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1.
A procedure for the analysis of geochemical samples has been developed based on direct atomic-emission spectrometry for the determination of silver, gold and the platinum-group elements. Instrumentation comprised a DC arc emission two-jet plasmatron coupled to a diffraction spectrograph and multichannel analyser for recording emission spectra. Spectrum analysis used a comprehensive library of spectral lines for practically all elements excited using this emission source. The software programme for the automatic registration of spectra and subsequent data processing are described and results presented for a number of geochemical reference materials.  相似文献   

2.
In order to meet the needs of geochemical mapping and geochemical exploration, 125 geochemical reference materials have been successively prepared by the Institute of Geophysical and Geochemical Exploration (IGGE) since 1978. They include certified reference materials of stream sediments (GSD1-14), soils (GSS1-16; ASA 1–6, for analysis of available elements), various rocks (GSR1-6, GSR13-15), biological material (GSV1-4 and GSB 1–10), synthetic silicates (GSES I 1–11) and limestones (GSES II 1–9 for spectral analysis). They also include geochemical reference materials for ore analysis: Cu-Pb-Zn ores (GSO1-4), Cu-Pb-Zn concentrates (GSO5-7), platinum-group element (PGE) ores (GPt5-6 and GPt9-10), silver ores (GAg1-6) and geochemical reference materials for Au (GAu8-14) and PGE determination (GPt1-4, and GPt7-8). A multi-laboratory collaborative analysis scheme was adopted in the certification procedure of the IGGE. Dozens of competent laboratories with hundreds of senior analysts in China participated in the certification analysis. These samples have been supplied to more than thirty countries and more than 4000 customers from national industrial, agricultural, environmental, scientific and educational fields. Most of the geochemical reference materials are used for the calibration of measuring apparatus, evaluation of analytical methods, certification studies, quality control and laboratory accreditation programmes.  相似文献   

3.
This review gives an overview of the literature on reference materials of geochemical and environmental interest for the two-year period 2008–2009. Reference materials play an increasingly important role in all fields of geoanalytical research. This is demonstrated by the large number of publications containing data on reference materials. Although many reference materials exist, there is still a great need for certified samples, so-called delta zero materials for stable isotopic work and homogeneous microanalytical reference materials. This review focuses on six topics: developments of certification processes of reference materials mainly postulated in ISO guidelines and the IAG protocol, new developments of the GeoReM database, investigations of powdered rock reference materials, Chinese reference materials published in Chinese journals, microanalytical reference materials and isotopic reference materials.  相似文献   

4.
We present high precision Ir, Ru, Pt, Pd, Re and rare earth element (REE) determinations by isotope dilution multiple collector-ICP-MS on the Cretaceous-Tertiary boundary sedimentary reference material FC-1. Samples for platinum-group element measurements were digested in Carius tubes followed by acid digestion. The platinum-group elements were subsequently separated by anion exchange chemistry and determined by multiple collector-ICP-MS. The accuracy of the platinum-group element analyses have been verified by comparative analyses of the reference materials WITS-1 and GP13 (sample size 0.5-1 g). Replicate analyses of FC-1 (sample size 0.2 g) exhibit good reproducibility (RSD < 5%) for all the analysed platinum-group elements. REE data also exhibit excellent reproducibility (RSD < 0.5%), which indicates that this sample is homogeneous for the determination of the platinum-group elements and REE at the 0.2 g level.  相似文献   

5.
6.
This review for the year 2003 deals with three relatively well-established, mature, analytical techniques (neutron activation analysis, atomic absorption spectrometry and X-ray fluorescence spectrometry) that nevertheless remain very important for the characterisation of geological and environmental samples. Developments in neutron activation analysis included modification to the technique in relation to the determination of platinum-group elements, as well as consideration of sample size in ore grade estimation. A considerable body of literature was published on the application of atomic absorption spectrometry in the analysis of environmental samples. Many of these proposed technical and methodological improvements, notably in extraction procedures. X-ray fluorescence spectrometry saw developments in in situ analysis, synchrotron micro-XRF (μ-SRXRF) and a confocal X-ray set-up for 3D elemental imaging. XRF technologies were used in the analysis of geological samples, reference materials, glasses, solutes and environmental materials.  相似文献   

7.
Three new certified reference materials (CRM), certified for the platinum-group elements (PGE), GPt-8, GPt-9 and GPt-10 were developed based on the previous CRMs IGGE GPt-1 to GPt-7. The PGE concentration of GPt-8 is about 1 ng g-1. GPt-9 and GPt-10 are ore samples with PGE concentrations of more than 1 μg g-1. A multi-laboratory collaborative analysis scheme was adopted in the certification procedure, in which nine highly-experienced institutes and laboratories participated. The samples were analysed for the six platinum-group elements by nickel sulfide mini fire assay, with Te coprecipitation, and were determined by ICP-MS. Osmium was determined by isotope dilution.  相似文献   

