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  • Gas chromatography  (108)
  • Springer  (108)
  • 2005-2009
  • 1980-1984  (108)
  • 1925-1929
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Year
  • 1
    Electronic Resource
    Electronic Resource
    Springer
    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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  • 2
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    Springer
    Chromatographia 13 (1980), S. 73-84 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas hold-up time ; Dead time
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The two approaches used for the calculation of the gas hold-up time and thus, the adjusted retention time are outlined, first for the restricted case when the carbon numbers of the three homologues used for the calculation are evenly spaced (c3−c2=c2−c1) and then, for the general case when (c3−c2) differs from (c2−c1). The basic difference in the philosophy of the two approaches is shown.
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  • 3
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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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  • 4
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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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  • 5
    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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  • 6
    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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  • 7
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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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  • 8
    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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  • 9
    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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  • 10
    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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  • 11
    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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  • 12
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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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  • 13
    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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  • 14
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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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  • 15
    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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  • 16
    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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  • 17
    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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  • 18
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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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  • 19
    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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  • 20
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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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  • 21
    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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  • 22
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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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  • 23
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    Chromatographia 17 (1983), S. 33-36 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Preparative scale chromatography ; Capacity ; Dual-step separation
    Source: Springer Online Journal Archives 1860-2000
    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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  • 24
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    Chromatographia 13 (1980), S. 686-692 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Micropacked columns in GC ; Microparticles
    Source: Springer Online Journal Archives 1860-2000
    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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  • 25
    ISSN: 1612-1112
    Keywords: Configuration ; Chiral phases ; Gas chromatography ; Isovaline
    Source: Springer Online Journal Archives 1860-2000
    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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  • 26
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    Chromatographia 14 (1981), S. 143-147 
    ISSN: 1612-1112
    Keywords: Capillary columns ; Gas chromatography ; Retention index ; Structure
    Source: Springer Online Journal Archives 1860-2000
    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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  • 27
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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
    Source: Springer Online Journal Archives 1860-2000
    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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  • 28
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    Chromatographia 14 (1981), S. 19-22 
    ISSN: 1612-1112
    Keywords: Teflon columns ; Chemically modified teflon ; Gas chromatography ; Capillary columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Wall-coated open tubular columns prepared from chemically modified teflon tubing have been developed for gas chromatography. Chemical reaction of the inner walls of teflon tubing allows bonding of an adhesive layer on which a variety of stationary phaes can be coated. Test mixtures of alkanes and alcohols were used to investigate the chromatographic properties of these columns and the stability and mixing of the adhesive and stationary phae layers. the results in dicate that mixing of the layers is negligible and that the column is stable for a long period of time.
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  • 29
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    Chromatographia 14 (1981), S. 576-578 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Tortuosity factor
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The relationship between the obstructive factor γ and velocity was restudied. The dependence of the obstructive factor on velocity was verified. The effects of diffusion coefficient and particle-to-column diameter ratio on the obstructive factor-velocity relationship were investigated. The results are consistent with Hawkes' hypothesis that values of γ at low velocities are averages over tightly packed and loosely packed domains while at high velocities they are weighted in favour of the loosely packed domains where there is more flow.
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  • 30
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    Chromatographia 14 (1981), S. 601-602 
    ISSN: 1612-1112
    Keywords: Ethanolamines ; Ethylene glycols ; Direct separation ; Gas chromatography ; Short glass capillaries
    Source: Springer Online Journal Archives 1860-2000
    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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  • 31
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    Chromatographia 14 (1981), S. 648-652 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas-liquid adsorption ; Bulk solution ; Mixed stationary phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary It is shown that the blending of some retention effects can make the resolution of complex mixtures on short classical columns as effective as on capillary columns.
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  • 32
    ISSN: 1612-1112
    Keywords: Gas chromatography ; C1−C5 Hydrocarbons ; Dimethyl ether
    Source: Springer Online Journal Archives 1860-2000
    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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  • 33
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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
    Source: Springer Online Journal Archives 1860-2000
    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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  • 34
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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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  • 35
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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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  • 36
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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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  • 37
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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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  • 38
    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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  • 39
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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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  • 40
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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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  • 41
    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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  • 42
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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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  • 43
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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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  • 44
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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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  • 45
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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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  • 46
    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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  • 47
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    Chromatographia 16 (1982), S. 26-31 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Ionization detectors ; Gaia
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    Topics: Chemistry and Pharmacology
    Notes: Summary This paper is an account of the development of the gaia hypothesis as seen through the eyes of a gas chromatographer. Gaia is a radical notion about the Earth which postulates the climate and chemical composition to be regulated at an optimum by and for life. Gas chromatography played an important role in the gathering of evidence for the hypothesis but most significantly the art of inventing detectors lead to the developement of a planetary life detector through which gaia was revealed.
