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  • Gas chromatography  (172)
  • Springer  (172)
  • Elsevier
  • 2015-2019
  • 2010-2014
  • 1985-1989  (172)
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Year
  • 1
    ISSN: 1432-1432
    Keywords: Primordial terrestrial atmospheres ; CH4, C2H2, CO2 ; Prebiotic synthesis ; High-frequency discharge ; Hydrocarbons ; Gas chromatography ; Mass Spectrometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Various hydrocarbons were synthesized by high-frequency discharge in a primordial terrestrial model atmosphere. The products were extracted by benzene or methanol and analyzed by GC-MS. The mean carbon chain length of the hydrocarbons formed by the discharge through pure CH4 gas was less than 6. Benzene was also obtained. Some isomers were obtained for each of the hydrocarbons containing a given number of carbons. When a small amount of C2H2 was added to the CH4, longer chain compounds were formed, as compared with discharge in CH4 only. However, when the amount of C2H2 was increased, unextractable high molecular weight compounds were produced. The amounts of products decreased as the mixing ratio of CO2 to CH4 increased. No hydrocarbons were detected when the ratio of CO2/CH4 exceeded 1.
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  • 2
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    Trees 1 (1987), S. 94-101 
    ISSN: 1432-2285
    Keywords: Monoterpenes ; Abies alba Mill ; Resin ; Seeds ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary Using gas-chromatographic methods, the variability of the contents of monoterpene hydrocarbons (α-pinene, β-pinene, Δ3carene and limonene) in the resin of silver fir seeds (Abies alba Mill.) was studied. Resin cavities were characterized according to their position on the seed surface. It was estabilished that the terpene content of the resin of cavities localized on the abaxialadaxial surfaces of the seed differs significantly, creating a gradient of resin composition around the circumference of the seed. The differences between various resin cavities of single seeds were greater than the differences between different seeds of a single cone and between seeds of various cones on a single tree. An accurate definition of the resin cavity location on the seeds appears to be a fundamental condition for the collection of a sample representing the resin composition of individual trees. Resin biosynthesis in the course of organogenesis and the control of terpene contents in the resin of various locations on the seed and the cone are discussed.
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  • 3
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary liquid, choice of ; Physico-chemical data
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A table of data for acidity, basicity, polarity and London potential for stationary phases is given. These provide guidance in choosing a stationary phase for a given task from the 26 substances listed. The indices are calculated from infra-red shifts of 1-chlorobutane and the visible wavelength shifts of l2 when they are dissolved in the stationary phases, from NMR estimates of acidity and basicity and from relative retention data. They replace the less reliable data of Burns and Hawkes. Methods of determining the indices are suggested that require only a gas chromatograph and can be applied by technicians with no specialized understanding of solution parameters. An attempt to add electron donoracceptor indices to the table was unsuccessful. A further table is given of the slopes of the log plots d(logt′)/dC for use in extrapolating from one homologue to another on these stationary phases.
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  • 4
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    Chromatographia 20 (1985), S. 343-346 
    ISSN: 1612-1112
    Keywords: Thermosorb ; Tenax GC ; Environmental Analysis ; Trace Organics ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A preliminary study has been carried out to evaluate a new adsorbent, Thermosorb, for trace level organic contaminants. For this purpose, a comparison was made with a well-characterized adsorbent, Tenax GC, using a prepared aqueous solution of trace organic components. In addition, a comparison was made of chromatograms of air contaminants obtained using both of these adsorbents, under equivalent conditions. The results clearly indicated the potential of this thermally stable, inorganic adsorbent for many trace organic substances of environmental interest.
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  • 5
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    Chromatographia 20 (1985), S. 371-375 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Flame photometric detector ; Sulphur
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The effect of experimental conditions such as gas flow rates, detector and column temperatures on sulphur response are discussed. It is concluded that the response of the flame photometric detector is affected by the O/H ratio and the total gas flow. Column temperature has an important influence upon S2 emission. It is shown that the sulphur response of the FPD is dependent on the compound containing the sulphur.
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  • 6
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Flame ionisation detection ; Cyanogen ; Cyanogen chloride
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The response of a flame ionisation detector (FID) to cyanogen ((CN)2) and cyanogen chloride (CNCI) has been studied. The lower limits of detection for (CN)2 and CNCl were 6×10−12 moles and 2×10−11 moles respectively. In a comparative study a thermal conductivity detector gave as its lower limit of detection for both (CN)2 and CNCl 4×10−11 moles. Both detectors showed excellent linearity over the range 0 to 10 micromoles. The ratio of the gradients of the FID calibrations (CN)2/CNCI were found to be approximately two suggesting the response depended on the cyanide group. The response and stability of the FID was investigated as a function of air and hydrogen flow-rates. The response increased with increasing air flow-rate for both (CN)2 and CNCI up to 300cm3min−1, thereafter no significant increase was observed. On raising the hydrogen flow from 10 to 25cm3min−1 only a slight increase in the sensitivity of the FID towards both (CN)2 and CNCI was observed. At higher flow rates the response for (CN)2 increased markedly whereas at the same flow rates the response for CNCI increased only slightly.
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  • 7
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    Chromatographia 21 (1986), S. 214-218 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Behaviour of metal acetylacetonates ; Adsorption isotherms ; Heat of solution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Specific retention volumes, adsorption isotherms, molar heats of solution and changes of the entropy were determined from chromatographic data, which was obtained by the gas chromatographic separation of metal acetylacetonates. The retention data for Cr(III), Co(III) and Al(III) acetylacetonates were measured at different temperatures and different flow rates. From the retention data other values associated with adsorption and solution phenomena were calculated.
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  • 8
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Immobilized stationary phase ; Carbowax-type stationary phase ; Cross-linked polyurethane
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The preparation of an immobilized stationary phase based on Carbowax 20M is described. The stationary phase cross-linking was carried out with Desmodur N 75 or Desmodur L 75, pluriisocyanates. The properties of the prepared stationary phases are compared.
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  • 9
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Volatile nitrosamines ; Fused silica capillary columns ; Linear indices
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Fused silica capillary columns of different diameters and polarities are linked to a thermal energy analyzer and a flame ionisation detector for comparison. Extra column effects are discussed. Unsymmetrical homologue nitrosamines are applied in order to assign the volatile nitrosamines most often to be determined by their linear indices rather than by their overall retention times.
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  • 10
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Thermionic detector ; Flame-forming agents ; CO2 and water gas
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The use of carbon monoxide were suggested as the flame-forming agent in the thermionic detector (TID). The main characteristics of this detector were studied. It was shown that the optimum flow rate of carbon monoxide is 40 ml/min at an air flow rate of 400–550 ml/min. The response increases twice with the positive potential on the collector. Molar responses of TID were compared with those obtained when using carbon monoxide and hydrogen. For instance, for phosphorus containing compounds they are approximately the same (∼102), while for nitrogen containing compounds in the case of carbon monoxide, there is a 2–5 fold increase in the response. The linear dynamic range for methaphose and azobenzene is 103.
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  • 11
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Metal complexes ; Chemically bonded phase ; Specific interactions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Packings consisting of chemically bonded diphenylphosphine complexes with CuCl2 and CuBr2 were synthesized and their retention parameters determined. The packings investigated are capable of specific interactions with electron-donating compounds and are characterized by particularly high selectivity in relation to cis and trans isomers allowing their complete separation.
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  • 12
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    Chromatographia 23 (1987), S. 818-824 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Selective sampling ; On-line fractionation ; Essential oil analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The paper describes the possibilities of on-line selective sampling as an on-line fraction technique for the analysis of essential oils. Selective sampling is a micro-separation method, on-line with on-column injection, carried out directly in the syringe body by means of a selective elution of the sample through a fraction cartridge. The paper reports a method of both preparing and standardizing silica gel cartridges, and illustrates through some examples the results of some elution series of solvents on different essential oils.
