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  • Gas chromatography  (172)
  • Springer  (172)
  • 2015-2019
  • 1985-1989  (172)
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  • 1
    ISSN: 1432-1432
    Keywords: Primordial terrestrial atmospheres ; CH4, C2H2, CO2 ; Prebiotic synthesis ; High-frequency discharge ; Hydrocarbons ; Gas chromatography ; Mass Spectrometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Summary Various hydrocarbons were synthesized by high-frequency discharge in a primordial terrestrial model atmosphere. The products were extracted by benzene or methanol and analyzed by GC-MS. The mean carbon chain length of the hydrocarbons formed by the discharge through pure CH4 gas was less than 6. Benzene was also obtained. Some isomers were obtained for each of the hydrocarbons containing a given number of carbons. When a small amount of C2H2 was added to the CH4, longer chain compounds were formed, as compared with discharge in CH4 only. However, when the amount of C2H2 was increased, unextractable high molecular weight compounds were produced. The amounts of products decreased as the mixing ratio of CO2 to CH4 increased. No hydrocarbons were detected when the ratio of CO2/CH4 exceeded 1.
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  • 2
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    Trees 1 (1987), S. 94-101 
    ISSN: 1432-2285
    Keywords: Monoterpenes ; Abies alba Mill ; Resin ; Seeds ; Gas chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary Using gas-chromatographic methods, the variability of the contents of monoterpene hydrocarbons (α-pinene, β-pinene, Δ3carene and limonene) in the resin of silver fir seeds (Abies alba Mill.) was studied. Resin cavities were characterized according to their position on the seed surface. It was estabilished that the terpene content of the resin of cavities localized on the abaxialadaxial surfaces of the seed differs significantly, creating a gradient of resin composition around the circumference of the seed. The differences between various resin cavities of single seeds were greater than the differences between different seeds of a single cone and between seeds of various cones on a single tree. An accurate definition of the resin cavity location on the seeds appears to be a fundamental condition for the collection of a sample representing the resin composition of individual trees. Resin biosynthesis in the course of organogenesis and the control of terpene contents in the resin of various locations on the seed and the cone are discussed.
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  • 3
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Step profile method ; Adsorption isotherm ; Water film pressure ; Surface free energy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Investigation of water adsorption by the step profile method (Glueckauf method) was carried out with the help of a modified gas chromatography equipped with thermal-conductivity detector. On the basis of the adsorption isotherm obtained, the water film pressure and the polar component of the surface free energy of quartz were calculated. The calculated value of the polar component of the surface free energy of quartz agrees with analogous values obtained by other methods.
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  • 4
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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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  • 5
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Linear temperature programming ; Thermodynamic chracteristics ; Calculation of k PT ′ for LPTGC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A simple method has been elaborated to calculate capacity ratios under programmed-temperature conditions (k PT ′ ) from the thermodynamic characteristics determined for the given column under isothermal conditions and the parameters of programmed-temperature operations.
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  • 6
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    Chromatographia 21 (1986), S. 157-160 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Alkylation ; Carboxylic acids ; Urine analysis ; Micelles
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Carboxylic acids can be converted to their methyl esters in an aqueous sample which contains no organic solvent. The reaction appears to be assisted by the presence of a quaternary ammonium salt surfactant. The procedure is best described as a pseudo-organic phase, or micelle-like, reaction. The important experimental variables have been optimized by Simplex procedures. The reaction proceeds in 80–100% yield, for common carboxylic acids, at room temperature in less than one hour. This reaction is superior to existing two-phase extractive alkylation procedures.
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  • 7
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Ethylene oxide ; HBr-treated charcoal tubes ; Pollution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Air sampling of ethylene oxide on HBr-treated charcoal tubes followed by capillary GC analysis of the 2-bromoethanol produced allows pollution control evaluation for concentrations ranging from 0.2 to 20 mgm−3. The adequacy of the method is assessed taking into account ambient temperature and relative humidity.
