顶空气相色谱法测定地表水中吡啶

采用顶空进样、毛细管柱HP -INNOWAX分离、GC -FID测定地表水中吡啶。水样顶空时通过加碳酸钠盐大幅度降低了检出限 ,最低检出浓度达到 0 0 2mg/L。本法加标回收率为 96 5 %～ 10 1% ,变异系数为 7 8%～ 9 8%。     

炸药爆轰气体产物中无机组份的离子色谱分析方法研究

采用超纯水、Na2CO3-NaHCO3NaOH3种不同的吸收液吸收爆轰气体产物、离子色谱进行样品分离、外标法定量,建立了爆轰气体产物中HF、HCl、HCN无机污染物的离子色谱分析方法。研究表明,炸药爆轰气体中合有一定量的HF、HCl和少量的HCN,选择3．2mmol／LNa2C03与1．0mmol／LNaHCO3混合溶液作为爆轰产物中无机组份的吸收液,吸收效率均值太于90％;离子色谱分析方法的相对标准偏差（RSD）小于5．0％,相关系数达到0．9990以上;进样量为100μL时,HF、HCl、HCN的检测限分别为0．04mg／m^3、0．03mg／m^3、0．05mg／m^3。该方法灵敏度高,回收率好,且样品预处理简单。     

水中阿特拉津的气相色谱法测定

采用正已烷液液萃取方法,萃取液经320m石英弹性毛细管柱分离,用电子捕获检测器(ECD)检测水中阿特拉津,得到了良好的分离效果和较高的灵敏度及精密度,达到GB3838—2003《地面水环境质量标准》中的要求。     

Artificial indoor streams as a method to investigate the impact of chemicals on lotic communities

The potential hazard of chemicals on aquatic communities are generally evaluated by standardised single-species bioassays. Safety assessment is based on results gained from organisms adapted to lentic systems and biological interactions in ecosystems are neglected. While lotic communities are often at first in contact with chemicals, it is astonishing that microcosms with lentic communities are mainly used as a bridge between laboratory bioassays and outdoor aquatic systems. Hence, we established five artificial indoor streams to simulate abiotic factors of small rivers. The closed-circuit system was filled with nutrients added to tap water. Washed pebbles were used as sediment. The dynamics of a simple biocoenoses consisting of aufwuchs, Lumbriculus variegatus Asellus aquaticus and Gammarus fossarum was investigated. The dynamic of aufwuchs and periphyton was determined as dry weight and chlorophyll-a, respectively and qualitatively by pigment pattern. The abundance of different developmental stages of L. variegatus was determined at the end of the experiment as well as the population dynamics of G. fossarum and A. aquaticus. Survival rates of gammarids and juveniles per female were investigated and data were used for modelling the population dynamics. The experiment was carried out to investigate the performance of the established artificial streams and the developed approaches to investigate effects of chemicals on a basic lotic community. The prime reason to establish this approach was to close a gap between complex artificial stream systems and laboratory single species tests to assess the impact of chemicals on the aquatic environment.     

混床填色谱柱在有机氯农药残留分析中的应用

在植物粮食、土壤有机氯农药残留监测，使用涂有ＯＶ－１７和ＱＦ－１固定液的白色载体ＣｈｒｏｍｏｓｏｒｂＷ，该种色谱柱对六六六的四种异构体分离比较好，但对ＤＤＴ的四种异构体分离不理想，采用红色载体ＣｈｒｏｍｏｓｏｒｂＰ和白色载体ＣｈｏｍｏｓｏｒｂＷ湿床填充的色谱柱，分离有机氯农药８种组份仅需１５分钟，提高了有机氯农药的分离分析效果。     

