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1.
高艳  李大伟  常洲 《甘肃地质》2017,26(4):82-86
本方法用HCl和H_2O_2分解试样,以泡沫塑料富集Au、Pt和Pd,在酸性介质中解脱,用电感耦合等离子体质谱法测定化探样品中痕量金铂钯,研究了富集解脱介质及浓度。结果表明,在0.5%NaI+0.5%KBr+20%HCl介质中泡沫塑料对Au、Pt、Pd的吸附率大于95%;在1%硫脲+2%KSCN+2%HCl解脱介质中Au、Pt、Pd的回收率高于90%。方法检出限为Au 0.072 ng/g,Pt 0.17 ng/g,Pd 0.096 ng/g,标准物质的测定值与标准值基本一致,准确度和精密度满足相关规范要求,因此该方法对化探样品中痕量金铂钯的测定有一定实用性。  相似文献   

2.
贵金属分析应用火试金法分离富集时,试金配料复杂、耗时较长,分析成本相对较高,空白较难控制.本文建立了采用过氧化氢-盐酸湿法分解样品,电感耦合等离子体质谱同时测定地质样品中Pt、Pd、Au的分析方法.在10％的盐酸介质中,以LSC-400巯基树脂和活性炭为混合吸附剂,采用动态吸附方式对样品中的Pt、Pd、Au分离富集,用Lu作内标元素,195 Pt、197 Au、108 Pd为待测同位素消除了非谱线干扰和谱线干扰,三元素的回收率均大于96.4％.方法检出限(3σ):Pt为0.06 ng/g,Pd为0.08 ng/g,Au为0.12 ng/g,优于火试金等其他分离富集方法的检出限.应用于测定国家标准物质,Pt、Pd、Au的测定结果与标准值相符,12次测定的相对标准偏差均小于16.1％,满足区域地球化学调查样品的分析要求.该方法操作简便、成本低廉,提高了分析速度,有效地降低了测试过程的空白值.  相似文献   

3.
王瑞敏 《岩矿测试》2011,30(3):295-298
样品采用王水溶解,二氯化锡还原,泡沫塑料富集,用Re作内标,电感耦合等离子体质谱法同时测定土壤中超痕量金、铂、钯。在盐酸-二氯化锡体系中,盐酸酸度为15%,二氯化锡浓度为45 g/L,吸附时间30 min时吸附效果明显,吸附温度为25℃时吸附率相对稳定。方法检出限Au为0.21 ng/g,Pt为0.18 ng/g,Pd为0.16ng/g,方法加标回收率Au为91.3%~97.8%,Pt为92.0%~96.7%,Pd为96.0%~101.6%。该方法用于测定国家一级标准物质,线性范围宽、重现性好,结果准确可靠,样品处理简便、快速。  相似文献   

4.
小试金光谱法同时测定地质样品中超痕量铂钯金   总被引：9，自引：2，他引：9  
林玉南  沈振兴 《岩矿测试》1991,10(4):247-253
用小试金光谱法同时测定地质样品中低至0·x×10~(-9)级Pt、Pd和Au,包括先用小试金熔炼和灰吹预富集10g样品中的Pt、Pd和Au于1mg的银合粒中,然后把银合粒装入石墨电极同锇-锑合金(ω(Os)=0.06)一起激发,以发射光谱法同时测定它们的含量。小试金法类同经典火试金,但采用纯化过的2PbCO_3·Pb(OH)_2(Pt、Pd和Au的含量皆<0.05 ×10~(-9)代替商品PbO,并且用50ml高铝坩埚在950℃进行熔炼。方法的检出限是Pt0.2×10~(-9),Pd和Au均为0.1×10~(-9)。对于3×10~(-9)的含量,全过程的相对标准偏差(％)是Pt15,Pd11,Au9。此法快速、简便,适用于地质物料的分析。  相似文献   