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  • 8
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Glass capillary column ; Retention indices ; Alkylcyclopentane and Alkenylcyclopentane ; Alkylcyclohexane and Alkenylcyclohexane
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Reaction products of the pyrolysis of n-dodecylpentane and n-hexylcyclohexane had been separated and identified on a glass capillary column coated with Polydimethylsiloxane OV-1. The identification of the components in the pyrolysis products and of the corresponding hydrogenated samples was performed from structure retention correlations, especially retention index increments (1CH2), homomorphy values (HOV-1) and the temperature coefficients of retention indices (δI/δT). Hence the presence of homologous 1-alkenes and of monoalkenylcycloalkanes could be confirmed. Based on the addition principle of index increments the determination of the side chain structure of alkenylcycloalkanes (straight chain) and the position of the double bond was ascertained. The calculation of the retention indices of these compounds was performed with high accuracy (deviation 〈1 index unit). Retention indices of 10 1-alkenes, 11 monoalkenyl-cyclopentanes, 11 monoalkylcyclopentanes, 5 monoalkenylcyclohexanes and 5 monoalkylcyclohexanes were determined on the liquid phase Polydimethylsiloxane OV-1.
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  • 9
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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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  • 10
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Multi-chromatography ; Selectivity tuning ; Column combination ; Theory
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The evolution of the use of mixed phases or serial column combinations is outlined, leading to systems with fixed-length columns to be used in selectivity tuning (“multi-chromatography”). The difference between multi-chromatography and multi-dimensional gas chromatography is outlined. After discussing the system used in subsequent work, the fundamental relationships of multi-chromatography are detailed. Among the basic relationships the additivity of retention data, the relationship between the individual and composite capacity factors and the relative retentivity serving as the fundamental parameter of a multi-chromatography system are discussed. The relative retentivity is derived as a function of gas holdup times, pressures, and average velocities or flow rates. Finally, the relationships between individual vs. composite relative retention, efficiency, and resolution values are deduced.
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  • 11
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    Chromatographia 23 (1987), S. 132-136 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Column liquid chromatography ; Thin-layer chromatography ; Analysis of lactulose in carbohydrate mixtures
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Lactulose is a disaccharide with important implications in medicine, nutrition and dairy technology. It has to be determined usually as a minor component in complex matrices containing many other sugars. This paper describes the different chromatographic techniques (planar, liquid and gas chromatography) which have been proposed for the separation and quantification of lactulose in mixtures with other carbohydrates; the advantages of each technique are compared and some features where more research is necessary are outlined.
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  • 12
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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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  • 13
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Ethylene oxide ; Active charcoal tubes ; Pollution
    Source: Springer Online Journal Archives 1860-2000
    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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  • 14
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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
    Source: Springer Online Journal Archives 1860-2000
    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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  • 15
    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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  • 16
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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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  • 17
    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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  • 18
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    Chromatographia 23 (1987), S. 50-52 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention indices ; C6 alkanols ; OV-101 ; Carbowax 20M
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic retention indices for 16 C6 alkanols measured on capillary columns coated with OV-101 methylsilicone and Carbowax 20M propylethyleneglycol liquid phases at 80° and 90°C were determined. The respective standard deviation values were 0.5 and 0.8 i.u. The correlation between the retention indices measured on non-polar and polar stationary phases and the boiling points of the alkanols was studied.
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  • 19
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Propyl esters of aliphatic hydroxy acids
    Source: Springer Online Journal Archives 1860-2000
    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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  • 20
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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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  • 21
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    Chromatographia 25 (1988), S. 547-559 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid column chromatography ; Process scale separations ; Review
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The relative merits of large scale gas chromatography (GC) and high performance liquid chromatography (HPLC) have not been reviewed for some considerable time. Although methodologies capable of manufacturing high efficiency (and hence cost effective) plant have existed for over a decade, commercial introduction has been remarkably slow. This has primarily been caused by confidentiality restrictions placed on equipment manufacturers, in turn severely limiting wide ranging applications data. These are necessary to raise potential end users confidence that both techniques offer viable large scale routes to separation and purification of mixtures as analysed by laboratory chromatographic methods. Considerable recent progress has been made with large scale HPLC plant, which has led to sufficient published data to make both technical and economic comparisons against GC possible.
