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  • 2020-2024
  • 1995-1999  (27)
  • 1975-1979  (85)
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  • 1
    Digitale Medien
    Digitale Medien
    Springer
    European food research and technology 209 (1999), S. 400-406 
    ISSN: 1438-2385
    Schlagwort(e): Key words Pumpkin seed oil ; Oil adulteration ; Δ7-Phytosterols ; Sample clean-up procedure ; Gas chromatography
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Werkstoffwissenschaften, Fertigungsverfahren, Fertigung
    Notizen: Abstract  A simple and accurate method for the determination of phytosterols by capillary gas chromatography was developed for the analysis of the seeds and oil of the pumpkin Cucurbita pepo L., the naked seed variety growing in the southern Styrian parts of Austria. After extraction of the oil and saponification, the remaining unsaponifiable material was isolated and purified using silica gel columns. For greater volatility, the sterols were derivatised to trimethylsilylethers, and gas chromatography was performed on a column of high polarity, allowing separation of the Δ5-sterols from the Δ7-sterols and thus yielding a typical chromatographical pattern. Quantification of the phytosterols using 5α-cholestan or cholesterol as internal standards led to a method of high accuracy. Comparison of the chromatographic pattern of the phytosterol fraction of pumpkin seed oil with those of other vegetable oil samples permitted the use of this method to detect adulteration of pumpkin seed oil.
    Materialart: Digitale Medien
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  • 2
    Digitale Medien
    Digitale Medien
    Springer
    International journal of legal medicine 112 (1999), S. 124-131 
    ISSN: 1437-1596
    Schlagwort(e): Key words Hydroxyproline ; D/L Aspartic acid ; N-TFA isopropyl ester derivatives ; Gas chromatography ; Collagen
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin , Rechtswissenschaft
    Notizen: Abstract The proportion of D- to L-enantiomers of aspartic acid in metabolically isolated proteins has been used by forensic scientists to estimate age at death. We have demonstrated the interference of a derivative of hydroxyproline (N-TFA isopropyl Hyp ester) with the N-TFA isopropyl L-Aspartic (Asp) acid ester during gas chromatography of amino acids. This has serious implications for the accurate quantification of the D- to L-Asp ratio extracted from collagenous proteins. Having demonstrated the potential for this co-elution in amino acid standards, acid-soluble dentine proteins and non-mineralised collagen, we argue that this problem can be overcome either by high resolution separation or by analysis of the (Hyp-poor) non-collagenous protein fraction.
    Materialart: Digitale Medien
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  • 3
    Digitale Medien
    Digitale Medien
    Springer
    Rechtsmedizin 9 (1999), S. 184-189 
    ISSN: 1434-5196
    Schlagwort(e): Key words Ethyl glucuronide ; Congeners of alcoholic beverages ; Alkyl glucuronide ; Gas chromatography ; Mass spectrometry ; Schlüsselwörter Ethylglucuronid ; Begleitstoffe ; Alkylglucuronid ; Gaschromatographie ; Massenspektrometrie
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin , Rechtswissenschaft
    Beschreibung / Inhaltsverzeichnis: Zusammenfassung Es wird die chemische Synthese von Alkylglucuroniden beschrieben, die nach Konsum von begleitstoffhaltigen Getränken als Metaboliten im Urin erscheinen. Von folgenden Alkoholen wurden die Glucuronide synthetisiert: Methanol, d5-Ethanol, Propanol, Isopropanol, Butanol, Isobutanol, R-(–)-2-Butanol, S-(+)-2-Butanol, Isopentanol, S-(–)-2-Methylbutanol. Die Retentionsindizes der Acetyl-, Pentafluorpropyl(PFP)- und Trimethylsilyl(TMS)-derivate werden mitgeteilt und der Einfluß der chemischen Struktur auf den RI-Wert diskutiert. Die Massenspektren der homologen Derivate erwiesen sich als sehr ähnlich, aber einige Fragmente sind spezifisch für die Kettenlänge der Alkylgruppe und können zur Identifizierung und Quantifizierung der Glucuronide in Urinproben herangezogen werden.
    Notizen: Abstract The chemical synthesis of alkyl glucuronides, which appear as metabolites in urine after the consumption of beverages containing congeners of ethanol, is described. Glucuronides of the following alcohols were synthesized: methanol, d5-ethanol, propanol, isopropanol, butanol, isobutanol, R-(–)-2-butanol, S-(+)-2-butanol, isopentanol and S-(–)-2-methylbutanol. The retention indices of acetyl, pentafluorpropyl (PFP) and trimethylsilyl (TMS) derivatives are given and discussed in relation to the chemical structures. Mass spectra of homologous derivatives were shown to be very similar but some fragments were specific for the chain length of the alkyl moiety and can be used for identification and a quantitative estimation of glucuronides in urine samples.
    Materialart: Digitale Medien
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  • 4
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Sorptive preconcentration ; Air monitoring ; Nicotine ; Hospital air
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A novel method for the enrichment of nicotine from gaseous samples is presented. It is based on the sampling of 6 liters of air onto a cartridge packed with 100% polydimethylsiloxane (PDMS) particles. The analytes are dissolved (partitioned) into the PDMS phase which results in much better recoveries and reproducibilities compared to those obtained on common adsorbents. The PDMS tube is then placed in a thermal desorption (TD) unit connected to a CGC-NPD or CGC-MS system. The procedure was employed for routinely monitoring air in a hospital. Nicotine was typically found at levels ranging from 5 to 250 μg m−3 (ppb) depending on the location and number of smokers present. Additionally, the efficiency of nicotine filters was determined by sampling simultaneously at the filter in- and outlet and was found to be 46%.
    Materialart: Digitale Medien
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  • 5
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; [60] Fulleropyrrolidine polysiloxane ; High temperature stationary phase
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary In this paper, a new type of [60]fulleropyrrolidine functionalized polysiloxane in which the fullerene moieties were incorporated in the main polysiloxane chain was synthesized the first time and used as a stationary phase for capillary gas chromatography. It demonstrated high column efficiency (2600–2866 plates m−1, on a 250 μm diameter column, for naphthalenek=3.1–3.2, 120 °C), a wide operational temperature range (90–360 °C) and outstanding thermostability. It can be used at 360 °C with a baseline drift of 5∼8×10−15A. Benzene homologues, aromatic hydrocarbons, polar compounds such as alcohols, esters, ketones, anilines and phthalic diesters can be seperated well on this column.
    Materialart: Digitale Medien
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  • 6
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 49 (1999), S. 333-337 
    ISSN: 1612-1112
    Schlagwort(e): Supercritical fluid chromatography ; Gas chromatography ; Solvating gas chromatography ; Peak capacity
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary In this paper, a general peak capacity expression was evaluated using columns containing various packing materials under solvating gas chromatography (SGC) conditions. Differing from column efficiency, peak capacity can describe both separation capability and speed when introducing the dead time into the peak capacity expression. Various factors that influence peak capacity in SGC are described, including particle pore size, chemical surface modification, particle size, column length, temperature, and pressure.
    Materialart: Digitale Medien
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  • 7
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Microwave and ultrasonic extraction ; River sediment ; Dioxin-like polychlorobiphenyls ; Toxic equivalency factors
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Microwave extraction and ultrasonication of dioxin-like polychlorobiphenyls (PCBs) from sediment samples were investigated. After separation of dioxin-like PCBs from a sample matrix on an acidic-alkaline silica gel column, dioxin-like PCBs were determined by GC-ECD, using dual capillary columns. Recoveries of dioxin-like PCBs in river sediment samples exceeded 80% by both extraction techniques. Toxic equivalency factors and their use for the PCB congeners investigated were applied.
    Materialart: Digitale Medien
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  • 8
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Reversed-flow gas chromatography ; Carbon monoxide oxidation ; Bimetallic Pt−Rh catalysts
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Catalytic fractional conversions of carbon monoxide to carbon dioxide over Pt−Rh alloy catalysts in the presence of excess oxygen, under steady-state or non steady-state conditions, as well as corresponding rate constants for the CO oxidation reaction were measured by using the reversed-flow gas chromatographic technique. From the variation of the conversions with temperature, maximum values of conversions were found, which depend on the catalysts nature (Pt content), while from the variation of the rate constants with temperature, activation energies for the CO oxidation reaction were determined, which also depend on the catalyst Pt content. The results suggest a synergism between Pt and Rh in the Pt−Rh bimetallic catalysts in accordance with previous works, showing that reversed-flow gas chromatography can be used with simplicity and accuracy for the kinetic study of the CO oxidation reaction, which is of technological importance for the control of air pollution.