5.
正自然资源部中国地质调查局郑州矿产综合利用研究所贵金属分析团队在学科带头人倪文山高级工程师的带领下,建立了铅试金分离富集与激光剥蚀-电感耦合等离子体质谱(LA-ICP-MS)联用技术测定地球化学样品中痕量、超痕量金(Au)、铂(Pt)、钯(Pd)的新方法,实现了固体样品前处理和直接进样技术的有效联合。该方法较传统铅试金分析方法节省了样品前处理时间,降低了Au、Pt和Pd的空白值,避免了溶液进样时大量O、  相似文献   

6.
郑浩  李红  曾扬  马龙 《岩矿测试》2005,24(4):299-302
采用717阴离子交换树脂-活性炭分离富集矿石中的微量Au、Pt、Pd。40μg待测元素富集结果表明,Au、Pt、Pd的回收率分别为100%、95.3%和96.3%。以HC l为介质在无火焰原子吸收仪上测定。方法经对国家一级标准物质GBW 07291、GBW 07292分析检验,结果与标准值相符。对GBW 07291国家一级标准物质测定7次,其精密度(RSD)分别为:Au 9.4%、Pt 11.2%、Pd 3.0%。方法适用于矿石中10-6~10-9量级Au、Pt、Pd的测定。  相似文献   

7.
DT—1016型阴离子交换树脂分离富集金铂钯   总被引：17，自引：5，他引：17  
研究了DT－1016型阴离子交换树脂对超痕量Au,Pt,Pd的吸附性能及条件。在0.025mol/L HCl介质中，流出速度为0.5-1.0mL/min时，Au,Pt和Pd的富集效果最佳，吸附率分别为99.72％，99.06％和97.95％，共存离子无显著性影响。用等离子体质谱测定标准物质中Au，Pt和Pd，其结果与标准值基本相符。检出限Au为0.27μg/L，Pt为0.40μg/L，Pd为0.19μg／L。对GBW 07294铂族元素国家标准物质进行精密度试验，RSD（n=8）Au为19．2％，Pt为28.1％，Pd为15.6％。  相似文献   

8.
采用717阴离子树脂活性炭联合交换分离富集技术,电感耦合等离子体发射光谱法同时测定富钴锰结壳中痕量金、银、铂、钯。方法检出限四元素分别为:Au1. 3、Ag0. 4、Pd0. 6、Pt4. 8ng/g。样品加标回收率在89. 0% ~110. 3%,相对标准偏差3. 5% ~7. 8% (n=4)。方法已用于富钴锰结壳中痕量金银铂钯的测定。  相似文献   

9.
沈毓琏 《岩矿测试》1989,8(4):272-276
在10％的王水介质中,采用717阴离子交换树脂交换富集Pt、Pd和Au,与大部分阳离子分离,被吸附的Pt、Pd和Au用硫脲解脱后以无火焰石墨炉原子吸收法进行测定。方法简便、快速,检测限低。各元素的特征量分别为Pt5.8γ×10~(-11)g,Pd8.9×10~(-12)g,Au7.72×10~(-12)g。方法已成功地用于岩石矿物中痕量Pt、Pd、Au的测定。  相似文献   

10.
等离子体质谱法直接测定地球化学样品中金铂钯   总被引：19，自引：0，他引：19  
建立了王水分解地球化学样品报直接用等离子体质谱法测定Au、Pd和Pt的分析方法。方法测定下限为Au4,0ng/g,Pd3.6ng/g,Pt2.4ng/g，方法精密度（RSD，n=12）为Au14.2%,Pd3.6%-5.2%,Pt6.6%-10.8%，三个元素的线性范围都为0.02-300μg/L。采用文中制定的分析方法直接测定了国家一级地球化学标准物质中的Au、Pd、Pt，在测定下限以上的测定结果与标准值吻合。  相似文献   

11.
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   

12.
喀拉通克铜镍矿床产于漏斗状基性岩体中下部的橄榄苏长辉长岩相中,矿石类型分特富铜镍矿石(Ⅰ)、富铜贫镍矿石(Ⅱ)、贫铜贫镍矿石(Ⅲ)及富镍富铜矿石(Ⅳ).由于矿床物质成分复杂特别是金银铂钯矿物颗粒细、品位低、种类多,故首先在进行矿物定性研究的基础上,确定目的矿物的特殊富集流程.然后在人工重砂大样中富集目的矿物,并制成砂光薄片,有代表性的排定视域,引入电子探针-图象分析-计算机联机定量并辅以显微镜定量的综合方法对贵金属元素和矿物进行定量.联机方法是用电子探针以扫描方式提供颗粒电子象和元素X射线面分布象信号给出元素或共存元素的化学信息,对矿物颗粒进行分类,统计出个数及面积百分比.这种方法对微细杂矿物的定量工作颇有成效.  相似文献   

