共查询到18条相似文献,搜索用时 140 毫秒
1.
锍镍试金-等离子体质谱法测定地球化学勘探样品中的铂族元素和金Ⅰ.分析流程的简化 总被引:22,自引:8,他引:22
报道了一个改进的锍镍试金一等离子体质谱测定铂族元素和金的分析流程,用封闭溶解贵金属硫化物滤渣与同位素稀释法测锇相结合,解决了包括锇在内的全部铂族元素和金的测定,避免了锇的蒸馏分离和(或)单独测定,简化了分析流程,以适应大批量化探样品的要求,用所拟方法分析了标准物质中铂族元素和金,其结果与参考值相符。 相似文献
2.
大洋多金属结核和深海沉积物标准物质中铂族元素的中子活化分析 总被引:7,自引:2,他引:5
采用镍锍试金预富集 中子活化分析方法,测定了大洋多金属结核标准物质GSPN 2、GSPN 3和深海沉积物标准物质GSMS 2、GSMS 3中的铂族元素;根据大洋样品成分特征,对常规的镍锍试金配方和熔炼条件作了改善;计算了活化分析中的铂族元素干扰核反应,校正了Au对Pt的二级干扰;选用羰基化镍粉配料,降低了铂族元素空白值。用国家一级标准物质GBW07102作了对照分析,结果与标准值相符。 相似文献
3.
激光剥蚀电感耦合等离子体质谱元素微区分析标准物质研究进展 总被引:9,自引:5,他引:4
激光剥蚀电感耦合等离子体质谱(LA-ICP-MS)是目前地球科学分析领域的重要技术手段,元素微区分析标准物质研制是该分析技术发展的重要方向。本文对当前LA-ICP-MS元素微区分析标准物质的种类、元素分布以及应用上的优缺点和标准物质的制备方法进行了评述。现有的有证标准物质数量不多、种类不齐全,部分元素浓度较低,定值不确定度较大,应用上受到较大的局限性;研制标准也不成熟,均匀性检验方面尚未有统一的方法。本文参照岩石粉末标准物质均匀性检验方法提出了两步均匀性检验法,同时指出在标准物质种类方面,铂族元素及Au元素浓度适当、Pb-S等不同硫化物基体标准物质,以及化学成分不同的碳酸岩和磷酸岩基体标准物质是当前的迫切需求;在标准物质研制技术方面,纳米岩石粉末压片技术的研发、原位微区分析标准物质(固体)均匀性检验判别标准研究是亟待解决的问题。 相似文献
4.
5.
6.
第一行过渡金属元素及痕量贵金属元素高度富集在硫化物矿物中,常形成具有工业意义的矿床,使得硫化物具有重大的经济价值。对天然硫化物矿物中的这些痕量金属元素丰度及其分布的研究,在矿石成因学、经济地质学、环境地球化学等领域具有重要的应用价值。激光剥蚀-电感耦合等离子体质谱(LA-ICP-MS)微区分析技术是一种强大的痕量元素分析工具,非常适合直接分析硫化物矿物中痕量元素的浓度及其空间分布。由于硫化物的激光剥蚀特性与硅酸盐及氧化物不同,分析校准用的标准物质又极度缺乏,严重阻碍了这一技术在硫化物矿物微区分析中的应用。本文评述了硫化物简介、硫化物中痕量金属元素分析的意义、LA-ICP-MS微区分析技术在硫化物矿物痕量元素分析中的优势及近年来的应用进展、硫化物分析中的干扰与校准、包含铂族元素及金的硫化物标准物质的研制进展及合成硫化物标准物质最有应用前景的方法。 相似文献
7.
硫化物矿物中痕量元素的激光剥蚀-电感耦合等离子体质谱微区分析进展 总被引:10,自引:3,他引:7
第一行过渡金属元素及痕量贵金属元素高度富集在硫化物矿物中,常形成具有工业意义的矿床,使得硫化物具有重大的经济价值。对天然硫化物矿物中的这些痕量金属元素丰度及其分布的研究,在矿石成因学、经济地质学、环境地球化学等领域具有重要的应用价值。激光剥蚀-电感耦合等离子体质谱(LA-ICP-MS)微区分析技术是一种强大的痕量元素分析工具,非常适合直接分析硫化物矿物中痕量元素的浓度及其空间分布。由于硫化物的激光剥蚀特性与硅酸盐及氧化物不同,分析校准用的标准物质又极度缺乏,严重阻碍了这一技术在硫化物矿物微区分析中的应用。本文评述了硫化物简介、硫化物中痕量金属元素分析的意义、LA-ICP-MS微区分析技术在硫化物矿物痕量元素分析中的优势及近年来的应用进展、硫化物分析中的干扰与校准、包含铂族元素及金的硫化物标准物质的研制进展及合成硫化物标准物质最有应用前景的方法。 相似文献
8.