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  • 22
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    Chromatographia 25 (1988), S. 598-602 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Steroid profiles
    Source: Springer Online Journal Archives 1860-2000
    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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  • 23
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    Chromatographia 25 (1988), S. 655-658 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Structure-retention relationships ; Connectivity indices, topological indices ; Alkenes
    Source: Springer Online Journal Archives 1860-2000
    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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  • 24
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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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  • 25
    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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  • 26
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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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  • 27
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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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  • 28
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    Chromatographia 25 (1988), S. 134-138 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Sulfur ; n-Octane adsorption
    Source: Springer Online Journal Archives 1860-2000
    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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  • 29
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    Chromatographia 27 (1989), S. 333-339 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Catalytic reactions ; Adsorption and desorption rate constants ; Reversed-flow techniques
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A small volume of reactant, 1-butene, is injected onto a catalytic bed and is allowed to diffuse away from it together with the product butane, along a narrow empty chromatographic tube; the latter is connected perpendicularly to the middle point of another similar tube through which hydrogen flows as reactant and carrier gas, transferring both 1-butene and butane to the detector through an analytical column. By using the reversed-flow GC technique, extra peaks are obtained in the chromatographic trace, sampling the concentration of both the readtant and product at the junction of the two tubes as a function of time. These concentrations are the result of the diffusion of the substances along the narrow empty tube, modified by the adsorption-desorption rates and the rate of the catalytic reaction. From the extra peaks of the reactant and product, a number of physicochemical quantities pertaining to the catalytic reaction can be calculated simultaneously, using appropriate mathematical analysis. These include adsorption rate constants, reaction rate constants, desorption rate constants, partition coefficients, and the overall mass transfer coefficients of the reactant across the gas-solid boundary of the catalytic bed.
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  • 30
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Coke oven gas evolution ; On-line gas analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatograph will thermal conductivity detector (TCD) connected on line via a cleaning train to the semi-industrial scale Coke Oven Text Plant of the Spanish National Coal Institute (INCAR), has been used to control the evolution of the permanent gases during the coking process. The undesirable presence of oxygen in the coke oven gas can be detected with this system that will be applied to determine the end of the coking process by quantitative analysis of the gas evolved.
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  • 31
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Adsorption studies ; Clinoptilolite ; Zeolite
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Adsorption properties of NH4-clinoptilolite, thermally treated at 400, 550 and 650°C, were investigated by gas-solid chromatography. Adsorption of ten hydrocarbons, including aliphatic, alicyclic, chlorinated and aromatic compounds is discussed in the light of adsorbate-adsorbent interactions. The imporatant thermodynamic parameters of adsorption are determined. A detailed discussion is presented on the alteration of the surface properties of NH4-clinoptilolite caused by thermal treatment. Experimental data obtained show that NH4-clinoptilolite treated at 650°C can be successfully employed as a column packing in analytical gassolid chromatography.
