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1.
激光剥蚀电感耦合等离子体质谱(LA-ICP-MS)适合于直接分析硫化物矿物中痕量元素的含量及空间分布,但硫化物矿物的激光剥蚀特性与硅酸盐及氧化物不同,受到的干扰也更严重,且由于硫化物标准物质(尤其是含铂族元素、Au、Ag等贵金属元素标准物质)极度缺乏,限制了LA-ICP-MS技术在硫化物微区分析中的广泛应用。本文以贵金属标准样品GPT-9和矿石标准物质为原料合成锍镍试金扣,并封入真空管中重熔,利用背散射电子图像和LA-ICP-MS分析元素分布的均匀性,探讨真空重熔锍镍试金扣制备硫化物原位微区分析标准样品的可行性。背散射电子图像(BSE)显示真空重熔后锍镍试金扣由单相S、Ni化合物组成。LA-ICP-MS线扫描和点扫描分析表明,锍镍试金扣中S、Ni、Cr、Co、Cu、Pb、Sb、Cd、Bi等主量及微量元素分析精密度(RSD)均小于10%,均匀分布;在镍扣制备过程中Zn相对于Cu、Pb、Sb更难进入硫化物相;贵金属元素Au、Ag、Pt均一性较好,其余贵金属元素由于含量低、仪器波动及质谱干扰等影响因素造成分析数据的RSD相对较大,但可通过提高原料中贵金属元素含量、降低熔融样品淬火温度等方法进一步提高其均匀性。锍镍试金扣的组成元素对铂族元素分析的质谱干扰研究表明,重铂族元素(Os、Ir、Pt)和Au受到的干扰可忽略不计;轻铂族元素(Ru、Rh、Pd)受金属氩化物干扰较为严重,需进行干扰校正。研究认为,真空重熔技术可有效提高锍镍试金扣中各元素(包括贵金属)的均一性,达到硫化物原位微区分析标准样品的要求,利用真空重熔锍镍试金扣制备LA-ICP-MS原位微区痕量及贵金属硫化物分析标准样品具可行性。  相似文献   

2.
Precious metals (Ag, Au, Pt, Pd, Rh) were determined by flameless absorption atomic spectrornetry. Aqua regia sample decomposition followed by Te coprecipitation was employed to preconcentrate the precious metals in geological materials. With 5 g sample take-up, the limits of determination were 1-2 ppb for Au, Pd and Rh, 5 ppb for Ag and 10-20 ppb for Pt. These elements were determined in some geochemical standards.  相似文献   

3.
Inductively coupled plasma-mass spectrometry (ICP-MS) after NiS fire assay-Te co-precipitation was employed in the determination of Ru, Rh, Pd, Os, Ir and Pt at ng g-1 levels in six platinum-group element (PGE) geological reference materials. In general, the average of several results was in good agreement with the certified values taking into account respective uncertainties. High relative standard deviations were observed for the reference materials GPt-3 and GPt-4. Problems associated with the NiS fire assay procedure and PGE determination at the sub-10 ng g-1 level are reviewed and discussed.  相似文献   

4.
NK8310螯合树脂分离富集地质样品中痕量金银铂钯及其测定   总被引：14，自引：3，他引：14  
李志强  沈慧君 《岩矿测试》2001,20(2):91-96,99
研究了硫脲螯合树脂（NK8310）分类富集地质样品中痕量Au、Ag、Pt和Pd的实验条件。在φ=10％的王水介质中，[AuCI4]^-、[AgCI2]^-、[PtCI6]^2-和[PdCI4]^2-定量吸附于树脂上并与大量贱金属分离；用5g/L硫脲－0.12mol/L HCI溶液洗脱Au、Ag、Pt和Pd，回收率为97％－104％。用硫镍矿管理样以及国家一级标准物质进行分析验证，分析结果与推荐值及标准值吻合，表明NK8310螯合树脂适用于地质样品中Au、Ag、Pt和Pd的分离富集。  相似文献   

