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1.
The Canadian Certified Reference Materials Project reports recommended values of lead-210 activity in four uranium reference materials previously certified for uranium and radium-226. Eleven laboratories participated in the interlaboratory program for DL-1a, BL-4a, DH-1a and BL-5; three measurement techniques were applied. Procedural and instrumental calibrations were performed with a certified lead solution from Amersham International Corp., thereby establishing traceability of the recommended values for lead-210. Activity ratios for uranium-238. radium-226 and lead-210 demonstrate these uranium reference materials to be in secular equilibrium, within experimental uncertainties.  相似文献   

2.
Lead-210, radium-226, thorium-228 and uranium-238 concentrations have been determined in five CCRMP reference samples using direct gamma-ray spectrometry. Literature data are available for only lead-210 and radium-226 levels in these samples.  相似文献   

3.
The Canadian Certified Reference Materials Project announces the availability of reference uranium tailings sample UTS-1, -2, -3 and -4. Eighteen laboratories participated in the interlaboratory program for total iron, titanium, aluminium, calcium, barium, uranium, thorium, total sulphur, sulphate and arsenic. Eight laboratories participated in the inter-laboratory program for thorium-230, radium-226, lead-210 and polonium-210 in all four samples and for thorium-232, radium-228 and thorium-228 in UTS-1 and UTS-2.  相似文献   

4.
The fifth version of natural river water certified reference material, SLRS‐5 (National Research Council – Conseil National de Recherches Canada), is commonly used to control the quality of major and trace element measurements. Concentrations of silicon and thirty‐one uncertified trace elements have been reported for the certified reference material SLRS‐4, but they are not yet available for SLRS‐5. Here, SLRS‐5/SLRS‐4 ratios were deduced from SLRS‐5 and SLRS‐4 measurements by inductively coupled plasma‐atomic emission spectrometry and high‐resolution inductively coupled plasma‐mass spectrometry for certified elements and thirty‐five uncertified elements (rare earth elements, B, Bi, Br, Cs, Ga, Ge, Hf, Li, Nb, P, Pd, Rb, Rh, S, Sc, Si, Sn, Th, Ti, Tl, Y). Both reference materials were measured directly one after the other, so that calculated elemental ratios would not be notably influenced either by calibration uncertainties or by eventual long‐term instrumental drift. The computed ratios are in good agreement with those deduced from the certified values. We also report concentrations for thirty‐three uncertified elements in SLRS‐5 by combining the measured SLRS‐5/SLRS‐4 ratios and the published SLRS‐4 values. The resulting new data set provides target SLRS‐5 values, which will be useful in quality control procedures.  相似文献   

5.
A basaltic certified reference material BEM, prepared by Chengdu University of Technology, has recently been approved as a Primary Grade Reference Material (GBW07126) by the General Administration of Quality Supervision, Inspection and Quarantine of China. BEM was sampled from the Emeishan Basalts in China, which is one of the largest basalt provinces in the world. After successfully completing homogeneity and stability tests, collaborative analyses were carried out in seventeen Chinese institutes and laboratories and two American laboratories. More than ten reliable analytical methods based on different principles of measurement were adopted, of which ICP-MS, NAA and ICP-AES contributed 60.5% of all results. Fifty-four elements and oxide components were characterised as certified values, four elements as recommended values and nine elements as information values. A minimum sampling mass of 40 mg for most elements is recommended for use.  相似文献   

6.
One or two gram aliquots of twelve reference materials with low platinum-group element (PGE) abundances (Ir concentrations ranging from 30 to 510 pg g-1) were analysed by isotope dilution ICP-MS using an on-line chromatographic matrix separation after acid digestion in a high pressure asher (HPA-S) to determine the concentrations of Ru, Pd, Re, Ir and Pt. Osmium concentrations were determined via ID-ICP-MS but as volatile OsO4, whereas Rh concentrations were calculated by comparing the peak areas of the chromatographic peak with that of a standard solution. Validation of the method was performed and the concepts of traceability and measurement uncertainty were applied to assure comparability. The reference materials BCR-2, BHVO-1, BHVO-2, BIR-1, DNC-1, EN026 10D-3, MAG-1, RGM-1, SCo-1, SDO-1, TDB-1 and W-2 were investigated to test for their usefulness for certification. The use of TDB-1 is highly recommended because it is homogeneous at the two gram level and many values based on several different analytical procedures have been published. It is recommended that our efforts should focus on the certification of this reference material to reduce the uncertainties of its currently certified values (Pd and Pt only) and to assign certified values to the other PGE and Re. It is necessary to have at least one well-characterised RM for validation of methods applied to the analysis of PGE and Re in low abundance samples, although the matrix of TDB-1 might not completely match those of many samples.  相似文献   

