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1.
岩石、土壤和水沉积物试样能够用氢氟酸、王水和氢溴酸——溴溶液分解。在两种氢溴酸浓度下,可采用二次MIBK(甲基异丁酮)萃取法自样品浸出液中萃取分离金、铊、铟和碲。金和铊首先从0.1M氢溴酸介质中萃取,然后在有抗坏血酸的情况下自3M氢溴酸介质中萃取钢和碲,以消除铁的干扰。随后可采用火焰原子吸收光谱法对各种元素进行测定。二次溶剂萃取法也可与电热原子吸收法一起使用,以降低地质物中料中四种金属的检出限。 金、铟、碲和铊在地质物料中含量极低。据估计,其在地壳中的丰度分别为:金0.001~0.0035ppm;铟0.11~0.14ppm;碲0.001ppm;铊0.3—1.3ppm。一种测定同一地质物料样品中所有四个元素含量的测试方法,在地化勘探中,能经济而快速地分析和检测岩石和风化产物中的矿物元素,并用其作为指示元素探明矿床的不同类型和研究元素的共生组合,因而具有特殊的优越性。 本文介绍的火焰原子吸收法,可提供一种相当迅速、简便的测定金、钢和碲的异常浓度(即比地壳丰度高许多)和铊的地壳丰度和异常浓度的方法。本法的特点是采用二次萃取,此时金和铊首先从0.1M氢溴酸的样品溶液中分离。然后铟和碲从3M氢溴酸介质中萃取,加抗坏血酸消除了铁的干扰。如采用电热原子吸收进行测定,四种元素的分析检出限还能相应地降低。  相似文献   

2.
铜精矿、镍精矿和锌精矿是金属硫化矿物,且为大宗进口商品,准确分析其中的稀散元素有利于矿物的综合利用。这类矿物中的稀散元素含量极低,各元素性质各异,尤其Ge和Se在湿法消解中由于挥发损失而无法准确定值,很难进行多种元素的同时测定,传统的方法需要通过预先分离富集,采用不同的仪器进行测定。本文以铜精矿、锌精矿和镍精矿为代表性硫化矿,采用微波消解对样品进行密闭前处理,电感耦合等离子体质谱法(ICP-MS)测定稀散元素含量,实现了多种元素的同时测定。条件实验表明在同时检测镓、锗、硒、镉、铟、碲、镧、铊的过程中,总固溶量、内标、质谱干扰消除的条件对三种金属硫化矿均一致,只是前处理过程中用酸的选择有些差异。硝酸-盐酸-氢氟酸-过氧化氢体系适合于测定镍精矿和锌精矿中的Ga、Ge、Se、Cd、In、Te、La、Tl和铜精矿中的Ga、Ge、Se、Cd、In、La、Tl,各元素的回收率在85.5%~116.6%之间;王水溶样法更适合测定铜精矿中的Te。  相似文献   

3.
研究了用钼酸铵浸渍处理石墨管、石墨炉原子吸比法测定镓、铟和铊的最挂条件。实验证明,采用硝酸—氢氟酸—硫酸体系溶解样品,涂钼石墨管直接测定样品中的镓、铟和铊,能有效地避免它们在原子化之前以氧化物形式挥发的损失,减少了测定干扰,提高测定的灵敏度。对6个地质标样的测定结果是满意的。木法对镓、铟和铊的检测下限分别为0.9×10 ̄(-11)g,1.7×10 ̄(-11)g和6.2×10 ̄(-11)g;相对标准偏差分别为1.4%、4.8%和3.0%。  相似文献   

4.
研究了用钼铵浸渍处理石墨管、石墨炉原子吸收法测定镓、铟和铊的最佳条件。实验证明,采用硝酸-氢氟酸-硫酸体系溶解样品,涂钼石墨直接测定样品中的镓、铟和铊,能有效地避免它们在原子化之前以氧化物形式挥发的损失。减少了测定干扰,提高测定的灵敏度。  相似文献   