5.
赵宏樵  赵建如 《现代地质》2007,21(4):654-658
对太平洋CL、CM海山调查时获取9个富钴结壳样品,采用化学处理及ICP-MS法进行分析。对贵金属元素含量分布特征、富集因子、标准化模式以及来源进行探讨和研究。结果表明：海山结壳中贵金属元素Ag、Au、Ru、Rh、Pd、Pt等的平均含量分别为： 1.05×10-6、2.3×10-6、15.6×10-9、22.3×10-9、2.39×10-9和432×10-9。与结核、洋壳及陆地矿石的Pd/（Pt+Pd）、Pt/（Pt+Pd）和Pd/Pt等贵金属元素的比值相比,大洋富钴结壳的 Pd/（Pt+Pd） 比值最低,为0.006;其次是结核,为0.06;洋壳为0.08;陆地矿石的Pd/（Pt+Pd）比值较大,为0.35～0.65。结壳的Pt/（Pt+Pd）比值最高,为0.99;其次是结核,为0.95;洋壳为0.93;陆地矿石的Pt/（Pt+Pd）比值相对较低,为0.33～0.65。统计分析显示了不同区域、不同环境中贵金属元素的特征参数变化,并且说明富钴结壳中富铂、金、钌、铑,而贫钯。贵金属元素标准化显示,海山富钴结壳均存在着Pt、Au正异常和Pd的负异常,其中Au异常幅度与结核的Au异常一致。  相似文献   

6.
安徽铜官山矽卡岩型铜铁矿床富含多种稀有贵金属金银铂钯和铀,本文应用偏光显微镜与电子探针技术对该地区贵金属和铀矿物的含量、矿物种类、赋存状态及其嵌布特征进行研究,并利用电子探针Th-U-Pb定年技术推测铀矿物的形成时期。研究表明:金主要以银金矿独立矿物存在,成色均值约为638,与铜的硫化物密切依存,金矿物形成于成矿中晚期的中低温环境;银的独立矿物有银金矿、碲银矿、辉银矿,还与铜铋铅等以类质同象形式结合形成不同种类的矿物组合,且含量在74.15%~0.12%不等;铂钯矿物以含铂碲钯矿为主;铀以晶质铀矿独立矿物存在且与磁铁矿密切依存,晶质铀矿的形成年龄约为124±14 Ma,晚于岩体形成年龄(约139 Ma),早于黄铜矿和含金银铂钯等矿物,而与磁铁矿同在燕山中晚期形成。结合镜下观察,认为铜官山矽卡岩型铜铁矿床主要矿物生成顺序依次是:石榴子石-磁铁矿、晶质铀矿,含金银铂钯矿物,黄铜矿。本研究为贵金属选矿提供了线索,同时利用晶质铀矿的年龄数据界定了伴生贵金属的形成年代。  相似文献   

7.
对利用铜试金预富集后辉光放电质谱法(GDMS)测定贵金属矿样中痕量Pt、Pd、Ir、Au的方法进行了探索性研究。着重考察了铜试金条件的选择和辉光放电电极的匹配、质谱的测定条件和测定方法等。分析结果表明,痕量(μg级)贵金属元素Pt的含量在1.99~15.0μg,回收率为92.0%~111.9%;Pd的含量在3.15~29.78μg,回收率为88.4%~113.3%;Ir的含量在0.12~0.60μg,回收率为68.3%~100.0%;Au的含量在10.43~24.08μg,回收率为98.9%~127.0%。方法可应用于矿石、矿物及其他物料中痕量贵金属的分析。  相似文献   

8.
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   

9.
根据西太平洋麦哲伦海山富钴板状结壳样品的成分特征，对常规的锍镍试金配方作了改进；酌情减少捕集剂羰基镍的加入量，可显著降低铂族元素的空白值。富集后的样品，采用电感耦合等离子体质谱测定铂族元素（PGE）。其中，Ru、Rh、Pd、Ir和Pt用常规外标法测定，^175Lu作内标；Os用同位素稀释法测定。用国家一级标准物质GBW07290和GBW07291作监控分析质量的参考样，结果满足要求。  相似文献   