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  • 48
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    Chromatographia 17 (1983), S. 65-69 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Oxygenates ; Fused-silica capillary columns
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method of analysing gasolines that contain oxygenates has been developed. The method uses a single fusedsilica capillary column and gives quantitative data for the oxygenates and the hydrocarbons in one analysis.
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  • 49
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    Chromatographia 13 (1980), S. 61-67 
    ISSN: 1612-1112
    Keywords: Optimization ; Carrier gas velocity ; Gas chromatography ; Influence of temperature on optimum velocity
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    Topics: Chemistry and Pharmacology
    Notes: Zusammenfassung Die Wahl der mittleren, linearen Trägergasgeschwindigkeit bei der Analyse von Mehrkomponentengemischen unter isothermen und temperaturprogrammierten Bedingungen wird diskutiert. Es wird gezeigt, daß stets eine Trägergasgeschwindigkeit gewählt werden sollte, die mindestens gleich, besser jedoch höher ist, als die optimale Gasgeschwindigkeit für den ersten Peak, gemessen bei der Starttemperatur (Temperaturprogramm) oder bei der eingestellten Ofentemperatur (isotherme Fahrweise).
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  • 50
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    Chromatographia 13 (1980), S. 752-754 
    ISSN: 1612-1112
    Keywords: Xylenol isomers ; Gas chromatography ; Polyols and polyethers as stationary phase ; Hydrogen bonding
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    Topics: Chemistry and Pharmacology
    Notes: Summary Xylenol isomers can be resolved on most polyols (sugars or sugar alcohols) and polyethers (polyethylene glycol or polypropylene glycol) with hydrogen-bonding interaction. They are separated on vinical polyols which have more hydroxy hydrogen than tetrol, and even on vicinal triol when its hydroxy hydrogen is acidic (stronger proton donor). The stronger is the hydrogen bonding interaction between xylenols and the liquid phase, the better is the separation of 2,4- and 2,5-xylenol, and the poorer the separation of 2,4-and 2,3-xylenol.
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    Chromatographia 13 (1980), S. 207-208 
    ISSN: 1612-1112
    Keywords: Trace determination ; Hydrogen chloride ; Ethylene oxide ; Gas chromatography ; Chlorinated solvents
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the determination of small quantities of hydrochloric acid in two chlorinated organic solvents (CHCl3 and CCl4). An excess of gaseous ethylene oxide is added to a liquid sample; the 2-chloroethanol formed is then analyzed by gas chromatography. The procedure is simpler and more sensitive in comparison with other conventional methods. It can be modified for other organic solvents.
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  • 52
    ISSN: 1612-1112
    Keywords: Gas chromatography ; On-column abstraction ; Aliphatic aldehydes ; Amine antioxidants
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    Topics: Chemistry and Pharmacology
    Notes: Summary The selective on-column abstraction of aliphatic aldehydes by gas chromatographic stationary phases containing N-iso-propyl N′-phenyl-p-phenylenediamine is described.
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    Chromatographia 13 (1980), S. 574-575 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Xylenol isomers ; Sugar derivatives as liquid phases
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    Topics: Chemistry and Pharmacology
    Notes: Summary Adenosine, guanosine and inosine used as liquid phases in gas chromatography permits the separation of all six xylenol isomers.
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    Chromatographia 14 (1981), S. 39-40 
    ISSN: 1612-1112
    Keywords: Xylidine isomers ; Heteroaromatic liquid phases ; Gas chromatography
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    Topics: Chemistry and Pharmacology
    Notes: Summary Nicotinic acid and 1H-benzotriazole appreciably resolved all the xylidine (dimethylaniline) isomers, while benzimidazole, nicotinamide and phthalimide can also separate all the isomers except 2,4- and 2,3-xylidines. The analyses were carried out on supports which were not treated with an alkali.
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    Chromatographia 14 (1981), S. 285-288 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Porous layer open tubular columns ; Kaolin as support ; Column performance
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    Topics: Chemistry and Pharmacology
    Notes: Summary PLOT columns have been prepared with kaolin as the liquid phase support. These columns show good efficiency with different stationary phases and good thermal stability with polar phases. The performance of columns is shown by the separation of various mixtures such as fatty acids, phenols and anilines which are of analytical importance.
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  • 56
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    Chromatographia 14 (1981), S. 345-350 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Silica capillaries ; Glass capillaries ; Mixed gum phases ; Polarity and selectivity
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    Topics: Chemistry and Pharmacology
    Notes: Summary Mixed phases of Superox 20M and OV-1 can be coated homogeneously on the untreated wall of fused silica capillary columns. Excellent columns with regard to efficiency, inertness and thermal stability can be obtained. (CE〉95% and MAOT≥250°). The polarity and selectivity were ascertained with Rohrschneider-Reynolds probes and a capillary polarity test mixture. The analysis of an essential oil mixture illustrates the possibilities of mixed phases in practical capillary GC.