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  • 13
    ISSN: 1612-1112
    Keywords: Organic pollutants determination ; Gas chromatography ; Thermal desorption
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The problem of the separation of 34 volatile organic chlorinated compounds is solved by using three different GC columns selected according to the needs of the particular separation required. The effect of water vapor contained as moisture in the trapped air on the retention of some characteristic compounds is studied. The influence of dead volumes on trap injection is also studied.
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  • 14
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    Chromatographia 23 (1987), S. 888-892 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Calculation of temperature programmed ; Retention indices
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new method is presented for the calculation of the retention indices under linear temperature programming with or without an initial isothermal period. The data calculated by the method are in good agreement with the isothermal retention indices.
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  • 15
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Propyl esters of aromatic polycarboxylic acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The direct esterification and gas chromatographic analysis of aromatic carboxylic acids as n-propyl esters is described. Derivatization is performed in aqueous solution with n-propanol in the presence of sulfuric acid. The n-propyl esters of benzoic, phthalic, trimellitic and pyromellitic acids permit their gas chromatographic separation from each other and from fatty acids and aliphatic dicarboxylic acids. At mode ratios of [H2O]/[n-PrOH]≤0.03 the water present does not interfere with the esterification reaction. At mole ratios above 0.03 anhydrous sodium sulfate is used for binding the water, at mole ratios of [Na2SO4anh.]/[H2O]=0.51–1.52 and of [H2SO4]/[Na2SO4anh.]=0.43–1.28, respectively.
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  • 16
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Micropacked columns ; Quantitation ; Fermentation products
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new method is proposed for the analysis by gas chromatography of volatile compounds found in alcoholic and acetic fermentation samples. The method represents a suitable choice for the accurate and precise determination of 19 compounds (including Methanol) by direct injection onto a single column. Chromatograms of synthetic mixtures as well as actual samples show the capabilities of the micropacked column used.
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  • 17
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    Chromatographia 23 (1987), S. 195-198 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Structure-retention relationships ; Polarity parameters ; Retention index
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The possibility of evaluation of the parameters representing the dispersive solute-solvent interactions is presented. BN and Bs values can be used to describe the liquid phase polarity and to predict the retention indices of alcohols when the model polyxyethylene glycol dialkyl ethers and their sulphur analogs are used as stationary phases. The possibility of the first ionization potentials estimation is also presented.
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  • 18
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Prediction of retention volume ; Porous polymers coated with liquid phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new expression which permits the prediction of the net retention volumes in gas chromatography with column packings of coated porous polymers is reported. The porous polymers Chromosorb 101 and Chromosorb 102 were used as supports and squalane, Ethofat and Carbowax 20M as stationary phases at three different column temperatures of 80°C, 100°C and 150°C. Several organic compounds of various polarity were used as test compounds and the net retention volumes, VNtheor, have been calculated according to this new expression. The VNtheor values were compared with the experimental net retention volumes, VNexp, and it was found that the difference between these two values is dependent on the type of compound and column packing. Nevertheless, the elution order could be predicted in most cases.
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  • 19
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    Chromatographia 23 (1987), S. 499-501 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Packed+capillary GC switching system ; Precolumn construction, oven and connector
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The constractional details of precolumns, its oven and connector have been given with two types of multiflow control modules. Two types of phases made in China, a silanized pellicular beads and a non silanized pellicular silica beads, with an optimum particle size of 20μm to 30μm were packed in the precolumn 20mm in length with the column efficiency of 4620 plates/meter at column temperature of 49°C. A 25m×0.22mm i.d. capillary column coated with bonded methylsilicone phase from Chrompack connected with the precolumn (250°C) has an efficiency of 5376 plates/meter for n-octane. But it decreased to 3149 plates/meter by decreasing the precolumn temperature to 130°C.
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  • 20
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Immobilized Carbowax-type stationary phases ; Free fatty acids analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Capillary columns coated with acid-modified poly-(ethylene glycol)-type immobilized stationary phases have been studied. The thermostability and chromatographic behaviour of the columns and the stability of the coated films after washing with different solvents were investigated.
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  • 21
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fourier transform IR detection ; Headspace sampling ; Solvents of abuse
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary After experimental intoxication of rats, gas chromatography — Fourier transform infrared spectrometry with headspace sampling (HS/GC/FT-IR) was used to identify solvents of abuse in biological material (blood, liver, lungs and brain). Limits of detection were measured for acetone, 2-butanone, ether, toluene and trichlorethylene with standard solutions. All the solvents have been identified in the organs of the intoxicated rats. For blood samples a salting-out effect was obtained with potassium carbonate. HS/GC/FT-IR allowed the identification of metabolites of acetone (isopropanol) and of 2-butanone (2-butanol) in blood and organs.
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  • 22
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Simultaneous distillation-extraction ; Cheese volatiles
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simultaneous distillation-extraction apparatus proposed by Godefroot has been used for the GC study of volatile components of cheese. 5–10 g of cheese provide a fraction that can be directly injected into a GC or a GC/MS. Two capillary columns (SE-30 and SP-1000) were evaluated, the second one being adequate for quantitative determinations. Camphor was used as internal standard. The coefficients of variation ranged from 1.4 to 11.8. The technique can be used as a fast method for the characterization of cheeses from their volatile component concentrations.
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  • 23
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    Chromatographia 25 (1988), S. 1087-1088 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Log plot ; Homologous series
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The slope of the log plot of the adjusted retention time of a homologous series usually varies from that of the n-alkane series by no more than 2%, though with unusual interactions between the functional group and the stationary phase the difference may be as high as 7%.
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  • 24
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Preparative scale separations ; Plate model
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two close-boiling materials, diethyl ether (DEE) and dichloromethane (DCM), were separated to investigate the effects of the pure components and the mixture on elution in preparative gas-liquid chromatography. Nitrogen was used as the carrier gas, and the chromatographic column (1 cm I.D. and 0.75m length) was packed with Chromosorb A with different quantities of dinonyl phthalate stationary phase and particle sizes. Below ca. 7% (by wt.) of feed concentration, the experimental elution curves of pure DEE and DCM were almost the same as those of the mixture, and the theoretical plate model can be used successfully to predict the elution curves.
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  • 25
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    Chromatographia 25 (1988), S. 404-408 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Silica surface modification ; Hexamethylcyclotrisilazane ; Hexamethyldisilazane ; Support materials
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The paper is concerned with the structure of an organic layer bonded to the silica surface modified with silazanes. The changes of the retention volumes of hydrocarbons is studied for the silicas modified with hexamethylcyclotrisilazane, hexamethyldisilazane and their mixtures. It is shown that most of the carbon in the layer after hexamethylcyclotrisilazane modification is bonded to the surface by Si−O−Si bonds. This fact supports the assumption of a fragmentation of the cyclosilane used for modification.
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  • 26
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Statistical criteria ; Non-linear models ; Constants for n-alkane retention curve ; Multiparametric least-squares adjustment
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Multiparametric, least-squares, regression treatment of G.C. data is extended to describe deviations from the usual linear model. Through statistical evaluation of results, four parameters models are generally found adequate and the use of higher degree empirical models is discouraged.
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  • 27
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    Chromatographia 25 (1988), S. 539-542 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Temperature programming ; Retention index
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method is presented for the calculation of retention indices at an assigned temperature from temperature-programmed data. If the retention times at two different program rates for the solutes and the n-alkanes are known, the retention indices at an assigned temperature can be calculated directly.