10.
A series of geochemical anomalies of Pt and Pd were found in 1 358 recombined samples from a geochemical stream sediment survey in eastern Yunnan (云南) Province, China. Chemical optical emission spectroscopy, X-ray fluorescence analysis, and inductively coupled plasmas atomic emission spectrometry analyses of 22 elements and chemical compositions of 21 samples from coal-bearing strata from the Late Paleozoic, Mesozoic, and Cenozoic show Pt and Pd concentrated to some extent in coal rocks, with Pd/Pt相似文献   

11.
The knowledge of the variability, the anthropogenic versus natural origin and corresponding environmental risk for potentially harmful elements in urban topsoils is of importance to assess human impact. The aims of the present study were: (1) to assess the distribution of heavy metals (Sn, Li, Ga, Ba, Fe, Mn, Co, Be, Ti, Al, Hg, Cr, Sb, As, Bi, Pd, Pt, Au, Ni, Cd, Zn, Cu, Pb, Se, Mo, Sc and Ag) in urban environment; (2) to discriminate natural and anthropogenic contributions; and (3) to identify possible sources of pollution. Multivariate statistic approaches (principal component analysis and cluster analysis) were adopted for data treatment, allowing the identification of three main factors controlling the heavy metal variability in Xuzhou urban topsoils. Results demonstrate that Hg, Cr, Sb, As, Bi, Pd, Pt, Au, Ni, Cd, Br, Zn, Cu, S, Pb, Se, Mo, Sc and Ag could be inferred to be tracers of anthropogenic pollution, whereas Al, Ti, Ga, Li, V, Co, Pt, Mn and Be were interpreted to be mainly inherited from parent materials. Iron, Ba, Sn, Pd and Br were interpreted to be affected by mixed sources.  相似文献   

12.
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   

13.
A method was developed for the determination of platinum‐group elements (PGE) in geological samples by isotope dilution‐inductively coupled plasma‐mass spectrometry combined with sulfide fire assay preconcentration. Samples were fused and PGE analytes were concentrated in sulfide buttons. The buttons were dissolved using HCl leaving PGE analytes in insoluble residues, which were digested in HNO3 and simultaneously processed for the distillation of Os. The remaining solutions were further prepared for the purification of Ru, Rh, Pd, Ir and Pt using a tandem assembly of cation and Ln resin columns. The eluents were directly analysed by membrane desolvation‐ICP‐MS. Ruthenium, Pd, Os, Ir and Pt were determined by isotope dilution, whereas Rh was determined by conventional reference material calibration combined with 193Ir as the internal standard element. The method was validated using a series of PGE reference materials, and the measurement data were consistent with the recommended and the literature values. The measurement precision was better than 10% RSD. The procedural blanks were 0.121 ng for Ru, 0.204 for Rh, 0.960 ng for Pd, 0.111 ng for Os, 0.045 ng for Ir and 0.661 ng for Pt, and the limits of detection (3s) were 0.011 ng g?1 for Ru, 0.008 ng g?1 for Rh, 0.045 ng g?1 for Pd, 0.009 ng g?1 for Os, 0.006 ng g?1 for Ir and 0.016 ng g?1 for Pt when a test portion mass of 10 g was used. This indicates that the proposed method can be used for the determination of trace amounts of PGE in geological samples.  相似文献   

14.
论金川硫化铜镍矿床中贵金属元素的分带机制   总被引：3，自引：1，他引：3  
在金川硫化铜镍矿床最大的寓矿体内,贵金属元素存在明显分带:Pt、Pd、Au、Ag含量在边部较低,向中心部位逐渐增高;Os、Ir、Ru、Rh含量在中心部位较低,向边部逐渐增高。通过对实际资料的分析,认为这种分带特征是硫化物液相结晶分异作用造成的。  相似文献   

