微区有机质激光热解GC/MS新技术及其应用

微区有机质激光热解GC/MS是国际上近年来发展起来的新分析技术。它利用激光的高相干性和高平行性准确地聚焦于有机质表面某个微小区域内 ,使之发生热降解而产生能反映有机质化学组成和结构的分子级产物 ,借助GC/MS系统进行分离和鉴定。这一新技术为生油岩和煤中单个显微有机组分的研究开辟了一条途径 ,在生油岩评价、油气源对比和油藏地球化学研究中有广泛的应用前景。     

废水中微量酚的气相色谱法测定

采用SP 370 0型气相色谱仪 ,配以SE 54玻璃毛细管柱 (35m× 0 .37mmi.d .)、氢焰离子化检测器 ,测定了以GDX 50 2为吸附剂富集的含酚废水样 .方法的最低检知浓度为 1 4 0× 1 0 - 9。     

双毛细管柱气相色谱法测定环境水体中取代苯

本文使用 GDX- 10 2大孔树脂对水中微量烷基苯类、硝基苯类、卤代苯类进行了同时富集 ,富集后的水样用两根极性不同的毛细管柱进行气相色谱双柱定性 ,外标法定量。本方法对十四种取代苯的加标回收率为 92 %～ 98% ,相对标准偏差在 5 %以下 ,最低检测限达 3.2 5× 10 -9g。采用的双毛细管柱定性方法操作简便 ,结果可靠     

Advanced analytical determination of volatile organic compounds (VOC) and other major contaminants in water samples using GC-Ion Trap MS

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典型畜禽粪污中雌激素排放特征

为探究畜禽粪污中雌激素的排放水平和分布特征,采用固相萃取-高效液相色谱串联质谱（SPE-HPLC-MS/MS）分析方法,对上海市典型畜禽养殖类型（猪、奶牛、鸡）排放粪污样品中雌激素含量进行测定.结果表明:猪场粪便、沼渣肥、还田土壤、尿液和沼液样品中5种雌激素（E1,雌酮;E2,雌二醇;E3,雌三醇;EE2,炔雌醇;DES,己烯雌酚）总量分别为94.5 ng/g、35.1 ng/g、0.1 ng/g和8 882.2 ng/L、4 388.6 ng/L,其中E1是排泄物中最主要的雌激素;奶牛场粪便、堆肥、还田土壤、尿液、污水进水及出水样品中雌激素总量分别为84.6 ng/g、16.2 ng/g、0.1 ng/g和2 636.7 ng/L、2 605.6 ng/L、615.7 ng/L,其中E1和E2含量最高;鸡场粪便和堆肥样品中雌激素总量分别为60.9和17.5 ng/g.研究显示,猪场、奶牛场和鸡场排泄物中均含有一定数量的天然和人工合成雌激素,雌激素含量水平总体表现为粪便高于有机肥、尿液高于污水;通过畜禽粪污向环境中排放的雌激素总量表现为猪场>奶牛场>鸡场;厌氧发酵对猪场污水中雌激素具有一定的去除效果,而污水厌氧-好氧净化处理和固体粪高温好氧堆肥对奶牛场排泄物中雌激素具有较高的去除效果.      

某酸性矿山排水中溶解性有机物的特征分析

采集安徽某酸性矿山排水（AMD）水库不同离岸距离的表水层水样,结合傅立叶变换离子回旋共振质谱（FT-ICR MS）与三维荧光光谱（EEMs）技术对水样中溶解性有机物（DOM）来源和组分特征进行分析.三维荧光结果表明,样品中内源性色氨酸类荧光峰峰强与离岸距离正相关,且基于三维荧光特征指数（FI,HIX,BIX）分析判断DOM主要来自于内源.FT-ICR MS在分子层面进一步表明,内源性组分（脂类,脂肪族/蛋白类,糖类）在近岸点样品DOM所占比重相对较低（66%）.AMD中DOM的主要成分为CHO（40%~50%）、CHON（25%~30%）、CHOS （22%~36%）等化合物.DOM包含有高比例的CHOS化合物主要与AMD水体高浓度硫酸盐有关.     

Seasonal variability of polychlorinated biphenyls (PCBs) and polychlorinated diphenyl ethers (PBDEs) congener profiles in butter in Poland: Dietary risk evaluation

Various statistical methods have been employed to analyse in details seasonal diversification of polychlorinated biphenyl (PCB)/polybrominated diphenyl ether (PBDE) congener profiles found in butter fat. The variability of the PCB/PBDE congener profiles indicates the presence of various sources of the milk fat contamination. The obtained results suggest that the environmental chemical background has the highest share in the contamination sources pattern. Ion trap mass spectrometry coupled to high-resolution gas chromatography with semi-permeable membrane dialysis sample cleanup was used for determination of PCBs and PBDEs in milk fat. Determined butter fat PCB profiles were similar to the profiles characteristic for Aroclor 1254 technical mixture. Our data indicate that dietary intake of PCB/PBDE with milk and milk products may be estimated to be about 717.5 pg kg b.w.^?1 day^?1 for six-indicator PCBs, 0.329 (equivalent toxicity, TEQ) pg kg b.w.^?1 day^?1 for 12 DL PCBs and 50 pg kg b.w.^?1 day^?1 for PBDEs (sum of 14 congeners).     

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.     

液相色谱质谱法测定水体及土壤中的类固醇激素

建立了水体和土壤中类固醇激素的液相色谱质谱分析方法。水样采用固相萃取方法富集,土壤样经加速溶剂萃取后由固相萃取净化和富集。处理好的样品经丹磺酰衍生化后上仪器分析。结果表明,类固醇激素在水体和土壤中的检出限分别为0.01~0.6ng/L和0.01~0.19ng/g,回收率分别为77%~97%和62%~119%,RSD小于6.04%和15.5%。该方法具有较高的准确度和精密度,适用于环境水体及土壤中类固醇激素残留的分析。     

Effects of temperature and composite alumina on pyrolysis of sewage sludge

An interactive dual-circulating fluidized bed system has been proposed in which the pyrolysis of sewage sludge(SS) and incineration of biomass proceed simultaneously, and alumina is used as the bed material and heat carrier. The alumina coated with biomass ash would mix with sewage sludge in the pyrolysis reactor of this device. It is important to know the influence of composite alumina(CA) on the pyrolysis progress. Sewage sludge was pyrolyzed in a fixed bed reactor from 400 to 600°C using CA as catalyst. The effects of temperature and CA additive ratio on the products were investigated. The product yields and component distribution of non-condensable gas were more sensitive to the change of temperature, and the maximum liquid yield of 48.44 wt.% and maximum Useable Energy of Liquid of 3871 k J/kg sludge were observed at 500°C with 1/5 CA/SS(mass ratio). The gas chromatography–mass spectrometry results showed that the increase of temperature enhanced devolatilization of organic matter and promoted cyclization and aromatization of aliphatics. The presence of CA could strengthen secondary cracking and interaction among primary products from different organic compounds, such as acid–amine condensation,and reduce the content of oxygenated compounds. When the CA additive amount exceeded a certain proportion, the aromatization was clearly strengthened. The effects of CA on decomposition of fatty acids and formation of aromatics were similar to that of temperature. This means that the reaction temperature could be lowered by introducing CA, which has a positive effect on reducing energy consumption.