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  • 32
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Perhalogenated compounds ; Relative retentions ; Identification by interpolation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Separation of perhalogenated compounds resulting from thermolysis, photolysis or radiolysis of mixtures of halogens in carbon tetrachloride was carried out by programmed temperature gas chromatography. Plots of relative retentions (to CBr4) vs the number of bromine atoms present for known compounds of the general formula CxBryClz (x=1 and 2; y+z=4 or 6) gave three linear correlations (all with r〉0.99). These correlations permitted projections of the identities of reaction products for which no standards were available. These projections were later confirmed by CG-MS. *** DIRECT SUPPORT *** A0732166 00010
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  • 33
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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
    Source: Springer Online Journal Archives 1860-2000
    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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  • 34
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Ethyl carbamate ; Direct injection quantification ; Cold injection system ; Optimised SIM
    Source: Springer Online Journal Archives 1860-2000
    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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  • 35
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    Chromatographia 28 (1989), S. 237-240 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Slope of log plot ; Homologous series ; Retention index ; Retention time ; Uncertainty ; Free energy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The free energy of partition of a methylene group $$\Delta G_{CH_2 }^ \circ $$ is constant within a homologous series down to C5 and nearly constant to C3, contrary to the finding of Golovnya and Grigoryeva [5]. Retention indices are linear with carbon number: values may be extrapolated from higher carbon numbers to C5 within experimental uncertainty, to C4 with error no greater than 5 units and to C3 with error no greater than 10 units. Error in extrapolating the logarithm of the adjusted retention time, log t′R, to C5 is thus negligible, to C4 has possible error up to 5b/100 and to C3 up to 10b/100, whereb is the slope of the plot of log t′R against carbon number.
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  • 36
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Optimization of gas-solid separations ; Plate height equation ; Computer mapping procedure
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    Topics: Chemistry and Pharmacology
    Notes: Summary This paper proposes an optimization model for gas-solid chromatographic separations in a non-linear programming form and an approximate equation of the plate height for the model. A computer-modified mapping procedure is also described for searching the optimum separation conditions. Just five experiments and about 20 minutes of the computer time are needed to establish the optima of column temperature and of the carrier gas linear velocity. The relative deviation between the predicted and the experimental values was found to be within 20% for the plate heights, and within 1.5% for the retention times.
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  • 37
    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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  • 38
    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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  • 39
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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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  • 40
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Macroporous silica ; Silica-adsorbent modification ; Low boiling halocarbons ; Analysis of water pollutants
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    Topics: Chemistry and Pharmacology
    Notes: Summary The use of the silica adsorbent Silochrom C-80 modified by a thin liquid stationary phase film is proposed for the gas chromatographic analysis of low molecular weight halocarbons. Such modified adsorbents are characterized by good retention of the volatile halocarbons and high selectivity with respect to halocarbons. The thermodynamic sorption characteristics of alkanes, chloroalkanes and chloromethanes on Silochrom modified by three liquid phases (Apiezon L, methylsilicone and polyethylene glycol 20M) and on Chromaton N with thick films of the same phases were studied. The heats of sorption (−ΔH) and free sorption energy changes (−ΔF) of these substances and the increments −Δ(ΔH) and −Δ(ΔF) per chlorine atom in the chloralkane molecule compared with n-alkanes with the same number of carbon atoms were determined. The “chlorine” retention indices of low molecular weight volatile halocarbons on three sorbents were determined to identify them in aqueous solutions using the electron-capture detector. The analysis of drinking water by this technique is demonstrated.
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  • 41
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    Chromatographia 21 (1986), S. 697-700 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Methyl silicones ; Unified retention index ; Hydrocarbons
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    Topics: Chemistry and Pharmacology
    Notes: Summary Gas chromatographic retention indices of 51 hydrocarbons were determined on OV-101 dimethylsilicone between 40 and 70°C. From the measured data the unified retention indices were calculated.
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  • 42
    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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  • 43
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    Chromatographia 21 (1986), S. 214-218 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Behaviour of metal acetylacetonates ; Adsorption isotherms ; Heat of solution
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    Topics: Chemistry and Pharmacology
    Notes: Summary Specific retention volumes, adsorption isotherms, molar heats of solution and changes of the entropy were determined from chromatographic data, which was obtained by the gas chromatographic separation of metal acetylacetonates. The retention data for Cr(III), Co(III) and Al(III) acetylacetonates were measured at different temperatures and different flow rates. From the retention data other values associated with adsorption and solution phenomena were calculated.
