超高效液相色谱法直接快速测定环境水样中硝基苯和苯胺

建立了超高效液相色谱直接快速测定环境水样中硝基苯和苯胺的分析方法。取900μL水样与100μL乙腈混匀,用微孔滤膜(0.2μm,有机系)过滤。采用1.7μm小颗粒填料的BEH phenyl柱,以乙腈/醋酸铵溶液为流动相,硝基苯和苯胺分别用紫外和荧光检测器检测,分析时间仅1.1 min。硝基苯和苯胺的线性范围分别是0.485～4850μg/L和0.495～1978μg/L,方法检出限分别是0.194μg/L和0.099μg/L,相关系数均在0.995以上。硝基苯9.70μg/L、194μg/L、1940μg/L三个浓度水平回收率在98.3%～101%,相对标准偏差在1.11%～2.03%。苯胺9.89μg/L、198μg/L、1978μg/L三个浓度水平回收率在98.6%～104%,相对标准偏差在0.75%～5.85%。与传统液相分析方法相比,本方法线性范围更宽,灵敏度更高;直接进样简化了前处理环节,减少采样体积和有机试剂的使用;分析效率高,适用于地下水、地表水等多种水质样品中痕量到常量范围的硝基苯和苯胺快速测定。     

浅析高效液相色谱-质谱/质谱法测定饮用水中的灭草松和2,4-D

利用高效液相色谱-质谱/质谱法,同时测定饮用水中灭草松和2,4-D,水样经0.45μm微孔滤膜过滤后直接上机,经高效液相色谱分离后,采用质谱/质谱法测定。结果表明,灭草松和2,4-D分别在0.25~8.00μg/L和1.00~30.0μg/L范围内线性良好,相关系数分别为0.9987和0.9980,检出限为0.002μg/L和0.004μg/L,相对标准偏差(RSD)分别为7.5%~8.0%和2.9%~4.8%,加标回收率分别在73.6%~90.4%和90.3%~103.0%之间。完全满足饮用水中灭草松和2,4-D的测定。     

微波消解-原子荧光光谱法测定化探样品中的砷和锑

准确测定砷和锑的含量是化探样品测定中的重要内容。本文介绍了测定这两种元素的一种新方法,笔者基于原子荧光光谱仪,试样经氢氟酸-盐酸-硝酸混酸微波消解,高氯酸-硫酸混酸蒸发除去氢氟酸,由盐酸-酒石酸混合溶液定容,从而得到样品中准确的砷、锑含量。本方法砷、锑校准曲线的线性相关系数均大于0.999;检出限分别为砷0.039μg/L、锑0.005 8μg/L。按照实验方法测定水系沉积物、土壤标准物质中砷、锑,结果的相对误差砷为1.52%～6.77%,锑为1.25%～7.17%;相对标准偏差(RSD,n=6)砷为2.27%～5.15%、锑为1.88%～5.81%。本方法适用于化探样品中砷含量在0.05～500μg/g、锑含量在0.05～300μg/g之间的样品测定。     

碱消解-高效液相色谱-电感耦合等离子体质谱法测定生物样品中的甲基汞和乙基汞

建立了碱消解-高效液相色谱-电感耦合等离子体质谱联用系统测定生物样品中甲基汞(MeHg)与乙基汞(EtHg)的分析方法。为提高灵敏度,选用微流量的PFA雾化器,在优化的检测条件下,MeHg及EtHg检出限可达到0.036μg/L和0.03μg/L;线性范围达到4个数量级,两条工作曲线线性相关系数为1。对1.78μg/L MeHg、1.65μg/L EtHg的混合标准溶液重复测定7次,色谱峰面积的相对标准偏差(RSD)分别为1.79%和1.44%。对标准物质BCR 464(金枪鱼)的分析结果表明,测定值与标准值基本吻合,但略低于标准值;甲基汞和乙基汞的加标回收率分别为85.9%和84.5%。高效液相色谱与质谱联用技术的高灵敏度和低检出限能够满足生物样品中汞形态定量分析的要求。     

微波消解-氢化物发生原子荧光光谱法同时测定化肥中的砷和汞

采用微波消解对样品进行前处理,建立了氢化物发生-双道原子荧光光谱同时测定化肥中砷和汞的方法。以20 g/L KBH4为还原剂,8%的盐酸为载液,测定砷和汞的负高压均为270 V,砷的灯电流为60 mA,汞的灯电流为20 mA。讨论了常见元素对测定的干扰,40 g/L的主量元素N、P、K,10倍于砷、汞浓度的杂质元素Te、Ca、Zn、Cu、Cr、Mn、Ni、Sb、Sn、Pb对砷和汞测定的影响满足分析要求。方法测定砷和汞的线性范围As为0.68～100μg/L,Hg为0.12～10μg/L;检出限As为0.68μg/L,Hg为0.12μg/L;方法精密度(RSD,n=5)低于8%。该方法具有前处理简便快速、易于操作、灵敏度高等特点,能满足化肥中砷和汞同时测定的要求。     

原子荧光光谱法测定芦荟中铅和镉

应用AFS-820型双道原子荧光测定芦荟中Pb和Cd,用HNO3-HClO4 消解样品,以KBH4 作还原剂分别测定Pb和Cd。Pb和Cd检出限分别为0. 58μg/L和0. 21μg/L,相对标准偏差(RSD,n=5)均小于10%,线性范围Pb为0~100μg/L,Cd为0~80μg/L,标准加入回收率Pb为88. 2% ~108. 6%,Cd为85. 3% ~112. 8%。方法经植物国家一级标准物质验证,结果与标准值相符。     

