电感耦合等离子体原子发射光谱法测定硅铁中微量元素   总被引：6，自引：1，他引：6  

刘先国  方金东 《岩矿测试》2002,21(1):63-65

应用电感耦合等离子体发射光谱法对硅铁中微量元素的测定进行了研究，采用基体匹配法消除了大量基体的干扰，选择了最佳激发条件，样品的加标回收率在97％－107％。方法用美国硅铁标样分析验证，测定结果与标准值吻合较好，各元素8次测定的RSD％＜7％。  相似文献   

Method of Laser Scanning Data Matching     

HE Lei  YU Chun-ping  LI Guang-yun 《测绘科学技术学报》2008,25(6)

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Niobium and Tantalum Concentrations in NIST SRM 610 Revisited     

Zhaochu Hu  Shan Gao  Yongsheng Liu  Juan Xu  Shenghong Hu  Haihong Chen 《Geostandards and Geoanalytical Research》2008,32(3):347-360

Niobium and Ta concentrations in MPI‐DING and USGS (BCR‐2G, BHVO‐2G, BIR‐1G) silicate rock glasses and the NIST SRM 610–614 synthetic soda‐lime glasses were determined by 193 nm ArF excimer laser ablation and quadrupole ICP‐MS. Measured Nb and Ta values of MPI‐DING glasses were found to be consistently lower than the recommended values by about 15% and 25%, respectively, if calibration was undertaken using commonly accepted values of NIST SRM 610 given by Pearce et al. Analytical precision, as given by the 1 s relative standard deviation (% RSD) was less than 10% for Nb and Ta at concentrations higher than 0.1 μg g^?1. A significant negative correlation was found between logarithmic concentration and logarithmic RSD, with correlation coefficients of ‐0.94 for Nb and ‐0.96 for Ta. This trend indicates that the analytical precision follows counting statistics and thus most of the measurement uncertainty was analytical in origin and not due to chemical heterogeneities. Large differences between measured and expected Nb and Ta in glasses GOR128‐G and GOR132‐G are likely to have been caused by the high RSDs associated with their very low concentrations. However, this cannot explain the large differences between measured and expected Nb and Ta in other MPI‐DING glasses, since the differences are normally higher than RSD by a factor of 3. Count rates for Nb and Ta, normalised to Ca sensitivity, for the MPI‐DING, USGS and NIST SRM 612–614 glasses were used to construct calibration curves for determining NIST SRM 610 concentrations at crater diameters ranging from 16 (im to 60 μm. The excellent correlation between the Nb/Ca_1μgg‐1 signal (Nb represents the Nb signal intensity; Ca_{1μg g‐1} represents the Ca sensitivity) and Nb concentration, and between the Ta/Ca_{1μg g‐1} signal (where Ta represents the Ta signal intensity; Ca_{1μg g‐1} represents the Ca sensitivity) and Ta concentration (R²= 0.9992–1.00) in the various glass matrices suggests that matrix‐dependent fractionation for Nb, Ta and Ca was insignificant under the given instrumental conditions. The results confirm that calibration reference values of Nb and Ta in NIST SRM 610 given by Pearce et al. are about 16% and 28% lower, respectively. We thus propose a revision of the preferred value for Nb from 419.4 ± 57.6 μg g^?1 to 485 ± 5 μg g^?1 (1 s) and for Ta from 376.6 ± 77.6 μg g^?1 to 482 ± 4 μg g^?1 (Is) in NIST SRM 610. Using these revised values for external calibration, most of the determined average values of MPI‐DING, USGS and NIST SRM 612–614 reference glasses agree within 3% with the calculated means of reported reference values. Bulk analysis of NIST SRM 610 by standard additions using membrane desolvation ICP‐MS gave Nb = 479 ± 6 μg g^?1 (1 s) and Ta = 468 ± 7 μg g^?1 (1 s), which agree with the above revised values within 3%.  相似文献   

Determination of Platinum‐Group Elements in OPY‐1: Comparison of Results using Different Digestion Techniques     

Liang Qi  Mei‐Fu Zhou 《Geostandards and Geoanalytical Research》2008,32(3):377-387

A new proficiency testing sample, OPY‐1 (ultramafic rock), the basis of the twentieth international proficiency test of analytical geochemistry laboratories (GeoPT 20), was recently prepared by the International Association of Geoanalysts (IAG). This paper reports analytical data for Os, Ir, Ru, Rh, Pt and Pd with different digestion techniques, including an improved Carius tube, Carius tube combined with HF dissolution and alkaline fusion. About 4–15% of the PGEs are in the silicate phase, which cannot be leached by aqua regia even when digested at 300 °C with the Carius tube technique. Both the Carius tube technique combined with HF dissolution and alkaline fusion can obtain reliable data. The results demonstrated that OPY‐1 is sufficiently homogeneous at a 2 g test portion level to be suitable as a reference material for method validation. The procedure for sealing the Carius tube was simplified and the recommended digestion procedures are provided.  相似文献   

Trace Element Determination by ICP‐AES and ICP‐MS: Developments and Applications Reported During 2006 and 2007     