7.
This report describes the location, collection, preparation, homogeneity testing, analysis, data-processing and assignment of certified values of a polymetallic nodule (GSPN-1) and marine sediment (GSMS-1). Materials used in the preparation of these reference materials were collected in 1986 and 1987 from the central Pacific Ocean, by the Chinese Ministry of Geology and Mineral Resources (MGMR). A total of fifty one recommended element concentrations and five proposed concentrations are reported for GSPN-1. For GSMS-1, a total of fifty recommended and seven proposed values are presented.  相似文献   

8.
The preparation and homogeneity study of three certified reference materials, Plastic Clay GBW 03115, Potassium Feldspar GBW 03116 and Soda-Lime Silica Glass GBW 03117 are briefly presented. The recommended values with their uncertainties were assigned, after a cooperative study with 18 laboratories.  相似文献   

9.
Wavelength dispersive X-ray fluorescence spectrometry (WD-XRF) is widely used for the analysis of soils and sediments using well characterised procedures. However, difficulties can occur with samples such as unknowns containing small amounts of ore materials and samples collected from contaminated sites where trace elemental concentrations can exceed the concentration range for routine analysis. We studied the performance of a commercially available method, based on fundamental parameters (FP) to correct matrix effects. The spectrometer was originally calibrated with elemental or simple compound calibrants. Samples were analysed as pressed powder pellets. Eighteen sediment and soil reference materials, three of them with certified values for some of their constituents, were used to evaluate accuracy, by comparing results with recommended values and their standard deviations (RV ± 2s) or certified values and their confidence intervals (CV ± Cl). When results fell systematically outside these intervals, calibrations were refined with geochemical reference materials. The best agreement of results with recommended and certified values was obtained when the contents of H2O and C in each sample were included as matrix constituents during calculations. The detection limits of trace elements tended to be relatively high, because the measuring conditions employed were not maximised for sensitivity. The main advantage of the method tested was that it enabled the analysis of samples with high concentrations of trace elements and the determination of elements such as F, Bi, Sb and W, which are not commonly included in quantitative XRF analysis of geological samples.  相似文献   

10.
A large number of certified and other reference samples are available for use in analytical geochemistry. Certified materials are preferred, but of much more limited availability than other reference samples for most geochemical applications. The availability of rock, sediment, soil, water, and plant reference samples is outlined; ore and mineral separate reference samples are not included in the discussion. The preparation of these materials, including the establishment of certified or recommended concentrations, is then reviewed. It is shown that comparable quality can be achieved for both certified and recommended concentrations, though it has not always been achieved in the past. Finally, the most appropriate ways to use reference samples in quality control and instrumental calibration are discussed.  相似文献   

11.
中国的大洋多金属结核及沉积物标准物质系列   总被引：8，自引：0，他引：8  
1986～1996年间我国研制了两批共６个海洋地质标准物质：3个多金属结核标准物质GSPN-1～3和3个深海沉积物标准物质GSMS-1～3,形成了两个标准物质系列。与美国、俄罗斯、印度和日本的同类标准物质相比,这些标准物质的主要特点是：①实用性强：这些样品主要取自世界上锰结核最富集、也是各国“先驱投资者”开辟区最集中的太平洋CC区;②系列性好：这些样品还可与美、俄的标准物质构成既具有较大的元素浓度范围又具有适当浓度梯度的标准系列;③被测定组分多（达79个）,定值组分达63个。其中包括58个组分的保证值和5个组分的参考值,全组分的加和均在99.5％～100.1％之间;④参加合作的国家数和实验室多:有18个国外实验室和包括台湾大学在内的14个国内实验室参加了合作分析。这就使这些标准物质具有较大的国际影响。  相似文献   