    Materialart: Digitale Medien
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  • 9
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 49 (1999), S. 321-326 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Headspace analysis ; Open-tubular trap ; Very thick film column
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An open-tubular trap with a very thick film was studied for “full on-line” headspace capillary gas chromatography, and was used as an enrichment trap for headspace sampling. The preparation of the open-tubular column with up to an 80 μm thick film, by combining both static and dynamic coating, is described in detail. The break-through volume for the open-tubular trap of different film thickness, as the loading capacity for HS sampling, does not increase linearly in proportion to the film thickness. A study of the difference between a packed adsorbent trap and an open-tubular trap shows that HS capillary GC with open-tubular trap loses less of the retention capacity, has better resolution ability and higher recovery. By independently and rapidly heating the open-tubular trap, the GC peaks may have higher resolution. Examples of successful analyses, by the opentubular trap with “full on-line” HS capillary GC, include trace aromatic hydrocarbon (1 ppm-100 ppm) in polybutadiene-styrene rubber and trace alcohol and acrylic esters (10 ppm–1000 ppm) in polyacrylate hydrous emulsion.
    Materialart: Digitale Medien
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  • 10
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 49 (1999), S. 385-390 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Structure correlations ; Polycyclic aromatic hydrocarbons ; Polychlorinated biphenyls ; Polychlorinated pesticides
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A composite chromatographic retention index system has been developed for identifying polycyclic aromatic hydrocarbons, polychlorinated biphenyls and polychlorinated pesticides. When retention indices and thermodynamic data of polycyclic aromatic hydrocarbons on 5% phenylmethylsiloxane stationary phase were compared with those obtained on polydimethylsiloxane a correlation was found between retention and electronic properties. Determination and quantitation of individual contaminants in water and sediment samples from Lake Mecoacán were achieved by capillary gas chromatography with flame ionization and electrocapture detection.
    Materialart: Digitale Medien
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  • 11
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 49 (1999), S. 268-272 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Mass spectrometry ; Analytical pyrolysis ; Chinese art objects ; Mercury analysis
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A few samples of polychrome Chinese archaeological objects of art have undergone analytical pyrolysis coupled with GC-MS to evaluated the possibility of contemporary characterization of the pigments as well as the organic media used. The red pigment cinnabar (HgS) is easily media used. The red pigment cinnabar (HgS) is easily detected, whereas in the case of organic components positive results are only found where the matrices are resistant to archaeological environmental conditions.
    Materialart: Digitale Medien
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  • 12
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Supercritical fluid chromatography ; Solvating gas chromatography ; Polybutadiene coated zirconia ; CO2 mobile phase
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary In this paper, practical considerations of column efficiency, separation speed, thermal stability, and column polarity of capillary columns packed with polybutadiene-coated zirconia were investigated under solvating gas chromatography (SGC) conditions using carbon dioxide as mobile phase. When compared with results obtained from conventional porous octadecyl obtained from conventional porous octadecyl bonded silica (ODS) particles, PBD-zirconia particles produced greater change in mobile phase linear velocity with pressure than conventional ODS particles under the same conditions. The maximum plate number per second (Nt) obtained with a 30 cm PBD-zirconia column was approximately 1.5 times higher than that obtained with an ODS column at 100 °C. Therefore, the PBD-zirconia phase is more suitable for fast separations than conventional ODS particles in SGC. Maximum plate numbers per meter of 76,900 and 63,300 were obtained using a 57 cm×250 μm i.d. fused silica capillary column packed with 3 μm PBD-zirconia at 50 °C and 100 °C, respectively. The PBD-zirconia phase was stable at temperatures up to 320 °C under SGC conditions using carbon dioxide as mobile phase. Polarizable aromatic compounds and low molecular weight ketones and aldehydes were eluted with symmetrical peaks from a 10 cm column packed with 3 μm PBD-zirconia. Zirconia phases with greater inertness are required for the analysis of more polar compounds by SGC.
    Materialart: Digitale Medien
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  • 13
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 49 (1999), S. 509-512 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Homologous series ; Retention times
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary It is shown how to estimate the retention times of homologous series members in linear temperature programmed gas chromatography with the aid of a spread-sheet. Both the ease of estimation and the accuracy of the estimation depend on whether the homologue is eluted during the rising portion of the temperature program or the hold time at the end, and also on whether the homologous series is eluted from one injection or a number of injections. When all members of the series elute in the one chromatographic run the percentage standard deviation of the predicted retention times from the experimental retention times is 0.1. When members of the series elute in different chromatographic runs, the percentage standard deviation of predicted times from experimental times is 0.6, compared with an experimental percentage standard deviation for replicates of 0.5.
    Materialart: Digitale Medien
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  • 14
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 49 (1999), S. 686-690 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Solid-phase microextraction ; Fibre coating ; Volatile organic compounds ; Semi-volatile organic compounds
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The efficiency of direct solid-phase microextraction (SPME) was determined for 27 selected volatile and semivolatile organic compounds (BTEX, chloro- and bromobenzenes, chlorinated pesticides and PCBs). The fibres used were 7μm polydimethylsiloxane (PDMS), 30μm PDMS, 100μm PDMS, 65μm PDMS-divinylbenzene, 85μm polyacrylate, 65μm Carbowax-divinylbenzene, 75μm Carboxen-PDMS and a new 65μm C8 fibre. Extraction yields for these compounds were calculated under standardised conditions: 75μm Carboxen-PDMS was found to be the most efficient fibre for compounds with low boiling points. Although 65μm C8 can be used for extraction of all compounds studied, in no one case is it the most effective coating. 100μm PDMS and the more polar coatings can be used for a broad range of compounds, whereas application of 7μm and 30μm PDMS cannot be recommended. Inter-fibre comparison revealed significant differences between three different Carboxen-PDMS fibres. The results enable suitable coatings to be chosen for each of the 27 compounds and for substances with similar properties.
    Materialart: Digitale Medien
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  • 15
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Cisplatin determination ; Blood analysis
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A capillary gas chromatographic method is described for the determination of cisplatin based on the complexation of platinum(II) with bis(isovalerylacetone) ethylenediimine (H2IVA2en) and extraction in chloroform. The chromatography was carried out on a BP1 or a BP5 column with an FID. Copper(II), nickel (II) and palladium(II) separated completely and did not affect the determination of platinum(II). The method was applied of the determination of cisplatin in a pharmaceutical preparation and blood samples of cancer patients after infusion of cisplatin. The amounts of cisplatin in blood were found to be within 246–283 ng mL−1 with a C.V. of 2.35–4.26%.
    Materialart: Digitale Medien
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  • 16
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 49 (1999), S. 273-280 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Complexation stationary phases ; Bonding metal complexes ; Capillary columns
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The use of polysiloxanes with cyano or thiol groups as stationary phases for complexation gas chromatography is discussed. The polymers were obtained via polycondensation followed by polymerisation of the corresponding dichloro- or dimethoxy-silanes. Both the phases were modified by bonding transition metal chlorides with were modified by bonding transition metal chlorides with cyano (CuCl2 or CoCl2) and thiol groups (NiCl2 or CoCl2). The phases were examined in order to determine their application to the analysis of ethers, thioethers and ketones. Due to the presence of lone electron pairs on oxygen or sulphur atoms, the compounds should be capable of specific interacting with the electron-withdrawing centre of the liquid stationary phases. A number of retention parameters (retention indices, molecular retention indices and specific retention volume) were determined, which allowed characterisation of specific interactions between the bonded metal and the compound analysed. The results also enabled assessment of the influence of the structure of the compounds on their retention. The measurements were also carried out for the phases with free SH and CN groups as reference phases. The work demonstrates that the phases obtained may be useful for effective separations.
    Materialart: Digitale Medien
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  • 17
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Average column pressure ; Average column flow ; Specific retention volume ; Distribution coefficient
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A systematic derivation of corresponding equations shows that averaging the pressure and the flow rate of the mobile phase in a gas chromatographic column over the column length and over the time that an unretained component resides in the column, requires the use of three different compressibility correction factors,j 2 1 ,j 3 2 , andj 4 3 . When multiplied by the adjusted retention volume,V R-VM, the Martin and James mobile phase compressibility correction factorj 3 2 , only, produces the value of specific retention volume,V g T , which is connected unambiguously with the thermodynamic phase distribution coefficient,K, of the sorbate.
