多接收器电感耦合等离子体质谱法测定土壤标准物质铜同位素组成

近年来,铜同位素在表生环境和生物地球化学中的应用越来越广泛,尤其是土壤的铜同位素组成可以示踪环境污染物来源及生物地球化学过程。目前,对土壤铜同位素进行研究时,主要以硅酸岩标准物质为标样来衡量土壤样品铜同位素测定的准确性和精确性。但土壤与硅酸岩中铜、基质离子及有机质的含量等存在很大差异(如:硅酸岩中的铜含量80μg/g,一些土壤中的铜含量很低,20μg/g),将硅酸岩标准物质作为标样来监测土壤样品的数据质量缺乏代表性。为了弥补这一缺陷,本文精确测定4个国家土壤标准物质(GBW07443、GBW07425、GBW07427、GBW07389)的铜同位素组成,并将其作为检验土壤样品铜同位素测定过程中的标准。实验中采用高温高压反应釜消解样品,利用AG MP-1M树脂进行纯化,全流程空白2ng,回收率≥98%,通过多接收器电感耦合等离子体质谱仪(MC-ICP-MS)采用标样-样品-标样间插法进行仪器分馏校正,δ~(65)Cu的长期测试外精度优于0.05‰(n=306, 2SD)。GBW07443、GBW07425、GBW07427和GBW07389的铜同位素组成分别为-0.04‰±0.04‰(n=9, 2SD)、-0.07‰±0.05‰(n=12, 2SD)、-0.06‰±0.04‰(n=12, 2SD)、-0.02‰±0.06‰(n=12, 2SD)。这些土壤标准物质的铜同位素组成均位于0附近,大致为自然界土壤铜同位素比值变化范围(-0.5‰～+0.5‰)的中间值,且样品容易获得,其化学和铜同位素组成均一,适合作为监控土壤铜同位素化学及质谱分析数据可靠性的标准物质。     

有机化学物质碳氮稳定同位素系列标准物质研制

实验室和研究人员所使用的碳、氮同位素标准物质一般由国际原子能机构(IAEA)获得,然而近年来,随着碳氮同位素在实验室质量监控、方法评价、仪器校准等方面的广泛应用,市场需求量不断增加, IAEA研制的碳、氮同位素标准物质的种类与数量逐渐不能满足科学研究快速发展的需求。我国急需研制适应当今分析技术水平的有机质碳氮同位素国家标准物质用以进行质量监控、方法评价、仪器校准。为保证量值传递精度,本文研制了4个有机化学物质的碳氮稳定同位素标准物质,其中3个为尿素样品,1个为L-谷氨酸。经检验4种标准物质的均匀性通过F值检验,标准物质的δ~(13)C和δ~(15)N值经过一年的稳定性检验,特征量值变化在测量方法允许的不确定度范围内,由此判定δ~(13)C和δ~(15)N值稳定性良好。由包括研制单位实验室在内的12家实验室协同定值,采用高温燃烧-气体同位素质谱法测定了δ~(13)C和δ~(15)N值,系列标准物质δ~(13)C和δ~(15)N认定值区间呈梯度分布,δ~(13)C值为-40‰～0‰,δ~(15)N值为-10‰～30‰,涵盖了我国天然样品中有机质碳氮稳定同位素组成范围;研制的系列标准物质δ~(13)C的定值扩展不确定度不大于0.08‰,δ~(15)N的定值扩展不确定度不大于0.09‰,定值水平与国际标准物质相当。该系列标准物质已被国家质检总局批准为国家一级标准物质,批准号为GBW04494～GBW04497。可被用于地质、生态、环境等多种样品δ~(13)C和δ~(15)N比值测定时的分析监控、仪器校准、方法评价、质量保证和质量监控。     

元素分析仪-同位素比值质谱仪测定海洋沉积物有机碳稳定同位素方法初探

初步建立了利用元素分析仪-同位素比值质谱仪(EA-IRMS)联用技术测定海洋沉积物中有机碳稳定同位素的方法。标定了标准工作参考气CO2(δ13CvsPDB为-32.053‰);验证了仪器的稳定性,标准偏差为0.009‰;当离子流强度范围为0.4～8.7 V时,总体线性为0.0337‰/V,小于仪器线性指标0.06‰/V的要求;同时测定了国家标准物质GBW 04408、国际标准物质Urea和海洋沉积物样品M01的精密度和准确度,标准偏差在0.04‰～0.13‰范围内;并在三家实验室进行了测量比对实验,标准偏差小于0.20‰,满足地质样品再现性0.5‰的要求。所选样品区域δ13Corg范围为-25.29‰～-22.30‰,表明该海域总有机碳是陆源和海源两种来源的混合物。     