作业环境空气中醋酸异丁酯的气相色谱测定方法

根据国外卫生标准的要求，建立了作业环境空气中醋酸异丁酯的气相色谱分析测定方法．     

分散固相萃取/高效液相色谱法测定土霉素菌渣中土霉素的残留量

文章拟建立一种从土霉素菌渣中提取并检测土霉素残留量的高效液相色谱法。用甲醇和冰乙酸作为提取剂提取样品,用分散固相萃取的方法净化样品,净化药剂为石墨化碳黑(GCB)和C18。通过加标回收实验,用高效液相色谱仪检测样品中土霉素含量。选用的色谱柱为PLRP-S,流动相为甲醇和0.05 mol/L草酸,两者比例为35:65(V:V)。检测波长为355 nm,柱温30℃。经检测,土霉素在0.1~2 000 mg/L范围内线性相关系数大于0.999,线性良好。1.0,4.0及8.0mg/g 3个加标水平的土霉素平均回收率范围是80.85%~109.59%,相对标准偏差(RSD)为2.45%~6.38%。土霉素菌渣中土霉素残留量平均为4.741 mg/g。实验表明,该方法具有简单、方便、快速、准确性强、灵敏度高的特点,可以应用于土霉素的分析检测。     

Application of chemometric analysis based on physicochemical and chromatographic data for the differentiation origin of plant protection products containing chlorpyrifos

The aim of this study was to investigate the similarities and dissimilarities between the pesticide samples in form of emulsifiable concentrates (EC) formulation containing chlorpyrifos as active ingredient coming from different sources (i.e., shops and wholesales) and also belonging to various series. The results obtained by the Headspace Gas Chromatography–Mass Spectrometry method and also some selected physicochemical properties of examined pesticides including pH, density, stability, active ingredient and water content in pesticides tested were compared using two chemometric methods. Applicability of simple cluster analysis and also principal component analysis of obtained data in differentiation of examined plant protection products coming from different sources was confirmed. It would be advantageous in the routine control of originality and also in the detection of counterfeit pesticides, respectively, among commercially available pesticides containing chlorpyrifos as an active ingredient.     

GC × GC--A New Analytical Tool For Environmental Forensics

Comprehensive two-dimensional gas chromatography, GC 2 GC, is a new analytical tool with a tremendous capability to separate and identify organic compounds in complex environmental samples. GC 2 GC uses two different chromatography columns coupled serially by a modulator to produce a volatility by polarity separation and distribute compound peaks across a two-dimensional retention time plane. The two-dimensional separation produces an order of magnitude more resolved peaks than traditional GC methods. The grouping or ordering of the peaks in the GC 2 GC chromatogram facilitates the identification of unknown compounds and the comparison of complex environmental samples. When a mass spectrometer detector is used, each resolved GC 2 GC peak yields a single-component, interference-free mass spectrum that leads to accurate matching with mass spectral libraries. GC 2 GC examination of marine sediment extracts identified a wide variety of chemical contaminants including polychlorinated biphenyls, p -nonylphenol isomers, polycyclic aromatic hydrocarbons, benzotriazoles, and the alkane, cycloalkane, alkylbenzene, alkylnaphthalene, and biomarker fractions of petroleum. The two-dimensional GC 2 GC chromatogram image permits rapid screening of the sediment extracts for these and other unknown contaminants.     

固相萃取—气相色谱法测定海水中的666、DDT

采用固相萃取技术富集海水中的666、DDT,并使用气相色谱进行测定。主要包括不同填料(C8、C18、C18-N)、SPE柱规格(500 mg/3 mL、500 mg/6 mL)、洗脱试剂、上样流速、水样pH和洗脱试剂体积6个因素对666、DDT富集效率的影响。最终确定最优条件为:采用500 mg/6 mL C18SPE小柱,调节海水pH=6,上样流速4~5mL/min,10 mL二氯甲烷洗脱。优化后的固相萃取-气相色谱方法测定海水中666、DDT加标10 ng/L回收率为75.7%~110.4%,精密度为1.16%~4.00%,方法检出限为0.19~1.20 ng/L。