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  • 44
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    Chromatographia 21 (1986), S. 397-401 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention time extrapolation ; Retention time interpolation
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    Topics: Chemistry and Pharmacology
    Notes: Summary An empirical method of extrapolating and interpolating gas chromatographic retention times obtained at three equally spaced isothermal temperatures is described. The accuracy of the method was evaluated from retention time data obtained using packed glass columns. A procedure for constructing retention time tables for homologous series and the derivation of an equation for calculating retention times as a function of temperature is also presented.
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  • 45
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Volatile nitrosamines ; Fused silica capillary columns ; Linear indices
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    Topics: Chemistry and Pharmacology
    Notes: Summary Fused silica capillary columns of different diameters and polarities are linked to a thermal energy analyzer and a flame ionisation detector for comparison. Extra column effects are discussed. Unsymmetrical homologue nitrosamines are applied in order to assign the volatile nitrosamines most often to be determined by their linear indices rather than by their overall retention times.
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  • 46
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    Chromatographia 22 (1986), S. 271-274 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Retention index calculation ; Epoxides
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    Topics: Chemistry and Pharmacology
    Notes: Summary The separation of C6 epoxides on a glass capillary column coated with OV-101 dimethylsilicone liquid phase was investigated. Retention indices were determined at four temperatures between 60 and 90°C. Linear regression equations permit the pre-calculation of the retention indices and the dI/dT values of the C6 epoxides from their properties.
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  • 47
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    Chromatographia 22 (1986), S. 278-282 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Mixed phases ; Chlorinated C1−C3 hydrocarbons
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    Topics: Chemistry and Pharmacology
    Notes: Summary A method to establish the optimum composition of mixed stationary phases used in GC is given for the case when only the retention times on the individual phases are known. The method has been empirically tested for the resolution of chlorinated C1−C3 hydrocarbons.
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  • 48
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    Chromatographia 20 (1985), S. 197-200 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Polyalcohol quantification ; Wine ; Vinegar
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    Topics: Chemistry and Pharmacology
    Notes: Summary A gas chromatographic method is described for the analysis of arabitol, mannitol, sorbitol and inositol in wine. The method is evaluated for repeatability using perseitol as internal standard. Perseitol can be added to wine before or after passing the wine through the ion-exchange column without showing significant differences in the polyalcohol content. The method is also applied to the analysis of vinegar from different substrates (wine cider and rice).
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  • 49
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Modified diatomaceous supports
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Diatomaceous earth type supports are modified with a liquid phase, by high-temperature thermal treatment in a closed system. It is shown that the retention characteristics of the support changes by this treatment. The main advantage of this method, as compared with modification in a flow-through system is that liquid phase evaporation and possibility of oxydation during the process can be avoided. This ensures a better uniformity of the modified support.
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  • 50
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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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  • 51
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    Chromatographia 23 (1987), S. 818-824 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Selective sampling ; On-line fractionation ; Essential oil analysis
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    Topics: Chemistry and Pharmacology
    Notes: Summary The paper describes the possibilities of on-line selective sampling as an on-line fraction technique for the analysis of essential oils. Selective sampling is a micro-separation method, on-line with on-column injection, carried out directly in the syringe body by means of a selective elution of the sample through a fraction cartridge. The paper reports a method of both preparing and standardizing silica gel cartridges, and illustrates through some examples the results of some elution series of solvents on different essential oils.
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  • 52
    ISSN: 1612-1112
    Keywords: Organic pollutants determination ; Gas chromatography ; Thermal desorption
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    Topics: Chemistry and Pharmacology
    Notes: Summary The problem of the separation of 34 volatile organic chlorinated compounds is solved by using three different GC columns selected according to the needs of the particular separation required. The effect of water vapor contained as moisture in the trapped air on the retention of some characteristic compounds is studied. The influence of dead volumes on trap injection is also studied.