    Materialart: Digitale Medien
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  • 18
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 49 (1999), S. 513-519 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Solid phase microextraction ; Open cap vials ; Volatile compounds (BTEX) ; Water matrix
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The testing of open cap vials in headspace solid-phase microextraction combined with capillary gas chromatography is reported. The losses of volatile analytes from such vials were analyzed theoretically and investigated experimentally. The benzene, toluene, ethylbenzene, and xylene isomers spiked in water were used as model compounds. Extraction yields and precision obtained under optimized experimental conditions as exposure time, desorption time and temperature were compared applying vials with open caps or sealed with teflon lined septa.
    Materialart: Digitale Medien
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  • 19
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 49 (1999), S. 567-571 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Mixed stationary phase ; Calixarenes ; Crown ethers ; Cyclodextrins
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Mixed stationary phases containing of 25,27-dibutoxy-5,11,17,23-tetra-tert-butyl-26,28-diundecenyloxy calix [4]arene (C[4]B)+ω-undecylomethyl-18-crown-6 polysiloxane (PSO-11-18-C-6) and C[4]B polysiloxane (PSO-C[4]B)+permethyl-β-cyclodextrin (PM-β-CD) were investigated in capillary gas chromatography. By comparing their selectivity for positional isomers with that of the corresponding individual pure stationary phases, synergistic effects were found.
    Materialart: Digitale Medien
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  • 20
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Electron capture detector ; Anti-picornaviral agent in dog serum ; Enteroviruses
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A gas chromatographic assay for the determination of SCH 48973, a potent broad spectrum anti-picornaviral agent, was developed and validated in dog serum. The method involved extraction with organic solvent followed by separation on a capillary column (DB-1) with quantitation by an electron-capture detector. The method was sensitive with a limit of quantitation of 10 ng mL−1. The linearity of the method was satisfactory as indicated by correlation coefficients of 〉0.999 and visual examination of the calibration curves. The method was precise with a coefficient of variation ranging from 2.3 to 13.2% and accurate with a bias ranging from −9.1 to 7.9%. Moreover, SCH 48973 was stable in dog serum after being subjected to three freeze-thaw cycles. The assay was shown to be sensitive, specific, accurate and precise, and reliable for use in pharmacokinetic or toxicokinetic studies.
    Materialart: Digitale Medien
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  • 21
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 49 (1999), S. 399-405 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Solid phase adsorption ; Supercritical fluid extraction ; Sewage ; Organic pollutants
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Analytical methods have been developed for the determination of organic pollutants of intermediate polarity in sewage. Water samples are first passed through a solid phase adsorption cartridge. The analytes are then extracted from the absorbent with supercritical CO2 into a small volume of trapping solvent. Finally, the extracts are analyzed directly by capillary gas chromatography and gas chromatography-mass spectrometer. The various parameters (pressure, temperature, type and concentration of modifiers, trapping solvent, flow rate and volume of supercritical fluid and equilibrium time) influencing the efficiency of extraction were studied. Extraction efficiencies for the test compounds are 〉70%, and relative standard deviations are 〈4.6% (n=3). The methods established were applied to the analysis of sewage at the Lanzhou Wastewater Treatment Plant, China. 66 organic pollutants were detected, of which 15 compounds appeared in the list of priority pollutants suggested by the US EPA.
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  • 22
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 24-28 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; ECD ; Micro-ECD ; GC detector ; organochlorine pesticides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A new ECD, the HP 6890 Series Micro-ECD, was designed to address inherent deficiencies in classical electron capture detectors (ECD), especially with respect to sensitivity, linearity, dynamic range, and ruggedness. Several novel technologies were incorporated in the totally new design and were refined through practical testing and user feedback. Validation of the micro-ECD performance was accomplished through side-by-side testing of the Micro-ECD with previous ECDs following US EPA Contract Laboratory Program methods for pesticides and PCBs. In addition, extensive interviews were conducted with early users of the Micro-ECD who also had experience with other designs running a variety of ECD methods. The design and resulting performance improvements are described.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 23
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 181-182 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; microwave induced emission spectrometry ; speciation ; mercury ; SPME, headspace SPME ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 24
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 294-296 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; capillary ; fused silica ; rotenone ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: No abstract
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 25
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 303-304 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; food analysis ; pesticide residues ; thiabendazole ; imazalil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 26
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 395-402 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; pulsed splitless injection ; pesticide residues ; matrix effects ; retention gap ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The applicability of pulsed splitless injection to the gas chromatographic analysis of pesticide residues in fruit and vegetables has been evaluated. 22 pesticides belonging to different chemical classes, including those known to be liable to matrix induced response enhancement, were selected for the study. The parameters of pressure pulse have been tested for optimum performance of injection. Application of the pressure pulse was found to decrease matrix effects during analyses of real samples. Further decline of matrix effects was obtained using higher sample injection volumes. The installation of a deactivated retention gap was necessary to obtain good peak shapes with injection volumes exceeding 1 μL of sample. Up to 4 μL was then injected without peak distortion and consequent loss of resolution. Using 4 μL pulsed splitless injection, matrix effects were almost completely eliminated even at very low concentration levels of analytes. The highest matrix effects observed for tested compounds at the lowest concentration level tested were in the range of 110-122%.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 27
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 565-588 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Kovats retention index ; vapor pressure ; boiling point ; Wilson activity coefficient ; binary phase diagrams ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Non-ideal mixing in a dimethylsilicone stationary phase is modeled according to the Wilson activity coefficient. Pure liquid vapor pressures of alkylated compound series are calculated from capillary GLC retention with the functional group heat of solution in a polymer solvent. The new method uses the Kovats index, molar mass, and functional group to determine the bubble line of a compound. Boiling points at reduced and normal pressure are compared to literature values of 194 gasoline components. An unlike molecular pair interaction parameter is derived, using only bubble line data of the pure liquids. Binary phase diagrams are constructed and compared to vapor liquid equilibrium data.
    Zusätzliches Material: 22 Ill.
    Materialart: Digitale Medien
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  • 28
    Digitale Medien
    Digitale Medien
    Springer
    Urological research 7 (1979), S. 227-234 
    ISSN: 1434-0879
    Schlagwort(e): Oxalic acid ; Acid metabolites ; Urine ; Back-flushing ; Gas chromatography
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Summary The known methods of oxalic acid determination are not suitable for reliable, rapid and economical routine analysis. A rapid gas chromatographic method has been developed which dispenses with separation operations and measures oxalic acid as a diethylester by means of back-flushing, and using malonic acid as an internal standard. One determination can be conducted within 6 to 8 min. and preparation of the specimen takes about the same amount of time. If the gas chromatographic conditions are changed and more time is permitted for analysis, numerous other extractable acidic metabolites can also be determined.
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  • 29
    Digitale Medien
    Digitale Medien
    Springer
    International archives of occupational and environmental health 42 (1979), S. 257-268 
    ISSN: 1432-1246
    Schlagwort(e): Phenol ; Cresols ; Gas chromatography ; High pressure liquid chromatography ; Photometry ; Urine ; Phenol ; Kresole ; Gaschromatographie ; Hochdruckflüssigkeitschromatographie ; Photometrie ; Harn
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Beschreibung / Inhaltsverzeichnis: Zusammenfassung Eine gaschromatographische und eine hochdruckflüssigkeitschromatographische Methode zur Bestimmung von Phenol und Kresolen im Harn wind beschrieben. Phenol wind in beiden Fällen selektiv erfaßt. o-, m- und p-Kresol wird beschrieben. Phenol wind in beiden Fällen selektiv erfaßt. o-, m- und p-Kresol werden hochdruckflüssigkeitschromatographisch nicht getrennt. Gaschromatographisch gelingt die Abtrennung von o-Kresol. Aufgrund der speziellen Probenaufbereitung sind beide Verfahren sehr empfindlich. Die Nachweisgrenzen liegen zwischen 0,2 und 1,3 mg/l. 24-h-Harne eines Normalkollektivs (n = 30) werden untersucht (xPhenol = 4,6 mg/l; xp-Kresol = 45,7 bzw. 52,6 mg/l). Die Ergebnisse werden mit denen eines photometrischen Verfahrens verglichen.
    Notizen: Summary Gas chromatographic and high pressure liquid chromatographic methods for the determination of phenol and cresols in urine are described. In both cases phenol is determined specifically; o-, m- und p-cresols are not separated by high pressure liquid chromatography. However, o-cresole is separated by gas chromatography. On account of the special preparation of urine samples both methods are very sensitive. The detection limits lie between 0.2 and 1.3 mg/l. 24-h samples of normal urines (n = 30) are analysed (xphenol = 4.6 mg/l; xp-cresol = 45.7 mg/l, respectively 52.6 mg/l). These results are compared with those of a photometric method.
