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用百分总和检查硅酸盐岩石全分析数据的质量是分析工作者的传统做法,但对于微量元素含量较高的样品,采用X射线荧光光谱法(XRF)进行测定,如果不考虑微量元素的含量及其对主量元素基体效应的影响,往往会使主量元素含量更加偏离真实值。本文针对Sr、Ba含量较高的硅酸盐样品,通过人工配制标准样品,扩大了Sr、Ba校准曲线的定量范围,主量元素校准中加入Sr、Ba的基体校正系数,达到了主量元素定量更加准确可靠的实际效果。采用此方法分析国家标准物质,各主量元素的精密度(RSD)均小于2%;分析不参加回归的标准物质和人工配制的标准样品,主量元素的测量值与标准值(或参考值)基本一致。该方法可以满足硅酸盐的测定要求,主量元素各项结果的加和能够达到《地质矿产实验室测试质量管理规范》的一级标准(99.3%～100.7%)。 相似文献
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基于X射线荧光光谱法测定常见生物样品中常量和微量元素 总被引：1，自引：1，他引：0
基于大米、小麦、玉米等23种国家生物成分系列标准物质,探讨了X射线荧光光谱法在常见生物样品中常量和微量元素测定中的应用。在对各待测元素的激发电流电压、分析线、背景位置、干扰谱线、分析晶体、准直器、探测器和脉冲高度分布等条件进行分析的基础上,采用粉末压片法制样,基于回归曲线法和康普顿散射线内标法求取各待测元素的标准曲线常数、元素间吸收效应的影响系数和谱重叠系数。结果表明:国家生物成分系列标准物质具有足够宽的含量范围和适当的含量梯度,基本能覆盖常见生物样品中各元素的含量范围。方法检出限能够保证测定结果的有效性,测量精密度为2.62%～14.79%,且标准物质各元素的测定值与标准值基本相符。方法具有简便、灵敏和准确的特点,能够满足分析的需求。 相似文献
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磷矿石化学成分分析标准物质研制 总被引：5，自引：4，他引：1
磷矿的开发与综合利用不仅需要分析磷等主要元素,也需要准确地测定稀土元素和微量元素。分析测试过程需要含量适中、定值组分全的磷矿石标准物质进行质量监控,国内外现有的磷矿石标准物质无论是从定值指标还是含量梯度范围等方面均无法满足此需求。本文研制了4个不同类型磷矿石成分分析标准物质。样品采集自河北张家口钒山磷矿、贵州织金新华磷矿、云南昆阳磷矿、湖北神农架火炼坡磷矿4个典型矿区,其中张家口钒山磷矿和织金新华磷矿为含稀土的磷矿。检验结果表明样品的均匀性、稳定性良好;通过11家实验室协作定值,定值元素包括造岩主量元素、稀土元素和痕量元素共37项,其中3个组分为参考值,其余均给出标准值和不确定度。4个磷矿石标准物质形成了一个从边界品位、工业品位到磷精矿较为完整的含量系列,P_2O_5的含量分别为10.57%、18.91%、27.78%、39.40%,稀土元素总量分别为0.16%、0.11%、0.032%、0.0083%,可满足磷矿勘查、评价和综合利用开发中对标准物质的需求。 相似文献
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中国与世界铂族元素地球化学标准物质评介 总被引：4，自引：0，他引：4
铂族元素分析一直是地质材料分析中最棘手的任务之一,是铂族金属矿产资源勘查、评价和相关研究工作的瓶颈。铂族元素标准物质作为铂族元素分析的计量标准,在分析质量监控、分析仪器校准、分析方法评价和仲裁分析中发挥着重要作用。笔者等评介了我国研制的超基性岩和铬铁矿铂族元素标准物质、铂族元素地球化学标准物质、铂族元素矿石标准物质和海山富钴结壳铂族元素标准物质共4个系列21个标准物质,也给出了其他地球化学标准物质中铂族元素的定值数据;并与南非、加拿大、俄罗斯和岩石矿物分析标准国际工作组(GIT-IWG)研制的13个铂族元素标准物质及其他国际地球化学标准物质中铂族元素的数据进行了对比。这些标准物质的研制与应用将大大提高铂族元素分析数据的可靠性,为我国和世界铂族金属矿产资源勘查、评价及研究提供了有力的技术支撑。 相似文献
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长江三角洲沉积物标准物质研制 总被引：3，自引：3，他引：0
美国、加拿大等国家先后研制了10余个海湾和河口沉积物标准物质,但定值成分较少,大多侧重于有机污染物和放射性核素值。我国于2007年研制了3个黄河三角洲沉积物标准物质,为进一步满足近海地球化学调查及资源勘探的需要,本文按照ISO导则35和国家一级标准物质技术规范,研制了2个长江三角洲沉积物标准物质。按照不同粒径采集两个候选物样品,样品经干燥、球磨至200目,采用电感耦合等离子体质谱和发射光谱法进行均匀性检验,结果表明F实测值小于列表临界值F0.05(24,25)=1.96,样品均匀性良好。在两年时间内采用X射线荧光光谱法进行了4次稳定性检验,未发现统计学意义上的明显变化,样品稳定性良好。由12家有技术权威的实验室共采用13种准确、可靠的分析方法进行协作定值,最终定值元素53项,涵盖了主量、微量及全部稀土元素,其中主量成分含量呈梯度分布,如Al2O3的含量分别为16.42%、11.48%。该系列标准物质定值元素种类多,定值方法准确,能够为河口三角洲地区地质及环境调查的分析测试工作提供可靠的质量保证。 相似文献
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铂族元素地球化学标准物质的研制 总被引：12，自引：3，他引：9
ＧＰｔ＿１～７系列标准物质由土壤、水系沉积物、富镁超基性岩、富铁超基性岩、含铜镍贫铂矿石及铬铁矿等不同类型７个样品组成。铂族元素的含量范围从土壤和岩石的背景含量到矿石达４～５个数量级。经方差检验样品均匀度良好。标准物质的定值分析采用了不同类型的试金和湿化学法分离富集,以原子吸收、催化比色、催化极谱、等离子体质谱、发射光谱和中子活化等方法进行测定。定值的元素为Ｐｔ、Ｐｄ、Ｏｓ、Ｒｕ、Ｉｒ、Ｒｈ６个铂族元素及Ａｕ。该系列标准物质主要适于作铂族元素地球化学勘查和铂矿勘查中铂族元素分析的量值标准与测试的质量监控。 相似文献
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用中子活化分析方法,定值测试了湖北岩矿测试中心研制中的GSS31~GSS35土壤底泥标准物质,测定了28个元素;定值测试捷克生物标准物质TY1~4,测定了12个元素,对谱干扰和U裂变干扰作了修正。这里列出了由国际地质分析协会(IAG)组织,有全球71个地球化学分析实验室参与测试的玄武岩BNV-1的平均值及本实验室的测试结果。 相似文献