大别造山带祝家铺辉长岩的铂族元素特征 总被引:10,自引:2,他引:8
采用镍锍火试金法结合ICP-MS分析了祝家铺14个辉长岩样品中的Ir,Ru,Rh,Pt和Pd的含量。结果显示其PGE的含量较低,原始地幔标准化后的PGE分布模式呈正斜率型,PPGE相对原始地幔略微亏损,而IPGE强烈亏损,Pd/Ir值(22—138)远高于相应的地幔比值,表明铂族元素发生了分异。对祝家铺辉长岩的铂族元素研究表明,在其源区发生过硫化物的分异作用,地壳的混入可能促进了硫化物的饱和。祝家铺辉长岩中铂族元素的分异是因为在地幔部分熔融和岩浆演化过程中,PPGE主要受硫化物控制,而Ir则存在于非硫化物相如尖晶石、可能还有合金之中。 相似文献
9.
采用镍锍火试金法结合ICP-MS分析了毛屋斜方辉石岩和石榴二辉岩样品中的Ir、Ru、Rh、Pt和Pd的含量,结果显示其铂族元素(PGE)的含量随岩石类型无规律性的变化,原始地幔标准化后的铂族元素分布模式呈负斜率,Pd、Ir发生了分异。毛屋超镁铁岩铂族元素特征的形成受岩石中铂族元素的存在相制约,PPGE富集在富Cu硫化物,而IPGE以类似残留相、不熔的单硫化物固熔体形式存在,其中地壳混染也起了一定的作用;同时,成岩过程中流体的存在造成了Pt和Pd的活化。因此,单硫化物固熔体和流体的共同作用形成了毛屋超镁铁岩类似残留地幔岩的铂族元素分布特征。 相似文献
10.
11.
Ivan Belousov Leonid Danyushevsky Karsten Goemann Sarah Gilbert Paul Olin Jay Thompson Elena Lounejeva Dieter Garbe-Schönberg 《Geostandards and Geoanalytical Research》2023,47(3):493-508
A new reference material, STDGL3, for the calibration of in situ analyses of sulfide minerals by LA-ICP-MS has been developed and characterised. It represents a lithium-borate-based glass containing a mixture of Zn- and Fe-sulfide concentrates doped with several chalcophile elements as well as Zr, Gd, Hf and Ta required for assessing common interferences on Ag, Au and Pt. STDGL3 has a wider range of elements and a better homogeneity compared with existing reference materials for LA-ICP-MS analysis of sulfides. Compositional variations for most elements are below 3% RSD, below 5% RSD for Ag, Au and Pt, and below 7% RSD for Se, when performing spot analyses with a 50 μm beam size. Its preparation recipe is reproducible allowing for multiple batches to be made. Use of STDGL3 significantly improves accuracy of sulfide mineral analysis by LA-ICP-MS when compared with use of other available reference materials. Performance of STDGL3 was evaluated using several different laser systems. No significant change was observed between 193 nm ArF excimer lasers with 5 and 20 ns pulse widths, but use of 213 and 248 nm lasers displays more systematic differences, especially when analysing galena. Correction coefficients are needed for some elements (Zn and Cd in particular) when analysing sulfide minerals using STDGL3 as a calibration reference material. 相似文献
12.
M.-Riitta Juvonen ras Bartha Tuula M. Lakomaa Leena A. Soikkeli Eva Bertalan Eeva I. Kallio Maria Ballok 《Geostandards and Geoanalytical Research》2004,28(1):123-130
We compared the recovery of gold, palladium and platinum by two fire assaying procedures, using nickel sulfide and lead as collectors. The presence of appreciable amounts of sulfide minerals in the sample caused interferences in both procedures. An in-house reference sample, a reference sample of high-grade sulfide ore and samples of high sulfide content from the Recsk porphyry copper ore in Hungary were analysed by both methods. The elements were determined by inductively coupled plasma-atomic emission (ICP-AES) and/or inductively coupled plasma-mass spectrometry (ICP-MS). It was found that for the sulfide ore samples, the recoveries of Au and Pd are sometimes lower by nickel sulfide fire assay than by lead fire assay. Recovery of Re by nickel sulfide fire assay was found to be low: the average recovery of five repeated analyses of the reference sample NIST SRM 330 was 9% with a relative standard deviation of 48%. Increasing the amount of S in the fusion flux gave better recovery. 相似文献
13.