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  • 30
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 12 (1979), S. 790-798 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Dead-time ; log ts=f(C) ; Retention index calculation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: Zusammenfassung In der vorliegenden Arbeit wird eine Methode zur Retentionsindex-Bestimmung beschrieben, die von einem kubischen Zusammenhang zwischen Bruttoretentionszeit-Differenzen der Referenzhomologen und der Kohlenstoffzahl ausgeht. Hieraus ergeben sich direkt die Nettoretentionszeiten. Der Fehler der Totzeitbestimmung entfällt bei dieser Methode. Mit den so gewonnenen Nettoretentionszeiten erhält man über einen kubischen Zusammenhang zwischen 1g ts=f(C) die Retentionsindices. Extrapolationen und Interpolationen sind über 300 Retentionsindexeinheiten mit einem mittleren Fehler von ±0,02 Retentionsindexeinheiten möglich. Das Verfahren bietet sich für eine automatische Berechnung der I-Werte mittels on-line-Datenverarbeitung an.
    Notizen: Summary The method for the calculation of retention indices described here is based on a third order relationship between the logarithm of differences of unadjusted retention times of homologues and the carbon number. From this adjusted retention times are directly calculated. A determination of the dead-time is not necessary thus avoiding the errors connected with this factor. A cubic equation for the logarithm of the adjusted retention time lg ts as a function of carbon number Cn is used for the retention index calculation. Extrapolations and interpolations can be done over a range of 300 index units with an average deviation of ±0.02 i.u.. The method offers the possibility of an automated on-line calculation of retention indices by computer merely on the basis of unadjusted retention times.
    Materialart: Digitale Medien
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  • 31
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 12 (1979), S. 523-526 
    ISSN: 1612-1112
    Schlagwort(e): Amantadine ; Gas chromatography ; Gas chromatography-mass spectrometry ; Biochemical analysis
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A simple, selective and sensitive method for the quantitation of amantadine in biological samples is described. After extraction from biological samples using a two-step procedure, amantadine is quantitatively converted into its isothiocyanate (NCS) derivative by treatment with carbon disulfide and then determined quantitatively using isobaric compounds, p-methoxyphenyl-ethylamine-NCS or N-acetylamantadine as external standards. The applicability of this method is illustrated by determining plasma levels of amantadine for pharmacokinetic studies and levels in dialysate samples of amantadine treated patients who were on dialysis machines.
    Materialart: Digitale Medien
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  • 32
    ISSN: 1612-1112
    Schlagwort(e): Polynuclear aromatic hydrocarbons ; Retention index ; Gas chromatography
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An equation has been derived allowing to predict retention index values on nematic phases from computable parameters and sizes of the molecules of polycyclic aromatic hydrocarbons. Another equation, which has also been derived, allows to determine the shape parameter of a molecule from chromatographic data.
    Materialart: Digitale Medien
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  • 33
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 12 (1979), S. 583-586 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Clinical analysis ; Meningitis detection
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Gas liquid chromatography was performed on cerebrospinal fluid from cases of purulent meningitis, and control subject. A relatively constant pattern of peaks was obtained in all samples. Four constant peaks in the chromatogram frequently showed a significant increase in purulent meningitis but not in aseptic meningitis or control cases. There was a gradual return to normal levels during clinical improvement, usually within 5–6 days of appropriate therapy. In one case of recurrent meningitis, an increase in the peaks was noted with relapse. Identification of the compounds represented by these peaks may provide further information regarding diagnosis, prognosis and pathogenesis of meningitis.
    Materialart: Digitale Medien
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  • 34
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 12 (1979), S. 168-170 
    ISSN: 1612-1112
    Schlagwort(e): Acid catalyzed esterification ; Amino acids ; Fatty acids ; Gas chromatography ; Isopropyl esters
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Acid-catalyzed esterification of carboxyl groups with acetyl chloride in isopropanol is investigated. Yields are equivalent to those obtained with reagent prepared conventionally by bubbling gaseous hydrogen chloride into isopropanol. The preparation of the former reagent is less time consuming and no special equipment is needed. The procedure is applicable for other alcohols as well.
    Materialart: Digitale Medien
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  • 35
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 12 (1979), S. 533-538 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Sorbents: liquid phases, supports, adsorbents ; Thermodynamical classification ; Polarity and selectivity
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Equations modifying Rohrschneider's relationship between ΔI and thermodynamical characteristics values are derived. Polarity in chromatography is discussed as a possibility of stationary phases or absorbents to enter into intermolecular interactions and is determined on the basis of the partial molar free energies of solution (ΔG) of six test substances. A simple method for the calculation of stationary phase polarity in terms of ΔG from retention indices and McReynolds constants is given. Equations are presented for the calculation of stationary phase selectivity utilizing ΔG data tabulated for selected test substances. The thermodynamical basis of selecting a reference phase for a unified system expressing the selectivity of stationary phases which can also be applied for adsorbents is suggested. The energy equivalent to an index unit, ΔGi.u., is discussed.
    Materialart: Digitale Medien
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  • 36
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 12 (1979), S. 803-807 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Ionization detector ; High frequency discharge ; Specific or no specific detection ; Gas adsorption (by flues)
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The response of a high frequency ionization detector according to various parameters: voltage, tuning capacitance, feed-back capacitance, space between the electrodes and direct flux-plasma distance is studied. The characteristic measure of v in accordance to high voltage for various mixtures of carrier gas argon-nitrogen gives a maximum which demonstrates that specific automatic analyses of oxygen, krypton and methane are possible with concentrations in the order of ppb. Complete adsorption of 0.8 ppb of methane by a flue of 120 cm in tube 2×4 mm at 50°C after twentieth recycling is essential.
    Materialart: Digitale Medien
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  • 37
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 12 (1979), S. 530-532 
    ISSN: 1612-1112
    Schlagwort(e): Hexetidine ; Triamine ; Gas chromatography ; On-column interactions
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Gas chromatography was used for the direct assay of hexetidine and triamine in a pharmaceutical formulation. During this work we came across a strong oncolumn interaction, in such a way that the GLC retention, selectivity and response parameters were seriously modified relative to the injections of hexetidine and triamine standard solutions. The interaction was traced to the coinjected hydrochloride form of a major component of the sample and in practical terms points to the potential quantitation errors that may be associated to similar systems.
    Materialart: Digitale Medien
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  • 38
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 12 (1979), S. 665-671 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Retention index ; Multiple correlation ; Molecular properties ; Prediction
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: Zusammenfassung Ein auf der linearen, multiplen Korrelation basierendes Verfahren wird vorgestellt, das es gestattet, den Retentionsindex von Substanzen in der gaschromatographischen Trennung aus einem Satz Säulenkonstanten und drei bis vier Substanzeigenschaften zu berechnen. Der Fehler der Berechnung liegt unter 2%. Der Ansatz wurde für isothermes und temperaturprogrammiertes Arbeiten getestet.
    Notizen: Summary A method based on linear multiple correlation is introduced allowing the calculation of gas chromatographic retention indices from a set of column constants and three to four physical properties of the solute. The error is less than 2%. The formulation has been tested for isothermal and temperature programmed working conditions.
    Materialart: Digitale Medien
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  • 39
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Porous polymer supports ; Retention behaviour-effect of support
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The gas chromatographic behaviour of a series of compounds of different polarity on columns of Ethofat 60/25 on Chromosorb P HMDS (an inactive support) and Chromosorb 101 (an active support) was investigated. To observe how the support influences the chromatographic process, we separated the contribution to the retention volume of the interaction phenomena associated with the stationary phase, the solid support and the corresponding interfaces. In some cases the Chromosorb 101 exerts an influence on the process even with high percentages (〉10%) of stationary phase. The values of the experimental partition constants of a series of compounds and the factors that contribute to adsorption on these columns are calculated.
    Materialart: Digitale Medien
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  • 40
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 12 (1979), S. 733-736 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Gas volume, influence of ; Preconcentration ; Wine headspace analysis
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Examination was made of the changes in composition of aroma volatiles trapped on Chromosorb 105 during dynamic headspace sampling of aged wine. Collections from different gas volumes were analysed and a subsequent collection made. It was demonstrated that analyses of headspace collections containing reduced quantities of the more volatile and more, hydrophobic compounds could aid in the identification and quantitative determination of alcoholic beverage components.
    Materialart: Digitale Medien
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  • 41
    ISSN: 1612-1112
    Schlagwort(e): Inclusion compound ; Urea-cetylalcohol adduct ; Gas chromatography ; Clathration process ; Phase changes
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Phase changes in urea-cetyl alcohol inclusion compounds prepared by various methods were monitored gas chromatographically. The decomposition temperature interval and the presence of the free components could be found from the temperature dependence of the retention data. Study of the clathration process yielded facts that can be used in the preparation of this type of inclusion compound.