催化动力学光度法测定痕量亚硝酸根

基于0.02mol/L的稀H2SO4介质中,痕量亚硝酸根对高碘酸钾氧化靛红的褪色反应有明显的催化作用,建立了痕量亚硝酸根的动力学光度测定法,方法检出限为0.072μg/L,线性范围为0～4.0μg/L。用于测定环境水样中的痕量亚硝酸根,结果与Griess法相符,6次测定结果的RSD<2.9%。     

离子色谱法测定水样中S2-、SO2-3、SO2-4、S2O2-3

该种方法利用离子色谱仪的电导检测器与电化学检测器串联,十几分钟即可连续完成水中S2-、SO2-3、SO2-4、S2O2-3的测定,方法具有快速、高效、方便、灵敏、选择性好等特点.方法的检出限分别为S2-12.5μg/L;SO2-3 22.4μg/L;SO2-4 5.0μg/L;S2O2-3 5.0μg/L.相对标准偏差在1.5%～6.9%之间,能够满足水中S2-、SO2-3、SO2-4、S2O2-3四种阴离子分析测试的需要.     

分散液-液微萃取—火焰原子吸收光谱法测定水样中的痕量铅

对萃取剂和分散剂进行了筛选,并研究了pH、APDC的用量、萃取时间等试验条件对萃取效率的影响。将分散液-液微萃取(DLLME)与火焰原子吸收光谱法(FAAS)相结合,建立了快速、高灵敏度测定水样中痕量铅的新方法。在优化条件下,富集6.0mL样品溶液,铅的检出限为1.35μg/L,线性范围10.0～600.0μg/L,对含有20μg/L和400μg/L Pb2+的标准溶液平行萃取测定11次,相对标准偏差分别为3.35%和2.78%。本方法应用于自来水、河水、地下水和海水中痕量铅的分析,加标回收率在95.5%～99.7%之间。     

计时电位溶出法同时测定锑样品中铜和铋

:探讨了以预镀汞膜玻碳电极为工作电极 ,同时测定锑类金属及其氧化物和硫化物中铜、铋的计时电位溶出法的适宜条件 ;试验了酸介质和常见元素对测定的影响 ;选择了仪器的最佳工作条件。结果表明 ,在 0 1mol/LHCl- 0 0 1mol/L抗坏血酸底液中 ,相对饱和氯化钾甘汞电极 ,铜与铋的溶出峰电位分别为 - 0 2 0V和 - 0 1 0V ,分辨效果较好。在测定条件下 ,铜和铋的线性范围分别为 0～ 30 0μg/L和 0～ 80 μg/L ,检出限分别为 7μg/L和 2 μg/L。用该法测定出口锑中铜和铋 ,结果与AAS及ICP -AES法测定值吻合 ,三次重复测定的RSD在 1 2 %～ 4 1 %。     

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.     

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).     

NONMETALS DEPOSITS

正20141520 Bo Ying(Key Laboratory of Metallogeny and Mineral Assessment,MLR,Beijing 100037,China);Liu Chenglin Saline Spring Hydrochemical Characteristics and Indicators for Potassium Exploration in Southwestern and Northern Tarim Basin,Xinjiang(Acta Geoscientica Sinica,ISSN1006-3021,CN11-3474/P,34(5),2013,p.594-602,5 illus.,3 tables,28 refs.)     

MATHEMATICAL GEOLOGY

正20141243Chen Ge(Hangzhou Research Institute of Petroleum Geology,PetroChina,Hangzhou 310023,China);Si Chunsong Study on Sedimentary Numerical Simulation Method of Fan Delta Sand Body(Journal of Geology,     

PROSPECTING EXPLORATION

正20142599Chen Sanming(Guangxi Key Laboratory of Concealed Deposits Exploration,Guilin University of Technology,Guilin541004,China);He Yuzhou Block Model and Reserves Estimation of Panzhihua Iron Deposit Based on 3D Geological Modeling(Journal of Guilin University of Technology,ISSN1674-9057,CN45-1375/N,33(4),2013,p.610-615,9illus.,1table,15refs.)     

STRUCTURAL GEOLOGY

正20140594 Bai Daoyuan(Hunan Institute of Geology Survey,Changsha 410016,China);Zhong Xiang Faults in the Jingzhou Basin and Their Tectonic Settings(Geotectonica et Metallogenia,ISSN1001-1552,CN44-1595/P,37(2),2013,p.173-183,6illus.,59refs.)Key words:basin evolution,tectonic setting,South China In the Upper Paleozoic and Jurassic se-     

STRUCTURAL GEOLOGY

正20141912Cao Hui(State Key Laboratory for Continental Tectonics and Dynamics,Institute of Geology,Chinese Academy of Geological Sciences,Beijing 100037,China)Gravitational Collapse and Folding during Orogenesis:A Comparative Study of FIA Trends and Fold Axial Plane Traces(Geology in China,ISSN1000-3657,CN11-1167/P,40(6),2013,p.1818-1828,9illus.,35refs.,with     

PALEOZOOLOGY

正20141609 Chen Guiying(College of Earth Sciences,Guilin University of Technology,Guilin 541004,China);Han Nairen New Materials of Stylophora from the Upper Cambrian of the Jingxi Area,Guangxi,South China(Acta Palaeontologica Sinica,ISSN0001-6616,CN32-1188Q,52(3),2013,p.288-293,2 illus.,12 refs.)Key words:Stylophora,Guangxi     

GEOPHYSICS

正20140634 Cao Lingmin(Key Laboratory of Marine Geology and Environment,Institute of Oceanology,Chinese Academy of Sciences,Qingdao 266071,China);Xu Yi Finite Difference Tomography of the Crustal Velocity Structure in Tengchong,Yunnan Province(Chinese Journal of Geophysics,ISSN0001-5733,CN11-2074/P,56(4),2013,p.1159-1167,6illus.,35refs.,with English abstract)