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1.
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.
D290树脂-活性炭吸附富集电感耦合等离子体质谱法测定铜精矿中铂钯 总被引：1，自引：1，他引：0
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
3.
泡沫塑料富集-电感耦合等离子体质谱法测定土壤中超痕量金铂钯 总被引：1，自引：1，他引：0
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.
阴离子树脂-活性炭分离富集等离子体发射光谱法测定富钴锰结壳中的痕量金银铂钯 总被引：10，自引：1，他引：10
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
5.
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
6.
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
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
7.
火焰原子荧光光谱法(FAFS)测定痕量金的灵敏度好、稳定性高及线性范围广,但在测定时干扰极为严重,如果干扰元素不加以分离或扣除,对0.5ng/g以下金无法进行准确测定。本方法在传统泡塑分离富集金的基础上,研究了FAFS法测定痕量金的最佳条件:在选定仪器条件下,提出了选择低背景值(≤0.25ng/g Au)泡塑分离富集Au,采用3.0g/L硫脲-1%盐酸为解脱液可消除记忆效应,在标准系列中加入5μg/mL的Fe3+溶液扣除铁对测定金的干扰。采用本分析方法对国家标准物质GBW07805、GBW07242、GBW07244a、GBW07245a和GBW07247进行测定,相对误差≤4.7%,相对标准偏差(RSD)≤23.2%;采用FAFS法与ICP-MS法对90个原生晕样品和4个控制样品中痕量金同时进行测定,两组测定结果数统计分析的F检验值为1.23,相关系数为1.01,符合性较好,无显著性差异。本分析方法简便、快速与实用,金检出限为0.08ng/g,线性范围为0.08~500ng/g,可达3个数量级。 相似文献
8.
9.
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
10.
铂-钯区域地球化学勘查 总被引：12，自引：2，他引：12
以Pt、Pd作为直接指示元素，利用1：20万全国区域化探扫面水系沉积物测量副样和全国超低密度泛滥平原沉积物测量样品，采用化学光谱法测定Pt、Pd和Au三种元素，进行了中国大陆超低密度Pt、Pd地球化学填图，在川滇等地球化学省开展了1：20万Pt、Pd区域化探，发现中国大陆存在几个重要的Pt、Pd地球化学省和一些区域异常。中国大陆Pt、Pd丰度低：Pt0.42ng/g,Pd0.35ng/g，呈不均匀分布。在活动带Pt、Pd有显著富集。川滇是一个重要的铂族元素成矿省，除镁铁-超镁铁岩及在关的铂族元素矿化外，在黑色岩系以及西南暗色岩系等岩层中Pt、Pd等显著富集，并且发现了非传统类型的铂族矿化。 相似文献
11.
Sabo Suleiman Jibrin Chaozhang Huang Jia Li Nan Zhang Bin Hu 《Geostandards and Geoanalytical Research》2009,33(4):469-476
A new method using a microcolumn (20 mm length × 2.0 mm i.d.) packed with Azadirachta Indica leaf powder (Neem leaf) as an adsorbent for the preconcentration/separation of Au and Pd prior to their determination by ICP‐OES in geological samples is presented. Various factors affecting the separation and preconcentration of the target analytes such as pH, sample flow rate and volume, eluent concentration and volume and interfering ions were studied and the optimal experimental conditions were established. The adsorption capacity of Azadirachta Indica leaf for Au and Pd was found to be 39.2 and 9.8 mg g−1, respectively. The detection limits (3s) of this method for Au and Pd with an enrichment factor of 50 were 47 ng l−1 and 59 ng l−1 and the relative standard deviations were 4.8% and 5.7% (n = 7, adsorption capacity C = 5 ng ml−1), respectively. In order to validate the proposed method, the certified reference material, GBW07293, was analysed, and a good agreement was obtained between the certified and determined values. 相似文献
12.
Determination of Platinum‐Group Elements in Geological Samples by Isotope Dilution‐Inductively Coupled Plasma‐Mass Spectrometry Combined with Sulfide Fire Assay Preconcentration 
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下载免费PDF全文 Minghao Ren Yali Sun Christina Yan Wang Shengling Sun 《Geostandards and Geoanalytical Research》2016,40(1):67-83
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
13.