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  • 28
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    Chromatographia 22 (1986), S. 183-186 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; C2−C5 hydrocarbons ; Pre-Concentration on silica gel ; Sorption efficiency
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A short stainless steel column packed with silica gel is cooled to −78°C and atmospheric hydrocarbons are preconcentrated from 3 I of air on it. Desorption to the analytical column is by heating for 10 min to 200°C. Analysis is by GC on OPN-Poracil C at 27°C. The sorption efficiencies were nearly 100% for most of the light hydrocarbons.
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  • 29
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    Chromatographia 26 (1988), S. 125-132 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Non-equilibrium frontal chromatography ; Nonlinear isotherms ; Variable velocity ; Multicomponent mixtures
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The paper presents a classification of various theoretical models for multicomponent gas chromatography at u=var for high concentrations of the mixture components with consideration of the major distinctive features of the interphase mass exchange inside the porous grains of the adsorbent and outside them within the porous medium of the chromatographic column. It has been shown that the conditions determining a given front behaviour of multicomponent gas mixture at u=var depend on: theoretical models for the kinetics and dynamics of adsorption; the values of mass exchange parameters inside the porous grains and in the porous medium. Formulae have been derived for calculating the values of the quantities characterising the frontal behaviour in the stage of adsorption and desorption of multicomponent mixture at u=var.
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  • 30
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Physico-chemical properties ; Retention indices ; Cycloolefins
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention indices of mono and polycycloolefins with endo or exo double bonds, on squalane or polypropylenglycol 425 are related to their physico-chemical properties such as boiling point, molar volume, molar refraction, and refractive index. Equations have been empirically obtained, from which accurate retention indices of these compounds can be predicted. Unknown boiling points of some of these compounds can also be calculated from their lineal relation with the retention index on squalane.
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  • 31
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    Chromatographia 23 (1987), S. 839-843 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary phases ; Porous polymer beads ; Polarity ; Adsorbents ; Breakthrough volume
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The breakthrough volume of ådsorbent traps made with porous polymer beads Porapak N, P. Q, R, S was evaluated by analysis of polarity reference substances proposed by Rohrschneider (ethanol, methyl ethyl ketone, nitrometane, benzene, pyridine) by McReynolds (butanol, methyl propyl ketone) and of the first term of some homologous series: alcohols, aldehides, carboxilic acids, nitrocompounds, iodoalkanes and nitriles. Adjusted retention times of the compounds were measured at 200°C and correlated with the physical properties and with polarity class according to Ewell. Trapping efficiency of the various Porapak types was evaluated and the theoretical breakthrough volumes at 25°C was calculated for the used test substances.
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  • 32
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    Chromatographia 23 (1987), S. 850-855 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Bacterial cellular fatty acids ; Stationary phase selectivity ; Solid phase preseparation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The importance of selectivity in the capillary gas chromatographic analysis of the cellular fatty acids of micro-organisms is underestimated. The analysis on apolar silicone phases can lead to erratic elucidation of the fatty acid structure. Qualitative errors have been detected in commercially available standards on which computer matching identification techniques are based. Using highly polar capillary columns of the cyanopropyl silicone type, the errors could be elucidated. The exact identification of the hydrolysis products of bacteria is a must for chemotaxonomic studies applying chromatographic techniques. The fatty acid methyl ester profiles can also contain other chemical components which are very important taxonomic markers. Fatty aldehydes, for example, are main components in someClostridium species. Fractionation techniques are described for selective enrichment of fatty aldehydes and hydroxy fatty acids.
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  • 33
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    Chromatographia 27 (1989), S. 37-43 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Methylbromide ; Charcoal tubes ; Pollution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Air sampling of methylbromide using 900 mg HBr-treated activated charcoal tubes, followed by solvent desorption and FID or ECD chromatographic analysis, makes it possible to evaluate concentrations ranging from 0.2 ppm (1 mg×m−3) to 250 ppm (1g×m−3) at ambient temperature even with a high hygrometric level. Thermal desorption does not lead to satisfactory results.
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  • 34
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    Chromatographia 27 (1989), S. 60-66 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Mass loadability ; Stationary phase capacity ; Capillary columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In GLC the mass load can be normalized with respect to the amount of stationary phase in one plate. This quantity can be used for a specified solute-liquid phase combination in any capillary or packed column, irrespective of the column dimensions or the number of plates. For each individual solute in a given stationary phase a unique factor β″ can be found, which accounts for the specific shape of the isotherm of this particular combination. this factor β″ corresponds well with the activity coefficients of the solutes in the stationary phase, by which a fairly good approximation of the mass loadability of the column at hand can be made without need for experiment.
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  • 35
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    Chromatographia 23 (1987), S. 215-219 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid chromatography ; Thermodynamic equilibria ; Solution and adsorption thermodynamics ; Gas adsorption isotherms
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary After a brief recall of the chromatographic principles, the different applications of gas chromatographic measurements of thermodynamic equilibria were reviewed. Gas and liquid chromatographies are now well known and elegant methods for measuring the physicochemical properties and phase equilibrium thermodynamic constants. Although fundamentally a dynamical method and mostly known as a powerful separation technique, chromatography can be schematized by a sucession of equilbria of a chemical species partitioning between a mobile phase and a fixed liquid or solid stationary phase. It can be operated in either infinite dilution or finite concentration conditions and permits to collect a large number of data for calculating molecular interactions for solutes which are either rare or available at the trace level. Gas chromatography permits the measurement of gas adsorption isotherm, gas-liquid equilibria, molecular diffusion and interaction virials. The modelization of successive partition equuilibria occuring in the chromatographic column leads to rather simple expression of differential enthalpy, entropy, free energy of adsorption or solution, variation of heat capacity, complexation constant, second virial coefficients, gas-solid and gasliquid isotherm and also binary or ternary equilibria. The possibilities of High Performance-Liquid Chromatography to investigate adsorption from solutions and chemical equilibria are also discussed.
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  • 36
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Aqueous samples ; Direct injection ; Traces of ketones and halogenated hydrocarbons ; Environmental analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary Procedures for the quantitative analysis of industrial effluents which involve concentration by solvent extraction or the purge-and-trap method are time-consuming, labor-intensive, and prone to error. Direct aqueous injection gas chromatography using an electron-capture detector for the analysis of volatile halocarbons at the ppb level is in routine use in many laboratories. We now discuss the development of a similar protocol for the analysis of volatile polar organics such as acetone, methyl ethyl ketone, methyl isobutyl ketone, and tretrahydrofuran using a flame-ionization detector.
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  • 37
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Nitrogen-specific detector ; Flash methylation ; Barbital and pentobarbital ; Blood analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary A sensitive and simplified method is described for the determination of barbital (B) and pentobarbital (PB) in blood using gas chromatography with a nitrogen-specific flame ionization detector. After a simple one-step extraction, B and PB were reconstituted in trimethylanilinium hydroxide and introduced directly into the gas chromatograph. Lower limits of detection was 0.14 μg/ml for B and PB in either water or blood solutions. The recoveries for B from water and blood were 90 and 88%, respectively; for PB they were essentially complete. The average between-run and within-run coefficients of variation for B from water and blood were lower than 7.8%, whereas those of PB were lower than 3.0%. The scale and sensitivity of detection for B and PB were found to be suitable for use in pharmacokinetic studies in the rat.
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  • 38
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    Chromatographia 23 (1987), S. 423-426 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Complexation ; Mercaptosilane chemically bonded phase ; Transition metal complexes ; Olefinic π-complexes
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    Topics: Chemistry and Pharmacology
    Notes: Summary A column packing containing thiol groups chemically bonded to the silica surface was synthesized. The thiol functional groups were used as ligands capable of forming stable complexes with Cu(II). The prepared material was characterized by gas chromatography using unsaturated linear and branched hydrocarbons as well as cyclic and aromatic hydrocarbons. The occurrence of specific metal—olefin interactions resulting from the formation of π-complexes during the chromatographic process was observed.