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我国海洋沉积物的研究近几年发展较快,但是缺少有定值的氮、有机碳标准物质。本文针对及其匮乏的氮、有机碳国家二级标准物质进行了我国近海沉积物总氮(TN)、总碳(TC)、总有机碳(TOC)含量的分析标准参考物质的研制。研究样品采自"我国近海海洋综合调查与评价"专项提供的表层沉积物,经过冷冻干燥、研磨至74μm,使用元素分析仪和氧化热解-气相色谱法分析总氮和总碳的含量;使用元素分析仪和氧化热解-电位法分析总有机碳的含量,制备了一系列16个有定值的总氮、总碳、总有机碳含量的近海沉积物标准物质。样品在均匀性检验中,F的实测值小于临界值,相对偏差较小,样品的均匀性较好。在稳定性检验方面,两年内多次测定的分析结果无方向性变化,统计计算结果显示稳定性良好。本文研制的这16个近海沉积物标准物质在3家实验室进行了联合定值,按照ISO导则35和国家一级标准物质研制规范,给出了该系列标准物质总氮、总碳、总有机碳含量的标准值和不确定度。这批标准物质分为不同海区,不同海区的标准物质又分为不同的沉积物类型,研制的不同海区不同沉积物类型的标准物质对现有的海洋沉积物标准物质进行了有效的补充。 相似文献
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This review gives an overview of the use and development of reference materials of geochemical and environmental interest in the literature of the years 2004 and 2005. In these years the performance of existing methods has been improved and new geochemical applications using new techniques have been developed. Accordingly, there was an increasing need for new reference materials, especially for in situ microanalysis and for precise stable isotope measurements. In addition, there was a notable trend for further characterisation of existing reference materials, mainly for the platinum-group elements. This review focuses on five topics: reference materials for platinum-group elements, reference glasses for in situ microanalysis, zircon reference materials, isotopic reference materials, and the development and certification of reference materials. 相似文献
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Reference Materials for Geochemical Studies: New Analytical Data by ICP-MS and Critical Discussion of Reference Values 总被引：13，自引：0，他引：13
Peter Dulski 《Geostandards and Geoanalytical Research》2001,25(1):87-125
Abundances of twenty four trace elements, including Y and fourteen rare earth elements (REE), are reported for eighty six geological reference materials and four proficiency testing samples. Analytical data were obtained by ICP-MS using solution nebulisation after mixed acid digestion (HF-HClO4 ) under pressure. Analysed samples cover a wide range of element concentrations and mineralogical compositions, including samples for which there are few previously published data. Precision for elemental determinations in nearly 90% of the samples analysed is better than 5%. Accuracy, estimated by comparison with data from compilations is better than 6% for well characterized reference materials. Results obtained for samples that are low in trace elements are often significantly lower than compiled reference values. A critical discussion of the compiled data sets, especially for Y and the REEs, indicates that some reference values seem to be erroneous. 相似文献
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Determination of Ga,Ge, Mo,Ag, Cd,In, Sn,Sb, W,Tl and Bi in USGS Whole‐Rock Reference Materials by Standard Addition ICP‐MS 
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下载免费PDF全文 Richard M. Gaschnig Roberta L. Rudnick William F. McDonough 《Geostandards and Geoanalytical Research》2015,39(3):371-379
