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碱性模式氢化发生原子荧光光谱法测定地质样品中痕量锗 总被引：7，自引：3，他引：7
实验选择了“碱性模式”氢化物发生-原子荧光光谱法测定痕量锗体系的最佳仪器和试剂条件，详细研究了Cu、CO、Ni、Au、Ag、Bi、Sb、Fe、Cl等元素的干扰情况及消除方法；对矿样的分解方法进行对比研究，选择出合理的样品分解方式。方法检出限为1．3μg／L，样品测定精密度较好，RSD为3．42％(n=12)。对多种国家一级标准物质进行测定，结果与标准值相符合。方法适用于多种地盾物料中痕量锗的测定。 相似文献
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本文采用HCl-HNO3-NH4HF2-KClO3封闭溶样,在(NH2)2CS介质中,原子吸收光谱法测定矿石中的Au、Ag。方法能有效避免AgCl、PbCl2沉淀和Au、Ag的硅酸盐包裹体,以及W、Mo和Sb、Pb等在Au富集过程中的竞争吸附与容量法测定的终点干扰。应用ICP-AES可在该介质中完成金矿样品中Ag、Cu、Pb、Zn、As、Sb等的同时测定。方法绿色环保,操作简单、快速,稳定性好,准确度和精密度高,适合于大批量金矿样品的分析测定。 相似文献
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地质样品中痕量Au的分析较多采用湿法溶解样品。最常见的是采用浓王水或1 1王水在烧杯或聚碳酸酯溶矿瓶中溶解样品。对于王水能否把地质样品中的痕量Au全部溶出,在酸不溶物中残留多少Au,残留量对分析质量是否有影响的问题,各文献提法不一。文献介绍:王水溶解低含量Au样时偏低15％;溶解石英岩尾矿,Au结果偏低10-30％。又指出:在金矿区围岩和某些酸难溶硅酸盐矿物中采用王水分解样品,在溶矿时不加入HF作助溶剂,其Au结 相似文献
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为分析金精矿中高含量Ag,加入浓HNO3处理样品中的S,采用王水溶样,使矿样分解完全并降低原子吸收测量时的背景干扰值。称取具代表性样品的最低重量,通过控制HCl介质的浓度,使溶液中的AgCl白色沉淀完全转化为[AgCl]2-配离子,在HCl介质中,用火焰原子吸收分光光度法直接测定Ag。选取2件不同含量的金精矿进行方法的精密度、准确度试验,分析结果表明,该方法的检出限为1×10-6,加标回收率99%～102%。 相似文献
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阳极泥及碲回收物料中高含量碲的测定 总被引：2，自引：0，他引：2
采用重铬酸钾容量法，测定铜铅阳极泥及碲回收物料中高含量碲。针对阳极泥样品成分复杂的特征，确定了最佳溶样介质；探讨了Cu^2 ,Cd^2 ,Bi^3 ,Ag^ ,Sb(Ⅲ）,As（Ⅲ），Pb^2 ,Se（Ⅳ），Sn（Ⅳ），Au(Ⅲ）等共存元素的影响及其消除方法；改善了滴定条件。方法适用于w(Te)＞1％碲的测定，样品分析结果与原子吸收法测定结果一致，RSD（n＝5）为0.4％－4.1％。 相似文献
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文章采用王水溶剂常压水浴溶样,在同一溶样体系分别采用原子荧光测试砷锑铋汞和原子吸收测试铜铅锌,砷、锑、铋、汞4种元素的溶样方法、测试方法和标准方法一致,所以没有再进行方法验证;铜、铅、锌分析方法的检出限、准确度、精密度符合规范要求。对我部矿区样品,用本文方法与标准方法进行了比对试验,2种分析结果吻合;用t检验法对2种方法进行了系统误差检验,结果表明2种方法间没有系统误差存在。 相似文献
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氢化物-原子荧光光谱法测定地质样中的痕量硒--不同溶样方式的比较 总被引：7，自引：1，他引：6
以确定测试基性岩中痕量硒的最佳溶样方式为目的,分别采用加压（PTFE）强酸消解和常压强酸消解两种方法消解标准参考物质和地质样品,直接用氢化物原子荧光光谱法（HG-AFS）测定。实验选用标准参考物质GWB07105、GWB07107对方法准确度和精确度进行验证,所测得总硒量与推荐值相符,标准偏差（SD）小于7．3ng／g,相对标准偏差（RSD）小于8．9％。实验测定了5个硒含量不同的岩石样品,不同方法所测数据基本一致。样品的均匀性在一定程度上影响痕量硒的测定结果。综合评价比较二者的测定结果,可知加压（PTFE）强酸消解（硝酸＋硫酸＋氢氟酸）为最佳溶样方式。 相似文献
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目前测定地质样品痕量、超痕量金常用的三种方法是活性炭吸附富集-发射光谱法、泡塑吸附富集-石墨炉原子吸收光谱法、活性炭吸附富集-电感耦合等离子体质谱法,这三种方法的检出限在0.1~0.3ng/g之间,由于矿石矿物的组成非常复杂,因此在有效富集和分离的基础上,采用合适的分析手段,能够对地质样品提供满意的分析结果。为保证试样要求的灵敏度和准确性,分析方法的选择需求应根据具体试样情况和实验室条件而定。根据田口玄一博士在测量工程学中提出的信噪比(S/N)能测量系统抗干扰能力,评价测量系统的稳健性和可靠性这一观点,本文利用田口测量质量控制理论,评价地质样品中痕量、超痕量金常用的上述三种分析测试方法,对这三种分析方法三个金标准物质的测试数据进行分类处理,计算S/N值和相对标准不确定度,通过比较三者的S/N值和相对标准不确定度值,确定更为可靠的测试体系。分析结果表明,对于地质样品中痕量金(含量大于1 ng/g)的测试,三种分析方法均能够满足要求;对于超痕量金(含量小于1 ng/g)的测试,活性炭吸附富集-电感耦合等离子体质谱法是较好的测试方案。 相似文献
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混合吸附剂分离富集-电感耦合等离子体质谱法测定地质样品中铂钯金 总被引：1，自引：1，他引：0
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
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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
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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
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
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本文评述了近年来地质样品中贵金属元素分析预处理技术的研究现状和应用进展,对样品分解过程中常用的火试金法、碱熔融法、酸分解法以及样品分离富集过程中的吸附法、碲共沉淀法、离子交换法、溶剂萃取法、蒸馏法、生物吸附法等手段进行了归纳总结,分析了各方法的特点与不足,展望了技术方法未来发展方向。分解方法中的火试金法经分析工作者不断探索及改进,已成为分解贵金属的最佳手段,但其仍存在试剂消耗量大、成本高、流程长等缺点;碱熔融法虽可分解几乎所有地质样品,但其处理后的溶液存在大量钠盐,需经进一步的纯化;酸分解法主要以高压密闭和卡洛斯管的消解方式为主,但受到样品性质的制约。而不同分离富集的手段都具有较强的针对性,如:吸附法多用于Au、Pt、Pd的富集,蒸馏法仅适用于Os、Ru的分析。由于贵金属元素具有颗粒效应强、赋存形式复杂多样以及超痕量等特殊性,需要针对样品的类型特点选择相适应的预处理方法。本文提出,应当在现有的贵金属分解方法基础上,结合当前新的实验设备及实验条件,寻求更加高效、快捷的分解技术,严格控制流程的本底及各个环节的污染问题,实现多技术、多方法联用,满足贵金属分析的要求。 相似文献