Liang Qi Mei-Fu Zhou Zheng Zhao Jing Hu Yan Huang 《Environmental Earth Sciences》2011,64(6):1683-1692
The emission of platinum group elements (PGE) from automobile catalytic converters has led to enrichment of PGE in road dusts
and roadside soils in urban areas that are well above the natural background levels. This paper evaluates the source of contamination
of all the PGE and Au in road dusts and roadside soils in the Pearl River Delta region, including three major cities, Shenzhen,
Guangzhou and Hong Kong, South China. Samples were digested using Carius tube and analyzed by isotope dilution ICP-MS; Os
was separated by distillation and other PGE by Te-coprecipitation. All samples have elevated PGE concentrations above the
background values of uncontaminated soils and contain higher Pt, Pd and Rh than other PGE. The maximum values are 181 ng/g
Pt, 514 ng/g Pd, 53 ng/g Rh and 1345 ng/g Au. There are clear positive correlations between Pt and Pd, Pt and Rh, and Pd and
Rh, indicating that the main emitted of PGE from automobile catalyst are Pt, Pd and Rh. High concentrations of Au were also
found in road dust samples from Hong Kong and Shenzhen. Dust samples with higher Os contents have lower 187Os/188Os ratios. Samples from Hong Kong show relatively high Pt/Rh ratios. Positive correlations between Pt and Ru, and Pt and Ir
were found in Shenzhen and Hong Kong, but only positive correlations between Pt and Ir were found in Guangzhou. These different
characteristics reflect different automobile catalytic systems used in Hong Kong and mainland China. 相似文献
14.
高纯硝酸银中痕量杂质元素的存在会影响其性能和质量,为提高现代测试技术分析痕量杂质元素的准确度,需要解决的首要问题是通过加入沉淀剂或还原剂将银除去,克服基体元素的基体效应。本文提出采用10 mL 10 g/L柠檬酸-5 g/L乙醇酸作络合保护剂,12 mL 100 g/L氯化铵作沉淀剂,建立了沉淀基体分离-电感耦合等离子体质谱同时测定高纯硝酸银中15种痕量杂质元素的分析方法。探讨了络合剂和沉淀剂浓度及用量、质谱干扰及同位素选择、非质谱干扰及内标选择、实验空白值等因素对测定结果的影响。在最佳的实验条件下,Cu、Pb、Ni、Mn、Au、Pd、Pt、Rh、Ru、Ir元素在0~100 ng/mL,Fe、Hg、Bi、Cr、Sn元素在0~250ng/mL浓度范围内呈良好的线性关系。方法检出限(3σ)为0.005~0.062 ng/g,方法精密度(RSD,n=11)为0.6%~2.6%,加标回收率为94.1%~103.1%。与现行的分析方法相比,本方法采用的络合剂和沉淀剂能将基体元素与杂质元素完全分离而不影响测定结果;实验流程简单快速,检出限低,准确度和精密度均满足了实际样品的分析要求。 相似文献
15.
通过野外地质调查资料、X衍射、主量及铂族元素测试分析，研究川南马边地区五峰-龙马溪组页岩的矿物学、主量元素地球化学特征和铂族元素组成特征。川南马边长河碥五峰-龙马溪组页岩有机碳TOC平均含量为2.47%；矿物成分主要由石英和黏土矿物两大类构成，石英平均含量37.95%，黏土矿物平均含量为40.2%；页岩SiO2平均含量为52.90%，Al2O3平均含量为11.47%；铂族元素总量在1.5～11.9 ng/g之间，平均值为5.16 ng/g。川南马边地区五峰-龙马溪组页岩铂族元素均以Pt与Pd含量高为特征，其中Pd平均含量为3.15 ng/g，Pt平均含量为1.48 ng/g。铂族元素碳质球粒陨石配分模式为Pt-Pd型，Pd含量约为Pt含量的2.12倍。剖面中富有机质页岩比贫有机质页岩更加富集铂族元素，铂族元素的富集可能与生物活动有关；黏土矿物含量与铂族元素含量呈负相关关系，铂族元素并未呈吸附态吸附在颗粒表面，黏土矿物的增加反而稀释了铂族元素含量。川南马边长河碥五峰-龙马溪组铂族元素并非来源于地外物质，可能来自地幔，且发生了明显分异，其富集程度在正常海洋沉积物范围内。 相似文献