Sample decomposition in an electrically heated cold-trap inlet system for high speed gas chromatography

Thermal decomposition of some hydrocarbon and chlorinated hydrocarbon compounds in metal capillary tubes used in an inlet system for high speed gas chromatography has been investigated. The metal tube is cooled to about ?75°C by a flow of cold nitrogen gas in order to focus a vapor sample cryogenically. A capacitive discharge power supply is then used to heat the metal tube resistively in order to revaporize the sample and introduce it to the separation column as a plug 5-10 ms wide. The effects of tube temperature, tube material, sample vapor residence time, and type of carrier gas on thermal cracking are described. Use of a copper-nickel alloy tube resulted in less cracking than either pure platinum or pure nickel. Cracking is more significant with hydrogen as carrier gas than with helium. Cracking also increases with increasing sample residence time in the hot tube. Quantitative sample injection with minimum decomposition can be obtained for a variety of aliphatic and aromatic hydrocarbons and chlorinated hydrocarbon compounds.     

Capillary gas chromatography of lower aliphatic C2?C5 aldehydes in the free form as a group of pungent odorants in air

The capillary gas chromatography of the C₂-C₅ lower aliphatic aldehydes (e.g.,acetaldehyde, propionaldehyde, n- and i-butyraldehydes, n- and i-valeraldehydes) which, in the free form in air, have unpleasant odors and low threshold odor values, has been studied using cold-trap preconcentration with liquid oxygen. The capillary column outlet was connected to enable simultaneous detection by FID, ECD, FPD AND FTD (SID).     

棕榈油中脂肪酸的GC/MS定性分析

本文介绍了进口棕榈油中的脂肪酸的色-质联用分析方法。其中,特别检测了油中的奇碳数脂肪酸,并和其它食用油中的脂肪酸作了比较。     

程序涂渍柱“柱效能程序效应”的研究

本文从理论上给出程序柱“柱效能程序效应”的概念并导出了函数关系式,通过计算机可计算柱效能程序效应与柱内各变量之间的关系,实践证明实验数据的变化趋势与理论数据相符。     

Ozone-based sulfur chemiluminescence detection: Its applicability to gas,supercritical fluid,and high performance liquid chromatography

The sensitive detection of sulfur-containing analytes is of interest in many industrial applications; selective detection is also desirable since these compounds are usually present at trace levels in difficult matrixes. The purpose of this article is to review the use of the Sievers® ozone-based sulfur chemiluminescence detector, and its coupling with gas chromatography, supercritical fluid chromatography, and high performance liquid chromatography. Detection limits, linearity, response factors, and selectivity are discussed for each of these techniques. Critical operational parameters for the SCD are also described. The use of other sulfur selective detectors for SFC and HPLC is also briefly summarized.     

Metabolic characterization of the early stage of hepatic fibrosis in rat using GC‐TOF/MS and multivariate data analyses

The aim of this study was to explore the changes in the urine metabolic spectrum in rats with the early stage of liver fibrosis using gas chromatography–time of flight/mass spectrometry (GC‐TOF/MS), try to search for potential biomarkers and elucidate the probably metabonomic pathogenesis. The early stage of liver fibrosis was established with a single subcutaneous injection of carbon tetrachloride twice each week for 4 weeks continuously. At the end of the experiment, GC‐TOF/MS technology with multivariate statistical approaches such as principal component analysis, partial least squares‐discriminant analysis and orthogonal partial least squares‐discriminant analysis was used to analyze the changes in the metabolic spectrum trajectory and identify potential biomarkers. Twelve potential biomarkers in the model group, such as succinic acid, threonine and lactose, were selected, which indicate that the metabonomic pathogenesis of the early stage of liver fibrosis may be related to disorders of energy metabolism, amino acid metabolism and fatty acid metabolism.     

Analysis of dinitrofluoranthenes by high resolution capillary gas chromatography/mass spectrometry

This paper reports the retention indices of eighteen of the possible twenty-five dinitrofluoranthene isomers.     

Single derivatives for GC-MS assay of reducing sugars and selective detection by the nitrogen-phosphorus detector (NPD)

Reduction of sugar methoximes with sodium cyanoborohydride followed by permethylation with CH₃SOCH₂^?/ICH₃ affords the corresponding deoxy(methylmethoxylamino)alditol O-methyl ethers, which are amenable to capillary gas chromatography. Derivatization proceeds under mild conditions with high yields. Only a single derivative is formed for each reducing sugar. All aldose derivatives can be separated in a single chromatographic run on glass capillaries coated with Carbowax 20 M or Superox 0.1. Good linearity was found. The introduction of the nitrogen atom in the sugar molecule makes these derivatives suitable for selective detection by the NPD. The El-mass spectra contain intense characteristics ions at m/z 74 for aldoses and at m/z 280 for reducing disaccharides, together with a (M - 15)⁺ion. These fragments are very suitable for highly sensitive GC-MS analysis by selective single ion monitoring.