12.
A precise, accurate and rapid method for the sequential determination of FeO and Fe2O3 in rocks, soils and some non‐refractory minerals by 1,10‐phenanthroline spectrophotometry is described. Fe(II) and Fe(III) were leached from the sample (?200 mesh) using a mixture of NH4HF2 and H2SO4 at 40–80 °C for 10 min on a hot plate. Both Fe(II) and Fe(III) could be conveniently estimated sequentially from the same reaction mixture at the μg g?1 to percentage level. The method is better than the existing wet chemical methods, including the commonly used Pratt's titrimetric redox method, for Fe(II) and Fe(III) determinations in rock and soil samples in terms of precision, accuracy and rapidity. The throughput of the method was very high; at least forty to fifty samples could be estimated easily in a day. The results obtained compare favourably with those obtained by Pratt's method, as well as for certified/recommended values of a set of eleven certified reference materials having FeO and Fe2O3 contents in the range 0.21–14.63% and 0.58–8.48%, respectively. The optimised 1,10 phenanthroline method was found to be accurate to within 0.21% m/m FeO and 0.30% m/m Fe2O3 compared with the literature values of the certified reference materials studied.  相似文献   

13.
重晶石矿石成分分析标准物质研制   总被引：3，自引：2，他引：1  
冯静  王瑞敏  张激光 《岩矿测试》2010,29(2):175-178
研制了7个重晶石矿石成分分析标准物质。其中,GSO-1为铁矿型重晶石,GSO-2、GSO-3为萤石型重晶石,GSO-4、GSO-5为石英型重晶石,GSO-6为硫化物型重晶石,GSO-7为黏土型重晶石。样品采用陶瓷衬里的球磨机加工,加工后样品粒度达到-0.074 mm。采用X射线荧光光谱法检验了钡、铜、铅、锌、锆、铝、硅、铁和钙共9种元素的均匀性,并进行振动试验。8个实验室参加定值工作,提供了硫酸钡、氧化钡、三氧化硫和锶的7个标准值,全三氧化二铁的2个标准值,氟化钙的1个标准值及铜、铅、锌和水溶盐等标准值或参考值。2009年4月,7个样品已被国家质量监督检验检疫总局批准为国家一级标准物质,编号为GBW 07811~GBW 07817。  相似文献   

14.
标准物质参考值的准确性在测试仪器校准、分析数据质量监控以及方法评价等方面具有非常重要的作用.为了检验国家地质标准物质参考值的准确性,本文应用高温高压密闭溶样-电感耦合等离子体质谱法分析了国家地质标准物质的18种岩石(GBW 07103 ～ GBW 07125)、19种沉积物(GBW 07301 ～ GBW 07318)和19种土壤(GBW 07401 ～ GBW 07430)中36种痕量与稀土元素.结果表明,除个别标准样品中的几个元素(Ni、Cr、Pb、Co、Cu、Sc、Yb、Lu)外,其余国家标准物质中36种元素测定结果的相对标准偏差均小于10％;绝大部分元素测定值的相对误差小于10％,测定值与参考值能较好地吻合.将误差较大元素的测定值与其他实验室的测定值以及文献报道值进行了比较,指出已有的参考值需要修正;针对部分沉积物和土壤中的元素未提供参考值,如GBW 07306的Ni、GBW 07313的Be、Hf、Ta,GBW 07314的Li、Be,GBW 07409、GBW 07410和GBW0741 1的Hf、Ta,GBW 07426的Gd、Ta,本文给出了相应的参考值.  相似文献   