原子吸收分光光度计测定银的两种工作曲线拟合方式的研究

原子吸收工作曲线的两种拟合方式的研究,采用国家一级标准物质GBW07209(矿石中金和银成分分析标准物质)、GBW07255(GAg1)(银矿石中银成分分析标准物质)、GBW07256(GAg2)(银矿石中银成分分析标准物质)、GBW07305a(水系沉积物成分分析标准物质)、GBW07307a(水系沉积物成分分析标准物质)、GBW07311(水系沉积物成分分析标准物质)、GBW07405(土壤成分分析标准物质-黄红壤)进行实验,得出两种拟合方式的使用条件以及在实际工作中如何取舍的结论。     

X射线荧光光谱法测定土壤中34种主、次痕量元素

采用粉末样品压片制样,水系沉积物及土壤国家一级标准物质作为标准,使用经验系数法和散射线内标法校正元素间的吸收增强效应,用X射线光谱仪对土壤样品中的Fe_2O_3、Cao、Cl、S、As、Ba、Br、Ce、Co、Cr、Ni、Cu、Zn等34种主次痕量元素进行测定,用国家一级标准物质GBW07452(GSS-23),GBW07405(GSS-5)和GBW07404(GSS-4)分析检验准确度和精密度,分析结果与标样标准值吻合,除Cl、S、As、Br、Ce、Co、Ni、Th、Sc、Hf、Nb、Nd的精密度小于10.00%以外,其他各元素精密度均在5.00%以内,各元素检出限均满足化探要求。     

新疆克因布拉克铜锌矿床富CO_2-N_2流体及地质意义

克因布拉克铜锌矿床位于新疆阿尔泰山南缘冲乎尔盆地。矿体主要赋存于早二叠世花岗岩外接触带的下泥盆统康布铁堡组上亚组内。克因布拉克矿床经历了两个成矿期:海相火山喷流沉积成矿期和变质热液叠加成矿期。变质热液叠加成矿期可包括2个阶段:早阶段顺层透镜状石英脉(Q1)和晚阶段切层含黄铁矿?黄铜矿石英脉(Q2)。石英脉中流体包裹体以富CO_2-N_2为特征,流体包裹体组合(FIA)发育。流体包裹体类型包括CO_2-N_2包裹体、H_2O-CO_2(±N_2)包裹体和水溶液包裹体(L-V型)。显微测温结果显示,Q1中CO_2-N_2包裹体三相点温度(T_(m,CO_2))范围在-61.2~-59.1℃,部分均一温度(T_(h,CO2))的范围是-42.3~-36.0℃。Q2中CO_2-N_2流体包裹体的T_(m,CO_2)为-61.6~-58.1℃,T_(h,CO_2)范围是-30.0~10.4℃;Q2中H_2O-CO_2(±N_2)包裹体的T_(m,CO_2)为-61.4~-58.1℃,T_(h,CO_2)为-11.9~5.3℃,CO_2笼合物融化温度(T_(m,clath))范围是2.9~13.1℃,完全均一温度(T_(h,total))为312℃,伴生的L-V包裹体T_(h,total)为201~389℃,求得CO_2相密度为0.91~0.97 g/cm~3,盐度为1.62%~12.02%NaCl_(eqv)。计算得到流体包裹体的最低捕获压力范围为250~320 MPa,具有极富CO_2-N_2、低盐度的特点,属于变质流体。变质热液期早阶段石英脉δD值为-90.5‰,δ~(18)O_(H_2O)值为7.8‰;晚阶段石英脉δD值为-82.1‰~-80.4‰,δ~(18)O_(H_2O)为6.2‰~8.6‰。海相火山沉积期硫化物的δ~(34)S为0.9‰~2.1‰,硫来自火山岩浆活动;变质热液叠加期硫化物的δ~(34)S为0.1‰~1.1‰,显示了与造山变质深源流体有关的来源。克因布拉克铜锌矿床矿石变形变质结构特征以及石英脉中富CO_2-N_2流体的大量出现,说明变质流体对矿床具有一定的叠加改造,矿床具有多阶段的特点。     