15.
A new technique for the in situ analysis of Re, Au, Pd, Pt and Rh in natural basalt glass by laser ablation (LA)-ICP-MS is described. The method involves external calibration against NIST SRM 612/613 or 614/615 glass certified reference materials, internal standardisation using Ca, and ablation with a 200 μm wide beam spot and a pulsed laser repetition rate of 50 Hz. Under these conditions, sensitivities for Re, Au, Pd, Pt and Rh analyte ions are ˜ 5000 to 100,000 cps/μg g-1. This is sufficient to make measurements precise to ˜ 10% at the 2-10 μg g-1 level, which is well within the range of concentrations expected in many basalts. For LA-ICP-MS calibration and a demonstration of the accuracy of the technique, concentrations of Re, Au, Pd, Pt and Rh in the NIST SRM 610/611 (˜ 1 to 50 μg g-1), 612/613 (˜ 1 to 7 μg g-1), 614/615 (˜ 0.2 to 2 μg g-1) and 616/617 (˜ 0.004 to 2 μg g-1) glasses were determined by solution-nebulisation (SN)-ICP-MS. Using the 612/613 or 614/615 glasses as calibration standards, LA-ICP-MS measurements of these elements in the other NIST glasses fell within ˜ 15% of those determined by SN-ICP-MS. Replicate LA-ICP-MS analyses of the 612/613 and 614/615 glasses indicate that, apart from certain anomalous domains, the glasses are homogeneous for Re, Au, Pd, Pt and Rh to better than 3.5%. Two LA-ICP-MS analyses of natural, island-arc basalt glasses exhibit large fractionations of Re, Au and Pd relative to Pt and Rh, compared to the relative abundances in the primitive mantle.  相似文献   

16.
ＩＮＴＲＯＤＵＣＴＩＯＮＬｏｗｅｒＣａｍｂｒｉａｎｂｌａｃｋｒｏｃｋｓｅｒｉｅｓｅｘｉｓｔｓｂｒｏａｄｌｙｉｎｍｏｒｅｔｈａｎ１０ｐｒｏｖｉｎｃｅｓｉｎＳｏｕｔｈＣｈｉｎａ（Ｃｈｅｎｅｔａｌ．,１９９０）．Ｔｈｅｂｏｔｏｍｏｆｔｈｅｓｅｒｉｅｓｓｐｏ...  相似文献   

17.
Concentrations of platinum group elements (PGE), Ag, As, Au, Bi, Cd, Co, Mo, Pb, Re, Sb, Se, Sn, Te, and Zn, have been determined in base metal sulfide (BMS) minerals from the western branch (402 Trough orebodies) of the Creighton Ni–Cu–PGE sulfide deposit, Sudbury, Canada. The sulfide assemblage is dominated by pyrrhotite, with minor pentlandite, chalcopyrite, and pyrite, and they represent monosulfide solid solution (MSS) cumulates. The aim of this study was to establish the distribution of the PGE among the BMS and platinum group minerals (PGM) in order to understand better the petrogenesis of the deposit. Mass balance calculations show that the BMS host all of the Co and Se, a significant proportion (40–90%) of Os, Pd, Ru, Cd, Sn, and Zn, but very little (<35%) of the Ag, Au, Bi, Ir, Mo, Pb, Pt, Rh, Re, Sb, and Te. Osmium and Ru are concentrated in equal proportions in pyrrhotite, pentlandite, and pyrite. Cobalt and Pd (∼1 ppm) are concentrated in pentlandite. Silver, Cd, Sn, Zn, and in rare cases Au and Te, are concentrated in chalcopyrite. Selenium is present in equal proportions in all three BMS. Iridium, Rh, and Pt are present in euhedrally zoned PGE sulfarsenides, which comprise irarsite (IrAsS), hollingworthite (RhAsS), PGE-Ni-rich cobaltite (CoAsS), and subordinate sperrylite (PtAs2), all of which are hosted predominantly in pyrrhotite and pentlandite. Silver, Au, Bi, Mo, Pb, Re, Sb, and Te are found predominantly in discrete accessory minerals such as electrum (Au–Ag alloy), hessite (Ag2Te), michenerite (PdBiTe), and rhenium sulfides. The enrichment of Os, Ru, Ni, and Co in pyrrhotite, pentlandite, and pyrite and Ag, Au, Cd, Sn, Te, and Zn in chalcopyrite can be explained by fractional crystallization of MSS from a sulfide liquid followed by exsolution of the sulfides. The early crystallization of the PGE sulfarsenides from the sulfide melt depleted the MSS in Ir and Rh. The bulk of Pd in pentlandite cannot be explained by sulfide fractionation alone because Pd should have partitioned into the residual Cu-rich liquid and be in chalcopyrite or in PGM around chalcopyrite. The variation of Pd among different pentlandite textures provides evidence that Pd diffuses into pentlandite during its exsolution from MSS. The source of Pd was from the small quantity of Pd that partitioned originally into the MSS and a larger quantity of Pd in the nearby Cu-rich portion (intermediate solid solution and/or Pd-bearing PGM). The source of Pd became depleted during the diffusion process, thus later-forming pentlandite (rims of coarse-granular, veinlets, and exsolution flames) contains less Pd than early-forming pentlandite (cores of coarse-granular).  相似文献   

