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  • Gas chromatography  (72)
  • Springer  (72)
  • Annual Reviews
  • Blackwell Publishing Ltd
  • 2020-2024
  • 2005-2009
  • 1990-1994  (40)
  • 1980-1984  (32)
  • 1975-1979
  • 1993  (40)
  • 1982  (32)
  • 1978
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  • 2020-2024
  • 2005-2009
  • 1990-1994  (40)
  • 1980-1984  (32)
  • 1975-1979
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  • 1
    ISSN: 1432-2285
    Keywords: Abies alba ; Abscisic acid ; Damage ; Gas chromatography ; Needles
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary The amount of abscisic acid (ABA) in needles of silver fir from a natural location was investigated with regard to position in the crown, damage, seasonal variation, and needle age. Because of problems of quantification of ABA in coniferous needles, which contain numerous secondary plant products, a method for reliable determination of both isomers cis-trans-ABA (c-ABA) and transtrans-ABA (t-ABA) was developed. By means of gas chromatography (GC) using an electron capture detector (BCD) and a programmed temperature vaporizer (PTV) injector complete separation of both compounds was achieved. Two different pairs of fir were investigated — in each case a damaged and a healthy tree. Needles from both trees from the first and the second pair collected in September contained 500–1100 ng c-ABA/g fresh weight (FW), and the concentrations of t-ABA varied from 400 to 700 ng/g FW. Investigations from the second pair show highest amounts of 2900 ng/g Fw c-ABA and 1800 ng/g FW of t-ABA in May and June. For the first pair a higher c-ABA content was found in needles from the top of the crown than in those from the middle and the base. This difference could not be confirmed in the analysis of the second pair. Because of the strong natural deviation no statistically significant difference between the healthy and the damaged tree was found. The first pair of firs examined showed a higher t-ABA concentration than the second one. In this case the highest amount was found in the top of the crown. Methodical mistakes during the clean-up procedure and in quantification by gas chromatography could be excluded. The presence of c- and t-ABA in the purified extract was corroborated by mass spectrometry. With regard to the seasonal variation both isomers of ABA show an unequivocal trend. The maximum concentration is achieved in May to June, whereas the content is minimal in August/September. In any case the level of t-ABA is lower than that of c-ABA. No correlation between the amount of ABA and the needle age could be established.
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  • 2
    ISSN: 1612-1112
    Keywords: Teflon capillary columns ; Chemically modified teflon ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of teflon capillary columns employing direct coating of the stationary phase to the chemically modified teflon surface and the role of the chemically modified teflon in the separation mechanism are described. Two types of contributions from the modified teflon have been observed: nonspecific adsorption of the carbon surface and specific interactions of polar groups in the carbon skeleton. The use of polar liquid phases can eliminate adsorption due to the presence of polar groups in the modified teflon.
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  • 3
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    Chromatographia 16 (1982), S. 60-62 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Amines ; Derivatization ; Chloroformate esters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The gas chromatographic analysis of amines after conversion to electron capture sensitive carbamates in two-phase systems has been studied. Hydrophilic compounds, for instance methylamine, are reacted with 2,2,2-trichloro-tert. butyl chloroformate. Quantitation below 10−7 M can be made by thermionic or electron capture detection. A hydrophobic amine, namely N,N-dimethyl-n-octylamine, was derivatized with 2,4,6-tribromophenyl chloroformate with addition of iodide ion to the aqueous phase. The favorable effect of iodide ion as well as the choice of pH and chloroformate ester is discussed.
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  • 4
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    Chromatographia 16 (1982), S. 98-102 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Rectangular channel ; Efficiency ; Capacity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic experiments have been performed in a truly rectangular channel with a 60∶1 cross-sectional aspect ratio, constructed according to the field-flow fractionation technology. It is shown that the peak broadening is controlled by the thickness of the channel while the maximum load is determined by the largest cross-sectional dimension. However, even with its elongated configuration, the side walls contribute significantly to the band broadening of solutes with a high diffusivity. Good agreement is found between the experimental plate height data and the recent theoretical calculations of Golay [13] taking into account the side-wall effect.
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  • 5
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    Chromatographia 35 (1993), S. 649-652 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Triglycerides in cheese ; Programme temperature (PTV) injection ; Silica capillary columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid gas chromatographic method for the analysis of triglycerides in cheese on a capillary column with a programmed temperature vaporizer has been developed. Fat were extracted with hexane to dryness. The reproducibility of the method was assessed and the coefficient of variation for the total triglycerides was 2.50%. Recovery of individual triglycerides ranged between 87 to 105%.
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  • 6
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Curie-point pyrolysis ; Multivariate analysis ; Sodium dodecylbenzene sulfonate
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Multivariate analysis can be applied to quantitative analysis of sodium dodecylbenzene sulfonate (DBS) by pyrolysis gas chromatography. The pyrograms obtained from mixtures of DBS and polyoxyethylene lauryl ether (PEG) were normalized for the peak heights and areas of several internal standards which appeared in every pyrogram, against the characteristics peaks for DBS and PEG. This normalization method gave smaller experimental errors than when using one internal standard. The normalization values were used for cluster analysis unchanged. The values were calculated correlation coefficients and principal component analysis was performed using 11 data base and a set of sample data simultaneously. One calibration curve was calculated from the principal component scores. The DBS content of a sample was obtained from the calibration curve. Calculated values were in fair agreement with theoretical values.
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  • 7
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    Chromatographia 36 (1993), S. 187-190 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Solid-phase extraction disks ; Pesticides ; Soil analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A systematic study comparing the methodology and analytical results obtained in an investigation of seven pesticide residues (Molinate, Atrazine, Carbofuran, Pirimicarb, Prometryn, Malathion and Tetrachlorvinphos) in soil samples is reported. Solid-phase extraction (SPE) using glass columns and 47 mm disks of octyl and octadecyl-bonded silica was used in the pesticide analysis. The best extraction efficiency and clearest extracts are obtained with C8 disks. The analyses were carried out by capillary gas chromatography with nitrogen and phosphorus detection. Recovery experiments were performed at ppb levels in spiked soil samples. The average recoveries of the compounds were 53–77%. Detection limits are between 5 and 30 ng g−1 based on 5 g moist soil sample. The method was validated by comparing it with conventional liquid-liquid extraction.