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  • 39
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Backflushing, peak-cutting technique ; Trace analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary A backflusing, peak-cutting method was developed for the analysis of trace components present in the tail of a major component peak. Using a helium-ionization detector, the minimum detectable concentration (MDC) was: oxygen in hydrogen, 0.5ppm; nitrogen in oxygen or argon, 1ppm; and methane and carbon monoxide in nitrogen, 1ppm. The corresponding MDC values for the conventional single-column method were 7.2ppm, 8.3ppm, and 14 and 5ppm, respectively. Equations used to predict the retention time are given. The accuracy of the predicted retention time is about two percent compared to experimental results.
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  • 40
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Alkylthiazoles ; Energy contributions of the alkyl groups ; Retention indices
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    Topics: Chemistry and Pharmacology
    Notes: Summary Retention indices and their energy equivalents were determined for ten alkylthiazoles analysed on the stationary phases Apiezon L, Triton X-305 and Carbowax 1000. It was found that the energy contributions of identical alkyl groups to the partial molar free energy of sorption of a molecule are not equivalent. Smaller energy contribututions are due to the α-position of alkyl groups with respect to the heteroatoms in the thiazole ring (α-effect). This effect was most pronounced for 2-alkylthiazoles. Higher sorption energies were found for dimethylthiazoles with two methylgroups in a vicinal position. The retention indices were predicted for ten other di- and tri-substituted methyl, ethyl and propyl thiazoles on the basis of the so-called α- and ortho-effects. The predicted values are in good agreement with the experimentally determined values.
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  • 41
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid crystal ; Capillary columns ; Retention data ; Stationary phase film thickness ; Column surface quality
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    Topics: Chemistry and Pharmacology
    Notes: Summary Glass capillary columns were prepared from non-deactivated and deactivated glass and coated with (2-methyl-4-[trans-4-n-propyl-cyclohexylcarbonyloxy]-benzoic acid-[4-n-heptyloxy-phenylester]) as the liqud phase, in different film thicknesses. The columns were tested using substances of different structures and polarities. It was verified that the capacity factors, retention indices and selectivity significantly depend on the thickness of the liquid crystalline stationary phase film and the quality of the tube, particularly in the case of columns with thin films. Trasition temperatures (melting and clearing point) of the liquid crystal are also dependent on these two factors.
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  • 42
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    Chromatographia 25 (1988), S. 21-24 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Sample concentration ; Chromatographic evaporation ; Solvent effect
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    Topics: Chemistry and Pharmacology
    Notes: Summary Several micro-techniques for the removal of solvent from dilute solutions of volatile compounds have been compared. Large solute losses were experienced when the conventional blow-down technique was applied. Better yields could be obtained with static evaporation procedures, as long as an effective reflux was maintained. However, careful optimization of the vessel design and operating conditions is necessary. The most efficient volume reduction technique was shown to be chromatographic evaporation. Quantitative recoveries were obtained for the compounds tested and the process was significantly faster than static concentration. Moreover, operating conditions (gas flow, temperature) are less critical. With modifications, the principle can be used for the concentration of large sample volumes down to a few microliters.
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  • 43
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Butyl esters of amino acids
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    Topics: Chemistry and Pharmacology
    Notes: Summary Amino acids have been esterified with n-butanol and isobutanol in the presence of perchloric acid. It has been established that in the concentration range of [H2O]/[n-BuOH]=0.10–0.40 esterification can be utilized for the determination of alanine, glycine, valine, leucine, proline, methionine, aspartic acid, phenylalanine, tyrosine, glutamic acid, lysine, arginine, histidine and cystine. In the case of [H2O]/[i-BuOH] =0.05–0.20 the esterification yield decreases from 100% to 70%, in proportion to the water content.
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  • 44
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    Chromatographia 20 (1985), S. 681-682 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Geothermal gases ; Molecular sieves ; Low temperature separations
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    Topics: Chemistry and Pharmacology
    Notes: Summary The gases evolved from geothermal fields, after condensation of H2O, CO2, H2S and NH3 in caustic solution, contain He, H2, Ar, O2, N2, CH4 and higher hydrocarbons. The analysis for the major components in these residual gas mixtures can be achieved by use of two simple gas chromatographs in parallel, and using 5Å molecular sieve. The separation of He and H2 to baseline is achieved by using low temperatures (30°C) coupled with a relatively long column; and the difficult separation of Ar and O2 is achieved by use of a cryogenically cooled column. The use of switching valves to backflush and bypass columns ensures that a minimum time for analysis can be achieved whilst retaining baseline separations of the He/H2 and Ar/O2 pairs.
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  • 45
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    Chromatographia 20 (1985), S. 685-688 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fuming sulphuric acid-ethanol esterification ; Ethyl and methyl esters of herbicides
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    Topics: Chemistry and Pharmacology
    Notes: Summary A fuming sulphuric acid-ethanol esterification method has been applied to chlorophenoxy acids and some other herbicides. This method is compared with esterification by iodoethane and diazomethane. The chlorophenoxy acids studied were: 2,4-D, dichlorprop, MCPA, MCPB, mecoprop and 2,4,5-T. Other herbicides studied were: benazolin, bentazone, bromophenoxime, bromoxynil, chlorthal, dicamba, 3,6-dichloropicolinic acid, dinoseb, ethephon, fluroxypyr, glyphosate, haloxyfop, ioxynil, picloram, 2,3,6-TBA and triclopyr. Fuming sulphuric acid-ethanol esterification can be successfully applied to chlorophenoxy acids, benazolin, 3,6-dichloropicolinic acid, dinoseb, fluroxypyr, haloxyfop, picloram and triclopyr. The reproductibility of the method is ±5%.
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  • 46
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stationary phase polarity ; Polarity parameters ; Structure-retention relationships
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    Topics: Chemistry and Pharmacology
    Notes: Summary The new stationary phase polarity parameters BN and BS evaluated from the concept of the electric intermolecular interactions are used to describe the polarity of polyoxyethylene glycol dialkyl ethers and their sulphur analogs. Relations between the discussed parameters and accepted measures of surfactants' polarity are presented and discussed. The considered parameters are correlated with the compound structures. Structural increments for characteristic fragments of the molecule are calculated and use to predict BN and BS values.
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  • 47
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    Chromatographia 25 (1988), S. 134-138 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Sulfur ; n-Octane adsorption
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    Topics: Chemistry and Pharmacology
    Notes: Summary From the adsorption isotherms of n-octane on the surface of sulfur at 29.8°C and 40.6°C some thermodynamic functions were determined. On the basis of these data the structure of the adsorbed layer of n-octane is postulated. The molecular interactions and adsorption mechanism are also discussed. It is stated that both quasi-liquid and quasi-sold layers may be formed on the surface of sulfur depending on the surface coverage with n-octane.
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  • 48
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Step profile method ; Adsorption isotherm ; Water film pressure ; Surface free energy
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    Topics: Chemistry and Pharmacology
    Notes: Summary Investigation of water adsorption by the step profile method (Glueckauf method) was carried out with the help of a modified gas chromatography equipped with thermal-conductivity detector. On the basis of the adsorption isotherm obtained, the water film pressure and the polar component of the surface free energy of quartz were calculated. The calculated value of the polar component of the surface free energy of quartz agrees with analogous values obtained by other methods.
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  • 49
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    Chromatographia 25 (1988), S. 313-318 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index ; Slope of log plot ; Homologous series ; Partition coefficient
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    Topics: Chemistry and Pharmacology
    Notes: Summary The slope of the n-alkane log plot dt′R/dnc (t′R=adjusted retention time; nc=carbon number) for a stationary phase can be used to obtain the retention index of an unidentified substance in a chromatogram containing only one peak with a known retention index, or to predict the retention time of a substance from that of a different homolog in the same series. It can also be used to translate retention indices into relative retention time, partition coefficient or specific retention volume. Published values of the slope are collected and critically evaluated. Equations are deduced that predict its approximate value at a specified temperature given the value at only one other temperature.