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  • 53
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    Chromatographia 23 (1987), S. 888-892 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Calculation of temperature programmed ; Retention indices
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    Topics: Chemistry and Pharmacology
    Notes: Summary A new method is presented for the calculation of the retention indices under linear temperature programming with or without an initial isothermal period. The data calculated by the method are in good agreement with the isothermal retention indices.
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  • 54
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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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  • 55
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Prediction of retention volume ; Porous polymers coated with liquid phases
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    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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  • 56
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Capillary columns ; Immobilized stationary phase ; Carbowax-type stationary phase ; Cross-linked polyurethane
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    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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  • 57
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Fused-silica capillary micro-packed columns ; Serial columns
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    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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  • 58
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Simultaneous distillation-extraction ; Cheese volatiles
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    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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  • 59
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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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  • 60
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    Chromatographia 25 (1988), S. 404-408 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Silica surface modification ; Hexamethylcyclotrisilazane ; Hexamethyldisilazane ; Support materials
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    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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  • 61
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Statistical criteria ; Non-linear models ; Constants for n-alkane retention curve ; Multiparametric least-squares adjustment
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    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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  • 62
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Physico-chemical properties ; Retention indices ; Cycloolefins
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    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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  • 63
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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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  • 64
    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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  • 65
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    Chromatographia 25 (1988), S. 725-730 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Structure-retention correlation ; Kováts retention index ; Alkylaromatics
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    Topics: Chemistry and Pharmacology
    Notes: Summary Relative retention data and Kováts retention indices were measured for several hydrocarbons (mainly for alkylbenzenes) on dinonylphtalate and polyethylenelycol 4000 stationary phase. Correlations were searched between these retention data and the following physical (boiling point, molrefraction, molvolume) and topological (connectiviity index and general index of molecular complexity) properties of solutes. The best fitting equations was choosen among more than 150 equations involving linear, quadratic, exponential, two variables linear and quadratic dependence of retention data and the properties mentioned as well as their inverses.
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  • 66
    ISSN: 1612-1112
    Keywords: Gas chromatography ; FAME fingerprinting ; Animal fats ; Transesterification
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    Topics: Chemistry and Pharmacology
    Notes: Summary The triglycerides of animal fats from milk, meat or cheese can also be characterized by the gaschromatographic pattern of the fatty acid methylesters (FAME) after conversion by an unsophisticated transesterification procedure. Even from the FAME pattern falsifications of commercial animal fats can be revealed by the fast separation of the FAME using a standard CW 20 M (polyethyleneglycol) capillary column. Characteristic patterns of FAME originating from different animals are shown. The patterns of the FAME from different races of the same animal are very similar, so that the characterisation according to the type of animal is not disturbed.
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  • 67
    ISSN: 1612-1112
    Keywords: Gas chromatography ; On-line process analysis ; Injection of volatile compounds
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    Topics: Chemistry and Pharmacology
    Notes: Summary A modified on-line liquid injection technique with rotary valves for gas chromatography has been developed. Applications for the on-line analysis of 2-methylpropene, cyclohexene and 1-butene are described. All samples were loaded under pressure. The results obtained show excellent reproducibility with less than 0.1% relative standard deviation (r.s.d.; n=6) for the peak areas measured. The method is particularly advantageous for samples containing both gas and liquid ccomponents at one bar.