A procedure for determining a wide range of chalcophile and siderophile elements in typical crustal rocks using standard addition and ICP‐SFMS (inductively coupled plasma sector field mass spectrometry) is presented. New results for Ga, Ge, Mo, Ag, Cd, In, Sn, Sb, W, Tl and Bi abundances in USGS whole‐rock reference materials AGV‐2, BHVO‐1, BIR‐1, G‐2, GSP‐1 and W‐2 are reported using this analytical procedure. Intermediate precision of means based on multiple dissolved aliquots of each USGS reference material was 10% RSD or better for Ga, Ge, In and Sn in all, and similarly good for Ag, Cd, Sb, Tl and Bi in most reference materials. Poorer intermediate precision of Mo and W measurements in several reference materials is probably due to higher analytical blanks on these elements and powder heterogeneity due to a sulfide‐related nugget effect in the specific case of Mo in GSP‐1. Results for all elements fell within the range of available published data with the exception of Ag, which yielded systematically higher concentrations than found in the literature for five of the six reference materials, likely reflecting interference from unresolved polyatomic species. 相似文献
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Qi‐Chao Yang Klaus Peter Jochum Brigitte Stoll Ulrike Weis Dmitry Kuzmin Michael Wiedenbeck Heike Traub Meinrat O. Andreae 《Geostandards and Geoanalytical Research》2012,36(3):301-313
To test whether the silicate reference glasses BAM‐S005‐A and BAM‐S005‐B from BAM (The Federal Institute for Materials Research and Testing, Germany) are suitable materials for microanalysis, we investigated the homogeneity of these reference glasses using the microanalytical techniques EPMA, LA‐ICP‐MS and SIMS. Our study indicated that all major and most trace elements are homogeneously distributed at micrometre sampling scale in both types of glass. However, some trace elements (e.g., Cs, Cl, Cr, Mo and Ni) seem to be inhomogeneously distributed. We also determined the composition of BAM‐S005‐A and BAM‐S005‐B. The EPMA data of major elements confirmed the information values specified by the certificate. With the exception of Sr, Ba, Ce and Pb, our trace element data by LA‐ICP‐MS were also in agreement with the certified values within the stated uncertainty limits. The reasons for the discrepancy in these four elements are still unclear. In addition, we report new data for twenty‐two further trace elements, for which the concentrations were not certified. Based on our investigation, we suggest that both of these materials are suitable for many microanalytical applications. 相似文献
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用于铂族元素分析的中外地质标准物质 总被引：2，自引：2，他引：0
标准物质作为地质分析的计量标准,在分析质量监控、仪器校准、方法评价和仲裁分析中发挥着重要作用。铂族元素分析一直是地质材料分析中最棘手的任务之一,铂族元素标准物质研制困难,数量少,严重影响了对铂族元素分析方法的评价和分析数据的质量监控,成为铂族金属矿产资源勘查、评价和相关研究工作的瓶颈。收集了中国及国际上现有的34个铂族元素标准物质和52个其他地球化学标准物质中的101个铂族元素定值数据。为便于使用也收集了这些标准物质中其他元素的含量信息,给出了铂族各元素按含量大小排列的信息简表以方便选择。充分利用这些标准物质对促进铂族元素分析方法研究,保证铂族元素分析数据质量,提高中国和世界铂族金属矿产资源勘查、评价及研究水平具有重要意义。 相似文献
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Shigeru Terashima 《Geostandards and Geoanalytical Research》2001,25(1):127-132
