on Silochrom modified by three liquid phases (Apiezon L, methylsilicone and polyethylene glycol 20M) and on Chromaton N with thick films of the same phases were studied. The heats of sorption (−ΔH) and free sorption energy changes (−ΔF) of these substances and the increments −Δ(ΔH) and −Δ(ΔF) per chlorine atom in the chloralkane molecule compared with n-alkanes with the same number of carbon atoms were determined. The “chlorine” retention indices of low molecular weight volatile halocarbons on three sorbents were determined to identify them in aqueous solutions using the electron-capture detector. The analysis of drinking water by this technique is demonstrated.
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  • 85
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    Chromatographia 21 (1986), S. 697-700 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Methyl silicones ; Unified retention index ; Hydrocarbons
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    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic retention indices of 51 hydrocarbons were determined on OV-101 dimethylsilicone between 40 and 70°C. From the measured data the unified retention indices were calculated.
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  • 86
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Coated porous polymers ; Adsorption phenomena ; Surface areas
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    Topics: Chemistry and Pharmacology
    Notes: Summary The behaviour of Chromosorb 101 and Chromosorb 102 supports coated with Ethofat 60/25, squalane and Fractonitril VI is compared. The adsorption constants of different solutes of varying polarity on these packings were calculated as well the surface areas for Chromosorb 102. The validity of the proposed equation used for correcting the specific surface areas of Chromosorb 102 for the molar volumes of each solute and the solubility parameters of the compounds, adsorbent and liquid phases is shown.
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  • 87
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    Chromatographia 21 (1986), S. 214-218 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Behaviour of metal acetylacetonates ; Adsorption isotherms ; Heat of solution
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    Topics: Chemistry and Pharmacology
    Notes: Summary Specific retention volumes, adsorption isotherms, molar heats of solution and changes of the entropy were determined from chromatographic data, which was obtained by the gas chromatographic separation of metal acetylacetonates. The retention data for Cr(III), Co(III) and Al(III) acetylacetonates were measured at different temperatures and different flow rates. From the retention data other values associated with adsorption and solution phenomena were calculated.
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  • 88
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    Chromatographia 21 (1986), S. 397-401 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention time extrapolation ; Retention time interpolation
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    Topics: Chemistry and Pharmacology
    Notes: Summary An empirical method of extrapolating and interpolating gas chromatographic retention times obtained at three equally spaced isothermal temperatures is described. The accuracy of the method was evaluated from retention time data obtained using packed glass columns. A procedure for constructing retention time tables for homologous series and the derivation of an equation for calculating retention times as a function of temperature is also presented.
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  • 89
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Volatile nitrosamines ; Fused silica capillary columns ; Linear indices
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    Topics: Chemistry and Pharmacology
    Notes: Summary Fused silica capillary columns of different diameters and polarities are linked to a thermal energy analyzer and a flame ionisation detector for comparison. Extra column effects are discussed. Unsymmetrical homologue nitrosamines are applied in order to assign the volatile nitrosamines most often to be determined by their linear indices rather than by their overall retention times.
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  • 90
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    Chromatographia 22 (1986), S. 271-274 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index calculation ; Epoxides
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    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of C6 epoxides on a glass capillary column coated with OV-101 dimethylsilicone liquid phase was investigated. Retention indices were determined at four temperatures between 60 and 90°C. Linear regression equations permit the pre-calculation of the retention indices and the dI/dT values of the C6 epoxides from their properties.
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  • 91
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    Chromatographia 22 (1986), S. 278-282 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Mixed phases ; Chlorinated C1−C3 hydrocarbons
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method to establish the optimum composition of mixed stationary phases used in GC is given for the case when only the retention times on the individual phases are known. The method has been empirically tested for the resolution of chlorinated C1−C3 hydrocarbons.
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  • 92
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    Chromatographia 20 (1985), S. 197-200 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Polyalcohol quantification ; Wine ; Vinegar
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    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method is described for the analysis of arabitol, mannitol, sorbitol and inositol in wine. The method is evaluated for repeatability using perseitol as internal standard. Perseitol can be added to wine before or after passing the wine through the ion-exchange column without showing significant differences in the polyalcohol content. The method is also applied to the analysis of vinegar from different substrates (wine cider and rice).