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  • 68
    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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  • 69
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    Chromatographia 27 (1989), S. 436-440 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid crystal stationary phases ; PAH ; FAME ; Mesomorphic polysiloxane phases
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    Topics: Chemistry and Pharmacology
    Notes: Summary The gas-chromatographic properties of two mesomorphic polysiloxane (MEPSIL) stationary phases, one smectic (SB) and the other nematic (N), were investigated. The retention indices and separation factors (relative retentions), α, of several pairs of polycyclic aromatic hydrocarbon (PAH) and fatty acid methyl ester (FAME) isomer solutes were used to gauge differences in the selectivity provided by each. The heats of solution of the PAH showed that the smectic MEPSIL is more selective for solutes with different length-to-breadth ratios. Also, five peaks were resolved for sixcis andtrans octadecenoic FAME isomers with this solvent. The nematic MEPSIL, on the other hand, was found to be more useful at higher temperatures because of its higher clearing point. In addition, solute capacity factors were smaller than those observed with the smectic MEPSIL, as evidenced by lower retention indices. The former was therefore more useful for the analysis of high molecular-weight PAH.
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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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  • 71
    ISSN: 1612-1112
    Keywords: Gas chromatography ; GC/MS and headspace GC ; Elastomeric stoppers for injectables ; Trace hydrocarbons
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    Topics: Chemistry and Pharmacology
    Notes: Summary Elastomeric stoppers for injectables have been surveyed by means of GC/MS screening. Residual contamination by hexanes (2-methylpentane, 3-methylpentane, n-hexane, methylcyclopentane, cyclohexane) toluene and xylenes occurred in all the samples tested. A headspace GC purity test is suggested, by using these residual chemicals as purity indexes.
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  • 72
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Renewal theory ; Monte-Carlo simulation ; Prediction of retention and peak widths
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    Topics: Chemistry and Pharmacology
    Notes: Summary A new method for prediction of gas chromatographic retention times and peak half widths is based on the renewal theory. The only requirements are the heats of vaporization of the compounds to be separated and one calibration measurement. With this data, retention times and peak half widths can be predicted for isothermal as well as temperature-programmed gas chromatography. For the separation of non-polar substances on non-polar stationary phases the prediction error for retention times is approx. 1–2%. First simulations of polar molecules and polar stationary phases indicate that this method is also applicable in these cases but some extension will be required.
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  • 73
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    Chromatographia 26 (1988), S. 413-416 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Gas analysis in incandescent lamps ; Gas chromatographic determination of O2 impurity in argon
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A sensitive GC method was developed to analyse O2 (∼10–400ppm) in argon, by using Ar as carrier gas. A sampling method was developed for lamp analysis, and the O2 impurity content in the gas filling of incandescent lamps was measured. The results of the GC and MS measurements were in good agreement.
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  • 74
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Reaction rate studies ; Dicyclopentadiene
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    Topics: Chemistry and Pharmacology
    Notes: Summary The gas chromatographic reactor technique was used to study the kinetics of dicyclopentadiene dissociation in several liquid phases (Versamid 900, neopentyl glycol sebacate, Triton X-305, Carbowax 6000, ethylene glycol phthalate and diethylene glycol succinate). Reaction rates and Arrhenius parameters are reported in the temperature range of 170–200°C. Kinetic data for the lower polarity liquid phases are in good agreement with literature values for liquid phases of the same nature reported previously. Reaction rates are higher when polar liquid phases are used. This behavior can be explained as a result of side reactions which lead to high molecular weight compounds which can be observed in the reaction chromatogram.
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  • 75
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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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  • 76
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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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  • 77
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Trichloroethyl ester ; Dicarboxylic acid ; Urine samples ; Electron capture ; Biological monitoring
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    Topics: Chemistry and Pharmacology
    Notes: Summary Dicarboxylic acids were esterified by 2,2,2-trichloroethanol by using trifluoroacetic anhydride and phosphoric acid as catalysts. The method was developed to facilitate the evaluation of workers' exposure to sensitising acid anhydrides and other compounds metabolised to acids in the body. The sensitivity of the acid determination in urine was in the order of 2–4 ng ml−1 for aliphatic and alicyclic acids and 15ng ml−1 for phthalic acid.