18.
The present study describes a method for the extraction of Pt, Pd, Rh, Ru, Ir and Au from various geological materials after fusion with sodium peroxide in zirconium crucibles involving samples that vary in mass from 1 g to more than 20 g. Precipitation is brought about by reduction of the platinum-group elements (PGEs) with Sn2+, using selenium and tellurium as carriers in the presence of a catalyst (KI). The extraction yields obtained by this method are between 95 and 100% for PGEs. Gold is less well extracted (around 80%). Detection of the noble metals in the extraction residues is carried out by using ICP-MS. The results obtained by this technique are reported for five CCRMP certified reference materials and are close to their certified values. The elements were also determined in a natural glass sample melted during a meteoritic impact and contaminated by PGEs at ultra-trace concentrations.  相似文献   

19.
矿产品中痕量贵金属元素的测定通常需要富集分离,在检测过程中谱线干扰较多。本文对铜精矿样品在高温下灼烧除去碳和硫,采用盐酸+王水+氢氟酸消解体系进行分解,利用D290阴离子交换树脂-活性炭作为吸附剂富集铂和钯,以Y、In、Bi为内标元素,105Pd和195Pt作为测量同位素,用电感耦合等离子体质谱法(ICP-MS)测定铂和钯的含量。铂和钯的吸附率均达到90%以上,加标回收率分别为92.0%和96.0%,检出限分别为0.126 ng/g和0.105 ng/g,方法精密度(RSD,n=6)小于4%。应用于实际铜精矿样品分析,测定值与锍镍试金-ICP-MS测定结果一致。本法的样品处理体系最大限度地减少了样品中其他金属离子对待测元素的影响,选择的内标元素和高纯氦碰撞反应可有效地减少基体效应和同质异位素干扰。相比于锍镍试金法,该方法的样品前处理简单,铂和钯的富集效果明显,测定检出限低。  相似文献   

20.
迄今为止文献中未见有铂矿原生晕研究的报道,通过对大岩子矿区地表和不同中段坑道原生晕的研究,发现在铂-钯矿体周围有清晰的F、Sb、Cd、Hg、As、Ag、Au、Pd、Pt、Cu、Ni元素的原生晕,其中F、Sb、Cd、Hg、As为前缘指示元素,Au、Ag为近矿指示元素,Pt、Pd、Cu、Ni为成矿指示元素.元素的垂直分带序列为(地表至矿体):(F、Sb、Cd、Hg、As)-(Ag、Au)-(Pd、Pt)-(Cu、Ni).地表岩石地球化学测量发现的Ⅲ号Pd、Pt异常带,具有多元素异常组合特征,判断为矿致异常,推测在该异常带下方可望找到隐伏矿体.坑道原生晕研究发现,在PD4中段出现浓集中心醒目、浓度分带清晰的F原生晕,推测在PD4中段下方可能存在新的盲矿体.  相似文献   

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