    Materialart: Digitale Medien
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  • 42
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 12 (1979), S. 265-270 
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Columns: open tubular ; Columns: capillary ; Efficiency ; Mean specific plate number
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A new parameter, the mean specific plate number, is proposed for assessing the efficiency of support coated open tubular (SCOT) and wall coated open tubular (WCOT) columns and for comparing the efficiency of different open tubular columns. It has the advantage over most previously used parameters in that it has only a small dependence on the partition ratio and it allows for the column diameter. A graphical presentation is given of the maximum theoretical mean specific plate number as a function of the partition ratio for SCOT columns having a range of relative porous layer thicknesses and for WCOT columns with a range of phase ratios. This presentation permits ready visual comparison of the potential efficiency of different columns and enables a simple evaluation of the percentage utilization of theoretical efficiency from experimentally determined values of the maximum mean specific plate number. For a given column the percentage utilization of theoretical efficiency at optimum average gas velocity and that at optimum practical gas velocity or at a higher average gas velocity are shown to be equal provided that corrections for column pressure drop are made.
    Materialart: Digitale Medien
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  • 43
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 12 (1979), S. 463-466 
    ISSN: 1612-1112
    Schlagwort(e): Hydrothermal treatment of Porasils ; Adsorption properties ; Gas chromatography
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A simple modification was employed by thermal or hydrothermal treatment of silica gel (Porasil). In this way chromatographic materials with advantageous properties were prepared. The changes of the adsorbent under different thermal and hydrothermal treatment were studied in more detail. The experimental results show that under controlled conditions material with required chromatographic properties can be prepared.
    Materialart: Digitale Medien
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  • 44
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Ethanolamines ; Ethylene glycols ; Porapak Q
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary GC separation of pure ethanolamines as well as mixtures with ethylene glycols, obtained from a real technological process is achived using Porapak Q coated with 15% Carbowax 20M. Symmetrical peaks, satisfactory resolution, and reasonable analysis times are obtained. The proposed method is suitable for a convenient, correct and express routine analysis.
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  • 45
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 12 (1979), S. 509-515 
    ISSN: 1612-1112
    Schlagwort(e): Optimization ; Carrier gas velocity ; Gas chromatography ; Influence of temperature on optimum velocity
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The selection of the average linear carrier gas velocity in the analysis of a multicomponent mixture under isothermal and programmed-temperature conditions is discussed. It is shown that one shouls always select a velocity which is at least equal but preferably higher than the optimum average gas velocity of the earliest peak at the initial column temperature.
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  • 46
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Retention index calculation ; lg ts=f(C) ; Dead-time ; Complex mixtures
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: Zusammenfassung Die bisher in der Literatur beschriebenen Verfahren zur Retentionsindex-Bestimmung beruhen auf einem linearen Zusammenhang zwischen dem Logarithmus der Nettoretentionszeit lg ts und der Kohlenstoffzahl C der n-Alkane. Wie genaue Meßwerte für Retentionszeiten zeigen, ist die Funkton lg ts=f(C) nicht streng linear. Die Krümmung des Funktionsbildes bedingt, daß lineare Regressionsmethoden, sowie auch die Methode nach Kovats, es nicht erlauben, extrapolativ sowie über weite Retentionsbereiche interpolativ I-Werte zu berechnen. In dieser Arbeit werden Retentionsindices aufgrund eines kubischen Zusammenhanges zwischen lg ts und der Kohlenstoffzahl ermittelt. Die hierzu notwendige Totzeit tm wird aus den Differenzen der Bruttoretentionszeiten der Referenzhomologen ermittelt.
    Notizen: Summary Methods of retention index calculation described in the literature have been based on a linear relationship between the logarithm of the adjusted retention times lg ts and the carbon numbers C of n-alkanes. Exact measurements of the retention times of n-alkanes show that the relationship lg ts=f(C) is in fact not strictly linear. Correct extrapolative or interpolative calculations of retention indices over a wide retention range are therefore impossible when using the original formula as given by Kovats or methods based on a linear regression concept. The method of retention index calculation presented here is based on a cubic relationship between lg ts and carbon number allowing extrapolative or interpolative calculations. The hold-up time (tm) is calculated on the basis of differences of retention times of the reference homologues.
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  • 47
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 12 (1979), S. 89-94 
    ISSN: 1612-1112
    Schlagwort(e): Determination of HCl ; Derivatization ; Trace analysis ; Gas chromatography
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Beschreibung / Inhaltsverzeichnis: Zusammenfassung In der vorliegenden Arbeit wird die Möglichkeit untersucht, kleine Mengen HCl durch derivatisierung mit 7-Oxabicyclo-(4.1.0)-heptan und anschließendem gas-chromatographischen Nachweis des Reaktionsproduktes 2-Chlorcyclohexanol zu bestimmen. Die Nachweisgrenze für das Produkt der Derivatisierung (2-Chlorcyclohexanol) entspricht 2 pg HCl. Durch verschiedene Probleme, die im Rahmen dieser Arbeit diskutiert werden, wird diese Nachweisgrenze in der Praxis nicht erreicht. Es zeigt sich jedoch, daß HCl-Konzentrationen im Bereich von ppm (bzw. HCl-Mengen〈1 μg) ohne weiteres zu bestimmen sind. Die Möglichkeiten dieser Analysenmethode werden diskutiert.
    Notizen: Summary This paper the possibility of determining small quantities of HCl by derivatization with 7-oxabicyclo-(4.1.0)-heptane and subsequent gas chromatographic identification of the reaction product 2-chlorocyclohexanol is examined. The detection limit for the derivative (2-chlorocyclohexanol) is equivalent to 2 pg HCl. On account of various problems, discussed in the paper, this detection limit is not achieved in practice. It is nevertheless apparent that concentrations of HCl in the ppm-region (quantities of HCl〈1 μg) can be determined without difficulty. The scope for this method of analysis is disscussed.
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  • 48
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Columns: open tubular ; Columns: capillary ; Columns: capillary: comparison ; Efficiency
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A detailed comparison is given of the various equations derived by Golay and that derived by Hawkes for assessing the theoretical efficiency of SCOT columns. The terms in these equations which describe the resistance to mass transfer in both the gas phase and in the liquid phase are given in a form which permits the equations to be compared directly. A numerical comparison is then made of the potential efficiency predicted by the different equations for five partition ratio values for a set of nine idealized SCOT columns with a wide range of porous layer thickness and liquid loading. The potential column efficiencies are expressed in terms of the maximum theoretical mean specific plate number. It is shown that appreciable differences occur between the theoretical efficiencies given by the different equations when the porous layer thickness and liquid loading are high, but these differences are small for most of the columns used in practice.
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  • 49
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 288-292 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Stationary phases, polar, gum type ; For temperatures up to 300°C ; For most of the common classes of organic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Most of the common classes of organic compounds chromatograph normally on Superoxes. There is no tailing or adverse effect from excessively different activity different activity coefficients. Superoxes are therefore universal phases for gas chromatography. This is also expressed by a wide useful temperature range from ∼50° to ∼300°. High MW Superox-4 has a MAOT about 20° higher than the lower MW Superox-0.1. Several applications illustrating the versatility of Superox phases in (GC)2 are presented.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
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  • 50
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 429-435 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Surface roughening by diatomaceous support (5 micron particles deposition) ; Organic glue (polar polymethacrylate acetate) used as intermediate material ; Reproducibility and durability of capillaries discussed ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A technique for adhesion of fine particles (ca. 5 μ) of the 405 white diatomaceous support on the inner wall of glass tube with organic glue [poly (diethylaminoethyl methacrylate) acetate] is described. The coated tube was drawn to capillary column by using a machine designed according to Desty's. The capillary column was then coated with stationary phase (such as squaiane, QF-1, Dexsil 300, PEG 20 M, OV-1, SE 30 and etc.) by the conventional dynamic or static method. This preparation method has proved easy to duplicate and is simple. The coating efficiency (UTE %) is within 60-90. The theoretical plate number per meter of an SE 30 column is about 4000, and per meter of a PEG 20 M column is about 2500. The columns thus prepared have been successfully used to analyze petroleum hydrocarbons, essential oils, petrochemicals, pheromone, steroid metabolites and others.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 51
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 635-636 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Cyclandelate quantitation ; In plasma. No sylilation needed ; Analysis within 16 min, range 5-50 ng/mikroliter ; Correlation coeff. 0.996 (N=6) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 52
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 177-183 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary ; Injection by tailored capsule-insertion technique ; Critical comparison with split-injection technique ; Competitive with best-known systems ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A capsule-insertion system tailored to the needs of capillary gas chromatography is described. It provides the basis for a truly quantitative and improved qualitative approach to open tubular capillary GLC. The advantages of the system lie in its simplicity of handling and in the possibility of using relatively low injection temperatures, thus reducing the risks to thermally unstable samples.The observed high efficiencies characterizing this capillary GLC capsule technique allow full advantage to be taken of the operating capacity of the superior capillary columns to give a performance competitive with the best known split-injection systems.
