C18固相膜萃取-气相色谱法测定饮用水中12种有机氯农药

利用C18固相萃取膜提取水样，气相色谱法（电子捕获检测器）测定饮用水中12种有机氯农药。对洗脱液、水样pH值、萃取压力等条件进行了优化选择，并与液-液萃取做了比较。结果表明，与液-液萃取相比，固相膜萃取具有操作简单、富集倍数高、节省溶剂和耗时短等优点，是萃取水中有机氯农药的有效方法。12种有机氯农药的回收率为85．97％～127．7％，相对标准偏差（RSD，n=5）为4．74％～12．2％，方法检出限为0．014～0．047μg/L。     

液液萃取-固相萃取富集地下水中毒杀芬的对比研究

应用液液萃取、固相萃取柱、固相萃取盘等传统和现代富集技术,对半挥发性有机物进行提取,建立了气相色谱-负化学电离质谱测定地下水中毒杀芬的方法。对性能较好的自制GDX-502固相萃取柱进行了条件优化。结果表明,使用填制的GDX-502固相萃取柱富集地下水中的毒杀芬,基体加标回收率为92.3%～98.5%,优于商品固相苯取柱LC-C18、ENVITM-C18以及固相萃取盘(92.8%～96.8%)和液液萃取(80.3%～88.5%);GDX-502固相萃取柱富集速度低于固相萃取盘,但远高于LC-C18和ENVITM-C18;GDX-502固相萃取柱的批量处理样品能力(12个)高于固相萃取盘(6个);同时所使用的有机试剂量远低于液液萃取。GDX-502固相萃取柱的萃取效率、分析通量、经济性和环保性具有更大的优势。     

气相色谱法测定地下水中15种有机氯农药

通过优化色谱分离条件,建立了一种以正己烷为液-液萃取溶剂,气相色谱法(电子捕获检测器)检测地下水中15种有机氯农药组分的分析方法。采用内标法降低了系统误差,定量分析结果更加准确。加标20ng/L时测定回收率为84.8%～101.0%,相对标准偏差(RSD,n=7)为1.9%～5.6%;基于5ng/L加标样品计算的检出限为0.6～1.4ng/L。方法适用于地下水中有机氯农药的检测。     

固相萃取-气相色谱法测定水中多环芳烃

以国家标准分析方法和美国环保局分析方法为基础,采用固相萃取-气相色谱法测定水中多环芳烃。探讨了各条件对测定的影响,确定选用HP 5毛细管柱,手动进样,程序升温。方法的检出限在4～10ng/L,适用于优先监控的16种多环芳烃的同时分析。对煤矿矿坑排水以及污灌区的地下水样中的16种多环芳烃进行测定,并与高效液相色谱法的测定值进行对比,结果基本符合国家标准(相对误差<30.0%)的要求。     

顶空固相微萃取-气相色谱-质谱联用法同时测定湖库水中12种氯苯甲醚的条件优化

氯苯甲醚类化合物(CAs)是地表水中普遍存在的嗅味物质,在世界各地水环境中均可发现CAs的存在,CAs易在食物链中富集和放大,且随着氯原子取代数增加其毒性逐渐增强。水体中CAs属于痕量物质,检测时需要先对其进行富集处理,以往研究大多是对单个物质进行检测。本文建立了采用顶空固相微萃取结合气相色谱-质谱联用技术同时测定湖库水中12种CAs的方法。对顶空固相微萃取过程中的萃取纤维、萃取温度、离子强度、萃取时间及搅拌速率等实验条件进行对比和优化,确认了最佳萃取条件为:萃取温度80℃,离子浓度0.35g/mL,萃取时间40min,搅拌速率1150r/min,样品体积10mL(15mL萃取瓶)。采用气相色谱-质谱选择性离子扫描方式进行定量分析,方法的线性范围为1～50ng/L,检出限为0.045～0.185ng/L,回收率为95.5%～115.1%,相对标准偏差≤13.02%。该方法相较于固相萃取及吹扫捕集法的检出限更低,对于样品浓度的变化感应度高,实验仪器的精密度优于其他方法。     

液-液萃取-气相色谱法测定水中9种有机氯农药

采用正己烷液-液萃取法提取,气相色谱法-电子捕获检测器测定水中9种有机氯农药。优化了实验条件:添加两种替代物作为分析过程的质量监控;使用浓硫酸磺化法净化去除杂质;采用Rtx-5MS和Rtx-1701柱双柱定性,保证数据准确可靠。9种有机氯农药的方法检出限为0.0017～0.0079μg/L,回收率为74.7%～105.1%,相对标准偏差(RSD,n=7)为4.2%～9.3%,9种农药在0.5～100μg/L内与峰面积呈良好的线性关系。方法检出限低,准确度和精密度高,简便,适用于批量样品的分析。     