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  • 50
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    Chromatographia 25 (1988), S. 393-396 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Separation of optical isomers ; Chirasil-Val capillary columns ; Amino acid esters
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    Topics: Chemistry and Pharmacology
    Notes: Summary D,L-amino acids were derivatized with (+), (±)-2-butanol or N-trifluoroacetyl-L-prolyl chloride (L-TPC) and then chromatographed. Four optical isomers were separated on a Chirasil-Val capillary column. By this method, the concentration of optical impurities arising from the commercial optically active reagents can be determined. The observed abnormal elution orders of enantiomeric amino acid esters may be caused by a selective intermolecular force.
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  • 51
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Essential oils ; Evaporation rate ; Perfume composition
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    Topics: Chemistry and Pharmacology
    Notes: Summary A simple method was developed for the determination of the evaporation rate of essential oils and perfumery composition using gas chromatography with temperature programming. The volatility of 19 essential oils and 17 perfumery composition was evaluated. The method is useful for different comparative measurements.
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  • 52
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    Chromatographia 25 (1988), S. 598-602 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Steroid profiles
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    Topics: Chemistry and Pharmacology
    Notes: Summary Steroid conjugates are hydrolysed enzymatically using β-glucuronidase after extraction from urine using a solid phase extraction cartridge. After hydrolysis the free steroids are removed from the matrix, again utilising solid phase extraction. Derivatisation of the free hydroxyl groups using Hydrox-Sil AQ produces the respective TMS ethers which are extracted into hexane, in which solvent they are stable for many days. Capillary GC analysis with flame ionisation detection produces a profile of the steroids present in the sample. This technique is suitable for following changes in the urinary excretion profiles of patients undergoing investigation for a variety of steroid production-related diseases.
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  • 53
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    Chromatographia 25 (1988), S. 609-612 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography ; Triglyceride composition of grapes ; Identification system
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    Topics: Chemistry and Pharmacology
    Notes: Summary The triglyceride composition of the Tempranillo grape (Vitis vinifera) has been examined by a combination of HPLC and GLC. To identify the triglycerides, equations were applied relating log k′ with the molecular variables: equivalent carbon number, chain length and number of double bonds in each of the fatty acids in the glycerides. Ten triglycerides were found, the principal ones being trilinolein (35.75%), dilinoleyl-olein (21.03%) and dilinoleyl-palmitin (17.02%).
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  • 54
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    Chromatographia 25 (1988), S. 655-658 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Structure-retention relationships ; Connectivity indices, topological indices ; Alkenes
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    Topics: Chemistry and Pharmacology
    Notes: Summary Retention indices of different alkenes are correlated with connectivity and topological parameters. The appropriate statistically valid relations hips are derived and discussed.
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    Chromatographia 25 (1988), S. 735-736 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; α,ω-diiodoperfluoroalkanes ; Separation ; identification
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    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of α,ω-diiodoperfluoralkanes on a glass capillary column coated with OV-101 methylsilicone was investigated. Retention indices were determined at three temperatures (140, 150 and 160°C). The correlation between the retention indices and the boiling points of the investigated compounds was studied.
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  • 56
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    Chromatographia 25 (1988), S. 731-734 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention Index (l) ; Temperature dependence of Retention Index
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    Topics: Chemistry and Pharmacology
    Notes: Summary A linear dependence of (T−T1)/[1(T)−1(T1)] on temperature (considering the retention index 1(T1) at temperature T1 as a standard value) is derived. Both ther retention index at an assigned temperature and the temperature dependence of the retention index can be calculated from retention data measured at two temperature-programing rates.
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  • 57
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    Chromatographia 26 (1988), S. 171-177 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; GC/MS analysis ; Polycyclic aromatic hydrocarbons ; Bituminous coal ; Brown coal ; Plant waxes ; Thermodesorption
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Polycyclic aromatic hydrocarbons (PAH) today are ubiquitous detectable constituents of recent sediments. The compounds are adsorbed on particulate emissions and are thus transferred to the environment. To date the analysis of PAH in sediments, dust samples and plant material is based mainly on the application of solvent-extraction methods followed by liquid chromatography and/or gas chromatographic separation of the extracts. An alternative approach for the analysis of PAH in solid samples such as coal, sediments, dust samples and plant waxes is shown in this contribution. A commercially available device for the analysis of volatile compounds present in solid matter is connected on-line to a GC/MS system. The device enables the thermal desorption of hydrocarbons at a temperature of 320°C. Subsequently, the hydrocarbons trapped on the initial part of the capillary column are analyzed by GC/MS. The application of mass chromatography provides the possibility of detection and quantitation of PAH in complex mixtures even when they coelute with other compounds. The sample amount required varies between 1 and 10 mg depending on the hydrocarbon content.
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    Chromatographia 26 (1988), S. 229-233 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Glass capillaries ; Chirasil-Val ; Immobilisation ; Enantiomeric separation
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    Topics: Chemistry and Pharmacology
    Notes: Summary Immobilisation methods of the chiral silicone stationary phase Chirasil-L-Val have been studied. In addition to the standard techniques of radical-induced immobilisation with dicumyl peroxide and azo tert-butane, immobilisation was solely achieved by thermal treatment: conditioning at low flow-rates or under stop-flow conditions led to unexpectedly high immobilisation despite mild temperatures. The presence of water vapor in the carrier gas accelerated the immobilisation process. While up to 75% immobilisation was attainable with both ATB and thermal methods, immobilisation with DCUP did not exceed 50%, despite relatively high DCUP concentrations. Whilst all immobilisation methods were accompanied by varying degrees of racemisation at the chiral centre, it was possible to establish conditions that yielded a high immobilisation (in excess of 70%) with a negligible loss in enantiomeric selctivity. The immobilisation reactions also slightly affected the polarity of the stationary phase, reflected in a shift of the Kovats-Indices of amino acid derivatives and in the accompanying “Squalane-Effect”. With respect to immobilisation, racemisation and polarity shift, thermal immobilisation with water-saturated carrier gas proved to be the optimum method.
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  • 59
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    Chromatographia 27 (1989), S. 552-558 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Radio gas chromatography ; 3H- and14C-labelled compounds ; Isotope effects
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    Topics: Chemistry and Pharmacology
    Notes: Summary Radio gas chromatography (RGC) is a valuable tool for the analysis of radioactively labelled compounds. Recent advances in capillary GC, especially in column technology and instrumentation have also induced new possibilities in this field. With regard to the preservation of the achieved separation efficiency, radioactivity detection is the main problem in capillary RGC. Based on published data and on our extensive experience in conventional RGC, a simple, reliable and versatile method has been developed for the radioactive detection: purge gas is added to the effluent of the capillary column and the RGC detection unit with conversion tube and flow-through proportional counter is used maintaining small dead volumes and dimensions. The influence of the extra-column volumes and of the total gas flow rate (of the carrier, purge and quenching gases) on the peak shape was investigated. It was also found that the isotopic effect commonly known in GC of2H- and3H-labelled compounds is hardly measurable for larger [G-14C] labelled species such as [G-14C] labelled higher fatty acids with high isotopic abundance of14C, even on the highly efficient capillary columns. The quantitative aspects of the detection method used are discussed and some applications to the analysis of labelled biochemicals (amino and fatty acids) are demonstrated.
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    Chromatographia 27 (1989), S. 644-648 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Ion exchange resins ; Polymeric supports ; Chloromethanes
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    Topics: Chemistry and Pharmacology
    Notes: Summary The retention of compounds of various classes on macroporous sulfonated cation exchangers in the form of the fourth period elements in Mendeleev's table (i. e. in the K, Ca, Co, Ni, Cu, Zn-forms) has been investigated. It has been shown that these sorbents are characterized by a high specificity of molecular interaction. It has also been established that the gas-chromatographic properties of cation exchangers depend on the nature and valency of the metal ion in the ionogenic group.