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  • 57
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    Chromatographia 14 (1981), S. 69-72 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Polynuclear aromatic hydrocarbons ; Retention index ; Vapour pressure
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    Topics: Chemistry and Pharmacology
    Notes: Summary The retention index of a planar polynuclear aromatic hydrocarbon on the GC phases OV-101, SE-52, and OV-17 is strictly related only to the boiling point, and less closely to the relative molecular mass. The very approximates relation with connectivity index ins only a consequence of the latter. On a nematic lqiuid crystal phase, a variation of activity coefficient, expressed in terms of a shape factor, also influences the retention of PAH.
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  • 58
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Fused silica ; Contact angle ; Wettability
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    Topics: Chemistry and Pharmacology
    Notes: Summary This paper describes the systematic characterization of glass and the newly introduced fused silica and quartz capillary columns from surface wettability measurements. Common gas chromatographic stationary phases were used in capillary-rise measurements at temperatures up to 300°C. By construction of Zisman plots and using the Cassie equation, the relative surface concentrations of wettable and non-wettable groups were determined. By application of the Fowkes equation, the dispersion force component of the surface energy was investigated. The influence of various surface treatments such as leaching, silylation, and polymeric film formation are discussed. Wettability measurements were also used to evaluate the thermostability of various treated surfaces and to compare the surface properties of glass, quartz, and fused silica. The wettability of the surfaces with selected stationary phases as a function of temperature is also discussed.
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  • 59
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    Chromatographia 14 (1981), S. 421-424 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid sulfur ; McReynolds' constants
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    Topics: Chemistry and Pharmacology
    Notes: Summary The McReynolds' constants for liquid sulfur as a stationary phase in gas-liquid chromatography (GLC) are presented. A simple graphical method of pattern analysis is used to indicate the uniqueness of the sulfur column as compared with other stationary liquid phases characterized by McReynolds. The limitations of using a single factor (as polarity) for the basis for the selection of GLC columns is discussed.
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  • 60
    ISSN: 1612-1112
    Keywords: Phthalides ; Umbelliferae ; Liquid-solid chromatography ; Gas chromatography ; Ligustilide
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    Topics: Chemistry and Pharmacology
    Notes: Summary A liquid-solid chromatographic pre-fractionation of naturally occurring phthalides has been developed. The LSC was carried out on a column of silica applying a 1–50% gradient elution of diethyl ether (containing 2% methanol) in pentane. The enrichment in the fractions led to better possibilities for a gas chromatographic separation and isolation allowing further studies by spectroscopic methods. Ligustilide may easily isomerize during GC as a result of ageing of the column.
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  • 61
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    Chromatographia 15 (1982), S. 180-182 
    ISSN: 1612-1112
    Keywords: Acidic fermentation products ; Characterisation ; Gas chromatography ; Methyl esters
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    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid and simple method for the identification of acidic fermentation products is described. Methyl esters of volatile and non-volatile acids are separated on a single chromatographic column. Retention time data for a number of acids are tabulated.
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  • 62
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    Chromatographia 15 (1982), S. 183-185 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Analysis of ethylbenzene hydroperoxide ; Time normalization method
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    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method, based on the time normalization technique, is described for the analysis of ethylbenzene hydroperoxide in mixtures containing ethylbenzene, acetophenone, 1-phenylethanol, benzaldehyde and phenol. Different liquid phases were tested and the best results were obtained with tricresyl phosphate and neopentyl glycol sebacate. The influence of the support, the liquid loading and the gas velocity are discussed.
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    Chromatographia 15 (1982), S. 30-32 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Arsenic ; Inorganic materials
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the quantitative chlorination and extraction of arsenic as arsenic trichloride from a number of alloys. The conditions for the quantitative gas chromatographic measurement of the volatile chloride have been studied. The proposed method for inorganic materials is very fast giving results within 10 min; sensitive, 1.5·10−13 g As can be detected, simple and accurate. At the ng level of As the error is about 20% with a standard deviation less than 20%, and at the 10pg level the error is about 36% with a standard deviation of 44%.
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  • 64
    ISSN: 1612-1112
    Keywords: Graphizized carbon black traps ; Organic air pollutants ; Work areas ; Gas chromatography
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    Topics: Chemistry and Pharmacology
    Notes: Summary The use of traps containing graphitized carbon black for the collection and pre-analysis of atmospheric pollutants in industrial areas is presented. The working conditions, in terms of trapping capability and effectiveness of release by thermal desorption are discussed. Some practical applications are also given.
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  • 65
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Van der Waals' volume ; Polarity of stationary phase ; Retention index
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    Notes: Summary Equations for Retention Index (I) versus Van der Waals, volume (Vw) on squalane are studied for alcohols, carbonyls, esters and ethers. Each equation includes linear and branching substances with different positions of the functional group in the carbon chain. The study is extended to stationary phases with polarities from 4.29 to 91.54 on the Tarjan et al. scale. Variations of the slope and origin ordinate values with the polarity of the stationary phase are discussed.