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Additional analytical data for the thirteen oxides usually determined in a rock analysis by wet methods and estimates and, conclusions from the analysis of variance are presented for the eight new USGS rock standards STM-1, RGM-1, QLO-1, SCo-1, MAG-1, SDC-1, BHVO-1 and SGR-1. The "single-solution" method of sample dissolution, and the "rapid methods" described by Shapiro were used. Three bottles of each standard were analyzed in duplicate, providing six replicate analyses of each sample. Relative standard deviations ranged from 0. 00 to 202 %, with only 12 of the possible 104 sample-oxide combinations exceeding 10 %. Most deviations exceeding 10 % occur with oxides at very low concentrations or with the determi-nation, of H2 O+ and CO2 , all of which often yield poor precision. These data indicate that the rapid wet chemical methods, except possibly for H2 O+ and CO2 , or when very low concentrations are present, can be considered reliable. Of the 104 F-ratios calculated during the analysis of variance for sample-oxide combinations, only eight equal or exceed the tabled value of 9. 55 for F0.95 (d. f. 2, 3). These data strongly support the conclusion that the contents of the bottles may be considered homogeneous for most oxides determined. When our data for an oxide in the several samples are plotted versus similar data in the USGS Prof. Paper 840 by several methods, the plots generally show good agreement for most sample-oxide combinations, but approximately thirty of the 104 show substantial differences, with no obvious correlation between the various methods used or the nature or magnitude of the differences. 相似文献
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《Journal of Geochemical Exploration》2005,85(2):81-98
Efficient exploration for new Au deposits is increasingly important as existing deposits become depleted. This is particularly relevant in Australia, where exploration can be difficult because of a thick regolith cover. New and effective methods of exploration need to be developed, and possibilities lie in geomicrobiological methods. For instance, Bacillus cereus, a common soil bacterium, has been shown to act as a biogeochemical indicator for concealed mineralisations, including vein-type Au deposits. We report the results of the first Australian case study of the association of B. cereus and Au at the Tomakin Park Gold Mine in southeastern New South Wales. Soil samples from the Ah horizon were analysed for B. cereus spores and 56 major and trace elements. The results show enrichment of Au, As, B. cereus spores and, to a lesser extent, Sb, Bi and Pb over the top of the Au deposit. Gold concentrations over the mineralisation range from 100 ppb to 1.1 ppm compared to a background of 2 ppb and As concentrations are enriched to 100 ppm from a background of 5 ppm. B. cereus spore counts were up to 10 times higher in soils with elevated concentrations of Au. Factor analysis indicates four main associations: TiO2+lanthanides+actinides; CaO+MgO+Cs+Be+Ba(+Ga+Pb+Rb); B. cereus+Au+As+Sb+Bi(+Pb); Fe2O3+MnO+Co+Ni+Cu+Mo. Selective sequential leaching was used to study the fractionation of Au and As in soils, other regolith materials and Au-bearing vein quartz to infer their mobility and bioavailability. In unweathered quartz vein material, the majority of the Au was extracted only in the strongest, final step, with aqua regia. However, in soils from the Ah horizon, 50% of the Au was present in the water-, ammonium acetate- and sodium pyrophosphate- and hydroxylamine hydrochloride-extractable fractions. In contrast, As displays little change in fractionation with an increasing degree of weathering, and is