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  • 8
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fatty acid methyl esters ; Diesel fuel substitute ; Glycerol
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A GC method for the determination of free glycerol in vegetable oil methyl esters used as diesel fuel is described. The sample preparation includes dissolving in dimethylformamide, silylation with bistrimethylsilyltrifluoroacetamide (BSTFA) and separation on a methyl silicone capillary column using either FID or MS detection. The recovery was tested using standard samples containing known amounts of glycerol. The results of the analysis of different samples were compared with those obtained by enzymatic determination. The method described offers a far more sensitive and quick determination of free glycerol compared to other methods.
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  • 9
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Electron capture detection ; Trichothecenes ; Cereal grain
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Various analytical methods developed for trichothecene determination, including TLC, HPLC, GC, supercritical fluid chromatography (SFC) and enzyme immuno assay (EIA) are reviewed. In addition a new method is described for the simultaneous determination of the trichothecene mycotoxins deoxynivalenol (DON), nivalenol (NIV), 3-acetyldeoxynivalenol (3-ADON), diacetoxyscirpenol (DAS), T-2 toxin (T-2), HT-2 toxin (HT-2) and T-2 triol (TRIOL), in Austrian wheat and corn samples by GC-ECD. A clean-up procedure has been developed using a combination of liquid-liquid and liquid-solid extraction. Trichothecenes were detected as their heptafluorobuturyl esters or alternatively as trimethylsilyl ethers (only sensitive for deoxynivalenol and nivalenol) using nandrolone or chloramphenicol as internal standard. Four derivatization techniques using HFBI, HFBA+DMAP on polystyrene, TMSI and TMSI+BSA+TMCS have been studied and the advantages and disadvantages of each are discussed. Quantification of trichothecenes from 10 to 1000 ppb in cereals could be accomplished routinely.
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  • 10
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    Chromatographia 37 (1993), S. 215-217 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Unified retention indices ; Dimethylsiloxane stationary phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic, unified retention-indices of 56 alkylbenzenes up to C15 on dimethylsiloxane OV-101 and SE-30 stationary phases are given. These values agree well with the corresponding experimental values used in the statistical treatment of the experimental data.
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  • 11
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    Chromatographia 37 (1993), S. 259-263 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Quantitative analysis ; Ethylene oligomer by-products ; n-Alkanes, n-alkenes and 2-alkyl-1-alkenes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method using temperature-programmed poly-dimethylsiloxane OV-101 and poly(pheny ether) (5 rings) capillary columns was developed to separate and quantify the reaction by-products in ethylene oligomers. It was found that the content of 2-alkyl-1-alkenes, 2-alkenes and n-alkanes in the C8−C18 α-olefin fractions amounts to 29, 10 and 2.6% respectively.
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  • 12
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    Chromatographia 37 (1993), S. 211-214 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Organic solvents ; Routine analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method for the analysis of organic solvents in chemical products is described. The analysis is performed by the use of a polar column, Supelcowax 10, and a non-polar column CP-Sil-5CB. Samples containing a non-volatile matrix or water were analysed by headspace analysis. The identification of the solvents in a sample, based on GC retention times on one column, is confirmed by GC of the sample on the second column. The method has been found to be suitable for the routine analysis of solvent mixtures.
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  • 13
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    Chromatographia 37 (1993), S. 264-270 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Temperature programmed ; Peak widths ; Polynomial interpolation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Isothermal chromatographic measurements lead directly to ΔH v o and A (entropy term) of solutes, and three constants of an empirical relationship between peak width and column temperature. From the thermodynamic parameters ΔH v o and A retention temperatures have been computed by means of a theoretical model including temperature dependence of carrier gas viscosity, and subsequently retention times; programmed retention indices have been determined by linear and polynomial interpolations. By substituting the value of the calculated retention temperature in the above-mentioned relationship, peak width at half-height for a linear temperature may be estimated. Predicted retentions correlate with observed data, with a P-value ≤0.01; simulation accuracy is generally 6–10% for peak widths. Retention indices of some organochlorine species, separated on an OV-101 capillary column, may differ by as much as 26 units depending on the method of calculation. Polynomial-calculated indices are more consistent with the retention index scheme, and have smaller standard deviations and better constancy at different heating rates.
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  • 14
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Inverse gas chromatography ; Poly(ethylene glycol) 20M ; Retention mechanisms
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The properties of poly(ethylene glycol) 20M (PEG 20M) coated on the hydroxylated surface of Chromaton N AW were investigated by inverse gas chromatography. It was found that the solid form of PEG 20M exhibits partition as the retention mechanism even below its melting range. The contribution of adsorption to the specific retention volume was also determined. It was demonstrated that inverse gas chromatography establishes the existence of a polymer surface layer but precise determination of its thickness is difficult. The limitation of the applicability of inverse gas chromatography results from the structure of the investigated surface layer which is thin and not coherent so that solute molecules can penetrate it.
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  • 15
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    Chromatographia 35 (1993), S. 33-37 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Crown ether polysiloxane phases ; Selectivity mechanisms
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The phase recognition mechanism of nine groups of position isomers on four crown ether polysiloxanes, OV-1701 and PEG 20M has been investigsated by measuring various thermodynamic parameters. The high selectivity of crown ether polysiloxane phases is due to hydrogen bonding and the extent of fitting between the analytes and the crown ethe cavity. The effects on selectivity of cavity size, heteroatoms and substituent groups on the crown ether are discussed.
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  • 16
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Equilibrium headspace sampling ; Partition coefficient determination ; Theory of chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The new phase ratio variation method is described which represents a convenient way for the determination of gas-liquid partition coefficients for practical purposes, utilizing equilibrium headspace-gas chromatography (EHS-GC). This method is based on the relationship between reciprocal peak area and the phase ratio in the vial containing the sample solution; it involves regression analysis of the EHS-GC measurements of a number of sample vials containing the same sample solution but with a wide variation of phase ratios. Examples are given for both aqueous systems and systems consisting of a stationary (liquid) phase used as the solvent; comparison of the measured values with results obtained by other methods shows satisfactory agreement. A critical discussion of the conditions influencing the accuracy of the analytical results is given.