样品质量对EA-IRMS法测量硫同位素组成的影响

研究不同样品质量对EA-IRMS法测量硫同位素组成的影响,通过对质量为47~1124μg国家标准物质硫化银GBW04414质量数66、65、64的SO2+和质量数50、49、48的SO+测试,结果表明该方法精密度受到样品质量的影响较大。当δ~(34)S的精密度要求标准偏差±0.2‰时,控制硫化银的样品质量应为(420±50)μg,即样品的硫含量应为(54±6)μg为佳。国家标准物质GBW04414的质量在380~420μg之间,δ~(34)S和δ~(33)S的精密度较高,标准偏差分别为±0.14‰、±0.09‰,精密度满足国家标准测量精度±0.2‰的实验要求。     

9种植物基体元素分析标准物质研制及量值特征

随着人们对食品安全关注度的提升,尤其是对植物源食品和保健品的元素组成与功效的关注,对评价可食性植物中元素分析标准物质需求日益增加。本文研制了红豆粉无机成分分析标准物质(GBW10228)、洋葱成分分析标准物质(GBW10232)、油菜成分分析标准物质(GBW10233)、金针菇粉中元素成分分析标准物质(GBW10247)、银耳粉中元素成分分析标准物质(GBW10248)、藕粉中元素成分分析标准物质(GBW10249)、山楂粉中元素成分分析标准物质(GBW10250)、三七粉中元素成分分析标准物质(GBW10251)、茉莉花成分分析标准物质(GBW10234)共9种植物基体分析标准物质。针对物料特点确定了候选物的采集地点、制备方法、封装工艺和保存条件,经检验均匀性、稳定性良好,通过方法研究制定了标准物质定值作业指导书,由11家实验室联合对Ag、Al、As、B、Ba、Be、Bi、Br、Ca、Cd、Ce、Cl、Co、Cr、Cs、Cu、Dy、Er、Eu、F、Fe、Gd、Ge、Hg、Ho、I、K、La、Li、Lu、Mg、Mn、Mo、N、Na、Nd、Ni、P、Pb、Pr、Rb、S、Sb、Sc、Se...     

高压密闭罐溶样-氢化物原子荧光法测定环境样品中的砷

使用高压密闭罐溶样方式,比较了利用浓HNO3、王水和HNO3+HF消解土壤、沉积物和植物样品,还原后用氢化物发生-原子荧光光谱法(HG-AFS)测定样品中砷的情况。使用优选的浓HNO3溶样法对土壤标准参考物质GBW(E)070009、GBW07404(GSS-4)、GBW07405(GSS-5)、GBW07407(GSS-7)、GBW07408(GSS-8)、GS-BZ50011-88(ESS-1)和植物标准参考物质GBW07604(GSV-3)、GBW07602(GSV-1)进行了分析,砷的测定结果与推荐值基本一致。加标回收实验的回收率在99.9%～105.6%。利用该法对实际样品进行了测定,并与土壤总砷国标法(GB/T22105.2-2008)的分析结果进行了比较,平行样的重现性好,表明砷的分析结果准确可靠。     

多接收等离子质谱（MC-ICP-MS )测定Mg同位素初步研究

常量元素Mg的同位素比值，应用在地球化学上有重要意义。笔者采用“样品-标准”交叉技术，以国际标准SRM980,AIdrich, Romil和实验室标准GSB作为实验材料，探讨浓度和基质效应影响，尝试建立高精度多接收等离子质谱(MC-ICP-MS)测定Mg同位素方法。相对于国际标准物质SRM980，本研究测得的国际标准物质Aldrich的δ26Mg和δ25Mg值分别为（2.64±0.15)‰(2σ）和（1.34±0.09)‰(2σ); Romil的δ26Mg和δ25Mg值分别为（2.46±0.15)‰(2σ）和（1.27±0.08)%(2σ)；国土资源部同位素地质重点实验室的实验室标准GSB的δ26Mg和δ25Mg值分别为（4.05±0.03)‰(2σ)和(2.05±0.03)‰(2σ)。     

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.     