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  • 93
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Modified diatomaceous supports
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Diatomaceous earth type supports are modified with a liquid phase, by high-temperature thermal treatment in a closed system. It is shown that the retention characteristics of the support changes by this treatment. The main advantage of this method, as compared with modification in a flow-through system is that liquid phase evaporation and possibility of oxydation during the process can be avoided. This ensures a better uniformity of the modified support.
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  • 94
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    Chromatographia 15 (1982), S. 765-768 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Preparative scale chromatography ; Capacity ; Dual-stage separation
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    Topics: Chemistry and Pharmacology
    Notes: Summary The capacity of different versions of single- and dual-stage separation of mixtures on a preparative scale is considered. It has been shown that dual-stage separation with intermediate condensation considerably enhances the capacity of the installation as compared with a single-stage process.
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  • 95
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    Chromatographia 23 (1987), S. 839-843 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary phases ; Porous polymer beads ; Polarity ; Adsorbents ; Breakthrough volume
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    Topics: Chemistry and Pharmacology
    Notes: Summary The breakthrough volume of ådsorbent traps made with porous polymer beads Porapak N, P. Q, R, S was evaluated by analysis of polarity reference substances proposed by Rohrschneider (ethanol, methyl ethyl ketone, nitrometane, benzene, pyridine) by McReynolds (butanol, methyl propyl ketone) and of the first term of some homologous series: alcohols, aldehides, carboxilic acids, nitrocompounds, iodoalkanes and nitriles. Adjusted retention times of the compounds were measured at 200°C and correlated with the physical properties and with polarity class according to Ewell. Trapping efficiency of the various Porapak types was evaluated and the theoretical breakthrough volumes at 25°C was calculated for the used test substances.
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  • 96
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    Chromatographia 23 (1987), S. 818-824 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Selective sampling ; On-line fractionation ; Essential oil analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary The paper describes the possibilities of on-line selective sampling as an on-line fraction technique for the analysis of essential oils. Selective sampling is a micro-separation method, on-line with on-column injection, carried out directly in the syringe body by means of a selective elution of the sample through a fraction cartridge. The paper reports a method of both preparing and standardizing silica gel cartridges, and illustrates through some examples the results of some elution series of solvents on different essential oils.
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  • 97
    ISSN: 1612-1112
    Keywords: Organic pollutants determination ; Gas chromatography ; Thermal desorption
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    Topics: Chemistry and Pharmacology
    Notes: Summary The problem of the separation of 34 volatile organic chlorinated compounds is solved by using three different GC columns selected according to the needs of the particular separation required. The effect of water vapor contained as moisture in the trapped air on the retention of some characteristic compounds is studied. The influence of dead volumes on trap injection is also studied.
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  • 98
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    Chromatographia 23 (1987), S. 888-892 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Calculation of temperature programmed ; Retention indices
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    Topics: Chemistry and Pharmacology
    Notes: Summary A new method is presented for the calculation of the retention indices under linear temperature programming with or without an initial isothermal period. The data calculated by the method are in good agreement with the isothermal retention indices.
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  • 99
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Silicone liquid phases ; Oxidation
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    Topics: Chemistry and Pharmacology
    Notes: Summary The on-column oxidation of apolar and polar silicones used as gas chromatographic stationary phases is investigated. Even at 225° the effects of oxidation are found to be slight. Of the materials investigated the methylphenylsilicones are the most stable.
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  • 100
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    Chromatographia 23 (1987), S. 286-288 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Macroporous copolymers of 2-hydroxyethyl ; methacrylate ; Graft polymers ; Polar sorbent for gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The gas chromatographic behaviour of crosslinked macroporous 2-hydroxyethyl methacrylate grafted with 2-methyloxazoline was investigated and the range of applicability of the copolymer was assessed. Retention index values were measured on this copolymer and compared with those obtained on the terpolymer 2-hydroxyethyl methacrylate-ethylene dimethacrylate-acrylonitrile. Rohrschneider constants and efficiency data for selected sorbates are given. The use of this type of polymer in the separation of various types of compounds is documented by various examples.
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