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  • 17
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    Chromatographia 35 (1993), S. 109-110 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Unified retention index ; Correlation of data ; Hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic unified retention indices for 43 hydrocarbons (alkanes and cycloalkanes) are given for squalane and OV-101. Comparison of these values and unified retention index increments are presented as linear regression equations with high correlation coefficients and acceptable standard deviations.
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  • 18
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    Chromatographia 35 (1993), S. 160-166 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Neural networks ; Classification ; Pattern recognition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Artificial Neural Networks are proposed for the classification of vegetable oils submitted to gas chromatography analysis through their FAME profiles. Three important neural networks are evaluated here: the Hopfield model as a content-addressable memory (CAM), the Hamming model and the multi-layer perceptron. A brief description of these nets is first presented and further implemented for the classification of known vegetable oils. After the learning step, unknown samples are presented to the nets and the identification step performed. The performances of these nets are compared for the recognition of popular vegetable oils, including several edible oils.
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  • 19
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Mass spectrometry ; Atomic emission spectroscopy ; Pulp mill effluents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Three chlorinated dimethyl sulfones and five chlorinated thiophenes have been identified in the alkaline extraction liquor from a bleach plant by gas chromatography with atomic emission detection (GC-AED) and with mass spectrometry (GC-MS). The information on elemental content obtained by GC-AED enabled a rapid screening of the sulfur compounds and provided important structural information complementary to the mass spectral data. Quantitation was accomplished by GC-AED based on universal calibration.
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  • 20
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    Chromatographia 35 (1993), S. 209-215 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas chromatography-mass spectrometry ; Tagetes ; Plant volatiles ; Extractions ; Natural insecticides ; Mosquitos
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Volatiles from three species of the genustagetes, commonly called marigold have been isolated and characterized. Simultaneous steam distillation extractions (SSDE) produced consistently extracts of higher insecticidal activity than Soxhlet extractions. Methylene chloride was the best solvent. Volatiles isolated from theminutae species showed higher activity than those frompatula anderecta. Comparison of extracts from the flower, foliage and roots of the plant showed that most of the activity is located in the flower. The volatiles are highly effective toward both larvae and adult mosquitoes.
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  • 21
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    Chromatographia 35 (1993), S. 237-240 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Enantioselectivity ; Polysaccharide chiral stationary phase ; Amylose tris(n-butylcarbamate) ; Grob test
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Seven aromatic and alkyl amylose and cellulose carbamates have been tested as chiral stationary phases in gas chromatography. One of them, amylose tris(n-butylcarbamate) can be used for enantiomer separation.
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  • 22
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    Chromatographia 35 (1993), S. 290-294 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Solid phase extraction ; Organochloride pesticides ; Water analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatography of chlorinated pesticides in water is carried out after adsorption of a 50 mL sample using a cartridge containing 100 mg CN-bonded porous silica and extraction with 500 μL pentane. The average recovery for eight organochloride pesticides at 1 ppb was 〉95%. The procedure described is simple, selective and reproducible.
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  • 23
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    Chromatographia 35 (1993), S. 339-343 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Preconcentration techniques ; Trace gas analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The blanks in preconcentration methods for determining trace amounts of impurities in ultra-pure gases, which include the preconcentration volume of sample gases, carrier gas impurities and atmospheric contamination are discussed and three concentration methods for eliminating blank errors are proposed. These are, the differential volume method by concentrating at the same flow-rate but different times (DVMSF), the differential time method by concentrating the same volumes at different flow-rates (DTMSV) and the differential volume method by concentrating for the same times but different flow-rates (DVMST). DVMST is proposed as the best method for its ability to eliminate all blank errors described. The methods are used to determine trace amounts of Ar+O2 and N2 in ultra-pure hydrogen. Calculations demonstrate that the methods can effectively improve analytical accuracy.
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  • 24
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Micropacked columns ; Retention behavior ; LC silica packing materials ; Silanol groups
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic retention of cyclohexane and benzene on microcolumns packed with silica-based materials for liquid chromatography has been investigated to elucidate the relationship with the surface properties of the packing materials. Differences in capacity factors (Δk′) for these two hydrocarbons were related to the surface area of the packing materials. For untreated silica gels, the Δk′ value increased with increasing total surface area of the column employed and measurement of Δk′ for chemically-bonded stationary phases allowed estimation of accessible residual silanol groups.
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  • 25
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Pesticides in groundwater ; Solvent extraction ; Multiresidue analysis ; Selective detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple multi-residue procedure has been developed and applied to the analysis of pesticides in groundwater samples from the Comunidad Valenciana, a predominantly agricultural area on the Mediterranean coast of Spain. The procedure includes a liquid-liquid extraction, after addition of NaCl on the samples, and a subsequent analysis by capillary gas chromatography using a dual detection system with electron capture and nitrogen-phosphorous detectors. This allows the determination of more than 30 compounds (organophosphorous, organochlorine and pyrethroid pesticides) at the low ppb (μg l−1) levels. Detection limits obtained varied between 0.01 μg l−1 (lindane, fonofos) and 0.5 μg l−1 (cypermethrin). An additional injection of the sample extracts into a gas chromatograph equipped with a column of different polarity and electron capture detector is used for the confirmation of chromatographic peaks. The recommended procedure has been applied to 66 ground water samples. Pesticides, including organophosphorus and organochlorine compounds were detected in 31 of them, in levels ranging from 0.02 to 0.7 μg l−1.
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  • 26
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace sampling ; PTV-System ; Ethephon in drinking water
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An indirect GC method is described for the determination of Ethephon in drinking water on the basis of the headspace analysis of the ethylene formed from Ethephon. In order to reach the necessary detection limit, the entire volume of the static headspace distribution is transferred into a cold injection system (CIS). There, the ethylene is adsorbed on Carbosieve SIII at 10°C and, subsequently, desorbed at 300 °C. The water vapour included in the headspace is completely eliminated through the splitting system. By means of this technique, a detection limit of 0.05 μg/l water was reached.