Inter-regional correlation of transgressions and regressions in the Cretaceous period

Well investigated platforms have been selected in each continent, and the history of Cretaceous transgressions and regressions there is concisely reviewed from the available evidence. The factual records have been summarized into a diagram and the timing of the events correlated between distant as well as adjoining areas.On a global scale, major transgressions were stepwise enlarged in space and time from the Neocomian, via Aptian-Albian, to the Late Cretaceous, and the post-Cretaceous regression was very remarkable. Minor cycles of transgression-regression were not always synchronous between different areas. Some of them were, however, nearly synchronous between the areas facing the same ocean.Tectono-eustasy may have been the main cause of the phenomena of transgression-regression, but certain kinds of other tectonic movements which affected even the so-called stable platforms were also responsible for the phenomena. The combined effects of various causes may have been unusual in the Cretaceous, since it was a period of global tectonic activity. The slowing down of this activity followed by readjustments may have been the cause of the global regression at the end of the Cretaceous.     

The lamprophyres of Afyon stratovolcano,western Anatolia,Turkey: description and genesis

The Afyon stratovolcano exhibits lamprophyric rocks, emplaced as hydrovolcanic products, aphanitic lava flows and dyke intrusions, during the final stages of volcanic activity. Most of the Afyon volcanics belong to the silica-saturated alkaline suite, as potassic trachyandesites and trachytes, while the products of the latest activity are lamproitic lamprophyres (jumillite, orendite, verite, fitztroyite) and alkaline lamprophyres (campto-sannaite, sannaite, hyalo-monchiquite, analcime–monchiquite). Afyon lamprophyres exhibit LILE and Zr enrichments, related to mantle metasomatism.     

METAMORPHIC PETROLOGY

正20140751 Guo Xincheng(Geological Party,BGMRED of Xinjiang,Changji 831100,China);Zheng Yuzhuang Determination and Geological Significance of the Mesoarchean Craton in Western Kunlun Mountains,Xinjiang,China(Geological Review,ISSN0371-5736,CN11-1952/P,59(3),2013,p.401-412,8     

GEOCHEMICAL EXPLORATION

正20141058 Chen Ling(Key Laboratory of Mathematical Geology of Sichuan Province,Chengdu University of Technology,Chengdu610059,China);Guo Ke Study of Geochemical Ore-Forming Anomaly Identification Based on the Theory of Blind Source Separation(Geosci-     

SEISMIC GEOLOGY

正20141334 Chen Kun(Institute of Geophysics,China Earthquake Administration,Beijing100081,China);Yu Yanxiang Shakemap of Peak Ground Acceleration with Bias Correction for the Lushan,Sichuan Earthquake on April20,2013(Seismology and Geology,ISSN0253-4967,CN11-2192/P,35(3),2013,p.627-633,2 illus.,1 table,9 refs.)Key words:great earthquakes,Sichuan Province     

HISTORICAL GEOLOGY & STRATIGRAPHY

正20141624 Cai Xiongfei(Key Laboratory of Geobiology and Environmental Geology,Ministry of Education,China University of Geosciences,Wuhan 430074,China);Yang Jie A Restudy of the Upper Sinian Zhengmuguan and Tuerkeng Formations in the Helan Mountains(Journal of Stratigraphy,ISSN0253-4959CN32-1187/P,37(3),2013,p.377-386,5 illus.,2 tables,10 refs.)     

PALEONTOLOGY

正20142263Lü Shaojun(Geological Survey of Jiangxi Province,Nanchang 330030,China)Early-Middle Permian Biostratigraphical Characteristics in Qiangduo Area,Tibet(Resources SurveyEnvironment,ISSN1671-4814,CN32-1640/N,34(4),2013,p.221-227,2illus.,2tables,22refs.)Key words:biostratigraphy,Lower Permian,Middle Permian,Tibet     

MATHEMATICAL GEOLOGY

正20142560Hu Hongxia(Regional Geological and Mineral Resources Survey of Jilin Province,Changchun 130022,China);Dai Lixia Application of GIS Map Projection Transformation in Geological Work(Jilin Geology,ISSN1001-2427,CN22-1099/P,32(4),2013,p.160-163,4illus.,2refs.)     

GEOCHEMISTRY

正20140692 Duo Tianhui(No.402 Geological Team,Exploration of Geology and Mineral Resources of Sichuan Authority,Chengdu611730,China);Wang Yongli Computer Simulation of Neptunium Existing Forms in the Groundwater(Computing Techniques for Geophysical and Geochemical Exploration,ISSN1001-1749,CN51-1242/P,35(3),