高温熔融研制钾长石玻璃标准物质初探   总被引：1，自引：1，他引：0  

宋佳瑶  袁洪林  包志安  陈开运  贺国芬  范超 《岩矿测试》2011,30(4):406-411

激光剥蚀多接收等离子体质谱(LA-MC-ICPMS)是进行原位微区分析微量元素和同位素的重要技术之一,标准样品与样品之间的基体匹配是解决影响该技术准确分析的基体效应和分馏效应的首选方案。长石(特别是长石微区)的Pb同位素组成是示踪岩石形成和演化历史的重要途径,而LA-MC-ICPMS技术则是进行长石Pb同位素原位微区分析的关键技术,然而目前国内外尚没有合适的长石Pb同位素分析标准。文章研究探讨了利用高温炉进行原位微区分析钾长石中Pb同位素组成所用外部标准物质合成条件,结果表明,常规的74μm(200目)碎样无法得到均一的钾长石玻璃,需要将初始钾长石粉末研磨至1300目以下;高温炉合成温度为1680℃;熔融时间为2 h;采用液氮方式淬火。制成的钾长石玻璃除表面具有轻微的不均一性外,内部的Pb同位素比值为1.90779±0.00009(208Pb/206Pb,2s),0.75899±0.00004(207Pb/206Pb,2s),20.909±0.002(206Pb/204Pb,2s),15.871±0.002(207 Pb/204 Pb,2s)和39.888±0.005(208 Pb/204 Pb,2s),相应的相对标准偏差(RSD)分别为0.007%、0.008%、0.016%、0.016%和0.021%。表明利用本研究方法合成的钾长石玻璃可作为潜在的钾长石中Pb同位素组成原位微区分析外部校准物质。  相似文献   

水浴消解-顺序注射-氢化物发生原子荧光光谱法测定铁矿石中砷和汞   总被引：2，自引：2，他引：0  

苏明跃  陈广志  王晶  姚传刚 《岩矿测试》2011,30(2):210-213

采用水浴加热低温消解浸取铁矿石样品,顺序注射-氢化物发生原子荧光光谱法测定铁矿石样品中砷和汞的含量.选择了消解试剂,研究了硼氢化钾浓度、载气流量、屏蔽气流量、溶液酸介质、载流、溶液酸碱比例、样品中的主要基体元素等因素对砷和汞测定的干扰,并确立了适宜的测定条件.砷浓度在0～100 μg/L与荧光强度呈良好的线性关系,砷的...  相似文献   

快速程序升温-石墨炉原子吸收光谱法测定地质样品中痕量镉     

吴峥  牟乃仓  王龙山  张飞鸽  高登峰  王光照 《岩矿测试》2011,30(2):186-189

建立了快速程序升温-石墨炉原子吸收光谱测定地质样品中痕量镉的分析方法.样品用硝酸-氢氟酸-高氯酸进行前处理,为提高分析效率,改进了石墨炉升温程序,省去了常规方法中的灰化步骤,使测定镉的程序升温时间由常规的90～100 s降至24 s,工作效率显著提高.方法检出限为0.011 μg/g,加标回收率为93.5%～106.0...  相似文献   

王水溶矿-等离子体光谱法测定砷矿石和锑矿石中砷锑硫铜铅锌   总被引：7，自引：7，他引：0  

马新荣  马生凤  王蕾  温宏利  巩爱华  许俊玉 《岩矿测试》2011,30(2):190-194

建立了王水溶矿-电感耦合等离子体发射光谱法测定砷矿石和锑矿石中主、次量元素砷、锑、硫及含量范围在100μg/g以上的铜、铅、锌等元素的方法。研究了放置时间、溶液酸度、氧化剂与络合剂对砷、锑、硫及其他元素测定的影响。不同王水浓度酸度对可同时测定的其他元素的影响不明显;当溶液酸度较小时,不能放置,应及时测定;如需放置,应在溶液定容前加入酒石酸防止水解。样品中砷、锑、硫的含量在0.74%～39.7%时,相对误差(RE)在-0.17%～7.74%,5次独立测定的相对标准偏差(RSD)均小于2%;含量在100～500μg/g以下的Sb,RE在-2.5%～4.79%,5次独立测定的RSD均小于2%。由于稀释倍数较大(DF=1000),不能准确测定含量在100μg/g以下的铜、铅、锌;含量在100μg/g以上的铜、铅、锌的RE在-10.3%～10.3%,5次独立测定的RSD基本小于5%。经标准物质验证获得满意结果。方法也可应用于砷、锑含量较高的硫化矿的测定。  相似文献   