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  • 27
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    Chromatographia 37 (1993), S. 399-401 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Viscosity ; Carrier gases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Equations are derived for viscosities of H2, He, N2 and Ar for use at chromatographic temperatures which are accurate to within 0.3% for H2, and 0.1% for the other gases. The effect of pressure is usually negligible but may increase the viscosity of N2 or Ar by as much as 0.5% at 25°C or lower and 5 atm or higher.
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  • 28
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    Chromatographia 15 (1982), S. 704-706 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Isopropyliden-sorboses ; TMS-derivatives ; GC-MS combined technique ; Mass spectra
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method has been developed using gas chromatography — electron impact mass spectrometry for the determination of the di-0-isopropylidene-sorbofuranose and mono-0-isopropylidene-sorbofuranose. The compounds are separated as their trimethylsilyl derivatives on a capillary column coated with the stationary phase SE-52. The mass spectra show that the silylation reaction is quantitiative and that the isopropylidene groups does not change.
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  • 29
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    Chromatographia 15 (1982), S. 183-185 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Analysis of ethylbenzene hydroperoxide ; Time normalization method
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method, based on the time normalization technique, is described for the analysis of ethylbenzene hydroperoxide in mixtures containing ethylbenzene, acetophenone, 1-phenylethanol, benzaldehyde and phenol. Different liquid phases were tested and the best results were obtained with tricresyl phosphate and neopentyl glycol sebacate. The influence of the support, the liquid loading and the gas velocity are discussed.
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  • 30
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    Chromatographia 15 (1982), S. 625-630 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Open-tubular (capillary) columns ; Comparison of liquid phases ; Influence of temperature ; Retention index data
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The influence of temperature and liquid phase film thickness of open-tubular (capillary) columns on the retention index values of hydrocarbons on methylsilicone liquid phases is discussed. Data obtained on methylsilicones and squalane are compared. Retention index values of 43 hydrocarbons between 40 and 70 °C on OV-101 liquid phase are listed.
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  • 31
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    Chromatographia 15 (1982), S. 351-354 
    ISSN: 1612-1112
    Keywords: Supported catalysts ; Reserved-flow GC ; Drying step ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Application of reversed-flow gas chromatography to study the drying step in the preparation of supported catalysts is proposed. It is demonstrated that this technique can be applied to investigate the kinetic law followed, as well as to obtain kinetic parameters of drying (rate constants, activation energies and frequency factors). Amaterial illustrating this application is γ-Al2O3 impregnated with usual organic solvents (n-C5H12,n-C6H14,n-C7H16, CH3COCH3 and CH3CH2OH). It was found that in all cases above a simple first-order law based onone kind of active site is followed. Moreover, it was observed that the activation energyE a of the drying process increases almost linearly with the relative molecular mass of the solvent, whereas for the same solventE a increases with the amount used. The operation of a kinetic compensation effect suggests “similar” activated complexes of the various solvents used.
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  • 32
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fused silica capillaries ; New polar phases: OV-1701 and RSL-310 ; Immobilization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The possibilities of OV-1701 and RSL-310, two new stationary phases, have been evaluated for capillary gas chromatography in fused silica columns. OV-1701 is a cyanopropylphenyldimethyl polysiloxane of moderate polarity possessing excellent chromatographic characteristics. The phase exhibits high coating and chromatographic efficiencies, high temperature stability and is suitable for cross-linking. RSL-310 is a polar liquid stationary phase yet to be permanently bonded in a capillary column. The selectivity of both phases extends the applicability of fused silica columns.
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  • 33
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    Chromatographia 35 (1993), S. 503-505 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Silanol terminated Chirasil-Val ; Cross-linking with polyfunctional silanes ; Enantiomer separation
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method for the immobilization of Chirasil-Val has been studied based on the cross-linking which takes place between terminal silanols of Chirasil-Val and polyfunctional silanes. A leached, dehydrated and tetramethoxysilane-treated glass capillary coated with silanol terminated Chirasil-Val containing 5% tetraacetoxysilane as a cross-linking agent showed a maximum extractability of 15% without any loss of chirality.
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  • 34
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    Chromatographia 37 (1993), S. 51-56 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Halogenated hydrocarbons ; Headspace sampling ; ECD detection
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    Topics: Chemistry and Pharmacology
    Notes: Summary Simple sampling and preconcentration technique for the analysis of volatile halogenated hydrocarbons in water is described. For the separation a selective capillary column is used in combination with an ECD. Quantitative data are given.
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  • 35
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fused silica open tubular columns ; Serial coupled columns ; Phase ratio optimization
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    Topics: Chemistry and Pharmacology
    Notes: Summary There are a number of parameters which have to be chosen depending on the analysis being done in gas chromatography. While the choice of stationary phase material is based on the solutes to be separated, the thickness is dependent on the concentration and the volatility of the components to be analyzed. This study undertakes a coupled column phase ratio optimization by connecting a short piece of a particular column prior to a normal length of an analytical column. Various columns of different dimensions (phase ratio), but of the same stationary phase material (methyl silicone), are coupled together by a deactivated glass press-fit connector, and the efficiency and capacity are measured. The coupling of fused silica open tubular columns is optimized in efficiency by matching or decreasing the phase ratio of successive columns. Capacity optimization is accomplished by increasing the phase ratio of consecutive columns. Capacity and efficiency optimization are opposing each other; therefore, if some efficiency can be sacrificed a substantial increase in capacity is possible.
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  • 36
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    Chromatographia 15 (1982), S. 241-244 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Monosaccharides ; Polyols ; GC of TMS derivatives
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    Topics: Chemistry and Pharmacology
    Notes: Summary This paper describes the gas chromatographic separation of the mixture of isopropylidene monosaccharides, and their trimethylsilyl derivatives. Based on the total analysis time and resolution the best stationary phase was SF-96 using Chromosorb G as the solid support and temperature programming.