    Zusätzliches Material: 11 Ill.
    Materialart: Digitale Medien
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  • 53
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 254-254 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Hydrodesulphurization products elution ; Room temperature two-column operation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Materialart: Digitale Medien
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  • 54
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 283-287 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Sampling technique ; Semi-automation of head space sampling ; Application to water pollution, coffee aroma, light hydrocarbons in crude oil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Head space GC using a special electropneumatic sampling system works well in combination with glass capillaries. Because a homogenous gas mixture is already present most problems inherent with inlet splitters are thus avoided. In cases where the high vapor pressure of the sample can cause problems with the pressure controlled sampling system, the use of narrow bore glass capillaries provides the necessary inlet pressure. The use of this powerful and convenient analytical tool for water pollution analysis, flavour analysis and the analysis of volatiles in crude oil samples is shown by examples.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 55
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 319-323 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Mobile phase flow programming ; Comparison with temperature programming ; Short capillaries offer considerable shorter analysis time when flow programmed ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The technique of programming the carrier gas flow rate in gas chromatography, especially in connection with the use of capillary columns shorter than 10 m can significantly accelerate GC analyses. Equations for calculation of the parameters of the exponential flow function and retention data are described. The effects of flow programming in a short capillary column are shown in a few chromatograms. Different programming rates are tested and compared with temperature programming.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 56
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 297-302 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Surface roughening ; Amorphous silica ; Deactivation ; Column performance ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A new method for the preparation of wall-coated glass capillary columns after surface roughening by means of amorphous silica is described. After the glass capillary has been leached, a small quantity of amorphous silica is deposited evenly on the inner surface. This is done by passing a plug of dilute water glass through the capillary, followed by a flow of gaseous hydrochloric acid. The roughened surface is stabilized, deactivated and finally coated.This paper furnishes details of the technique and information about the performance of a number of columns prepared by the method.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 57
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 324-328 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Theory in contrast to traditional approaches ; Very practical formulas for peak width, maximum load, concentration in mobile phase ; Optimizing procedure for trace analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: In contrast to traditional theoretical approaches by calculation of (nonexistent) theoretical plates, a unified theory of gas chromatography as given by a definition of the resolution analogue to methods in signal processing or spectroscopy using the well-known Kovacz indices as fundamental scale. A derivation of the thusly defined resolution from basic physical principles yields very practical formulae for peak width, maximum load, substance flow in peak maximum, concentration of substance in the carrier gas and other interesting parameters in dependence of capillary diameter, capillary length, film thickness, carrier gas speed, viscosities etc. Diagrams show favourite conditions for detectors responding on absolute substance flow (e.g. FID) or on concentrations.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 58
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 400-404 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Low temperature plasma etching ; Polymer film on the inner surface from organosilicone monomer ; Flexibility of this new method discussed ; Discharge chamber described ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A novel method is described for the preparation of stable glass capillary columns (glass open tubular columns), including the etching and formation of a polymer film on the inner glass capillary surfaces. The approach used here is based on low-temperature plasma etching and polymerization. Under the influence of a field of radio frequency discharge, low pressure gases of fluoric compounds, introduced into the glass capillary tube, generate excited fluorine radicals which etch the inner surface. The plasma of organosilicone monomer in the glass capillary yields a uniform polymerized film on the inner surface. The resultant material functions as a good stationary phase for glass capillary gas chromatography (GC2). The inner surfaces treated with such a plasma, can be studied by means of a scanning electron microscope (SEM). The flexibility of this method permits the use of various stationary phases and surface modification.
    Zusätzliches Material: 8 Ill.
    Materialart: Digitale Medien
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  • 59
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 416-422 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; SECAT-technique=stepless fine tuning of capillary selectivity by serial column temperature optimization ; Exponential influence of temperature on selectivity over a wide range found ; SECAT-technique ready for automation of column adjustment on sample composition polarity ; Instrumental and methodological details for primitive self made solution given ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: GC, including capillary GC, is rather inflexible, if a certain column length and stationary phase has been fixed for a given analytical problem. If the sample composition changes, one often has to change the column length and/or stationary phase, at least when something like optimum analytical conditions are needed. Temperature changes (or heating rates) can change the selectivity of a given column only within very limited ranges, due to the exponential effect of temperature on retention time. By serial coupling two chemically different capillaries, each run at another temperature, even the slightest changes of these two temperature values have a dramatic effect on the selectivity of the system for polar substances. We call this technique the SECAT mode of GC. Results are reported as retention index shifts, dependent on SECAT temperature data. This technique can in future easily be automated, thus enabling the analyst, for polar sample analysis, to adjust a given chroma-tographic system to his specific sample composition without touching the instrument.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 60
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 487-496 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Comparison of FID, ECD, FPD for detection limit. linearity, peak shape etc. ; Practical results for pesticide residue and coal hydrogenation products given ; Concentration dependent detectors in capillary GC interesting, when optimized ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A comparison of the characteristics and Performance of the flame ionization, electron capture, and flame photometric detectors with capillary columns is described. Factors which may affect the limits of detection, linearity, chromatographic peak shape, and other detector performance characteristics are discussed and compared with the results of a model derived for the behavior of concentration and mass flow-rate dependent chromatographic detectors used with capillary GC systems. Examples are given of highly complex and labile mixtures such as pesticide residues and products from coal hydrogenation.
    Zusätzliches Material: 13 Ill.
    Materialart: Digitale Medien
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  • 61
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 581-582 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Retention indices and substituent constants ; Phenols ; Polar stationary phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Tab.