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    Chromatographia 27 (1989), S. 109-112 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Packed columns ; Immobilized stationary phase ; Poly(ethylene glycol) phase
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    Topics: Chemistry and Pharmacology
    Notes: Summary Carbowax 20M poly(ethylene glycol) stationary phase was immobilized on Chromosorb W by cross-linking with pluriisocyanate. The properties of the prepared packing material were investigated. Column efficiencies of 10,960 and 7,510 theoretical plates/meter were obtained for n-pentadecane and 1-heptanol, respectively.
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    Chromatographia 27 (1989), S. 159-163 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Flame photometric detector ; Sulfur compounds ; Response quenching
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    Topics: Chemistry and Pharmacology
    Notes: Summary The long time retardation of the main hydrocarbon peak in the chimney of the flame photometric detector greatly reduces the responses of later-eluting sulfur compounds. In the absence of hydrocarbons in the flame, the slope (s) of the log I vs. log [S] plot (where I is the sulfur response and [S] is the sulfur concentration in the sample) is of the highest value and is constant for all experimental conditions tested. Flame hydrocarbons cause the s value to decrease, and this is dependent on the oxygen to hydrogen ratio in the flame (O/H) and, under certain conditions, also on the sulfur to carbon ratio (S/C) of the sample. The abnormalities observed in the determination of methyl thiol in natural gas are explained on the basis of the present study.
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    Chromatographia 27 (1989), S. 631-632 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Wide-bore glass capillary columns ; End-sealing ; Static coating
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    Topics: Chemistry and Pharmacology
    Notes: Summary An end-sealing method to be used for static coating of wide-bore glass capillaries is described. After the capillary was completely filled with the coating solution, one end is connected to a gas-tight syringe (10-ml volume) via silicone tubing and the other end is fixed with shortcutted silicone tubing for sealing with a plug. The method is highly successful.
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  • 64
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Ethyl carbamate ; Direct injection quantification ; Cold injection system ; Optimised SIM
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    Topics: Chemistry and Pharmacology
    Notes: Summary An integrated procedure is described which allows direct injection quantitative screening to single figure parts per billion (μg/L) levels of ethyl carbamate in the natural matrix of distilled alcoholic beverage. Injection and detection performance was studied and optimized to allow this routine, reproducible, trace analysis without any sample pre-treatment. All aspects of the analysis including autosampler run sequences and automated internal standard report generation are initiated and controlled from a single GC/MS workstation.
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    Chromatographia 27 (1989), S. 455-460 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Surface free energy ; Silane-covered materials ; Film pressure
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    Topics: Chemistry and Pharmacology
    Notes: Summary The surface free energy, or film pressure, π0, is measured for mica (Mica HK), silane-covered mica (Mica NP), Chromosorb W DMCS and glass beads. The film pressure is obtained from gas chromatography. The materials are used as adsorbents and benzyl alcohol and n-dodecane are used as molecular probes. Adsorption isotherms at 353 K are obtained from gas chromatography data and the surface free energy is computed with the help of the Gibbs equation. Values of π0 for a given surface are found to vary with the molecular probe. With benzyl alcohol π0 varies from 44 erg/cm2 for Mica 60 HK to 76 erg/cm2 for glass. In the case of n-dodecane π0 is found to vary in the same manner but the values range from 25 to 45 erg/cm2. The results are in good agreement with the values obtained with the contact angle method.
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    Chromatographia 27 (1989), S. 469-471 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Headspace analysis ; Ethylene oxide ; Capillary column
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    Topics: Chemistry and Pharmacology
    Notes: Summary A headspace gas chromatographic method for determination of traces of ethylene oxide (EO) in sterilized materials has been developed. The method allows the determination of the amount of EO by putting the samples directly into acetonitrile and analysing by means of headspace GC. The procedure described is simple, sensitive, reproducible and linear. The lower limit of detection is 0.015 μg/g of sterilized material.
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    Chromatographia 28 (1989), S. 24-26 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Anesthetics ; Pharmacokinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A sensitive capillary gas chromatographic method is described for the simultaneous determination of lidocaine, tetracaine, procaine and dibucaine. The method was applied to the determination of anesthetics in tissue homogenates incubated at 38°C at doses between 10 and 400 mg/kg. In the liver tissue thein vitro metabolization of the studied anesthetics is most rapid for tetracaine, also fast for procaine, while for lidocaine and dibucaine the metabolization is very slow. In brain tissue thein vitro metabolization of anesthetics is very slow. The method shows good analytical parameters: linearity between 5 and 40 μg/ml; day-to-day reproducibility ca. 8% for a concentration of 20 μg/ml, precision ca. 7% for a concentration of 20μg/ml. Accuracy is also very good.
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  • 68
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    Chromatographia 28 (1989), S. 639-642 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Split injection ; Sample tailing and cold trap effects
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    Topics: Chemistry and Pharmacology
    Notes: Summary Sample plug tailing together with a cold trap effect brings about discrimination against low boiling components at an initial column temperature above the boiling point of the solvent. In conventional split injection, this compensates for the opposite effects of such factors as the gas phase viscocity change and the pressure wave during the split period, and reasonable results are obtained. In stop-flow injection, however, since the influences of the opposite factors are diminished, the sample plug tailing and the cold trap effect may produce results showing lower than true concentrations for the low boiling components.
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  • 69
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    Chromatographia 28 (1989), S. 313-314 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fused-silica columns ; Static coating ; Sealing method
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    Topics: Chemistry and Pharmacology
    Notes: Summary In this paper a new sealing method for the static coating of capillary columns is described. When one end of the fully filled capillary was immersed into liquid nitrogen in a Dewar flask, the coating solution at this end would be frozen and became a temporary seal, and an air-free solvent/seal interface was obtained. No bumping has ever been found at the interface, even when butane was used as solvent. By applying this sealing method, several capillary columns, including some narrow bore capillary, had been successfully coated.
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  • 70
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    Chromatographia 28 (1989), S. 502-504 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention variation ; Effect of sample composition on retention
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    Topics: Chemistry and Pharmacology
    Notes: Summary The variation of the retention index of a solute due to the presence of a closely neighboring peak is discussed. The neighboring peak is likely to modify the original stationary liquid by forming a temporary “mixed” stationary phase. The extent of the retention index variation is influenced by many experimental parameters and becomes pronounced when the stationary phase is overloaded by the neighboring peak and the film thickness of the stationary phase is not very large. However, the exact extent of this variation is rather unpredictable. The practical significance of this finding is also discussed.
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  • 71
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Electron-capture ; Thermal-energy electrons
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    Topics: Chemistry and Pharmacology
    Notes: Summary The products resulting from the reaction between thermal energy electrons and organic compounds have been investigated to further our knowledge of the mode of action of the electron-capture detector. Thermal energy electrons were generated by maintaining a corona discharge between a stainless steel cathode and a silver/silver chloride anode. The effects of electrode geometry, gas composition, gas flow rate, and the physical properties of the test substances were investigated. The design of the reactor was modified to minimize losses of unchanged substrate. Reaction products of benzaldehyde, tolualdehydes, chlorobenzaldehydes, and dichlorobenzenes were identified by combined gas chromatography — mass spectrometry.