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  • 37
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    Chromatographia 15 (1982), S. 312-314 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Injection-port modification ; Oxygen and nitrogen traces
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    Topics: Chemistry and Pharmacology
    Notes: Summary The paper presents a new device modifying normal injection port of a gas chromatograph for eliminating air contamination thus enabling determination of traces of oxygen or nitrogen. Further modification is also proposed which enables the analysis to be carried out with a limited quantity of sample gas. Potential application of this device in the analysis of reactive gases like florine has been indicated.
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  • 38
    ISSN: 1612-1112
    Keywords: Phthalides ; Gas chromatography ; Chromosorb W ; Isomerization ; Ligustilide
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    Topics: Chemistry and Pharmacology
    Notes: Summary During GLC of naturally occurring mixtures of phthalides on packed columns an artefact was sometimes detected that originated from Z-ligustilide. Active sites of Chromosorb W were responsible for the formation of the artefact, that was assumed to be E-ligustilide as GC-MS revealed that its mass spectrum was identical with that of Z-ligustilide. No isomerization was observed when freshly coated Chromosorb W was used or the support was deactivated by benzoyl chloride or melamine. The identity of the artefact was confirmed by UV irradiation experiments.
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  • 39
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    Chromatographia 15 (1982), S. 30-32 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Arsenic ; Inorganic materials
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the quantitative chlorination and extraction of arsenic as arsenic trichloride from a number of alloys. The conditions for the quantitative gas chromatographic measurement of the volatile chloride have been studied. The proposed method for inorganic materials is very fast giving results within 10 min; sensitive, 1.5·10−13 g As can be detected, simple and accurate. At the ng level of As the error is about 20% with a standard deviation less than 20%, and at the 10pg level the error is about 36% with a standard deviation of 44%.
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  • 40
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    Chromatographia 15 (1982), S. 765-768 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Preparative scale chromatography ; Capacity ; Dual-stage separation
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    Topics: Chemistry and Pharmacology
    Notes: Summary The capacity of different versions of single- and dual-stage separation of mixtures on a preparative scale is considered. It has been shown that dual-stage separation with intermediate condensation considerably enhances the capacity of the installation as compared with a single-stage process.
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  • 41
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    Chromatographia 15 (1982), S. 117-124 
    ISSN: 1612-1112
    Keywords: Various packed GC column ; Gas chromatography ; Porous layer beads ; GC/MS analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary Theoretical comparisons of various packed GC column types are presented with respect to analysis time, efficiency, sample dilution, and sample capacity for a given maximum inlet pressure. In particular, totally porous particles, porous layer beads, and glass beads are compared with one another. It is shown that 30 μm porous layer beads offer a useful compromise between analysis time and plate count with relatively good sample capacity. Moreover, when using 1 mm i.d. columns (microbore), outlet flow rates that are reasonable for direct coupling to magnetic sector mass spectrometers are achieved making these columns suitable for GC/MS. Using 30 μm Zipax porous layer beads, columns yielding 8,000 to 10,000 plates/meter have been produced with inlet pressures of 13 to 26 atm. A simple modification of the injection port converts the maximum inlet pressure of a commercial gas chromatograph to 26 atm. With such pressures, columns in excess of 20,000 plates can be achieved. Chromatograms are presented illustrating the promise of these microbore columns for GC and GC/MS analysis.
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  • 42
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    Chromatographia 15 (1982), S. 245-248 
    ISSN: 1612-1112
    Keywords: Chromatoscopy ; Gas chromatography ; Graphitized carbon black ; Molecular structure and retention ; Aromatic hydrocarbons
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    Topics: Chemistry and Pharmacology
    Notes: Summary A molecular-statistical calculation of the retention volumes at zero sample size on graphitized thermal carbon black is carried out for quasi-rigid molecules of fluorene, indene, 1-methylindene, 2-methylindene and three dimethylindenes. A reasonable agreement is observed between the calculated and the available experimental gas chromatographic data. The potential barrier to internal rotation and the torsional angle in styrene molecules are estimated by comparing theoretically calculated and measured retention volumes.
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  • 43
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Silicone liquid phases ; Oxidation
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    Topics: Chemistry and Pharmacology
    Notes: Summary The on-column oxidation of apolar and polar silicones used as gas chromatographic stationary phases is investigated. Even at 225° the effects of oxidation are found to be slight. Of the materials investigated the methylphenylsilicones are the most stable.
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  • 44
    ISSN: 1612-1112
    Keywords: Glass capillary ; Gas chromatography ; Methyl chloroacetates ; Methyl chloropropanoates ; Methyl chlorobutanoates
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    Topics: Chemistry and Pharmacology
    Notes: Summary The gas chromatography of all chlorinated methyl acetates, methyl propanoates and methyl mono- and dichlorobutanoates has been studied on Carbowax 20M and SE-30 glass capillary columns under various running conditions. The order of elution on a non-polar column was largely determined by the boiling point of esters, whereas on a polar column it was much influenced by the structure of compounds. Complete separation of the combined mixture of all 27 compounds could not be achieved, however, methyl 3,3-dichlorobutanoate was the only ester overlapped on both columns in spite of the various column temperatures used. The best separation of the mixture was on Carbowax 20M with a temperature program from 50°C at 8°C/min, isothermal running conditions leading either to poor separation of volatile components or long analysis time and broad peaks of higher chlorinated esters. The relative retention times for compounds at the various column temperatures are given and the retention order on a polar and on a non-polar column discussed.
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  • 45
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    Chromatographia 15 (1982), S. 517-520 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carbon-silica adsorbents ; n-Octadecanol film ; Phase transitions
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    Topics: Chemistry and Pharmacology
    Notes: Summary The properties of the n-octadecanol film on carbon-silica adsorbent (Carbosil) were investigated. It was found that n-octadecanol forms an oriented film on the Carbosil's surface. If the surface of the basic silica gel is not completely covered with carbon, then the phase transition takes place in this film at a temperature higher than the melting temperature of n-octadecanol. One may distinguish two forms of this film, characterised by the different structures and the temperatures of the phase transitions. The first exists on the surface of silica gel unblocked by carbon. This part of the film is a monolayer, in which the alcohol molecules are vertically oriented. The solid compact-liquid expanded type phase transition at the well-defined temperature occurs in this film. In the second part of the film formed on the carbon surface, there is a multilayer of n-octadecanol. Its molecules are probably parallely oriented in relationship to the adsorbent surface. This film desintegrates progressively when the temperature increase. Maximum temperature of this phase transition is lower than the temperature of its analogue on pure silica gel surface.