8.
地质标准物质均匀性检验方法评介与探讨   总被引:6,自引:6,他引:0  
评介了目前中国地质标准物质研制中样品均匀性检验与评价所用方法,包括:检测方法,统计判别模式,结果的定性、定量表达和最小取样量确定等。对照国家相关技术规范、国际标准化组织导则和国际地质分析者协会的地质标准物质定值协议,探讨了我国地质标准物质均匀性检验与评价中的难点及现存问题。  相似文献   

9.
The platinum-group elements (PGE) and gold have been determined in twenty international rock reference materials by inductively coupled plasma-mass spectrometry (ICP-MS) after pre-concentration by a nickel sulfide fire assay. It was possible to achieve determination limits for a 50 g sample that ranged from 1 pg g-1 (Rh) to 23 pg g-1 (Au). Compared to published certified and recommended values for rock reference materials, the trueness of the method was found to be good. However, in some cases we observed large deviations for all elements in the sub 10 ng g-1 range within individual reference sample splits. Our results show that the PGE and Au are inhomogeneously distributed in the reference materials analysed here, where they are present in low concentrations, using 50 g test portions.  相似文献   

10.
New concentrations for Au, Ir and Ag obtained by instrumental neutron activation analysis are presented for seventy geochemical reference materials. Results in agreement with literature values for Au and Ir down to concentrations of a few ng g−1 were obtained. For Au and Ir concentrations above 10 ng g−1, the repeatability of replicate analyses of reference materials was mostly better than 10%. For concentrations between 1 and 10 ng g−1 the RSD for Ir was 10–30%, whereas for Au it was higher and more variable (20–50%). In addition, concentrations for Cd and Hg are presented for some of the same reference materials. The high RSD at relatively high concentrations seen in gold for some RMs (e.g., WMG-1, WMS-1) did not exist for Ir and suggests homogeneity for this platinum-group element at the sub-sample size used in this study. For the following eight RMs, mostly ultramafic rocks (CHR-Pt+, OREAS-13P, OREAS-14P, PCC-1, UMT-1, WMG-1, WMS-1, WPR-1), Ir measurements agreed within ± 10% of mostly certified or recommended concentrations, which ranged from 2 ng g−1 to 6 μg g−1. For the reference material UB-N, iridium concentration compared favourably to published results obtained by isotope dilution ICP-MS methods and a previously unrecognised heterogeneity is inferred for Au, Hg and Sb, but not for the other measured elements.  相似文献   

11.
A novel method is described for the rapid dissolution of various geological, geochemical and related reference samples for the determination of Au and the platinum-group elements. The decomposition procedure is based on reaction with the fluoroxidants, liquid bromine trifluoride or molten potassium tetrafluorobromate. Results by this novel procedure are compared with data obtained by traditional methods of sample decomposition, including fire assay, autoclave techniques and an aqua regia leach. The oxidative fluorination procedure with the subsequent conversion of fluorocomplexes into the chloride form was found to be an effective and rapid method for the quantification of all the precious metals in a range of sample types.  相似文献   

12.
主编絮语     
罗立强 《岩矿测试》2011,30(2):I-II
自2011年第2期起,我刊推出"主编絮语"这个栏目,目的在于及时表达我刊的办刊思想和办刊动态,推介重点文章,加强与读者、作者和各位编委的信息沟通和交流。正如在本卷卷首语中指出的,文章质量是刊物的生命线。因此,如何提高发表在我刊文章的质量,是本届编委会的第一要务和工作重点。编委会将通过多种途径,从  相似文献   

13.
中国地质标准物质研制和标准方法制定的成果与思考   总被引:10,自引:2,他引:10  
简介了我国地质标准物质研制与标准方法制定的主要成果,重点讨论了其中在管理和技术方面值得思考的问题,并就提高我国地质标准物质水平,加速走向国际,提高国际影响力提出建议。  相似文献   

14.
A total of twenty-five bibliographic reviews were published between 1979 and 2004 in Geostandards Newsletter, subsequently renamed Geostandards and Geoanalytical Research, which list more than 5500 papers. These cited references contain information about geochemical reference materials, analytical methods or address general issues concerning the use of reference materials (protocols for sampling, certification, or new analytical techniques). In support of emerging fields of interest in geoanalysis, frequently associated with environmental research, and reflecting the increased breadth in the topics addressed by the Journal, new reference headings were added over time, while retaining the original style and format of the review. Reference management software was used to extract information from these publications related to methods, reference materials and analytes. Major developments during these 25 years, reflecting both advances in laboratory hardware as well as shifts in research interests, can readily be seen in both the types of reference materials being studied and in nature of the new analytical protocols that were developed. These two topics were the core foci of the twenty-five reviews, though much more information might also be extracted from this extensive resource.  相似文献   