全国地下水调查中12种半挥发性必检组分的测定

经过优化组合建立了适用于全国地下水调查中六六六、滴滴涕、苯并[a]芘等12种必检组分测定的分析流程。方法利用正己烷液-液萃取,以气相色谱法(电子捕获检测器)检测11种有机氯组分,高效液相色谱法(紫外、荧光检测器)检测苯并[a]芘。建立了分析过程的质量控制流程程序与质量管理指标范围,确保检测数据达到允许的范围之内。所建分析方法检测限低、精密度好,方法简便、准确,适用于批量样品分析。方法报出限在1.00~1.50 ng/L,8次测定相对标准偏差为2.52%~6.07%,加标回收率为85.3%~106.0%,满足了全国地下水调查评价规范的要求。     

小体积液液萃取气相色谱-质谱法测定地下水中的克百威与3-羟基克百威

克百威和3-羟基克百威是一对典型的农药母体及其代谢产物,由于其水溶性高、毒性大,可通过地表水或地下水进行长距离迁移,对人类健康和环境安全造成危害。以往通常采用液相萃取或固相萃取的方式提取样品中的克百威和3-羟基克百威,但这些方法操作繁琐、耗时较长,不利于室内模拟实验中多组样品的检测。为实现克百威与3-羟基克百威在地下水中的快速定量,本文建立了一种小体积液液萃取的前处理方法进行提取,并采用气相色谱-质谱(GC-MS)进行检测,对影响克百威和3-羟基克百威萃取效率的因素进行了研究。通过实验对比不同萃取剂、不同pH、不同离子强度条件下克百威与3-羟基克百威的回收率,优化了前处理条件。结果表明,选择二氯甲烷作为萃取剂且用量为1mL,调节水样pH=5,氯化钠用量为40g/L时克百威和3-羟基克百威的回收率最高,分别为75.1%～98.6%、55.0%～66.3%。性能评价结果显示,方法精密度和方法准确度满足测试要求(相对标准偏差10%,n=5),克百威和3-羟基克百威的方法检出限分别为15.3μg/L、10.2μg/L。该方法操作简便、快速、消耗溶剂少,与传统的液液萃取法相比,本方法耗时约为前者的1/8,消耗溶剂量约比前者小2个数量级,能够满足室内模拟实验需求。     

顶空进样-固相微萃取测定饮用水源水中吡啶

用75μm CarboxenTM-Polydimethylsiloxane(CAR-PDMS)固相微萃取头顶空萃取15 mL水样中的吡啶,萃取物用气相色谱-质谱法进行分离和检测,采用内标法和质谱的选择离子监测模式进行定量分析。优化了顶空进样-固相微萃取条件,获得较佳的萃取温度(58.0℃)和萃取时间(40 min)。在优化的条件下,方法检出限为1.5μg/L,标准曲线的线性相关系数为0.9994,线性范围为2.5～50.0μg/L;饮用水源水和纯水加标平均回收率为75.6%～81.3%,相对标准偏差(RSD,n=6)为9.60%～12.21%。使用顶空萃取方式可避免样品基体的复杂性,有利于保护萃取头涂层,同时无需使用有机萃取溶剂;使用质谱检测器可减小假阳性带来的影响。顶空进样-固相微萃取操作简单、环保、灵敏度高,适合用于饮用水源水中吡啶的监测分析。     

圆盘固相萃取富集-气相色谱法测定地表水中有机氯和有机磷农药

采用环境友好的圆盘固相萃取新技术富集水体中有机氯农药和有机磷农药,分别用微池电子捕获检测器(μECD)和火焰光度检测器(FPD)气相色谱法检测,实现了水中有机氯和有机磷农药残留物的测定。结果表明,16种有机氯农药的平均回收率为64.7%~102%,精密度(RSD,n=6)为2.9%~15%;13种有机磷农药的平均回收率为65.9%~104%,精密度(RSD,n=6)为1.7%~17%。方法快速、灵敏、低污染,可用于水体中多种有机氯农药和有机磷农药的残留分析。     

The terrestrial fauna of the Late Triassic Pant-y-ffynnon Quarry fissures,South Wales,UK and a new species of Clevosaurus (Lepidosauria: Rhynchocephalia)

Pant-y-ffynnon Quarry in South Wales yielded a rich cache of fossils in the early 1950s, including articulated specimens of new species (the small sauropodomorph dinosaur Pantydraco caducus and the crocodylomorph Terrestrisuchus gracilis), but no substantial study of the wider fauna of the Pant-y-ffynnon fissure systems has been published. Here, our overview of existing specimens, a few described but mostly undescribed, as well as freshly processed material, provides a comprehensive picture of the Pant-y-ffynnon palaeo-island of the Late Triassic. This was an island with a relatively impoverished fauna dominated by small clevosaurs (rhynchocephalians), including a new species, Clevosaurus cambrica, described here from a partially articulated specimen and isolated bones. The new species has a dental morphology that is intermediate between the Late Triassic Clevosaurus hudsoni, from Cromhall Quarry to the east, and the younger C. convallis from Pant Quarry to the west, suggesting adaptive radiation of clevosaurs in the palaeo-archipelago. The larger reptiles on the palaeo-island do not exceed 1.5?m in length, including a small carnivorous crocodylomorph, Terrestrisuchus, and a possible example of insular dwarfism in the basal dinosaur Pantydraco.     