    Materialart: Digitale Medien
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  • 62
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Surface deactivation, persllylation ; Discussion of variable parameters ; Suggested practical procedure ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Materialart: Digitale Medien
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  • 63
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 629-630 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary glass ; Nitrogen-specific detection ; TMSN ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 64
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 31-35 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Surface deactivation, silylation ; Inertia stable to 350° ; Free acids and bases, simultaneous injection ; On-column injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A deactivation procedure is described based on a published method using hexamethyldisilazane in the gas phase. In addition to unusually high inertia and thermostability, the method produces truly neutral columns which allow simultaneous analysis of moderately strong free acids and bases. The silylated columns show their full potential only with on-column injection. Preliminary experimental directions are given; more elaborate directions will become available after extended optimization work.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 65
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 529-530 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Requirements with respect to pressure controllers ; Design of pressure controllers ; All-metal controllers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 66
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 186-186 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Carrier gas ; Flow control by flattened tube restriction ; Fine tuning by adjustable twisting ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 67
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 187-188 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Whiskers, OV-17 ; Steroid profiling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 68
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 357-360 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Whisker production ; Violent explosion at the „ether etching“ step ; Modification of pyrex glass etching leads to more uniform whiskers in size and shaep, simple, safe ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Recent attempts to reproduce a literature method for etching of Pyrex glass capillary columns with „etching ether“ resulted in reduction of the columns to dust through a violent explosion. Although modifications of the method produced etched columns, we found that less than satisfactory results were achieved. Introduction of etching ether by simply coating the column with a thin film of the ether produced an evenly etched column with well defined whiskers. Several observations made during the etching process will also be discussed.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 69
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 361-365 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Sample preparation by pre-chromatographic reaction at the 7 microliter level ; Reproducibility of methylation and allylation of barbiturates ; Application to blood analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Pre-chromatographic reactions are no longer a necessary evil. Equipment such as the microrefluxer now allows reproducible 7-μl-reactions to be carried out in a short time. Thus multiple derivatisations can be used together with glass capillary GC for routine identifications. The method has been succesfully applied to barbiturates. Retention data of their methyl-, allyl- and benzyl-derivatives are given.Quantitative blood level determinations are briefly discussed.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 70
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 411-415 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Enantiomer amino acids separated on chirally functionalized polysiloxane phase ; McReynolds constants of chiral phase given ; HCl gas pretreatment, colloidal silicic acid deposition best wall preparation ; Racemisation tested ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Glass capillaries coated with Chirasil-Val, a chirally functionalised polysiloxane, are capable in principle of resolving all protein amino-acid enantiomers in a single run and within a short analysis time, thus allowing for example the quantitative amino acid determination by enantiomer labelling. The elution characteristics of the individual amino acids however are also dependent upon the chemical nature of the capillary wall surface, and a surface pretreatment is found to be necessary if all protein amino acids are to be analysed. Of the various methods of pretreatment tested, etching of borosilicate glass with gaseous HCl followed by deposition of colloidal silicic acid is considered to be the most suitable.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 71
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 436-440 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; „bo“ data (starting peak width) in valveless multidimensional operation studied ; Heart cutting, trapping, re-injection effects measured ; Band broadening caused by connections small (160 ms2) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: In order to permit valveless MDSS operation and easy column change, the hardware designed contains several connections. These can give rise to extra-column band broadening effects. In order to quantitate such effects, the packed-capillary column configuration (without trap) was used. The band broadening caused by the connections was found to be small: 120 ms2. A more practical approach was used to check the performance of the trap (re-injection) in the capillary-trap-capillary column configuration. Here the results obtained with re-injection from the trap were compared with results obtained in transfer and heart-cutting modes while the trap was heated. Re-injection was tested with n-alkanes ranging from n-C6 to n-C28. A starting peak width of 1.6 s was found.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 72
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 456-460 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary ; Theory ; Linearity between peak width and retention data ; Evaluation of GC equipment ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The linearity of the relationship between σT,t2 and (1 + k)2 is studied with the view of using it for the evaluation of GC equipment. Based on appropriate analytical expressions it is concluded that in general this relationship is not linear and that practical procedures for column evaluation should be developed that take this non-linearity into account.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 73
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 461-474 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Limitations by temperature, in trace analysis, by irreversible adsorption ; Sample capacity, separation efficiency ; Multidimensional GC advantageous ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Glass capillary gas chromatography is a high resolution separation method which allows the qualitative and quantitative analysis of even complex mixtures, which may contain many components-also isomeric-in a wide range of volatilities, polarities and concentrations.The principal limitation of gas chromatographic application is given by an insufficient volatility of the species to be separated. Elevated temperatures have to be applied if the application range is to be extended and to achieve steep peak profiles, i.e. low detection limits at high resolution. The use of elevated temperatures is limited, of course, by the temperature stability of both the solvent (stationary liquid and support) and the solutes.The problems of trace analysis for low volatility compounds at high resolution and its limitational parameters regarding sampling, separation and detection are discussed.The applicability of glass capillary columns in this field is influenced by the following parameters: tailing behaviour; irreversible adsorption of polar and decomposition of unstable solutes; thermal stability of stationary liquid (including the support deactivation); separation efficiency and sample capacity (film thickness).Multidimensional gas chromatography using capillary columns coupled either with a packed or another capilllary column for preseparations may be applied with advantage in the analysis of complex mixtures.
    Zusätzliches Material: 7 Ill.
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  • 74
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 527-528 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Leaching compared to etching ; Leaching by 20% HCI at 240°C ; Metal ions eliminated from glass surface ; Silica layer formed on leached surface ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 75
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 712-714 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Cholesteric liquid crystal phase ; Separation of geometrical isomers ; Cholesteryl cinnamate ; Insect pheromones ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 76
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 72-73 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary ; Split injection problems even at ratios 1:100 and 0.06 ml injection ; Band broadening effects, leading tail caused by reverse solvent effect for early peaks rel. to late solvent peak ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 77
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 303-311 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Overview, preparation and evaluation techniques ; Quantitation is the least satisfactory aspect of (GC)2 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The preparation of (glass) capillary columns of high quality is still not without difficulties. Six problems in this context are highlighted. Column material choice(l), glass wall modification(2) and coating(3) are considered to have reached a satisfactory level. Deactivation(4) is still in a state of flux. Quantitation(5) is the least satisfactory aspect of capillary GC. Scope expansion(6) will be helped by the introduction of new phases of high thermal stability and by the adoption of solutions exclusively applicable to capillary GC.Evaluation of (glass) capillary GC columns is a rapidly developing field. Hopefully the number and complexity of test or polarity mixtures will not expand much further and it will be possible to make a clear and generally acceptable choice.The preparation and evaluation of ever-improving capillary columns is important to an ever-widening group of chromatographers. Our opinion on selected topics in this already vast field is summarized in the following overview.
    Zusätzliches Material: 7 Ill.
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  • 78
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 405-410 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Stationary phases of polysiloxane-type degrade in acidic solution ; Several salt traces affect stability at high temperature NaCl on Duran-5O: no effect at 260°C ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A number of polysiloxanes have been shown to be sensitive to acids when dissolved in chloroform.At 26O°C polysiloxanes were found to degrade under the influence of several compounds used or produced during the preparation of glass capillary columns.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 79
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 577-578 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; support and packing production technique and device ; drying, removal of fines, silanization, solution coating, total evaporation ; in one system ; normal transport results in partial mechanical partlkel damage, causing tailing, decomposition on uncoated surfaces ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 80
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 221-224 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary ; Vapor-phase sampling ; Sample preparation, extraction by carbon dioxide under high pressure, Freon 12 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Two new sample preparation procedures that produce solvent-free extracts especially suitable for use with high resolution GC are described. One is based on Soxhlet extraction in a pressurized container that permits the use of liquid carbon dioxide as the extractant; the other utilizes refluxing difluorodichloro-methane (Freon 12) to isolate entrained volatiles from gas streams.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 81
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 216-220 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, at 25O°C ; Sampling via precolumn enrichment ; Precolumn backflush, reinjection after trapping the volatiles ; Rejection of non-volatiles ; Automation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A novel sampling system for isothermal capillary gas chromatography of medium- or low-volatility mixtures is described and test results are reported using flame ionization detection. The system features a loading and positioning chamber for glass vials which can carry a dilute sample in up to 0.2 ml of a volatile solvent. The output from the glass vaporization chamber is trapped onto a packed precolumn operated in the backflush mode. The analytes are further transferred over a wall-coated capillary trap prior to isothermal capillary GLC. Repeat-cycle operation of the sampling system requires 10 channels of a processor for time control over 5 solenoid valves and 3 static heaters. Preliminary results with long-chain n-alkanes in the submicrogram range showed no unwanted effects. The principal claim of the system is an improved rejection of non-volatiles.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 82
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 249-250 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Deactivation stable up to 35O°C ; High temperature phase ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A method of deactivating the inner surface of glass capillary columns is described, which can be used at 350°C without detoriation. A non-polar liquid phase was prepared from a commercially available liquid phase which, when coated on a glass surface, can withstand temperatures of 325°C for isothermal analysis and 350°C for temperature-programmed analysis.After deactivation, the column was coated using the static coating method. Then it was conditioned, tested and kept for 48 hours at 35O°C before being used for the analysis of a mixture of chlorinated pesticides.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 83
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 378-384 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Glass capillaries for low volatile polar natural products analysis ; Application to N-TFA-dipeptide, TMS-ribose, TMS-manno-samin, peptide sequence analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Two published procedures for glass capillary column production are applied to produce capillaries for chromatography of polar natural compounds. Soda lime glass capillaries, after leaching with aqueous HCL, are either treated with colloidal silicic acid or with barium carbonate and coated with either Silar 7CP or SE 52. A test mixture as well as polar carbohydrate and peptide mixtures are chromatographed on the different columns and their chromatographic properties are evaluated. Combined capillary gas chromatography-electron impact and chemical ionization mass spectrometry are used for identification of the peptide sequence.
    Zusätzliches Material: 8 Ill.
    Materialart: Digitale Medien
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  • 84
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 444-446 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Micropacked columns ; Sample capacity under comparable conditions forty times larger than in capillaries ; Equations given ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Equations have been derived from which the maximum sample size which may be loaded on a column without significantly affecting the performance may be calculated. It is shown that micro-packed columns can handle a sample which is as much as forty times larger than that which can be loaded onto wall-coated open tubular columns with comparable conditions.