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  • 46
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    Chromatographia 15 (1982), S. 546-558 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Quantitative analysis ; Sample inlet systems ; High-speed analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary The attainment of precise quatitative analytical data using open-tubular (capillary) columns in standard, commercially available gas chromatographic instrumentation is demonstrated. Key elements in the design and proper utilization of the instrumentation are discussed. The function of the various sample introduction systems is elaborated and their quantitative performance demonstrated. The extra-column contribution to band-spreading is determined and the resultant data is used assessing the suitability of commercial instrumentation for highspeed capillary gas chromatography. The quantitative analysis of a sample containing some eleven components in less than thirty seconds is shown.
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  • 47
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Crystal hydrates as stationary phases ; Mobile Phases containing water ; Selective retentions
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    Topics: Chemistry and Pharmacology
    Notes: Summary The use of crystallohydrates, crystallohydrate solutions and melts as stationary phases in gas chromatography has been proposed. Crystallohydrates have been shown to display high selectivity in the separation of polar organic compounds when use is made of water vapours as the mobile phase. Some aspects of gas-liquid chromatography in water vapours and with the stationary phase comprising crystallohydrates have been studied, and the preliminary results obtained point to the desirability of further progress in this field.
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  • 48
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    Chromatographia 16 (1982), S. 201-203 
    ISSN: 1612-1112
    Keywords: Phenols ; Whisky ; Gas chromatography ; Aroma compounds
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    Topics: Chemistry and Pharmacology
    Notes: Summary Twelve volatile phenols were identified in whisky by combined gas chromatography-mass spectrometry. Of these phenols 2,4-dimethylphenol was found for the first time in the aroma of whisky. The content of phenol, o-, m-, and p-cresol, guaiacol, p-ethylphenol, p-ethylguaiacol and eugenol in whiskies originating from different countries was determined by gas chromatography as their 2,4-dinitrophenyl ethers using electron capture detection. The results show that Scotch whiskies differ from others in the content of o-, m-, and p-cresol. The odour threshold values of phenols studied were determined in a 10% (v/v) ethanol-water mixture and in some cases also in the whiskies. Cresols have been found to make contribution to the aroma of Scotch whisky.
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  • 49
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    Chromatographia 16 (1982), S. 26-31 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Ionization detectors ; Gaia
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    Topics: Chemistry and Pharmacology
    Notes: Summary This paper is an account of the development of the gaia hypothesis as seen through the eyes of a gas chromatographer. Gaia is a radical notion about the Earth which postulates the climate and chemical composition to be regulated at an optimum by and for life. Gas chromatography played an important role in the gathering of evidence for the hypothesis but most significantly the art of inventing detectors lead to the developement of a planetary life detector through which gaia was revealed.
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    Chromatographia 16 (1982), S. 282-285 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Naphtha analysis ; Gasoline analysis ; Hydrocarbon type analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary Two different gas chromatographic methods are used for the determination of hydrocarbon type distribution in naphtha and gasoline samples with final boiling points up to 275 °C. The methods are based either on a single capillary column or on a valve-switched packed column system. Both methods give extensive information on paraffins, olefins, naphthenes and aromatics in total as well as by carbon-number. In each case the analysis is fully automated with a computer controlling the entire analysis from injection to results presentation. The advantages and limitations of both methods are discussed.
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  • 51
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    Chromatographia 16 (1982), S. 322-324 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Graphitized carbon black supports ; Determination of hydroxyacids
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    Topics: Chemistry and Pharmacology
    Notes: Summary Acid-washed graphitized carbon black (Carbopakc B) modified with trimesic adic and PEG 20M has proved to be effective for quantitative analysis of underivatized low molecular weight hydroxyacids. Calibration data revealed good linear relationships between relative peak area and concentration for lactic and 3-hydroxybutyric acids down to 0.05 mmol/l. The packing material was suitable for the analysis of aqueous solutions of hydroxyacids as it is tolerant to injections of water over a prolonged period of use. The GC system developed has been applied to the analysis of some hydroxyacids of biomedical interest in blood plasma and lactic acid contained in wine and beer.
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  • 52
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Modified thermal energy analyzer ; Selective detection of nitrogen compounds
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    Topics: Chemistry and Pharmacology
    Notes: Summary A modification to the TEATM Analyzer is described, which allows it to be used as a highly selective GC detector for nitrogen compounds as well as for N-nitrosamines and nitro compounds. The modified Analyzer is as sensitive as the AFID, but has a much higher selectivity towards nitrogen compounds than the AFID. Its response appears to be molar, with an output that is dependent only on the number of nitrogen atoms present. The performance of the modified Analyzer for the analysis of ammonia, amines,N-nitrosamines, nitriles and organonitro compounds is reported and discussed, as is its application to the detection of these compounds in bacon and beer samples.
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  • 53
    ISSN: 1612-1112
    Keywords: Supercritical fluid chromatography ; Gas chromatography ; High speed analysis ; Thermal desorption ; Two dimensional analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary A two-dimensional supercritical fluid-gas chromatography system was constructed and evaluated. A 50-μm i.d. capillary column coated with a 50 % cyanopropyl polysilixane stationary phase was used as the firstdimensional column. Group-type separations of polycyclic aromatic hydrocarbons, based on the number of aromatic rings, were achieved using this column under SFC conditions. A 25-μm i.d. liquid crystal column was used as the second-dimensional column under GC conditions. The effluent from the first column (SFC) was received continuously by the second column (GC) through a thermal desorption modulator. The thermal desorption modulator (prepared at the head of the second column) generated a series of concentration pulses from the first column effluent. These concentration pulses served as injections to the second column, and were developed into a corresponding series of high-speed chromatograms. Grouptype sample bands from the first column were separated into individual components on the second column. All sample substances passed through both columns to generate two sets of retention data, which could be used for more accurate compound identification.