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  • 72
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    Chromatographia 20 (1985), S. 195-196 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Wide-bore capillaries
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    Topics: Chemistry and Pharmacology
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  • 73
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    Chromatographia 20 (1985), S. 403-406 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Separation of sugars ; Oxime formation ; Silylation
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    Topics: Chemistry and Pharmacology
    Notes: Summary The procedure involving oxime formation followed by silylation for the analysis of standard hexoses by GC resulted in unseparated peaks for D-glucose, D-mannose and D-galactose. This procedure was therefore modified to obtain clear separation of hexoses. STOX (hydroxylamine containing phenyl-β-D-glucopyranoside as the internal standard) was mixed with trimethylsilylimidazol or hexamethyldisilazane, and then added to a standard sugar mixture containing D-glucose, D-galactose and D-mannose. The mixture was analyzed by gas chromatography with OV-17/OV-22 as the stationary phase, resulting in three distinct peaks.
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  • 74
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Butyl esters of aliphatic hydroxy acids
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    Topics: Chemistry and Pharmacology
    Notes: Summary Aliphatic hydroxy acids were esterified in aqueous solution in the presence of sulfuric acid. Esterification of lactic, tartronic malic and citric acids in water/n-butanol mixtures with mole ratios between 0.02 and 2.53 can be utilized for the determination of these aliphatic hydroxy acids by gas chromatography. Water does not interfere at water/n-butanol mole ratios below 0.02. For mole ratios above 0.02 anhydrous sodium sulfate is used for the binding of water. The mole ratio range was 0.25–2.53 for anhydrous sodium sulfate/water, and 0.32–1.27 for sulfuric acid/anhydrous sodium sulfate.
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  • 75
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Nitrogen dioxide ; Diethyl ether ; Photo-induced reaction
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    Topics: Chemistry and Pharmacology
    Notes: Summary When dissolved in diethyl ether, nitrogen dioxide reacts with the solvent, slowly at room temperature, more rapidly on heating of UV irradiation. A complex mixture of products is formed in which further changes are observed after prolonged storge: these are less pronounced if the unreacted nitrogen oxides are removed. A gas chromatographic method was applied for the identification of the majority of products. Irradiation does not change significantly the qualitative and quantitative composition of the reaction products. The reaction is thus the so-called photo-induced process [ΔG〈0]. Preliminary suggestions are made concerning the reaction mechanism.
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  • 76
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Preparation of methyl esters ; Tetramethylammonium hydroxide
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Tetramethylammonium hydroxide in methanol has been proposed as a catalyst for preparing methyl esters of both free fatty acids and glycerides of fats. Nevertheless, procedures normally recognized as suitable can be inadequate when the fat under study contains noticeable amounts of low relative molecular mass esters. The method using tetramethylammonium hydroxide has been examined and modified in order to analyze milk fats by capillary GC. The pyrolysis methylation of free fatty acids in capillary injectors has been also studied. The modified method was satisfactory for both neutral and acid milk fats.
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  • 77
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Multi-chromatography ; Selectivity tuning ; Column combination ; Theory
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    Topics: Chemistry and Pharmacology
    Notes: Summary The evolution of the use of mixed phases or serial column combinations is outlined, leading to systems with fixed-length columns to be used in selectivity tuning (“multi-chromatography”). The difference between multi-chromatography and multi-dimensional gas chromatography is outlined. After discussing the system used in subsequent work, the fundamental relationships of multi-chromatography are detailed. Among the basic relationships the additivity of retention data, the relationship between the individual and composite capacity factors and the relative retentivity serving as the fundamental parameter of a multi-chromatography system are discussed. The relative retentivity is derived as a function of gas holdup times, pressures, and average velocities or flow rates. Finally, the relationships between individual vs. composite relative retention, efficiency, and resolution values are deduced.
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  • 78
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    Chromatographia 20 (1985), S. 538-542 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fluidized beds ; Industrial chromatography
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    Topics: Chemistry and Pharmacology
    Notes: Summary Chromatography is carried out under the conditions of fluidization, in long, straight tubes under organized and non-organized conditions. Under non-organized conditions the column is filled only with a sorbent. In organized conditions, either metal coils are added into the column or a segmented column is utilized with metal grids. The results obtained are compared to those obtained under fixed-bed conditions when the column is completely filled with the sorbent. Organized fluidized beds provide a significant decrease in longitudinal bandspreading.
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  • 79
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Coated porous polymers ; Partition coefficients
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    Topics: Chemistry and Pharmacology
    Notes: Summary Following previous work on the solute-stationary phase-adsorbent interaction phenomena associated with the use of Chromosorb 101 support in gas chromatography, the retention of different polarity compounds on columns of Ethofat, squalane and Fractonitril VI on Chromosorb 102 has been studied. The experimental partition coefficients in these three liquid phases have been compared with those ones obtained earlier on Chromosorb 101 and Chromosorb P. The values have been related to the geometry of the support surface and the different coating of the liquid phases by scanning electron microscopy.
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  • 80
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    Chromatographia 21 (1986), S. 149-151 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention indices ; Comparison of data ; Alkenes
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    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic retention indices for 47 C5 to C8 alkenes on OV-101 dimethylsilicone at 50 and 70 °C were determined within a standard deviation of 0.3i.u. Data obtained on OV-101 are compared with those measured on squalane. The comparison of the retention index and dl/dT values from both columns is presented as linear regression equations with correlation coefficients greater than 0.98.
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  • 81
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    Chromatographia 21 (1986), S. 157-160 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Alkylation ; Carboxylic acids ; Urine analysis ; Micelles
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    Topics: Chemistry and Pharmacology
    Notes: Summary Carboxylic acids can be converted to their methyl esters in an aqueous sample which contains no organic solvent. The reaction appears to be assisted by the presence of a quaternary ammonium salt surfactant. The procedure is best described as a pseudo-organic phase, or micelle-like, reaction. The important experimental variables have been optimized by Simplex procedures. The reaction proceeds in 80–100% yield, for common carboxylic acids, at room temperature in less than one hour. This reaction is superior to existing two-phase extractive alkylation procedures.
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  • 82
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Coated porous polymers ; Adsorption phenomena ; Surface areas
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    Topics: Chemistry and Pharmacology
    Notes: Summary The behaviour of Chromosorb 101 and Chromosorb 102 supports coated with Ethofat 60/25, squalane and Fractonitril VI is compared. The adsorption constants of different solutes of varying polarity on these packings were calculated as well the surface areas for Chromosorb 102. The validity of the proposed equation used for correcting the specific surface areas of Chromosorb 102 for the molar volumes of each solute and the solubility parameters of the compounds, adsorbent and liquid phases is shown.
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  • 83
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Ethylene oxide ; Active charcoal tubes ; Pollution
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    Topics: Chemistry and Pharmacology
    Notes: Summary Air sampling of ethylene oxide on active charcoal tubes followed by GC analysis is a frequently proposed method. This paper studies just to what extent it can be used, defining its limitations (concentration range, influence of ambient temperature and relative humidity), which are seldom taken seriously into account. This method proves inadequate to determine low pollution levels, i.e. around 2 mg m−3.
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  • 84
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    Chromatographia 22 (1986), S. 333-336 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Split sampling ; PTV-sampling ; Discrimination ; Quantitation
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    Topics: Chemistry and Pharmacology
    Notes: Summary Parallel studies on split-sampling and PTV-sampling procedures have been made to highlight the difficulties in quantitative analysis for capillary columns. Parameters such as total sample amount, carrier gas and packing material used for the injector glass insert were studied. The results clearly demonstrate the importance of optimizing all experimental parameters which give rise to discrimination effects during injection.
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  • 85
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    Chromatographia 21 (1986), S. 538-540 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Micropacked column ; Milk ; Carbohydrate quantification
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    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method using a micropacked column is described for the analysis of lactose, galactose, lactulose and epilactose in processed milks. The method is evaluated for precision and accuracy using phenyl-β-glucoside as an internal standard. Recoveries near 100% were found for lactulose concentrations higher than 0.1 mgml−1, showing coefficients of variation from 5.9 to 9.4%.