Meeri Suominen Esko Kontas Heikki Niskavaara 《Geostandards and Geoanalytical Research》2004,28(1):131-136
The classical lead fire assay is still the most important method for the pre-concentration and separation of Ag, Au and some of the platinum-group elements (PGE) in the analysis of geological materials. The most frequently used fire assay procedure is the determination of Au, Pd and Pt with Ag as collector. When Au is used instead of Ag as a collector, Pd, Pt, Rh and possibly Ir can also be determined. In this study the recoveries by Au and Ag collectors, also called inquarts, were compared in the fire assay analysis of Pd, Pt and Rh in geological reference materials. The amount of gold to be added was optimised. Variable recoveries were obtained with Ag inquart for Rh, but a 2 mg inquart of Au gave good recoveries for all three of these elements in the analysis of reference samples of different geological materials. A procedure, alternative to scorification, to overcome interferences caused by base metals in the cupellation step is presented. The procedure involves cutting the Pb button into pieces and analysing the pieces separately. Prior to this, a homogeneity study of the lead button was made, and it showed that Pd, Pt and Rh were evenly distributed in the Pb button. All determinations were made using inductively coupled plasma-atomic emission spectrometry (ICP-AES). 相似文献
14.
Platinum-Group Elements and Gold Determination in NiS Fire Assay Buttons by UV Laser Ablation ICP-MS
Alexandre P.de S. Jorge Jacinta Enzweiler Elisa K. Shibuya Jorge E.S. Sarkis Ana Maria G. Figueiredo 《Geostandards and Geoanalytical Research》1998,22(1):47-55
The direct analysis of nickel sulfide fire assay buttons by UV laser ablation ICP-MS was used to determine the platinum-group elements and gold in the following reference materials: UMT-1, WPR-1, WMG-1, GPt-4, GPt-6 and CHR-Bkg. The instrument was calibrated with buttons prepared using quartz doped with the appropriate standard solutions. Analytical precision (RSD) was generally better than 10%, although occasional higher RSDs may infer local heterogeneities within nickel sulfide buttons. Good or excellent agreement was observed between analysed and reference material values except Rh in UMT-1 and WMG-1, which suffered an interference from copper. Detection limits calculated as 10 s quantitation limits were Au (1.7 ng g−1 ), Pd (3.3 ng g−1 ), Pt (8.3 ng g−1 ), Os (1.3 ng g−1 ), Rh (1 ng g−1 ), Ru (5 ng g−1 ) and Ir (0.7 ng g−1 ). 相似文献
15.
Improved Platinum-Group Element Extraction by NiS Fire Assay from Chromitite Ore Samples Using a Flux Containing Sodium Metaphosphate 总被引:1,自引:0,他引:1
Many chromite-rich rocks contain relatively high concentrations of the platinum-group elements (PGE). In many cases, the phases carrying PGE occur as either platinum-group minerals (PGM) or as base metal sulfides in solid solution in sulfides. In some cases, such as the UG-2 unit of the Bushveld Complex, the PGM are occluded inside chromite grains. Chromites are notably difficult to dissolve in most fluxes and if the chromite contains some PGM the possibility exists that not all the PGE will be recovered during fusion. In this work, shortcomings in published methods of analysis based on the nickel sulfide fire assay procedure were investigated and a new procedure developed based on the addition of sodium metaphosphate to the fusion mixture. Optimum composition of the fusion mixture was found to be 10 g sodium metaphosphate and 9 g silica to 10 g sample, 15 g sodium carbonate, 30 g lithium tetraborate, 7.5 g nickel and 4.5 g sulfur to achieve complete dissolution of chromite grains. The new flux mixture was evaluated by the analysis of reference material CHR-Pt+ (which is known to contain PGM inside chromite grains) and no undissolved chromite grains were found in the glassy slag. Analysis of the nickel sulfide beads from this fire assay using neutron activation analysis showed similar results for Rh and Ru when compared with published conventional true (or accepted) values, while Au, Ir, Os, Pd and Pt values determined here were 10 to 30% higher than the corresponding published conventional true values. It was concluded that the addition of sodium metaphosphate improved chromite dissolution in the flux and appears to improve PGE recovery. 相似文献
16.
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
17.
锍镍试金-等离子体质谱法测定地球化学勘探样品中的铂族元素和金Ⅱ.分析流程空白的降低 总被引:26,自引:8,他引:26
对锍镍试金富集-等离子体质谱法测定贵金属流程中的试剂空白进行了检查,并对空白主要来源-捕集剂镍的各种纯化方法作了对比,提出了回收试金流程中溶扣后滤液中的镍循环使用。在有效降低空白的基础上,满足了化探样品所要求的0.0x ng/g级检出限,对超痕量贵金属标样分析结果与标准值符合。 相似文献
18.
Chunsheng Li Chifang Chai Xiaolin Li Xueying Mao 《Geostandards and Geoanalytical Research》1998,22(2):195-197