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  • 54
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary column sampling ; Additivity of variance in GC ; Aqueous samples ; PAHs
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    Topics: Chemistry and Pharmacology
    Notes: Summary The possibility of using capillary columns for both sampling and gas chromatographic analysis of aqueous micropollutants has been studied. Factors influencing gas chromatographic band dispersion of the solute were investigated and a mathematical relationship developed correlating the properties (ID, df) of the capillary columns to the degree of dispersion of adsorbed substances has been derived. The experimental results obtained with aqueous samples are in good agreement with the theoretically forecast data. The method developed allows gas chromatographic dosing of traces of organic substances, reducing inconvenience deriving from excessive sample handling to a minimum. Non-refocusing of the analyte does not, in any significant way, compromise column efficiency for substances that are not very soluble in water.
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  • 55
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace analysis ; Steam distillation ; Phenols
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    Topics: Chemistry and Pharmacology
    Notes: Summary High-temperature headspace analysis performed under static conditions above 100°C increases the sensitivity of gas chromatographic determination of volatile phenols in aqueous solutions 20–100 fold and reduces the detection threshold, to 10 μg×1−1. To improve the sensitivity and reduce the threshold still further, preliminary concentration by high-temperature microdistillation at elevated pressure is proposed. A theoretical model of this process has been developed. The possibility of concentrating volatiles by high-temperature microdistillation has been experimentally confirmed.
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    Chromatographia 36 (1993), S. 215-217 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Polar columns ; Vegetable oils ; Sterols ; Unsaponifiable matter
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    Topics: Chemistry and Pharmacology
    Notes: Summary The analysis of both the total unsaponifiable matter and the sterol fractions in vegetable oils has been performed with a new polar column (TAP, Chrompack). The use of a polar column, which is characterized by high thermal stability, has led to the identification of a greater number of constituents than the use of a nonpolar column (i.e. SE 52, SE 54). The polar column enhances the separation of the main classes of unsaponifiable matter (sterols, 4-methyl sterols and 4,4′-dimethyl sterols). When used for the unsaponifiable and sterol fraction analyses, it offers a powerful tool for characterizing the lipid source.
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  • 57
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid chromatography ; Mass spectrometry ; β-agonists
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    Topics: Chemistry and Pharmacology
    Notes: Summary Different chromatography — mass spectrometry techniques for the analysis of β-agonists have been compared. Gas chromatography — mass spectrometry (electron impact) has been used, as also has liquid chromatography coupled to the mass spectrometer by either thermospray or electrospray interfaces. The results obtained by the three method were compared in terms of sensitivity, selectivity, and richness of information provided by the analysis. It was found that using electrospray ionization, very powerful analysis could be achieved with high sensitivity, thus providing significant potential for the analysis of β-agonists.
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  • 58
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Crown ether polysiloxane phases ; Capillary columns
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    Topics: Chemistry and Pharmacology
    Notes: Summary Two crown ethers, di(tert-butylbenzo)-propyl-15-crown-5 polysiloxane (PSO-DTB-15C5) and dibenzo-propyl-15-crown-5 polysiloxane (PSO-DB-15C5) have been synthesized and coated onto fused-silica capillary columns. The chromatographic characteristics, including column efficiency, polarity, phase transition temperature, operating temperature range and selectivity, were studied. Excellent selectivity was obtained for the separation of polar position isomers, especially phenol and dinitrotoluene isomers. The separation mechanism is discussed.
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  • 59
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention indices ; Adsorption effects ; n-Tetradecenes ; n-Tetradecynes
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    Topics: Chemistry and Pharmacology
    Notes: Summary The correction of the reproducibility of retention indices on polar capillary columns with different film thickness, using more polar reference standards instead ofn-alkanes, was investigated. It was found that the replacement ofn-alkanes by 1-alkenes, 3-alkynes and n-alkylbenzenes as standards significantly improves the reproducibility of retention indices and diminishes their temperature increments forn-alkanes,n-alkynes and arenes on PEG 20M columns.
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  • 60
    ISSN: 1612-1112
    Keywords: Graphizized carbon black traps ; Organic air pollutants ; Work areas ; Gas chromatography
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    Topics: Chemistry and Pharmacology
    Notes: Summary The use of traps containing graphitized carbon black for the collection and pre-analysis of atmospheric pollutants in industrial areas is presented. The working conditions, in terms of trapping capability and effectiveness of release by thermal desorption are discussed. Some practical applications are also given.
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  • 61
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Van der Waals' volume ; Polarity of stationary phase ; Retention index
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    Topics: Chemistry and Pharmacology
    Notes: Summary Equations for Retention Index (I) versus Van der Waals, volume (Vw) on squalane are studied for alcohols, carbonyls, esters and ethers. Each equation includes linear and branching substances with different positions of the functional group in the carbon chain. The study is extended to stationary phases with polarities from 4.29 to 91.54 on the Tarjan et al. scale. Variations of the slope and origin ordinate values with the polarity of the stationary phase are discussed.
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    Chromatographia 15 (1982), S. 125-132 
    ISSN: 1612-1112
    Keywords: Capillary columns ; Fast analysis ; Gas chromatography ; Instrumental effects ; Optimization
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    Topics: Chemistry and Pharmacology
    Notes: Summary The efficiency of fast GC columns depends largely on the quality of the chromatograph. A theoretical and experimental study shows the relative importance of the various phenomena involved and permits the optimization of a GC System. Extremely good performances, exceeding 2,500 plates per second have been routinely obtained.
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    Chromatographia 15 (1982), S. 180-182 
    ISSN: 1612-1112
    Keywords: Acidic fermentation products ; Characterisation ; Gas chromatography ; Methyl esters
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    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid and simple method for the identification of acidic fermentation products is described. Methyl esters of volatile and non-volatile acids are separated on a single chromatographic column. Retention time data for a number of acids are tabulated.