predominantly associated with the operationally defined Mn- and Fe-oxides and oxyhydroxides. These results indicate that: (i) Au is mobilised during the weathering of the host rock; (ii) Au is bioavailable in these soils; and (iii) the increase in B. cereus spores is likely to be linked to elevated concentrations of bioavailable Au in these soils. The results indicate also that an effective biogeochemical exploration technique may be developed, where B. cereus spore counts are measured in the field and used as a pre-screening method to target areas useful for further sampling and complete geochemical analysis. 相似文献
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A consistent pattern has been observed in the results obtained for Au in three soil and two porphyry copper ore samples serving as control reference standards in geochemical analyses. The mean reported by wet chemical methods (regardless of the measurement technique) was less than the mean by fire assay-based methods which, in turn, was less than the mean reported by laboratories using direct instrumental neutron activation analysis (INAA). These data have been obtained from 16 laboratories, some employing more than one method. Compared to INAA, values obtained for Au (at the 30–300 ppb level) using aqua regia (AR) dissolution were low by 24–42%, while those reported by fire assay-based methods were low by 14–26%.Studies of these samples and 32 rocks of widely varying composition revealed that the amount of Au remaining in the residue after AR attack ranged from 4% to 59% of the total. Gold dissolved by AR was determined by graphite furnace atomic absorption spectrometry (GFAAS) after extraction into MIBK (methyl isobutyl ketone), whereas Au remaining in the residue was determined by INAA. The slope of the line obtained by plotting Au by INAA vs. the sum of Au by AR/GFAAS and Au in the residue was not significantly different from 1.0.Modifications to the AR procedure such as prior attack by HCl or HF did not improve the recovery of Au in the three reference soils. However, reduction of sample size from 10 g to 1 g while maintaining the volume of AR at about 30 ml did increase results for Au. Furthermore, addition of HF in the attack on 1-g samples yielded results virtually identical to those obtained by INAA. It is thought that the poor extraction efficiency by AR is due to non-wetting of the larger sized sample, a lack of intimate, prolonged contact between the grains of the sample and the acid mixture and the presence of insoluble gangue surrounding Au particles. Constant agitation of the sample during evaporation with AR is desirable.The mean values obtained for Au in the soils by fire assay methods were not significantly different from the results by INAA (low by 14–19%); this was not the case for the two copper ore samples (low by 26%). This probably reflects the difficulties encountered in fire assay by high concentrations of Cu which hinder effective collection and separation of Au into the Pb button. However, the accuracy of the INAA method has not been established and is dependent upon measurement procedures and the degree of certainty associated with the Au values assumed for the reference materials employed for calibration. While estimation of precision does not present a problem, accuracy is difficult to assess in the absence of certified reference materials for Au at concentrations in the 10–300 ppb range. However, it is concluded that methods based upon AR dissolution can lead to low results, the magnitude being dependent upon the sample matrix and the mineralogical association of the Au present. 相似文献