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    Chromatographia 15 (1982), S. 517-520 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carbon-silica adsorbents ; n-Octadecanol film ; Phase transitions
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    Topics: Chemistry and Pharmacology
    Notes: Summary The properties of the n-octadecanol film on carbon-silica adsorbent (Carbosil) were investigated. It was found that n-octadecanol forms an oriented film on the Carbosil's surface. If the surface of the basic silica gel is not completely covered with carbon, then the phase transition takes place in this film at a temperature higher than the melting temperature of n-octadecanol. One may distinguish two forms of this film, characterised by the different structures and the temperatures of the phase transitions. The first exists on the surface of silica gel unblocked by carbon. This part of the film is a monolayer, in which the alcohol molecules are vertically oriented. The solid compact-liquid expanded type phase transition at the well-defined temperature occurs in this film. In the second part of the film formed on the carbon surface, there is a multilayer of n-octadecanol. Its molecules are probably parallely oriented in relationship to the adsorbent surface. This film desintegrates progressively when the temperature increase. Maximum temperature of this phase transition is lower than the temperature of its analogue on pure silica gel surface.
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    Chromatographia 16 (1982), S. 201-203 
    ISSN: 1612-1112
    Keywords: Phenols ; Whisky ; Gas chromatography ; Aroma compounds
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    Topics: Chemistry and Pharmacology
    Notes: Summary Twelve volatile phenols were identified in whisky by combined gas chromatography-mass spectrometry. Of these phenols 2,4-dimethylphenol was found for the first time in the aroma of whisky. The content of phenol, o-, m-, and p-cresol, guaiacol, p-ethylphenol, p-ethylguaiacol and eugenol in whiskies originating from different countries was determined by gas chromatography as their 2,4-dinitrophenyl ethers using electron capture detection. The results show that Scotch whiskies differ from others in the content of o-, m-, and p-cresol. The odour threshold values of phenols studied were determined in a 10% (v/v) ethanol-water mixture and in some cases also in the whiskies. Cresols have been found to make contribution to the aroma of Scotch whisky.
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  • 68
    ISSN: 1612-1112
    Keywords: Glass capillary ; Gas chromatography ; Methyl chloroacetates ; Methyl chloropropanoates ; Methyl chlorobutanoates
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    Topics: Chemistry and Pharmacology
    Notes: Summary The gas chromatography of all chlorinated methyl acetates, methyl propanoates and methyl mono- and dichlorobutanoates has been studied on Carbowax 20M and SE-30 glass capillary columns under various running conditions. The order of elution on a non-polar column was largely determined by the boiling point of esters, whereas on a polar column it was much influenced by the structure of compounds. Complete separation of the combined mixture of all 27 compounds could not be achieved, however, methyl 3,3-dichlorobutanoate was the only ester overlapped on both columns in spite of the various column temperatures used. The best separation of the mixture was on Carbowax 20M with a temperature program from 50°C at 8°C/min, isothermal running conditions leading either to poor separation of volatile components or long analysis time and broad peaks of higher chlorinated esters. The relative retention times for compounds at the various column temperatures are given and the retention order on a polar and on a non-polar column discussed.
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    Chromatographia 16 (1982), S. 107-111 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Thermionic ionization ; Catalytic flame ionization
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    Topics: Chemistry and Pharmacology
    Notes: Summary A newly designed thermionic detector was operated in two modes of thermionic ionization detection (TID), and a third mode of catalytic flame ionization detection (CFID). Operating modes were varied by changing the composition of the electrically-heated thermionic/catalytic source, and the composition of gases supplied to the detector. A TID-2 source activated by a low concentration of Cs/ceramic was operated in a dilute H2/air environment and provided specific responses to nitrogen and phosphorus compounds. A TID-1 source activated by a high concentration of Cs/ceramic was operated in a N2 environment and provided very high specificities and picogram detectivities to compounds containing electronegative functional groups such as the NO2 group. A CFID source formed from Ni/ceramic was operated in a H2/air flame environment and provided universal responses to all organics with enhanced responses to some heteroatom compounds.
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  • 70
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fused silica capillaries ; New polar phases: OV-1701 and RSL-310 ; Immobilization
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    Topics: Chemistry and Pharmacology
    Notes: Summary The possibilities of OV-1701 and RSL-310, two new stationary phases, have been evaluated for capillary gas chromatography in fused silica columns. OV-1701 is a cyanopropylphenyldimethyl polysiloxane of moderate polarity possessing excellent chromatographic characteristics. The phase exhibits high coating and chromatographic efficiencies, high temperature stability and is suitable for cross-linking. RSL-310 is a polar liquid stationary phase yet to be permanently bonded in a capillary column. The selectivity of both phases extends the applicability of fused silica columns.