Metamorphic veining and mass transfer in a chemically closed system: a case study in Alpine metabauxites (western Vanoise)   总被引：2，自引：0，他引：2  

B. GOFFÉ  F. BRUNET  C. POINSSOT  O. VIDAL  N. FINDLING  D. MENUT 《Journal of Metamorphic Geology》2011,29(3):275-300

In western Vanoise (French Alps), karstic pockets of Triassic‐to‐Jurassic metabauxites embedded in carbonate rocks and containing several generations of metamorphic veins were studied. During blueschist facies metamorphism, a cumulative amount of ～13 vol% of water is inferred to have been produced locally by successive dehydration reactions, and part of this fluid remained in the bauxitic lenses during most of the metamorphic cycle. Field and geochemical evidence show that these rocks have been isolated from large‐scale fluid flow (closed‐system behaviour). It is proposed that the internally derived fluid has promoted the opening of fluid‐filled open spaces (as attested by the euhedral habits of vein minerals) and served as medium for mass transfer from rock to vein. Indeed, the vein infill is obviously the result of chemical interactions, at the millimetre‐to‐centimetre scale, between the rock minerals and the locally produced aqueous fluid. Two vein types can be distinguished based on mineralogical and textural features: (i) some veins are filled with newly formed products of either prograde (chloritoid) or retrograde (chlorite) metamorphic reactions; in this case, fluid‐filled open spaces seem to offer energetically favourable nucleation/growth sites; (ii) the second vein type is infilled with cookeite or pyrophyllite, that were present in the host rock prior to the vein formation. In this closed chemical system, the components for the vein infill minerals have been transferred from rock to vein through the fluid, in a dissolution–transport–precipitation process, possibly stress‐assisted. These different vein generations all contain Al‐rich mineral infills, suggesting that Al was a mobile element (cm scale) during metamorphism. In these HP rocks, fluid flow may have been restricted, and if so mass transfer occurred by diffusion in an almost stagnant fluid. Metamorphic veins can be seen as witnesses of fluid and mass redistribution that partly accommodate the rock deformation (lateral segregation).  相似文献   

微波消解-电感耦合等离子体质谱法测定土壤和沉积物中痕量稀土元素   总被引：11，自引：6，他引：5  

陈永欣  黎香荣  韦新红  吕泽娥  谢毓群  蔡维专 《岩矿测试》2011,30(5):560-565

建立了微波消解-电感耦合等离子体质谱法测定土壤和沉积物中15种痕量稀土元素的分析方法。研究了溶样试剂、微波消解程序、标准溶液配制、质谱干扰与内标元素对稀土元素测定的影响。加入氢氟酸能有效打开样品,以HNO3-HF-H2O2混合酸溶解样品,稀土元素的溶出率较高。采用模拟土壤、沉积物中稀土元素天然组成比值的校正溶液,对稀土元素间的干扰具有明显的抑制作用。通过测定单个La、Ce、Pr、Nd和Ba的氧化物及氢氧化物产率,计算出等效干扰浓度,进而校正多原子离子干扰。利用103Rh内标校正系统,有效地抑制了分析信号的动态漂移。方法检出限为1.2～7.1 ng/g,精密度(RSD)≤5.3%(n=6),加标回收率为86.1%～110.1%。使用土壤、沉积物标准物质进行验证,测定结果与标准值相符。建立的方法样品处理程序简单快速、线性范围宽、分析重现性好、结果准确,适用于大批量地质样品的分析。  相似文献   