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    Chromatographia 15 (1982), S. 521-524 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index ; Connectivity index ; Van der Waals' volume ; Alkanes
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    Topics: Chemistry and Pharmacology
    Notes: Summary The relationships between retention index and Van der Waals' volume and between retention index and connectivity index have been studied for 58 different alkanes (C1−C9) on squalane. The correlation coefficient for the former is higher than for the latter. From these equations a linear relationship between Van der Waals' volume and connectivity index is obtained which indicates that the two parameters are equivalent. A simple method for calculating the Van der Waals' volume of alkanes is proposed.
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  • 65
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Fused silica capillaries ; Capillary drawing ; Glass capillaries
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    Topics: Chemistry and Pharmacology
    Notes: Summary A compact description is given of a simple and reliable method of drawing flexible fused silica capillary for gas chromatography. Some emphasis is given to the fact that the practices of drawing optical fibres should not be followed too slavishly so this leads to unnecessarily complicated and expensive equipment. Satisfactory capillary column silica tubing can be made with straightfoward extension of the method developed earlier for drawing thick walled capillary. A simple glass/silica hydrogen oxygen diffusion flame bumer is described for fusing the preform tubing at the draw point which is enclosed by a water cooled glass enclosure to trap evaporated silica and maintain the operation under dust free conditions. The uniformity of the capillary diameter is better than 5% which is adequate for most gas chromatographic purposes. The second part of the paper yet to be published will cover the methods developed for coating the capillary both internally and externally.
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  • 66
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    Chromatographia 16 (1982), S. 107-111 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Thermionic ionization ; Catalytic flame ionization
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    Topics: Chemistry and Pharmacology
    Notes: Summary A newly designed thermionic detector was operated in two modes of thermionic ionization detection (TID), and a third mode of catalytic flame ionization detection (CFID). Operating modes were varied by changing the composition of the electrically-heated thermionic/catalytic source, and the composition of gases supplied to the detector. A TID-2 source activated by a low concentration of Cs/ceramic was operated in a dilute H2/air environment and provided specific responses to nitrogen and phosphorus compounds. A TID-1 source activated by a high concentration of Cs/ceramic was operated in a N2 environment and provided very high specificities and picogram detectivities to compounds containing electronegative functional groups such as the NO2 group. A CFID source formed from Ni/ceramic was operated in a H2/air flame environment and provided universal responses to all organics with enhanced responses to some heteroatom compounds.
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    Chromatographia 35 (1993), S. 539-542 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid crystals ; Diffusion coefficients ; Xylenes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The molecular diffusion coefficients of xylene isomers have been determined at different temperatures in the three phases (smectic, nematic and isotropic) of 4,4′-bis(heptyloxy)azoxybenzene (BHOAB) by gas chromatography. The results obtained are discussed in terms of molar volume, polarity and length-to-breadth ratio of several isomers. The activation energy of diffusion processes of solutes in the three phases of the liquid crystal has been calculated.
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    Chromatographia 36 (1993), S. 225-233 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Selective ionization detectors ; Organic fuelled flames ; Lead, tin, phosphorus, halogens
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The selectivities of two flame-based ionization detectors identified as a Remote FID (RFID) and a Flame Thermionic Ionization Detector (FTID) have been improved by introducing methane as a fuel for the flame. Both the RFID and FTID feature a detector struture in which the ionization polarizer and collector are located several centimeters downstream of an oxygen-rich flame, rather than immediately adjacent to the flame as in a flame ionization detector. The RFID detects long-lived negative ions produced in the flame by the combustion of lead, tin, phosphorus, or silicon compounds. The FTID re-ionizes and detects neutral electronegative products generated by combustion of nitrogen, halogen, or phosphorus compounds. An organic-fuelled RFID can detect 1 pg Pb (Sn, P)/sec with a selectivity of the order of 106 versus hydrocarbons. An organic fuelled FTID is applicable to detection of compounds at nanogram and higher levels. FTID selectivity for PCB compounds in a transformer oil matrix is of the order of 105∶1. The improved selectivity achieved by using an organic-fuelled flame is also applicable to the detection of phospholipid and other non-volatile N, P, or Cl compounds using an FID/FTID detector accessory for a TLC/FID analyser.
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    Chromatographia 37 (1993), S. 105-106 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Occupational hygiene analysis ; Epichlorohydrin in air ; Trace analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new method has been developed for the determination of trace amounts of epichlorohydrin in workplace atmospheres. Collection is peroormed in two bubblers in series both containing dichloromethane. Optimum conditions for sampling and analysis have been established. The lower limit of determination is 0.05 μg/mL with an RSD of ±5%.
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    Chromatographia 37 (1993), S. 277-280 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Hydrogenation of 1,5,9-cyclododecatriene ; Retention index
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of the products obtained by the hydrogenation of 1,5,9-cyclododecatriene stereoisomers on fused-silica capillary columns coated with dimethylsilicone and cyanopropylmethylsilicone stationary phases was investigated. Retention indices of cyclododecatrienes, cyclododecadienes, cyclododecenes and cyclododecane were determined at three temperatures. The respective standard deviations were 0.3 and 0.6 i.u. The influence of the polarity of the stationary phases on the chromatographic retention of these cyclic hydrocarbones is discussed.
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    Chromatographia 37 (1993), S. 250-258 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention data ; Stationary phases ; Phase constants ; Linear free energy relationships
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Specific retention volumes and retention indices for selected compounds can be predicted from different sets of stationary phase constants by multiple regression. Errors in the corresponding calculated retention times are between 5 and 15%. Intercept (A) and slope (B) values are given for 72 McReynolds stationary phases. The A value can be predicted from the retention index of benzene with a standard deviation of 9%.
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    Chromatographia 37 (1993), S. 546-548 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace sampling ; Methyl methacrylate monomer ; Contact lens
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A modified gas chromatographic method is described for the determination of free monomer in contact lenses, irrespective of the method of production. It thus becomes possible to assess very quickly the conformity of such lenses with hygiene regulations. This method allows direct supervision of production or determination of the quality of a product of unknown origin in only 15 min. Production tests of new polymerization initiators, reactors for polymerization, etc. can also be carried out.
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