The indium (In) and tellurium (Te) contents of fifty nine geological reference materials, issued by several reference material producers (USGS, CRPG, ANRT, GIT-IWG and GSJ) have been determined by graphite furnace atomic absorption spectrometry, after aqua regia and HF digestion, and extraction of iodide complexes with trioctylmethylammonium (TOMA) - metyl isobutyl ketone (MIBK). Although the interferences from most elements can be minimised by the addition of palladium solution as the matrix modifier, large concentrations of Bi, Cu, Pb or Sn suppress the absorbance of In and/or Te. Samples for analysis were therefore restricted to those in which the concentrations of these interfering elements did not cause a significant interference. The limit of detection was 0.2 ng g−1 In and Te for 1 g test portions. The agreement between the reported results and published data is satisfactory. 相似文献
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Compared with solution ICP‐MS, LA‐ICP‐MS studies have thus far reported comparatively few external reference data for accuracy estimates of experiments. This is largely the result of a paucity of available reference materials of natural composition. Here, we report an evaluation of natural glass (obsidian) as an inexpensive and widely available external reference material. The homogeneity of over forty elements in six different obsidian samples was assessed by LA‐ICP‐MS. Accuracy was tested with two obsidian samples that were fully characterised by electron probe microanalysis and solution ICP‐MS. Laser ablation experiments were performed with a variety of ablation parameters (fluence, spot sizes, ablation repetition rates) and calibration approaches (natural vs. synthetic reference materials, and different internal standard elements) to determine the best practice for obsidian analysis. Furthermore, the samples were analysed using two different laser wavelengths (193 nm and 213 nm) to compare the effect of potential ablation‐related phenomena (e.g., fractionation). Our data indicate that ablation with fluences larger than 6 J cm?2 and repetition rates of 5 or 10 Hz resulted in the most accurate results. Furthermore, synthetic NIST SRM 611 and 612 glasses worked better as reference materials compared with lower SiO2 content reference materials (e.g., BHVO‐2G or GOR128‐G). The very similar SiO2 content of the NIST SRM glasses and obsidian (i.e., matrix and compositional match) seems to be the first‐order control on the ablation behaviour and, hence, the accuracy of the data. The use of different internal standard elements for the quantification of the obsidian data showed that Si and Na yielded accurate results for most elements. Nevertheless, for the analysis of samples with high SiO2 concentrations, it is recommended to use Si as the internal standard because it can be more precisely determined by electron probe microanalysis. At the scale of typical LA analyses, the six obsidian samples proved to be surprisingly homogenous. Analyses with a spot size of 80 μm resulted in relative standard deviations (% RSD) better than 8% for all but the most depleted elements (e.g., Sc, V, Ni, Cr, Cu, Cd) in these evolved glasses. The combined characteristics render obsidian a suitable, inexpensive and widely available, external quality‐control material in LA‐ICP‐MS analysis for many applications. Moreover, obsidian glass is suited for tuning purposes, and well‐characterised obsidian could even be used as a matrix‐matched reference material for a considerable number of elements in studies of samples with high SiO2 contents. 相似文献