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  • 71
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    Chromatographia 16 (1982), S. 98-102 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Rectangular channel ; Efficiency ; Capacity
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    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic experiments have been performed in a truly rectangular channel with a 60∶1 cross-sectional aspect ratio, constructed according to the field-flow fractionation technology. It is shown that the peak broadening is controlled by the thickness of the channel while the maximum load is determined by the largest cross-sectional dimension. However, even with its elongated configuration, the side walls contribute significantly to the band broadening of solutes with a high diffusivity. Good agreement is found between the experimental plate height data and the recent theoretical calculations of Golay [13] taking into account the side-wall effect.
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  • 72
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Modified thermal energy analyzer ; Selective detection of nitrogen compounds
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    Topics: Chemistry and Pharmacology
    Notes: Summary A modification to the TEATM Analyzer is described, which allows it to be used as a highly selective GC detector for nitrogen compounds as well as for N-nitrosamines and nitro compounds. The modified Analyzer is as sensitive as the AFID, but has a much higher selectivity towards nitrogen compounds than the AFID. Its response appears to be molar, with an output that is dependent only on the number of nitrogen atoms present. The performance of the modified Analyzer for the analysis of ammonia, amines,N-nitrosamines, nitriles and organonitro compounds is reported and discussed, as is its application to the detection of these compounds in bacon and beer samples.
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  • 73
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    Chromatographia 17 (1983), S. 600-604 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index ; Alkyl benzenes
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    Topics: Chemistry and Pharmacology
    Notes: Summary The additivity concept in the retention index system of Kovats has been examined for a series ofn-alkylbenzenes and theiro- andp-monosubstituted nitro-, amino-, and chloro-derivatives. Anomalous behaviour is exhibited by the first three members of the series on both polar and non-polar stationary phases. For addition of a methylene group ton-propylbenzene or ap-substituted derivative, it is found that the retention increment, Δl CH2, approaches 100 units. However, the strong inductive effect of the group in the ortho position and the steric effects apparent in ano-substituted alkylbenzene lead to large variations of retention increment upon addition of-CH2-to the alkyl chain. A study ofn-alkylbenzene retention on Apiezon L and Carbowax 20M over a wide range of temperatures has verified the linearity of the retention increment with temperature and has revealed that this gradient increases with increasing carbon side-chain length for the first few members of the series, thereafter becoming constant. Functional retention increments, Δlx, for substitution of nitro-, amino- and chloro-groups into the benzene ring are given.
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  • 74
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    Chromatographia 17 (1983), S. 191-194 
    ISSN: 1612-1112
    Keywords: Thermal treatment of MgO and MgCO3 ; Adsorption properties ; Gas chromatography
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    Topics: Chemistry and Pharmacology
    Notes: Summary The changes in the chromatographic properties of MgO and MgCO3 due to thermal treatment was investigated. The experimental results show that thermally treated MgO and MgCO3 can be used as stationary phase for the gas-adsorption chromatography of hydrocarbon mixtures.
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  • 75
    ISSN: 1612-1112
    Keywords: Esterification in aqueous solution ; n-Butyl esters of fatty acids ; Gas chromatography ; Fatty acid analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary The esterification of C1−C8 fatty acid in aqueous solutions and in the presence of sulfuric or hydrochloric acid and with n-butanol is described. It has been established that the esterification can be used for the quantitative determination of these fatty acids in the concentration ratio range of [H2O]/[n-BuOH]=0.01–5.3. In the concentration ratio range of 0.01–0.8 the water present does not interfere. In the concentration range of above 0.8 anhydrous sodium sulfate is used for binding the water, in the amount of [Na2SO4.anh.]/[H2O]≥0.2.
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  • 76
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    Chromatographia 18 (1984), S. 202-204 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Polysiloxane stationary phases ; Heat of adsorption ; Heat of solution
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    Topics: Chemistry and Pharmacology
    Notes: Summary The changes in the heat of solution of polar compounds and xylene isomers in methylsilicone fluid OV-101 deposited on Chromosorb W AW DMCS were studied. It was shown that the heat of solution increases with an increase of the percentage loading of the OV-101 up to 10%. Solution and adsorption thermodynamic characteristics of the studied system are briefly discussed.
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  • 77
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    Chromatographia 18 (1984), S. 234-238 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open-tubular columns ; On-column injection ; Stopped-flow operation
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    Topics: Chemistry and Pharmacology
    Notes: Summary A simple, inexpensive, on-column injector of the septum moving-needle kind is described for quantitative analysis using open-tubular columsn. when operated in the stopped-flow mode an improvement incolumn efficiency is observed combined wit a diminished tendency to produce split-top peaks, particularly for late eluting peaks. Using electronic integration a relative error of about 2.7% was observed for peaks spanning a wide range of sample concentrations and volatilities.
