Headspace SPME–GC Method for Acetone Analysis and its Biomedical Application

A new method for extraction and analysis of acetone in human urine based on headspace solid phase microextraction using a mixture of activated carbon and zeolite as sorbents in a PVC matrix coated on a silver wire and its application to the determination of ketone bodies is described. Unlike commercial fibers, which are coated on fused silica, the coating adheres strongly to the silver wire and is thermally stable up to 250 °C. After optimization of coating composition and microextraction conditions the fiber was used for the analysis of acetone in human urine.     

Determination of styrene in olive oil by an automatic purge-and-trap system coupled to gas chromatography-mass spectrometry

Summary A new gas chromatographic method using an automatic purge-and-trap system coupled to a GC with mass selective detection to analyze styrene at the parts-per-trillions (ng kg^–1) level is described. The method shows a good sensitivity and the detection limit is 10 ng kg^–1 with a relative standard deviation (RSD) of 4.7% for 164 ng kg^–1 styrene in olive oil. This analytical method has been successfully applied to the analysis of styrene in extra-virgin olive oil from the European market.     

Critical evaluation of gas standards based on hydrogen

Summary Six commercial hydrogen standards containing helium, oxygen, nitrogen, methane and carbon dioxide at trace levels were analyzed by gas chromatography, for periods up to 105 days. The concentrations, in the range of 0–120 μmol mol⁻¹, were stable (with the exception of oxygen) but often significantly different from the certified values provided by the suppliers, especially for helium, oxygen and nitrogen. Concurrently, some experiments were carried out to verify the stability of gas mixtures based on hydrogen stored in cylinders submitted to different chemical and physical treatments. The causes that led to the deviations observed, as well as the decreases in oxygen, are discussed. Presented at the 21^st ISC held in Stuttgart, Germany, 15^th–20^th September, 1996.     

A Pseudo-Random Frequency Modulation Continuous Wave Coherent Lidar Using an Optical Field Correlation Detection Method

We propose a new detection method for a pseudo-random frequency modulation continuous wave (RM-CW) coherent lidar. The feature of this method is modulation of local beam with a time delayed pseudo-random sequence. Heterodyne detection and correlation detection between the received beam and the local beam are simultaneously carried out in an optical field. In the RM-CW coherent lidar using the optical field correlation detection method, the received equipment is greatly simplified. We carried out preliminary experiments and demonstrated that the new method is effective for detection of a CW coherent lidar.     

镁掺杂对In2O3电导和气敏性能的影响

用共沉淀法制备了Mg2 + 掺杂的In2 O3 纳米粉 ,研究了镁掺杂对In2 O3 电导和气敏性能的影响 .结果表明 :MgO和In2 O3 间可形成有限固溶体In2 -xMgxO3 (0≤x≤ 0 .40 ) ;MgIn× 电离的空穴对材料导带电子的湮灭 ,使掺镁纳米粉的电导变得很小 ;n(Mg2 + )∶n(In3 + ) =1∶2共沉淀物于 90 0℃下热处理 4h ,用所得的纳米粉制作的传感器在 32 0～ 370℃下 ,对 45 μmol/LC2 H5OH的灵敏度达 10 2 .5 ,为相同浓度干扰气体Petrol的 12倍多 .     

Automated derivatization for on-line solid-phase extraction-gas chromatography; phenolic compounds

An automated system for derivaatization was coupled on-line with solid-phase extraction-gas-chromatography (SPE-GC). The system was optimized for the determination of phenol and chlorinated phenols in aqueous samples. The test analytes were acetylated with acetic anhydride; proper buffering of the sample was a critical factor. Next, the phenol acetates were enriched on a SPE cartridge and transferred to a GC; two appraoaches were studied. In the first approach, the derivatives were enriched on disposable C18 cartridges (ASPEC type) and desorbed with methylacetate. Aan aliquot of the final eluate was injected on-line the GC by means of a loop-type interface. In the second approach, trace enrichment was performed on 10 × 2 mm i.d. LC-type precolumn packed with polystyrenedivinylbenzene copolymer (PLRP-S) this precolumn was dried with a mitrogen purge and the phenol acetates were desorbed with ethyl acetate which was injectedon-line into the retention gap of the GC under partially concurrent solvent evaporation (PCSE) conditions. The Derivatization-SPE-GC system which was based on the loop-type interface has the advantage of simplicity and easy operation, the main drawback is the impossibility to determine phenol acetates which elute prior to trichlorophenol acetates. With the derivatization-SPE-GC approach using PCSE-based desorption, even the most volatile analyte of the test series, phenol acetate, can be determined successfully. The entire procedure, including the derivatization step, was fully automated and integrated in one set-up. The precision data for the integrated on-line derivatization-SP-FID system were fully satisfactory, with RSD values of 1–12 % at the 1 μg/1 level. When a sample volume of 2.2 ml was analyzed, The detection limits for the chlorinated phenol acetates were in the 0.1–0.3 μg/1 range.     

The variation of carrier gas viscosities with temperature

After describing simplified equations exspressing the temparature dependency of the viscosity of carrier gases (helium, nitrogen and hydrogen ) relative to a base value, absolute relationships based on the kinetic theory of gases are discussed. Comparative data obtained using various calculation methods are given and are compared to measured values. Based on the kinetic relationshipsm, of viscosity. Finally, the influence of pressure on the viscosity is also briefly discussed. As a supplement, Viscosity data are tabulated for the three gases in the range of 0°C to 400°C in increments of 2 K, calculated using the kinetic relationships.     

Identification of chlorinated sulfur compounds in pulp mill effluents by GC-MS and GC-AED

Summary Three chlorinated dimethyl sulfones and five chlorinated thiophenes have been identified in the alkaline extraction liquor from a bleach plant by gas chromatography with atomic emission detection (GC-AED) and with mass spectrometry (GC-MS). The information on elemental content obtained by GC-AED enabled a rapid screening of the sulfur compounds and provided important structural information complementary to the mass spectral data. Quantitation was accomplished by GC-AED based on universal calibration.     

人工神经网络方法预测气相色谱保留值

本文运用一典型的人工神经网络模型－“反向传播“模型的改进形式，研究了诱导效应指数Ｉ，摩尔折射度Ｒｏ，疏水亲脂参数ＩｇＰ，以及分子联通性指数与气象色谱保留行为的关系，实现了对色谱保留植的预测。神经网络预测模型的最大相对误差不超过８．７％。结果表明，该方法性能良好，可望成为色谱保留值预测的有效手段。