王水溶样-电感耦合等离子体发射光谱法同时测定铁铜铅锌硫化物矿石中8个元素   总被引：5，自引：5，他引：0  

温宏利  马生凤  马新荣  王蕾  范凡  巩爱华 《岩矿测试》2011,30(5):566-571

建立了王水溶样-电感耦合等离子体发射光谱法同时测定铁、铜、铅、锌硫化物矿中Cu、Pb、Zn、As、Ag、Cd、Hg和Mo等8个元素的分析方法。确定了方法的溶矿及测定条件,用国家一级标准物质GBW07162(多金属贫矿石)和GBW07164(多金属矿石)进行精密度实验,除个别元素外,大多数的元素精密度(RSD,n=11)小于5%,准确度(RE)小于10%。通过一系列硫化物矿石标准物质进行方法验证,检测结果基本都在标准值的误差范围内,符合地质矿产开发的要求。方法简单,同时测定元素较多,线性范围宽,检出限低,尤其有利于硫化物矿石中的亲硫元素As、Ag、Hg的分析,实用性强。  相似文献   

顶空进样-固相微萃取测定饮用水源水中吡啶   总被引：2，自引：1，他引：1  

赖永忠 《岩矿测试》2011,30(5):596-600

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。  相似文献   

水中氯代烃单体碳同位素分析中预富集方法进展     

凌媛  黄毅  尚文郁  谢曼曼  刘舒波  孙青 《岩矿测试》2011,30(6):795-801

高精度准确测定氯代烃单体碳同位素对示踪污染物来源,了解污染物的生物降解过程具有重要意义。在环境转化过程中,有机污染物的同位素组成可能是稳定不变的,也有可能发生改变。若污染物的同位素组成在迁移转化过程中不变,根据其同位素组成可以示踪污染物的来源;若同位素组成变化,根据同位素分馏结果,可以评价环境中有机污染物降解发生的可能性和程度。本文综述了固相微萃取、静态顶空进样、吹扫-捕集、多级串联技术等前处理方法与气相色谱-燃烧-同位素比值质谱仪(GC-C-IRMS)联用分析水中氯代烃单体碳同位素的研究进展,比较了分析方法的优缺点。液-液萃取较少用于水中氯代烃的单体同位素分析。静态顶空进样、固相微萃取、吹扫-捕集都是无溶剂富集技术,与GC-C-IRMS联用分析水中氯代烃单体同位素过程中不存在或存在小且恒定的可校正的同位素分馏,分析精度一般优于1‰,没有二次污染,降低了杂质干扰,提高了GC-C-IRMS的分辨率和分析精度,降低了检测限。从静态顶空进样、固相微萃取、吹扫-捕集,到多级串联等技术与GC-C-IRMS联用分析水中氯代烃单体同位素比值,检测限逐渐降低。目前,吹扫-捕集-GC-C-IRMS在分析水中氯代烃中应用最广泛,重现性好、检测限低。针内微萃取、管内微萃取、搅动棒吸附萃取和顶空进样吸附萃取等前处理方法与GC-C-IRMS仪联用具有一定的应用前景。  相似文献   

Numerical modeling of multiphase fluid flow in deforming porous media: A comparison between two- and three-phase models for seismic analysis of earth and rockfill dams     

A.R. Khoei  T. Mohammadnejad 《Computers and Geotechnics》2011

In this paper, a fully coupled numerical model is presented for the finite element analysis of the deforming porous medium interacting with the flow of two immiscible compressible wetting and non-wetting pore fluids. The governing equations involving coupled fluid flow and deformation processes in unsaturated soils are derived within the framework of the generalized Biot theory. The displacements of the solid phase, the pressure of the wetting phase and the capillary pressure are taken as the primary unknowns of the present formulation. The other variables are incorporated into the model using the experimentally determined functions that define the relationship between the hydraulic properties of the porous medium, i.e. saturation, relative permeability and capillary pressure. It is worth mentioning that the imposition of various boundary conditions is feasible notwithstanding the choice of the primary variables. The modified Pastor–Zienkiewicz generalized constitutive model is introduced into the mathematical formulation to simulate the mechanical behavior of the unsaturated soil. The accuracy of the proposed mathematical model for analyzing coupled fluid flows in porous media is verified by the resolution of several numerical examples for which previous solutions are known. Finally, the performance of the computational algorithm in modeling of large-scale porous media problems including the large elasto-plastic deformations is demonstrated through the fully coupled analysis of the failure of two earth and rockfill dams. Furthermore, the three-phase model is compared to its simplified one which simulates the unsaturated porous medium as a two-phase one with static air phase. The paper illustrates the shortcomings of the commonly used simplified approach in the context of seismic analysis of two earth and rockfill dams. It is shown that accounting the pore air as an independent phase significantly influences the unsaturated soil behavior.  相似文献