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  • 78
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Thermodynamic relationships ; Retention index ; Peak identification
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    Topics: Chemistry and Pharmacology
    Notes: Summary A thermodynamic criterion, ΔQ, is suggested which permits to estimate the difference in the functional group energy of interactions for two different stationary phases. The linear dependence of ΔQ on the homolog number m of any series Rm X can be used as the thermodynamic criterion for the identification of substances by GC analysis.
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  • 79
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    Chromatographia 18 (1984), S. 477-488 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open tubular (capillary) columns ; Sample capacity ; Column comparison ; Film thickness ; Column diameter
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    Topics: Chemistry and Pharmacology
    Notes: Summary Wall-coated, open-tubular (capillary) columns prepared from different diameter tubing, with different liquid phase film thickness, are compared with each other and with packed and support-coated open-tubular columns. The comparison is based on the variation of the phase ratio and the capacity factor, and includes column efficiency (HETP, theoretical plate number), resolution, retention time, and sample capacity. Problems associated with the evaluation of the sample capacity are outlined. The influence of temperature on column performance is discussed in detail. Finally, the possibilities of short, wide-bore open-tubular columns prepared with a thick liquid-phase film are demonstrated.
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  • 80
    ISSN: 1612-1112
    Keywords: Esterification in aqueous solution ; iso butyl esters of C1–C20 fatty acids ; Gas chromatography ; Fatty acid analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary C1–C20 carboxylic acids have been esterified in aqueous solutions with i-butanol. Gas chromatographic analyses have been performed from a single chromatogram. It has been established that esterification in the concentration range of [H2O]/[i-BuOH]=0.01–10.3 can be utilized for the quantitative determination of these carboxylic acids. The presence of water does not interfere in the range of [H2O]/[i-BuOH]=0.01–1.03. In the cases of [H2O]/[i-BuOH]〉1.03, anhydrous sodium sulfate has been used for binding the water, in an amount of [Na2SO4]anh./[H2O]≥0.2.
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  • 81
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    Chromatographia 18 (1984), S. 309-312 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carboxylic acids ; Acetonyl derivatives
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    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of the acetonyl esters of nine aliphatic carboxylic acids is described, the general formula of the derivatives being RCOOCH2COCH3 where R=alkyl or H. The derivatives show good chromatographic properties on both packed and capillary columns. The electron impact and chemical ionisation mass spectra of the derivatives are discussed.
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  • 82
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column characterization ; Oxidation ; Stationary phases
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    Topics: Chemistry and Pharmacology
    Notes: Summary The on-column oxidation of hydrocarbons commonly used as stationary phases in column characterization is investigated. In each case significant shifts of retention are observed, which may be negative or positive depending upon the polarity of the test solutes and the adsorptivity of the support material. In order to reduce the consequent uncertainties in the Rohrschneider [1] and McReynolds [2] polarity values, a new method of column characterization is proposed. The applicability of the new method is illustrated by a consideration of a range of silicone liquid phases.
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  • 83
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Fused silica capillaries ; Capillary drawing ; Glass capillaries
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    Topics: Chemistry and Pharmacology
    Notes: Summary A compact description is given of a simple and reliable method of drawing flexible fused silica capillary for gas chromatography. Some emphasis is given to the fact that the practices of drawing optical fibres should not be followed too slavishly so this leads to unnecessarily complicated and expensive equipment. Satisfactory capillary column silica tubing can be made with straightfoward extension of the method developed earlier for drawing thick walled capillary. A simple glass/silica hydrogen oxygen diffusion flame bumer is described for fusing the preform tubing at the draw point which is enclosed by a water cooled glass enclosure to trap evaporated silica and maintain the operation under dust free conditions. The uniformity of the capillary diameter is better than 5% which is adequate for most gas chromatographic purposes. The second part of the paper yet to be published will cover the methods developed for coating the capillary both internally and externally.
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  • 84
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    Chromatographia 17 (1983), S. 44-46 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Natural gas analysis ; Poropak N
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    Topics: Chemistry and Pharmacology
    Notes: Summary A simple gas chromatographic method is described for the rapid analysis of natural gas using thermal conductivity detectors and programmed-temperature operation of a single Poropak N column. The method permits the determination of nitrogen, carbon dioxide and hydrocarbons containing one to seven carbon atoms.
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  • 85
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    Chromatographia 17 (1983), S. 553-559 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open-tubular (capillary) columns ; Immobilized liquid phases ; Thick-film columns ; Diffusion coefficients
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The influence of the liquid phase film thickness in open-tubular (capillary) columns on the individual resistance-to-mass-transfer terms and on the overall column efficiency is examined from the theoretical point of view. Methods for the calculation of the diffusion coefficients are discussed.