15.
Trace amounts (from nanogram to microgram levels) of bromine and iodine were determined by inductively coupled plasma-mass spectrometry (ICP-MS) in twenty-three geochemical reference materials issued by the GSJ, USGS, IAEA etc. The pyrohydrolysis technique was used to separate bromine and iodine from samples analysed in the form of powder. The accuracy and precision of the experimental values were assessed by the comparative analysis of well established reference materials such as USGS AGV-1, BCR-1 and IGGE GBW07312. The measured values agreed well with reported values within a 10% error range. We also report reliable new data for these elements in these geochemical reference materials.  相似文献   

16.
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  
王毅民  王晓红  高玉淑  樊兴涛 《地质通报》2009,28(10):1486-1498
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   

17.
Four CGSP (Chinese Geological Standard Powders) carbonate matrix element reference materials were prepared by a coprecipitation method. The major and trace elements were dissolved from natural rare earth carbonate raw materials in strong acid and precipitated with ammonium bicarbonate or ammonia to form carbonate matrix phases. The carbonate reference materials were ground and pressed into tablets for microanalysis. The element homogeneity and stability in CGSP reference materials were tested by LA-ICP-MS using a calibration strategy without an internal standard element and evaluated mainly following ISO Guide 35: 2017 and JJF 1343-2012. Although the homogeneity of most of elements in the CGSP series were comparable to the repeatability obtained from homogeneous glasses, some elements (e.g., Mo, Se, Ga, Ge, Cd, Ni, Co, U) were found to have some degree of heterogeneity. All of elements passed the t-test evaluation in a 32-month stability examination except for Mo in CGSP-A, Na, Ge, Mo in CGSP-B, Ni, Cd, Sn in CGSP-C, and Al, P, Tb, Ho in CGSP-D. The certified element mass fraction values and uncertainties were determined with the characterisation of a non-operationally defined measurand using various bulk analysis methods in eight laboratories. GGSPs will provide a new carbonate calibration reference option for microanalysis.  相似文献   

18.
Platinum-Group Element Geochemical Certified Reference Materials (GPt1-7)   总被引:2,自引:0,他引:2  
Unlike the situation for other elements, few reference materials certified for the platinum-group elements are currently available. Therefore, the GPt1-7 series of PGE geochemical CRMs, prepared by the IGGE, represent an important addition and comprise a range of matrix types, including a soil, stream sediment, Mg-rich ultramafic rock, Fe-rich ultramafic rock, platinoid ore depleted in Cu, Ni and Fe, and a chromitite. The concentration of PGE in these samples ranges over 4-5 orders of magnitude and the samples were shown to have good homogeneity as assessed by a variance test. Analytical methods based on different principles were used in sample certification, including several fire assay and wet chemical procedures used for decomposition and preconcentration. Certified values for the elements Pt, Pd, Os, Ru, Ir, Rh and Au were determined by AAS, catalytic colourimetry (COL), catalytic polarography (POL), atomic emission spectrometry (AES), ICP-MS and NAA. Recently, the GPt1-7 samples were approved as national primary CRMs by the State Bureau of Technical Supervision of China.  相似文献   

19.
20.
We report new data on the trace element concentrations of Mg, Cr, Mn, Co, Ni, Cu, Zn, Sr, Cd, Ba, La, Ce, Nd, Pb and U in USGS carbonate reference materials (MACS-1 and MACS-2) and compare solution ICP-MS and LA-ICP-MS trace element determinations on landfill calcites using calibration to different reference materials (MACS-1 and MACS-2 carbonate and NIST SRM 612 glass). Very good agreement (differences below 10% relative) was found between laser ablation and solution ICP-MS data for MACS-1 with higher concentrations of trace elements (values between 100 and 150 μg g−1), with the exception of Cu and Zn. Similarly good agreement was found for MACS-2 with lower trace element concentrations (units to tens of μg g−1), with the exception of Cr, Co and Zn. The MACS-1 reference material for calibration of LA-ICP-MS was found to be extremely useful for in situ determination of trace elements in real-world carbonate samples (landfill calcites), especially those present in calcite in higher concentrations (Mn, Sr, Ba; < 5% RSD). Less accurate determinations were generally obtained for trace elements present at low concentrations (∼ units of μg g−1). In addition, good agreement was observed between the instrument calibration to MACS and NIST SRM 612 glass for in situ measurements of trace elements in landfill calcites K-2, K-3 and K-4 (differences below 15% relative for most elements). Thus, the application of MACS carbonate reference materials is promising and points to the need for the development of new carbonate reference materials for laser ablation ICP-MS.  相似文献   

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