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  • 86
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Glass capillary columns ; Pre-treatment of column surface ; n-Octadecanol films
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    Topics: Chemistry and Pharmacology
    Notes: Summary The properties of n-octadecanol films on bare surface of glass capillary columns, leached with hydrochloric acid, HMDS treated and covered with BaCO3 have been investigated. Using the “inverse” gas chromatography method it was found that the structure of the n-octadecanol film distinctly depends on the glass surface preparation. The influence of the properties of the treated glass surface was particularly strong on the structure and properties of the n-octadecanol monolayer directly adjacent to the column wall.
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  • 87
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    Chromatographia 22 (1986), S. 329-332 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-propyl esters of C1−C22 fatty acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary C1−C22 carboxylic acids have been esterified in aqueous solution with n-propanol. Gas chromatographic analyses have been performed from a single chromatogram. It has been proven that esterification in the concentration range of [H2O]/[n-PrOH]=0.022–8.45 can be utilized for the quantitative determination of these carboxylic acids. The presence of water does not interfere in the range of [H2O]/[n-PrOH]=0.22–1.27. In the cases of [H2O]/[n-PrOH]〉1.27, anhydrous sodium sulfate has been used for binding the water, in an amount of [Na2SO4 anh.]/[H2O]〉0.7.
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  • 88
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Carbohydrate TMS-ethers ; Tautomeric equilibrium mixtures of aldoses ; MS and NMR identification
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Equilibrium tautomers of aldopentoses (arabinose, ribose, xylose and lyxose) and aldohexones (allose, altrose, gulose, idose and talose) have been analyzed as their trimethyl-silyl ethers by capillary GC. Pentoses were separated on SE-54 and hexoses on OV-225. The four components of the tautomer equilibrium mixture have been identified using GC/MS and NMR data.
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  • 89
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    Chromatographia 23 (1987), S. 722-726 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Adsorbents for gas chromatography ; Strong adsorption sites ; Heterogeneity of silica surface
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple gas chromatographic method is presented for the determination of the quantity of the strongest adsorption sites on an adsorbent's surface. The method consists of the blockage of the sites with quasi-irreversibly adsorbed, known amount of a strongly interacting compound and subsequent measuring of the retention of a hydrocarbon during the presence of the blocking compound in the column. Heterogeneity of chromatographic grade silicas is investigated with this method.
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  • 90
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Propyl esters of aliphatic hydroxy acids
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    Topics: Chemistry and Pharmacology
    Notes: Summary Aliphatic hydroxy acids were esterified in aqueous solution in the presence of different amounts of sulfuric acid. Esterification of lactic, tartronic, malic and citric acids in water/n-propanol mixtures with mole ratios between 0.03 and 2.15 can be utilized for the determination of these acids by gas chromatography. Water does not interfere at water/n-propanol mole ratios below 0.03. For mole ratios above 0.03 anhydrous sodium sulfate is used for the binding of water. The mole ratio range was 0.24–2.13 for anhydrous sodium sulfate/water, and 0.16–1.28 for sulfuric acid/anhydrous sodium sulfate.
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  • 91
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography ; Bonded silica ; Residual silanol groups
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Silanol groups of chromatographic material surfaces were determined by chemical reaction with methyl-lithium. Evolved methane was measured by a gas chromatographic method using a column packed with molecular sieves. This chromatographic technique leads to very reproducible results, particularly for the control of the hydroxylation of a silica gel and for the analysis of residual groups at the surface of bonded silica.
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  • 92
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    Chromatographia 23 (1987), S. 790-795 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns in series ; Variable polarity columns ; Essential oils analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary By connecting capillary columns of different polarity in series and by changing the temperature program gradient, a system of variable polarity is obtained. The working conditions can be adjusted to optimize separations of complex mixtures. Application to the analysis of essential oils of: lavender, thyme, lemon petit grain, bergamot, and tangerine, are reported.
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  • 93
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    Chromatographia 23 (1987), S. 240-242 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Stillingia oil ; Quantitative lipid analysis ; Chinese tallow,Sapium sebiferum
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Contemporary stillingia oil from China is qualitatively similar to the oil described earlier, but it exhibits significant quantitative differences reflecting a degree of autoxidation of the unsaturated fatty acids either before or after crushing of the seeds.
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  • 94
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Chemically bonded phases ; Specific interactions ; Chloroderivatives of alkanes and alkenes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Interactions of Cu(II) complexes chemically bonded to the surface of silica with chloro-derivatives of alkanes and alkenes were investigated. It was found that chlorine as a substituent exerts a considerable influence on the retention of the individual chloro-derivatives. In the case of chloroalkenes this influence is negative while in the case of chloroalkanes it is positive. The magnitude of the observed effect depends on the number of substituents and on the way of their distribution within the molecule.
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  • 95
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    Chromatographia 23 (1987), S. 286-288 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Macroporous copolymers of 2-hydroxyethyl ; methacrylate ; Graft polymers ; Polar sorbent for gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The gas chromatographic behaviour of crosslinked macroporous 2-hydroxyethyl methacrylate grafted with 2-methyloxazoline was investigated and the range of applicability of the copolymer was assessed. Retention index values were measured on this copolymer and compared with those obtained on the terpolymer 2-hydroxyethyl methacrylate-ethylene dimethacrylate-acrylonitrile. Rohrschneider constants and efficiency data for selected sorbates are given. The use of this type of polymer in the separation of various types of compounds is documented by various examples.
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  • 96
    ISSN: 1612-1112
    Keywords: Gas chromatography ; (S)-(+)-Naproxen ; Amino acid methyl esters ; Resolution of diasteroisomers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A GC method has been elaborated for the separation of enantiomers of some amino acid methyl esters after derivatization with activated (S)-(+)-naproxen. Nine amino acid ester paris were completely resolvede in a single run on a fused silica capillary column.
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  • 97
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    Chromatographia 25 (1988), S. 993-998 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; HPLC system ; Micropacked column ; Organic mobile phase ; UV detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Retention behaviours of aromatic hydrocarbons were examined by using the vapour of an organic substance as the mobile phase and silica gel as the stationary phase. Gas chromatographic separation of aromatic hydrocarbons was demonstrated by using a system comprising a liquid chromatographic (LC) pump, a micropacked column for LC, a column oven and a UV detector.
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  • 98
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index ; Hydrocarbons
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    Topics: Chemistry and Pharmacology
    Notes: Summary The retention of hydrocarbons present in the C5 pyrolysis fraction of gasolines on the stationary phases squalane and methylsilicone oil JXR at 30, 40 and 50°C was investigated by capillary gas chromatography. The unified retention indices of the hydrocarbons were also calculated on squalane. The retention indices obtained on these two phases were interrelated and the quantitative relationship with the structure of the solutes was studied. Equations based on the unified retention indices calculated on squalane and some selected structural elements of the solutes permit the calculation of their retention on methylsilicone with sufficient accuracy.
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  • 99
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fused-silica capillary micro-packed columns ; Serial columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary For the first time gas chromatographic characteristics of fused-silica capillary micro-packed columns consisting of two segments (i.e., serial columns) and packed with two different particle size fractions of the same sorbent have been investigated. The height equivalent to a theoretical plate (HETP) and the specific separation number vs. carrier gas velocity dependence has been studied. The expediency of empolying serial columns in which the segment containing the finer sorbent fraction is located near the column outlet has been theoretically and practically expalined. Serial columns with such an arrangement of the two segments show a better performance from the view point of efficiency and mass transfer coefficient.
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  • 100
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    Chromatographia 25 (1988), S. 589-592 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Hold-up time determination
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary New versions are suggested for the gas hold-up time calculation in gas chromatography. The results are compared with those obtained by using other methods. The advantages of the suggested ways of calculation are pointed out.
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