Comparison of methods to enhance flame ionization detector (FID) signals in gas chromatography

The performances of some numerical methods to improve the signal to noise ratio are compared and applied to enhance noisy signals obtained in gas chromatography with capillary columns and a flame Ionization detector. Several methods have been considered: cutoffs In the Fourier transform of the recorded signal; real time numerical filtering; theoretical model curve fitting; and the correlation of a chromatogram recorded from a pseudorandomly injected sample with the pseudorandom injection function. Numerical real time filtering is shown to be the most convenient method when the main periodic component of the noise has been determined by Fourier analysis.     

GC-MS法测定粮谷及油料中55种有机磷农药残留量

采用ASE-300快速溶剂萃取仪提取样品中农药残留量,提取液经二氯甲烷液-液分配、凝胶色谱柱（GPC）净化,固相萃取柱（活性炭）再净化,浓缩定容后,用气相色谱-质谱仪（GC-MS）测定,外标法定量.采用选择离子检测进行阳性确证.选择玉米、糙米、大豆、花生为实验样品、敌敌畏等55种农药添加水平在0.5～2.00 mg/kg时,该方法回收率为68%～117%;精密度为4.04%～11.76%;方法测定低限为0.005～0.100 mg/kg,各项指标均满足有关要求.     

The use of glass capillary columns for the analysis of polar natural products

Two published procedures for glass capillary column production are applied to produce capillaries for chromatography of polar natural compounds. Soda lime glass capillaries, after leaching with aqueous HCL, are either treated with colloidal silicic acid or with barium carbonate and coated with either Silar 7CP or SE 52. A test mixture as well as polar carbohydrate and peptide mixtures are chromatographed on the different columns and their chromatographic properties are evaluated. Combined capillary gas chromatography-electron impact and chemical ionization mass spectrometry are used for identification of the peptide sequence.     

Development and validation of an analytical methodology for the determination of p,p′-DDT, p,p′-DDE and p,p′-DDD in fish oil pills

An analytical methodology was proposed and validated to be applied to the determination of p,p′-DDT and its metabolites p,p′-DDE and p,p′-DDD in fish oil. The analytical procedure presented in this paper involves a single-step clean up process prior to the analysis. A solution of 1,2,3,4-tetrachloronaphtalene was used as internal standard.The analytical technique used was gas chromatography coupled to an electron capture detector. Details on the validation process are provided.The limits of detection ranged from 2.6 to 4.7 pg μL^− 1. The BCR 598 standard reference material (cod liver oil) was used to evaluate the performance of the methodology with satisfactory recoveries for all the compounds.The analytes were determined in three different fish oil pills sold in Spain as a supplementary vitamin support. The sum of p,p′-DDT and metabolites was from 13.2 to 51.3 ng g^− 1, the dominant compound being p,p′-DDE.     

Imide-siloxane block copolymer/silica hybrid membranes: preparation, characterization and gas separation properties

Imide-siloxane block copolymer/silica hybrid membranes with covalent bonds were prepared via sol–gel reaction. The structural informations of these hybrid membranes were obtained by using Fourier transform-infrared spectrometry (FT-IR), ²⁹Si nuclear magnetic resonance (²⁹Si NMR), XPS and thermogravimetric analysis (TGA). The gas separation properties of the hybrid membranes were also investigated in terms of organosiloxane (PDMS) or silica content at various temperatures. In the hybrids, the addition of PDMS phase increased the permeabilities of gases such as He, CO₂, O₂, and N₂, indicating that the gas transport occurred mainly through rubbery organic matrix. Meanwhile, the PDMS phase contributed the decreased gas selectivities to nitrogen but the reduction in selectivities was very small in comparison with other siloxane containing polymeric membranes. This might be due to the restriction of chain mobility by the existence of inorganic component such as silica network in the hybrids. Additionally, the increase of silica content in these hybrid membranes considerably retarded the falling-off of gas selectivity at elevated temperature. The increase of silica content in hybrid membranes resulted in well-formed silica networks and hence these inorganic components restricted the plasticization of organic matrix by the thermal segmental motion of organic components, leading to preventing the large decrease of the gas selectivity.     