Kathryn L. Linge 《Geostandards and Geoanalytical Research》2008,32(4):453-468

This review describes developments in trace element determination using inductively coupled plasma‐atomic emission spectrometry (ICP‐AES) and inductively coupled plasma‐mass spectrometry (ICP‐MS) that were reported in 2006 and 2007. It focuses on the application of ICP techniques to geological and environmental samples; fundamental studies in ICP‐MS and ICP‐AES instrumentation have largely been ignored. New advances in ICP‐MS and ICP‐AES were incremental over this period, partly because both techniques are now well‐established. A continuing shift towards the hyphenation of low‐flow separation techniques has sparked activity in the development of appropriate low‐flow interfaces, and papers discussing interference removal also contribute significantly to the volume of research for both ICP‐AES and ICP‐MS. Whereas the majority of new ICP publications concerned advances in ICP‐MS analysis rather than ICP‐AES, development for ICP‐AES still occurs in almost all areas, particularly in sample introduction and hyphenated techniques.  相似文献   

感耦等离子体质谱法测定商代原始瓷中的稀土   总被引：7，自引：1，他引：6  

古丽冰  邵宏翔 《岩矿测试》2000,19(1):70-71

以混合酸溶样电感耦合等离子体质普法测定了商代古陶瓷中稀土元素,采用Ｉｎ内标补偿测定信号所受的影响,同时讨论了干扰因素及其校正方法。方法经国家一级标准物质分析验证,其分析结果与标准植吻合;经１０次重复测定同一样品,方法的精密度ＲＳＤ在１．６％～７．３％。该方法已用于不同地区的商瓷样品中稀土的测定,并对古瓷的地球化学特征作了探讨。  相似文献   

江西银山火山岩型铜、金多金属矿床成矿特点   总被引：4，自引：1，他引：3  

李培铮  陶红 《大地构造与成矿学》2000,24(3):244-249

江西银山铜、金多金属矿床的矿化紧紧围绕多个中心呈有规律地分布,成矿物质既由岩浆从地壳深部带来,又部分来自基底围岩;成矿作用既受燕山期火山机构控制,也受基底构造控制;矿化具有多个中心复合叠加分带的特点,是一个典型的地洼型多因复成矿床。  相似文献   

类太阳活动恒星表面黑子结构的多普勒成像(Ⅰ)：技术     

顾盛宏  谭徽松 《天文学进展》2000,18(4)

回顾了恒星表面结构多普勒成像研究工作的发展历史,重点评述了该项技术在类太阳活动恒星研究领域的应用。介绍了该项技术在国际上的发展现状,给出了恒星表面黑子结构形态的多普勒成像技术的基本原理,讨论了该项技术对观测仪器、观测过程和观测对象的要求,并对未来这一领域的研究工作进行了展望。  相似文献   

Characterisation of Apatites as Potential Uranium Reference Materials for Fission‐track Dating by LA‐ICP‐MS          下载免费PDF全文

Cleber J. Soares  Regina Mertz‐Kraus  Sandro Guedes  Daniel F. Stockli  Thomas Zack 《Geostandards and Geoanalytical Research》2015,39(3):305-313

We report homogeneity tests on large natural apatite crystals to evaluate their potential as U reference materials for apatite fission‐track (AFT) thermochronology by laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS). The homogeneity tests include the measurements of major element concentrations by electron probe microanalysis (EPMA), whereas for U concentration, isotope dilution (ID) ICP‐MS and laser ablation (LA) ICP‐MS were employed. Two apatite crystals are potential reference materials for LA‐ICP‐MS analysis: a 1 cm³ fraction of a Durango crystal (7.5 μg g^?1 U) and a 1 cm³ Mud Tank crystal (6.9 μg g^?1 U). The relative standard deviation (1 RSD) of the U concentration determined by ID‐ICP‐MS of both apatite crystals was ≤ 1.5%, whereas 1 RSD for the LA‐ICP‐MS results was better than 4%, providing sufficient homogeneity for fission‐track dating. The results on the U homogeneity for two different apatite samples are an important step towards establishing in situ dating routines for AFT analysis by LA‐ICP‐MS.  相似文献   

An Evaluation of the Effects of Primary and Cross‐Contamination during the Preparation of Rock Powders for Chemical Determinations          下载免费PDF全文

José P. Sertek  Sandra Andrade  Horstpeter H. Ulbrich 《Geostandards and Geoanalytical Research》2015,39(3):381-397

Quartz crystals from the Batatal site, Minas Gerais, southern Brazil, were used to determine quantitatively primary contamination when submitting the samples to milling processes. Crushing devices used were a primary steel jaw crusher (br1), a secondary tungsten carbide (WC) crusher (br2) and a hydraulic press with stainless steel plates (pr). Fragments with suitable sizes were then ground in different Fritsch planetary mills, equipped with agate, WC and chromium‐steel rings for 7, 4 and 3 min, respectively. Solutions of the powders were analysed initially with the TotalQuant^? method in a quadrupole ICP‐MS instrument, providing semi‐quantitative results for seventy‐five elements. Contamination from crushers and mills was visible in major and minor elements such as Fe, Mn and Ti, and noticeable in trace elements such as Cr, Co, Ni, Cu and also V, Zr, Sc; significant contamination was observed from W, Mo, Co, Ta and Nb (mainly by use of the WC devices). Little or no contamination was observed for Pb, REE, Sr and Rb, elements that are important in routine isotopic determinations. Cross‐contamination was tested by grinding either a granite or a basalt sample, followed by conventional cleaning with mica‐free quartz sand, before the working quartz powder was prepared.  相似文献