13.
建立了一个用酸（HF、HCI、HNO3、HCIO4）溶解通古斯地区沉积物样品，以Re为内标元素，用电感耦合等离子体质谱（ICP－MS）测定其中铂族元素的分析方法。方法检出限为0．001－0．06μg/L，回收率大于85％。用该方法分析了9个取自通古斯地区的沉积物样品，发现了Ru、Rh、Pd、Ir、Pt等元素的异常。  相似文献   

14.
The Jingbaoshan platinum-palladium deposit is China＇s largest independent PGM （platinum-group metals） deposit so far discovered. There are eleven kinds of useful components in the ore： Pt, Pd, Os, Ir, Ru, Rh, Au, Ag, Cu, Ni, and Co. The platinum-group elements, gold and silver occur in the form of minerals in ores. twenty-five kinds of precious metal minerals have been found, of which twenty one belong to the platinum-group minerals. The minerals are very small in grain size. Copper occurs mainly as copper sulfide with a small amount of free copper oxide, and the beneficiated copper accounts for 95.21%. Nickel occurs mainly as nickel sulfide, and some nickel silicate and nickel oxide occur in the ore. The beneficiated nickel accounts for 72.03%. Cobalt occurs mainly as cobalt sulfide, and there are some cobalt oxide and other kinds of cobalt. The beneficiated cobalt accounts for 77.58%.  相似文献   

15.
The Kaalamo massif is located in the Northern Ladoga region, Karelia, on the extension of the Kotalahti Belt of Ni-bearing ultramafic intrusions in Finland. The massif, 1.89 Ga in age, is differentiated from pyroxenite to diorite. Nickel–copper sulfide mineralization with platinoids is related to the pyroxenite phase. The ore consists of two mineral types: (i) pentlandite–chalcopyrite–pyrrhotite and (ii) chalcopyrite, both enriched in PGE. Pd and Pt bismuthotellurides, as well as Pd and Pt tellurobismuthides, are represented by the following mineral species: kotulskite, sobolevskite, merenskyite, michenerite, moncheite, keithconnite, telluropalladinite; Pt and Pd sulfides comprise vysotskite, cooperite, braggite, palladium pentlandite, and some other rare phases. High-palladium minerals are contained in pentlandite–chalcopyrite–pyrrhotite ore. Native gold intergrown with kotulskite commonly contains microinclusions (1–3 μm) of Pd stannides: paolovite and atokite. Ore with 20–60% copper sulfides (0.2–6.0% Cu) contains 5.1–6.6 gpt PGE and up to 0.13–2.3 gpt Au. Pd minerals, arsenides and sulfoarsenides of Pt, Rh, Ir, Os, and Ru are identified as well. These are sperrylite, ruthenium platarsite, hollingworthite, and irarsite; silvery gold and paolovite have also been noted. All these minerals have been revealed in the massif for the first time. The paper also presents data on the compositions of 25 PGE minerals (PGM) from Kaalamo ores.  相似文献   

16.
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   

17.
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   

18.
A measurement procedure for determining of Ru, Pd, Ir, Pt and Au mass fractions in ferromanganese deposits by inductively coupled plasma‐mass spectrometry after acid digestion and anion exchange preconcentration is presented. To eliminate incomplete recovery after sorption preconcentration of the platinum‐group elements (PGE) and Au, a standard addition method was used. Detection limits ranged from 0.02 ng (Pd, Ir) to 0.19 ng (Ru). The measurement results for ferromanganese nodule reference material NOD‐A‐1 and NOD‐P‐1 agree with earlier reported values. Intermediate precision of PGE concentration data for nodule reference materials in this work was 5–24% (1s) and could reflect sample heterogeneity.  相似文献   

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