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  • 78
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    Chromatographia 27 (1989), S. 499-508 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Electron capture detector ; Space-charge model
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    Topics: Chemistry and Pharmacology
    Notes: Summary Mathematical analysis, allowing the determination of the distribution of the electron and positive ion concentration in an electron-capture detector with a cylindrical electrode arrangement and with constant and pulsed voltage supplies, has been carried out. The measurements obtained confirm the assumptions concerning the “space change” model of the ECD introduced by Gobby et al. and cast doubt upon the general assumption of the complete removal of the electrons from the detector by the voltage pulse. The physical factors influencing the current characteristics of the detector and the possible distortions connected with the electrode geometry have been explained on the basis of the measurements carried out.
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  • 79
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    Chromatographia 20 (1985), S. 5-8 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; H2SO4-coated silica gel ; Air pollution (foundries) ; Tertiary amines
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    Topics: Chemistry and Pharmacology
    Notes: Summary After a brief review of the main publications dealing with air-sampling and analysis of aliphatic amines, the authors propose and investigate two sampling methods (bubbling through a sulfuric acid solution, trapping on sulfuric acid-treated silica-gel) for three tertiary aliphatic amines commonly encountered in foundries.
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  • 80
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Liquid crystals ; Substituted benzenes and selectivity
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    Topics: Chemistry and Pharmacology
    Notes: Summary The retention mechanisms of polymethylbenzenes and n-alkylbenzenes on the inert solid support Chromaton (spec-surface area: 1m2/g) and the adsorbent-support Silochrom (C-80 (80 m2/g) coated with p-n-butyl oxybenzoic acid have been investigated.
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  • 81
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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
    Source: Springer Online Journal Archives 1860-2000
    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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  • 82
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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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  • 83
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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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  • 84
    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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  • 85
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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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  • 86
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Flame ionisation detection ; Cyanogen ; Cyanogen chloride
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    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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  • 87
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    Chromatographia 20 (1985), S. 681-682 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Geothermal gases ; Molecular sieves ; Low temperature separations
    Source: Springer Online Journal Archives 1860-2000
    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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  • 88
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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
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    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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  • 89
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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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  • 90
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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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  • 91
    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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  • 92
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    Chromatographia 23 (1987), S. 53-54 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Dual-column system ; Thermal conductivity detector ; Anesthetic gas mixtures
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    Topics: Chemistry and Pharmacology
    Notes: Summary A simple dual-column system with a thermal conductivity detector is described, that can be used for the quantitative analysis of anesthetic gas mixtures of halothane (2-bromo-2-chloro-1,1,1-trifluoroethane), nitrous oxide and oxygen. The separation was performed on a Carbopack (SP 1000) column and a Porapak Q column arranged in series across the detector.
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  • 93
    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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  • 94
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Esterification in aqueous solution ; n-Butyl esters of aliphatic hydroxy acids
    Source: Springer Online Journal Archives 1860-2000
    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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  • 95
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    Chromatographia 23 (1987), S. 265-268 
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Dicarboxylic acid analysis ; n-Propyl esters of C2−C16 dicarboxylic acids ; Esterification in aqueous solution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary C2−C16 dicarboxylic acids were esterified in aqueous solution in the presence of sulfuric acid. Esterification in water/n-propanol mixtures with mole ratios between 0.03 and 2.21 can be utilized for the quantitative determination of dicarboxylic acids by gas chromatography. The presence of water does not interfere at water/n-propanol mole ratios below 0.45. For mole ratios above 0.45 anhydrous sodium sulfate has been used for binding the water. The mole ratio range tested was 0.12–0.99 for anhydrous sodium sulfate/water, and 0.16–2.55 for sulfuric acid/anhydrous sodium sulfate.
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  • 96
    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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  • 97
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Alkylthiazoles ; Energy contributions of the alkyl groups ; Retention indices
    Source: Springer Online Journal Archives 1860-2000
    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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  • 98
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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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  • 99
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Backflushing, peak-cutting technique ; Trace analysis
    Source: Springer Online Journal Archives 1860-2000
    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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  • 100
    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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