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  • 86
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    Chromatographia 17 (1983), S. 691-692 
    ISSN: 1612-1112
    Keywords: Dichlorophenol isomers ; Sodium benzenesulfonate ; Gas chromatography
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    Topics: Chemistry and Pharmacology
    Notes: Summary It is difficult to separate all the dichlorophenol isomers as free phenols by gas-liquid chromatography. However they were effectively separated on 4,4′-dimethoxyazoxybenzene (liquid crystal), and all the isomers were separated appreciably well on sodium 1-naphthalenesulfonate, 2-naphthalenesulfonate and dodecylbenzenesulfonate.
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  • 87
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    Chromatographia 13 (1980), S. 263-270 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Metal complexes ; Enantiomers ; Isotopic composition
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    Topics: Chemistry and Pharmacology
    Notes: Summary The high selectivity of complexation gas chromatography has been employed for enantiomer resolution and isotope separation. Thus, a chiral olefin, 3-methylcyclopentene, has been resolved analytically on optically active dicarbonyl-rhodium(I)-3-trifluoroacetyl-1R-camphorate in squalane. The deuterated ethylenes C2H4−nDn have been separated on the same rhodium(I)-containing stationary phase. The chiral aliphatic oxiranes epoxypropane andtrans-2,3-epoxybutane have been resolved on optically active nickel(II)-bis-3-trifluoroacetyl-1R-camphorate in squalane.
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  • 88
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Graphitised carbon black ; Phenols ; Water pllutants
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    Topics: Chemistry and Pharmacology
    Notes: Summary The fractionation of eleven phenols which may be contaminants in drinking water has been accomplished by using acid-washed graphitised carbon black modified with trimesic acid and PEG 20 M.
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  • 89
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    Chromatographia 14 (1981), S. 699-703 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace analysis ; Aromatic hydrocarbons ; Water analyses
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    Topics: Chemistry and Pharmacology
    Notes: Summary The possibilities of using headspace analysis of aromatic hydrocarbon traces in aqueous solutions with changing values of the partition coefficients are discussed. A variant of headspace analysis of the simplest aromatic hydrocarbon in natural and waste water is described. It involves two-step gaseous extraction of a sample in vessels of varying volume before and after the equilibrium phase is replaced with a pure gas (air or nitrogen). This method permits to analyse 5–50 ml water samples with benzene and toluene contents varying from the ppb to the ppm range within an error not exceeding 155. The analysis time is about 1.5 h. The presence of non-volatile organic or mineral substances does not influence the determination. This method is unsuitable to heterogeneous systems (aqueous oil emulsions): before carrying out the analysis for the hydrocarbon content these systems have to be homogenized first.
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  • 90
    ISSN: 1612-1112
    Keywords: Teflon capillary columns ; Chemically modified teflon ; Gas chromatography
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    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of teflon capillary columns employing direct coating of the stationary phase to the chemically modified teflon surface and the role of the chemically modified teflon in the separation mechanism are described. Two types of contributions from the modified teflon have been observed: nonspecific adsorption of the carbon surface and specific interactions of polar groups in the carbon skeleton. The use of polar liquid phases can eliminate adsorption due to the presence of polar groups in the modified teflon.
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  • 91
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    Chromatographia 15 (1982), S. 704-706 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Isopropyliden-sorboses ; TMS-derivatives ; GC-MS combined technique ; Mass spectra
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method has been developed using gas chromatography — electron impact mass spectrometry for the determination of the di-0-isopropylidene-sorbofuranose and mono-0-isopropylidene-sorbofuranose. The compounds are separated as their trimethylsilyl derivatives on a capillary column coated with the stationary phase SE-52. The mass spectra show that the silylation reaction is quantitiative and that the isopropylidene groups does not change.
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  • 92
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    Chromatographia 14 (1981), S. 269-276 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Detector performance ; Trace analysis ; Catalytic conversion ; Multidimensional gas chromatography
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    Topics: Chemistry and Pharmacology
    Notes: Summary Relationships are derived describing how the detection limit of a chromatographic system depends on the minimum detectable limit of the detector and the chromatographic parameters such as column length, efficiency, carrier gas flow rate and the capacity factor. Performance data of detectors developed in the last 25 years at the Dalian Institute of Chemical Physics of the Chinese Academy of Sciences are given and a few selected application examples are listed. These include trace analysis by preconcentration and by direct analysis and the utilization of multidimensional gas chromatography with two columns, two detectors, a 12-port valve, and a catalytic conversion reactor.
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  • 93
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    Chromatographia 15 (1982), S. 125-132 
    ISSN: 1612-1112
    Keywords: Capillary columns ; Fast analysis ; Gas chromatography ; Instrumental effects ; Optimization
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    Topics: Chemistry and Pharmacology
    Notes: Summary The efficiency of fast GC columns depends largely on the quality of the chromatograph. A theoretical and experimental study shows the relative importance of the various phenomena involved and permits the optimization of a GC System. Extremely good performances, exceeding 2,500 plates per second have been routinely obtained.