    Materialart: Digitale Medien
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  • 85
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 481-486 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Splitting conditions for quantitative sampling investigated ; Injection amount and temperature should remain constant ; Standard deviation below 1% ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Sample inlet splitters are used in capillary column gas chromatography. We have investigated the sample band broadening in the splitter and studied reproducibility and accuracy in quantitative analysis using a simple lab-made splitter. It was found that the results were dependent upon the operating conditions such as split ratio, splitter temperature, glass wool plug, injected sample volume and solvent.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 86
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 423-428 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, nickel ; „Transevaporator“ into packed pre-column as sampling technique prior capillary described ; Application to volatile metabolite body fluid analysis for early detection of disease ; Serum and human breast milk as examples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Nickel capillary columns coated with moderately polarstationary phases such as Witconol can be used for the separation of the organic volatile fraction from biological fluids. A “transevaporator” sampling technique for the collection of the organic volatiles on glass beads from as little as 5 to 500 μl of biological fluids (e.g. urine, serum, amniotic fluid, breast milk, saliva, etc.) is described. The organic volatiles are thermally desorbed from the glass beads into a short precolumn cooled in liquid nitrogen, which overcomes the problems associated with sample introduction onto narrow-bore capillary columns. The application of the full analytical technique to problems associated with the early detection of disease is illustrated.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 87
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 441-443 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Methodological and instrumental solution of the recirculation problem ; In-line miniature switching valves used ; Column length optimization possible ; Over 3500 theoretical plates per second generated ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A multiple repass system, utilizing an in-line switching valve and suitable for use with small-bore glass open tubular columns, is described. The advantages of the system, which include higher OPGV, large plate numbers and optimization of column “length”, are discussed.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 88
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 475-480 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Photoionization detector (PID) ; Detection limit 50 to 100 pg nitrosamines at 10.2 eV ; Nitrosamine analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The use of a photoionization detector (PID) coupled to a glass capillary gas chromatography (GC2) separation system for the detection of carcinogenic nitrosamines was investigated. The components analyzed gave a linear response with a lower detection limit of 50 to 100 pg with the 10.2 eV ionization source. No detector response was obtained with an ionization energy of 9.5 eV.Chromatography of meat extracts indicated their complex molecular composition. Simple liquid chromatographic cleaning procedures significantly decreased the complexity of these samples, but not sufficiently for the accurate quantition of nitrosamine components.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 89
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 512-516 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Packed columns ; Glass transition temperatures of 3 polymers ; Polystyrene ; Poly(vinyl chloride) ; Poly(methyl methacrylate) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The glass transition temperatures, Tg, of polystyrene, poly (vinyl chloride) and poly(methyI methacrylate) have been determined from gas chromatographic measurements using n-hexane, n-heptane, meta-xylene and para-xylene solvents. The glass transition temperatures were detected on the z-shaped retention diagrams which were produced from the plot of the logarithm of the specific retention volumes of the above-mentioned solvents against the reciprocal of temperature, i.e. log Vgº vs. 1/T. The glass transition temperature is specified by the temperature where the slope of log Vgº vs. 1/T changes abruptly. The observed glass transition temperature of polystyrene produced by this technique was found to be in good agreement with those produced by other techniques such as the differential scanning colorimeter.The industrial importance of the glass transition temperature, Tg, might be due to the dramatic changes in the physical properties of the polymer, such as hardness and elasticity, which take place in the vicinity of this temperature. However, perfectly crystalline polymers do not exhibit glass transitions, because their chains are incorporated in regions of three-dimensional order, called crystallites. Completely amorphous polymers and semi-crystalline polymers usually exhibit both glass transition and melting.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 90
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 536-539 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary columns ; Photoionization detector ; Detector cell volume contribution to band broadening ; Flow rate effects on volumetric-based peak variance ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 91
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 580-580 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; support and packing production device ; drying, removal of fines, solution coatig, total evaporation ; principal virtue of the system: solvent can be recovered ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 92
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 715-719 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Sample introduction ; Direct manual operation at the capillary inlet ; Micro pipette is coupled onto cold separation capillary ; PTFE connection used ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 93
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Separation of polychloro biphenyls ; Separation of organochlorine pesticides ; Splitless automated injection ; Residue level ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Complicated PCB mixtures can be separated in individual compounds using glass capillary gas chromatography, (GC)2. Depending on extraction and clean-up procedure it is also possible to separate and determine organochlorine pesticides at the same time.This (GC)2 technique can be used to determine the contents of individual chlorinated biphenyls in milk products and animal feedstuffs and in the analysis of complicated extracts of soil and vegetable material.Practical aspects concerning connection of the capillary, automatic splitless injection, repeatability of the retention time, quality of the column with respect to separation and adsorption and degradation of DDT are discussed.The detection of individual chlorinated biphenyls is possible at the ppb level in fats and vegetable materials, using an extraction and clean-up procedure, based on saponification of the sample.Preliminary results for milk, obtained from several areas, are shown.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 94
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 746-748 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Pt/Ir tubing ; Interfacing and coupling of columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 95
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 312-318 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Subnanogram analysis of estrogens as heptafluorobutyric esters ; ECD, quantitative analysis, automatic injection ; Run-to-run precision at the 50 picogram level between 2 and 7% rel. standard deviation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Subnanogram detection of steroids has become increasingly important today. One applicable method for gas chromatographic determination of subnanogram quantities of estrogens as halogenated derivatives is electron capture detection. HFB-derivatives of 7 different estrogens were automatically injected onto a prolonged narrow bore wall-coated glass capillary column. Normal split injection could not be used for this trace analysis because of too much loss of sample. Only small amounts of sample were available from which double analysis had to be performed.Cross-contamination of the automatic sampling system as well as precision of retention times and peak areas were determined.The type of injection described showed better quantitative results compared to the splitless injection technique.All details of the system used together with the results are this discussed in this paper.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 96
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 343-350 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Analysis up to C50 in GC/quadrupole MS combination ; No special procedures necessary when using commercially available instruments ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The analysis of low volatile compounds by (GC)2/MS using high-temperature stable glass-capillary columns and a commercially available GC/quadrupole MS instrument is described.It will be shown that no special modifications or procedures are required in analyzing organic compounds exceeding carbon numbers of 50. The application to industrially and naturally occuring high boiling mixtures will be discussed.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
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  • 97
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 351-356 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Potash soda lead and fused silica as wall material investigated ; Thin-walled fused silica is an ideal material ; Inherently more inert than normal glass ; High flexibility avoids fragility problems ; Application examples (alcohols, mercaptanes, sulfides, phenolsamines, acids) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: An investigation was conducted of various glasses, other than soda lime or borosilicate, for use in glass capillary gas chromatography. The work has uncovered some unique chromatographic qualities in the use of potash soda lead and fused silica glasses as materials for making glass capillary columns. The fused silica proved to be an ideal material for capillary column construction, being inherently more inert than glass containing metal oxides. It has been shown that through the use of thin wall capillary tubing of high flexibility many of the mechanical problems associated with glass capillary columns, such as fragility and column straightening, can be avoided.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 98
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 366-370 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Sampling problems by syringe needle temperature ; Technical solution of the problems by cooling and heating up minimized masses ; Discrimination and standard deviation measured with test mixtures C18-C38 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: On-column injection into a hot gas chromatograph oven involves the danger that the bottom part of the needle is warmed up above the boiling point of the solvent in the sample. Consequently parts of the sample are evaporated out of the needle instead of being introduced as a liquid into the capillary column. This causes losses and hence discrimination of the less volatile parts of the sample which remain in the needle.A technical solution is proposed using a system for cooling the capillary during the injection, down to the injection point in the oven.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 99
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 447-455 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary, glass ; Surface roughening by direct deposition of suspension particles ; NaCl used ; High reproducibility when coated with polar phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A method is described for roughening the surface of glass capillary columns for subsequent coating with polar stationary phases. A suspension of sodium chloride, obtained by addition of a saturated solution of sodium chloride in methanol to 1,1,1-trichloroethane, is passed through the column at velocities of 1-5 cm/s. During passage of the suspension, particles of sodium chloride deposit spontaneously on the column wall. The amount of sodium chloride deposited on the column wall is a function of the volume of the suspension passed through and of the contact time of the suspension and the column wall. Ultimately the amount of sodium chloride per unit surface area approaches a maximum. Columns covered with this maximum amount of sodium chloride were prepared with high reproducibility and coated with a number of polar stationary phases. Various factors that influence the stability of the suspension and the deposition of sodium chloride are discussed and minimum requirements are given. A theoretical model is proposed for the mechanism of deposition of sodium chloride particles on the glass wall.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
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  • 100
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 749-750 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Packed column, glass ; Dichloroacetic acid ; In biological fluids, at 50 ng level ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A method for the measurement of dichloroacetic acid in plasma or urine has been developed. The method involves extraction of dichloroacetic acid into diethyl ether, evaporation of the etheric phase to a small volume and derivatization with diazomethane. Trichloroacetic acid was used as an internal standard. Concentrations as low as 50 ng/ml can be determined.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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