Définition d'une limite multicritère ; stratigraphie du passage Campanien–Maastrichtien du site géologique de Tercis (Landes,SW France)Definition of a multi-criteria boundary; stratigraphy of the Campanian–Maastrichtian interval of the geological site at Tercis (Landes,SW France)

Lithostratigraphy, physicochemical stratigraphy, biostratigraphy, and geochronology of the 77–70 Ma old series bracketing the Campanian–Maastrichtian boundary have been investigated by 70 experts. For the first time, direct relationships between macro- and microfossils have been established, as well as direct and indirect relationships between chemo-physical and biostratigraphical tools. A combination of criteria for selecting the boundary level, duration estimates, uncertainties on durations and on the location of biohorizons have been considered; new chronostratigraphic units are proposed. The geological site at Tercis is accepted by the Commission on Stratigraphy as the international reference for the stratigraphy of the studied interval. To cite this article: G.S. Odin, C. R. Geoscience 334 (2002) 409–414.     

The effect of water on accessory phase solubility in subaluminous and peralkaline granitic melts

The solubilities of columbite, tantalite, wolframite, rutile, zircon and hafnon were determined as a function of the water contents in peralkaline and subaluminous granite melts. All experiments were conducted at 1035 °C and 2 kbar and the water contents of the melts ranged from nominally dry to approximately 6 wt.% H₂O. Accessory phase solubilities are not affected by the water content of the peralkaline melt. By contrast, solubilities are affected by the water content of the subaluminous melt, where the solubilities of all the accessory phases examined increase with the water content of the melt, up to 2 wt.% H₂O. At higher water contents, solubilities are nearly constant. It can be concluded that water is not an important control of accessory phase solubility, although the water content will affect diffusivities of components in the melt, thus whether or not accessory phases will be present as restite material. The solubility behaviour in the subaluminous and peralkaline melts supports previous spectroscopic studies, which have observed differences in the coordination of high field strength elements in dry vs. wet subaluminous granitic glasses, but not for peralkaline granitic glasses. Lastly, the fact that wolframite solubility increases with increasing water content in the subaluminous melt suggests that tungsten dissolved as a hexavalent species.     

Quaternary stresses revealed by calcite twinning inversion: insights from observations in the Savonnières underground quarry (eastern France)

Calcite samples were extracted both from the rock matrix and the superficial coating of a karstified fault plane of an underground quarry, located in the eastern border of the Paris basin. The karstification is dated as Quaternary. Analysis of mechanical calcite twinning reveals that only the calcite matrix has also undergone a compression trending WNW that can be attributed to the Mio-Pliocene alpine collision. Both coating and matrix have undergone a strike-slip regime with σ₁ roughly trending north–south, that could correspond to the regional present-day state of stress, a strike-slip compression rather trending NNW, modified by local phenomena. To cite this article: M. Rocher et al., C. R. Geoscience 335 (2003).     

HYDROGEOLOGY

正20141756 Chen Ruige(Mathematical College,China University of Geosciences,Beijing100083,China);Zhou Xun Numerical Simulation of Groundwater Level Fluctuation in a Coastal Confined Aquifer with Sloping Initial Groundwater Level Induced by the Tide(Geological Bulletin of China,ISSN1671-2552,CN11-4648/P,32(7),2013,p.1099-1104,6 illus.,16 refs.) Key words:confined water,groundwater level     

METAMORPHIC PETROLOGY

正20141408 Cai Jia(Institute of Geology,Chinese Academy of Geological Sciences,Beijing100037,China);Liu Fulai Petrogenesis and Metamorphic P-T Conditions of Garnet-Spinel-Biotitebearing Paragneiss in Danangou Area,Daqingshan-Wulashan Metamorphic Complex Belt(Acta Petrologica Sinica,ISSN1000-0569,CN11-1922/P,29(7),     

SERIALS

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GEOPHYSICAL EXPLORATION

正20142386An Guoying(China Aero Geophysical Survey and Remote Sensing Center for Land and Resources,Beijing 100083,China)Application of Satellite Remote Sensing in Regional Hydrogeological Investigation:Taking Cenozoic Strata in Wenquan Sheet(1∶250 000)of Karakoram Range as an Example(Geosci-     

QUATERNARY GEOLOGY & GEOMORPHOLOGY

正20141016An Chengbang(Key Laboratory of Western China’s Environmental Systems,Ministry of Education,Lanzhou University,Lanzhou 730000,China);Zhao Yongtao Lake Records during the Last Glacial Maximum from Xinjiang,NW China and Their Climatic Impli-     

PETROLEUM GEOLOGY

正20141538 Cao Qing(School of Earth Sciences and Engineering,Xi’an Petroleum University,Xi’an 710065,China);Zhao Jingzhou Characteristics and Significance of Fluid Inclusions from Majiagou Formation,Yichuan Huangling Area,Ordos Basin(Advances in Earth Science,ISSN1001-8166,CN62-1091/P,28(7),2013,p.819-828,7 illus.,3 tables,43 refs.)