15.
This study investigated the leaching of radium-226 from phosphogypsum (PG) waste produced from the fertilizer industry by synthetic solutions that replicate water that may contact the waste in natural conditions. The results indicated that the activity concentration of Ra-226 in the PG was 461 ± 12 Bq kg?1 and compared with other studies carried out worldwide. The leached percentage of Ra-226 represents the exchangeable fraction loosely bounded in the matrix of the PG waste. The leached fraction of Ra-226 was 6.5 ± 0.6 and 9.0 ± 0.5% when the waste was exposed to rainwater and saline solution, respectively. It is also found that the leaching fraction increased 10–12 ± 0.4% when the waste was exposed to the admixture of saline solution containing Sr2+ or Ba2+ cations, whereas it was lowered to 4–5 ± 0.5% in the presence of carbonate or sulfate anions. When the PG is used as an economic fertilizer, the irrigation water can leach 7.8 ± 0.6% of Ra-226 that could contribute to plant uptake, thereby to animal and/or human consumption. The primary tests of the drinking water (well and tap resources) consumed by the populations surround the PG facility showed that the activity concentration of Ra-226 was below the minimum detectable activity.  相似文献   

16.
The Institute of Hydrogeology and Environmental Geology, Chinese Academy of Geological Sciences recently prepared four certified reference materials for hydrogen and oxygen stable isotopes in water, which are called ‘China Standard Water' (CSW)‐HO1–HO4 (hereafter referred to as HO1–HO4). These reference materials are intended for calibration purposes and provide reference values of their relative difference in 2H/1H and 18O/16O isotope‐amount ratios expressed in delta notation, normalised to the VSMOW–SLAP scale. The certified values of the reference materials were determined by an interlaboratory comparison of results from eleven participating laboratories. This paper describes in detail the production and certification procedure of the four reference materials. The first analytical data for the reference materials are also provided using a variety of analytical techniques, namely CO2–H2O equilibration and laser spectroscopy for δ18O and Cr reduction, as well as H2–H2O equilibration, laser spectroscopy, and high‐temperature conversion for δ2H. The reference values for materials HO1–HO4 and their associated uncertainties are assigned.  相似文献   

17.
In this study, we used the modified Horwitz expression (Hc= 0.01c0.8495, which gives the precision as a function of concentration) to evaluate and control the accuracy of results of silicate rock analysis obtained by X-ray fluorescence spectrometry. This expression is currently used by the organisers of the GeoPT international proficiency tests, to assign the precision limits of each analyte and subsequently to evaluate the data provided by laboratories whose main application is geochemistry. Results for major and trace elements, determined in glass disk and pressed pellets, respectively, were evaluated. Nine international silicate rock reference materials were analysed and results were compared to the recommended values plus and minus the limits given by the above expression. Those limits are easily attained for most major elements, but not for trace elements. Sample preparation and sub-sampling contributions to precision were evaluated by analysis of an in-house reference sample. In our results, precision does not follow the Horwitz expression relationship with concentration. It is known that the final accuracy in XRF analysis depends strongly on instrumental settings and on the uncertainties associated with the certified or recommended values of the reference materials used to calibrate the spectrometer, but our results indicate that the precision expression can be useful, especially to inspect and correct calibration curves and to check routine instrumental accuracy.  相似文献   

18.
A method for the determination of total sulfur in geological materials by inductively coupled plasma‐optical emission spectrometry (ICP‐OES) is described. We show that good results were obtained using this method even for sample types with very low (< 20 μg g?1) sulfur concentration (e.g., peridotite). Sulfur was determined in fifteen geological reference materials with different sulfur contents. For reference materials with certified sulfur contents, the ICP‐OES method gave results in excellent agreement with certified values, and uncertainties better than 4% RSD. ICP‐OES results for sulfur in other reference materials yielded RSDs better than 10%, where S concentrations were > 100 μg g?1 (except for diabase W‐2a, 16% RSD). Reference materials with lower sulfur contents (< 40 μg g?1) showed much higher RSDs (17–18%). Except for RMs with certified values for sulfur, most data obtained by the combustion infrared detection method generally showed higher concentrations than those measured by ICP‐OES and a better RSD (≤ 8% for all materials except DTS‐2b).  相似文献   

19.
In 1990, the Institute of Geophysical and Geochemical Exploration prepared a series of certified reference materials of synthetic silicates and limestones. The silicate series (GSES I * ) is composed of 11 samples with 28 ingredient elements and the limestone series (GSES II*) is composed of 9 samples with 29 ingredient elements. The standard series were prepared in ascending element concentration order of 1, 2 and 5. The synthetic standards were analyzed by a large number of laboratories with various reliable methods and then certified values were derived.  相似文献   

20.
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   

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