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  • 94
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    Chromatographia 15 (1982), S. 241-244 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Monosaccharides ; Polyols ; GC of TMS derivatives
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    Topics: Chemistry and Pharmacology
    Notes: Summary This paper describes the gas chromatographic separation of the mixture of isopropylidene monosaccharides, and their trimethylsilyl derivatives. Based on the total analysis time and resolution the best stationary phase was SF-96 using Chromosorb G as the solid support and temperature programming.
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  • 95
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    Chromatographia 16 (1982), S. 282-285 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Naphtha analysis ; Gasoline analysis ; Hydrocarbon type analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary Two different gas chromatographic methods are used for the determination of hydrocarbon type distribution in naphtha and gasoline samples with final boiling points up to 275 °C. The methods are based either on a single capillary column or on a valve-switched packed column system. Both methods give extensive information on paraffins, olefins, naphthenes and aromatics in total as well as by carbon-number. In each case the analysis is fully automated with a computer controlling the entire analysis from injection to results presentation. The advantages and limitations of both methods are discussed.
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  • 96
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    Chromatographia 16 (1982), S. 322-324 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Graphitized carbon black supports ; Determination of hydroxyacids
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    Topics: Chemistry and Pharmacology
    Notes: Summary Acid-washed graphitized carbon black (Carbopakc B) modified with trimesic adic and PEG 20M has proved to be effective for quantitative analysis of underivatized low molecular weight hydroxyacids. Calibration data revealed good linear relationships between relative peak area and concentration for lactic and 3-hydroxybutyric acids down to 0.05 mmol/l. The packing material was suitable for the analysis of aqueous solutions of hydroxyacids as it is tolerant to injections of water over a prolonged period of use. The GC system developed has been applied to the analysis of some hydroxyacids of biomedical interest in blood plasma and lactic acid contained in wine and beer.
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  • 97
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Trace analysis ; GC-concentration ; Enrichment factor ; Theoretical evaluation
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    Topics: Chemistry and Pharmacology
    Notes: Summary Based on gas chromatographic retention data obtained on a given adsorbent and at a given trap efficiency at different temperatures new equations are proposed for the evaluation of the enrichment factor. These equations are suitable under various preconcentration conditions such as: equilibrium saturation, complete trapping and permissible losses. Compared to known expressions for the evaluation of the enrichment factor the equations suggested consider the band broadening of the impurity in a trap causing a loss of the substance at the adsorption stage and dilution of the sample during desorption when the desorbed impurities are directed into the gas chromatographic column without intermediate freezing out in an graphic column without intermediate freezing out in an empty tube. The new equations may be used to select the optimum preconcentration conditions providing the necessary sensitivity.
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  • 98
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    Chromatographia 17 (1983), S. 269-284 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid chromatography ; Phenols
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    Topics: Chemistry and Pharmacology
    Notes: Summary Gas and high-performance liquid chromatographic methods in the analysis of phenols are reviewed. Among the great number of phenolic compounds analyzed, alkylphenols, chlorophenols, dihydroxy- and trihydroxybenzenes and biphenols are chiefly considered. The advantages and drawbacks of the methods are discussed, quoting the most important work. Relationships between the structural characteristics of phenols, the stationary phase structure, the mobile phase composition and the retention data are treated. Typical examples of the conditions for GC and HPLC analysis are summarized in tables. The literature comprises over 270 references, most of them recent.
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  • 99
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Average molecular polarizability ; Retention index ; Polycyclic aromatic hydrocarbons
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The Kováts retention indices of 10 polycyclic aromatic hydrocarbons were determined on SE-30, OV-101, SE-52, OV-7 and OV-17 stationary phases. A significant correlation has been found between the retention indices and the average molecular polarizabilities of the analyzed substances. Equations were derived for the direct determination of the average molecular polarizabilities from the retention index values. The influence of the temperature on this relationship is also indicated.
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  • 100
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    Chromatographia 18 (1984), S. 260-264 
    ISSN: 1612-1112
    Keywords: Parabens and their dissolution ; Pharmaceutical dosage forms ; Derivatization ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A specific, sensitive and general applicabla gas chromatographic method is described for the determination of parabens in various liquid pharmaceutical preparations: propylparaben and butylparaben in a liquid antacid dosage form (I); methylparaben, ethylparaben and propylparaben in a syrup (II); methylparaben and propylparaben in a solution for injection (III). Each time one of the parabens is used as internal standard. The parabens are extracted with diethylether and derivatized by silylation. Different columns are used for the analysis of the parabens: 3% SE-30 column, a 3% QF-1 column for different selectivity, a 2% OV-1 column for isothermal operation. Special attention is attributed to the standard: the parabens are dissolved in a minimal amount of 0.1 M sodium hydroxide and extracted in the same way as the pharmaceutical dosage form.
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