铸膜溶剂对CAB膜形态和性能的影响

以ＣＡＢ高分子为膜材料，研究了铸膜液的溶剂体生添加剂对膜形态及选择性渗透Ｎ２、Ｏ２、ＣＨ４、ＣＯ２等气体的影响。溶剂体系以丙酮为基本组分，混合甲酰胺或乙酸，可得到具有好的气体渗透性或气体选择性的非对称膜，通过溶剂的红外光谱羰基吸收峰的偏移，认为溶剂体系有可能存在Ｌｅｗｉｓ酸；碱络合物。     

New stationary phase polarity parameters considering the electric intermolecular interactions in gas chromatographic column

Summary The possibility of evaluation of the parameters representing the dispersive solute-solvent interactions is presented. B_N and B_s values can be used to describe the liquid phase polarity and to predict the retention indices of alcohols when the model polyxyethylene glycol dialkyl ethers and their sulphur analogs are used as stationary phases. The possibility of the first ionization potentials estimation is also presented.     

Evaluation of a PTV injector for quantitative analysis of volatile compounds at low concentrations

The performance of a PTV injector operated in the solvent venting mode with Tenax in the glass insert was evaluated with synthetic mixtures containing 5 to 50 ng of n-alkanes, ethyl esters, n-alcohols, and carboxylic acids. The influence of the sampled amount, the injected volume, and the nature of the solvent on accuracy and precision were studied. Coefficients of variation of relative (normalized) peak areas and absolute peak area ratios of each compound to the standard are of the order of 5 %.     

Kubische Berechnung der Retentionsindices ohne Kenntnis der Totzeit tm

Zusammenfassung In der vorliegenden Arbeit wird eine Methode zur Retentionsindex-Bestimmung beschrieben, die von einem kubischen Zusammenhang zwischen Bruttoretentionszeit-Differenzen der Referenzhomologen und der Kohlenstoffzahl ausgeht. Hieraus ergeben sich direkt die Nettoretentionszeiten. Der Fehler der Totzeitbestimmung entfällt bei dieser Methode. Mit den so gewonnenen Nettoretentionszeiten erhält man über einen kubischen Zusammenhang zwischen 1g t_s=f(C) die Retentionsindices. Extrapolationen und Interpolationen sind über 300 Retentionsindexeinheiten mit einem mittleren Fehler von ±0,02 Retentionsindexeinheiten möglich. Das Verfahren bietet sich für eine automatische Berechnung der I-Werte mittels on-line-Datenverarbeitung an.

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Cubic calculation of retention indices without determining the dead-time t_m

Summary The method for the calculation of retention indices described here is based on a third order relationship between the logarithm of differences of unadjusted retention times of homologues and the carbon number. From this adjusted retention times are directly calculated. A determination of the dead-time is not necessary thus avoiding the errors connected with this factor. A cubic equation for the logarithm of the adjusted retention time lg t_s as a function of carbon number C_n is used for the retention index calculation. Extrapolations and interpolations can be done over a range of 300 index units with an average deviation of ±0.02 i.u.. The method offers the possibility of an automated on-line calculation of retention indices by computer merely on the basis of unadjusted retention times.

     

Capillary gas chromatography of C1−C4 alkyl tert-butyl ethers

Summary The separation of C₁–C₄ alkyl tert-butyl ethers with the general formula (CH₃)₃C–O–R (R-alkyl substituent) on fused-silica capillary columns coated with dimethylsilicone and cyanopropylmethylsilicone stationary phases was investigated. Retention indices were determined at two temperatures in order to understand their chromatographic behaviour. The respective standard deviations were 0.3 and 0.5 i.u.