5.
灰化酸溶-电感耦合等离子体质谱法测定煤炭中的镓锗铟   总被引:2,自引:2,他引:0  
准确测定煤炭中的镓、锗和铟为煤炭中稀散元素的地球化学勘查提供了重要依据,对稀散金属的综合利用具有重要的经济意义。采用现有的分析方法处理煤炭样品时,由于镓、锗和铟灰化温度不同,而锗的灰化条件严格,测定结果受灰化温度影响大,因此三元素不能同时进行前处理和测定。本文通过试验优化了煤炭中镓、锗、铟的最佳灰化温度为625℃;采用硝酸-硫酸-氢氟酸溶解灰分,8 mol/L硝酸进行复溶,避免了锗的挥发损失;通过优化仪器工作条件和干扰实验,以103Rh为内标元素,选择71Ga、74Ge和115In作为测定同位素,消除了各元素的干扰,建立了电感耦合等离子体质谱法同时测定煤炭中镓、锗和铟的分析方法。结果表明:镓、锗和铟的标准曲线线性相关系数均在0.9999以上,三元素检出限分别为0.004、0.003、0.002μg/L,精密度为1.17%~3.15%,加标回收率为96.6%~102.0%。应用本方法分析标准物质GBW07363、GBW07457和GBW07428的测定值与认定值相符。与传统的分光光度法和原子吸收光谱法比较,本方法操作更为简便快速,具有更低的测定下限,并且可以多元素同时测定。  相似文献   

6.
郑民奇 《岩矿测试》1986,(4):282-284
地质样品中微量铊的分析,常采用有机试剂萃取分离后,进行比色法测定,其分析手续较繁、灵敏度低。近年来,随着原子吸收分析技术的发展,使用石墨炉原子吸收法测定痕量铊已有报导,也有用钒作为基体改进剂测定矿石中痕量镓、铟、铊。本文提出在盐酸-碘化钾-抗坏血酸介质中,用甲基异丁基甲酮(MJBK)萃取铊,不加基体改进剂,直接用自制的简易石墨炉平台测定有机相中的铊。  相似文献   

7.
报道了用HF—HNO3—HClO4分解样品,以^103Rh为内标元素,采用电感耦合等离子体质谱法直接同时测定地球化学样品中痕量镓、铟、铊的方法。方法检出限(6s)Ga、In、Tl分别为0.059、0.002、0.004μg/g,方法精密度(RSD,n=12)为2.6%—5.3%。用国家一级标准物质进行验证,测定结果与标准值吻合。  相似文献   

8.
稀散元素也称分散元素,是指在地壳中丰度很低(多为10?9级)、且在岩石中极为分散的元素,包括镉(Cd)、锗(Ge)、镓(Ga)、铟(In)、铊(Tl)、硒(Se)、碲(Te)和铼(Re)等八种元素(涂光炽等,2003)。铊(Tl)是一种典型稀散元素,也是一种剧毒元素。铊的地壳丰度为0.45×10?6(温汉捷等,2020),主要以“稀”、“伴”、“细”特征共伴生于其他矿床中(陈骏,2019;温汉捷等,2019;翟明国等,2019;侯增谦等,2020;胡瑞忠等,2020)。  相似文献   

9.
铊和铟均属稀散元素,丰度值低(T10.48 ppm;In 0.1ppm常与硫化矿物伴生。近年来,化探工作者发现,铊和铟可作为寻找金和硫化物矿床的重要指示元素。由于铊和铟在硫化物中含量甚微,因此,若要提高利用其寻找金和硫化物的成功率,必须发展铊和铟的高灵敏的试测方法。  相似文献   

10.
MIBK-HBr体系萃取分光光度法测定镓铟铊   总被引:1,自引:0,他引:1  
萃取分离测定同一样品中镓、铟和铊的工作,国内外近年来都有研究。本文在A.E.HuberT等工作的基础上提出,在氢溴酸介质中,以甲基异丁基甲酮(MIBK)为萃取剂,甲苯为稀释剂,调节水相酸度,分步萃取,有机相直接显色分光光度法测定同一样品浸提液中镓、铟和铊。该方法的特点是分步萃取后,有机相既不经反萃取也不经蒸干,直接用分光光度法进行测定,具有简便,准确的优点并成功地应用于矿样分析。 实验 1.仪器及试剂 721分光光度计(上海第三分析仪器厂) 氢溴酸 分析纯40%约为7mol/L(用时可进行标定)。  相似文献   

11.
山西平朔安太堡露天矿9号煤层中的微量元素   总被引:12,自引:0,他引:12       下载免费PDF全文
庄新国  曾荣树 《地球科学》1998,23(6):583-588
使用ICP-AES方法对安太堡露天矿9号煤层中的微量元素进行了系统测定,检测出53种微量元素,将研究煤样的平均微量元素质量分数与世界范围微量元素平均质量分数相比较,煤样中Li,Ga,Sr,Zr,Nb,Sn和Ta具有较高的富集,而Cr,Co,Ni,Ge,Rb,Y,Cs和Ba具有较低的富集,研究资料表明不同微量元素在垂向剖面上其质量分数具有不同的分布特征。经相关分析表明:(1)与镜质组含量相关的元素有  相似文献   

12.
熊英  吴赫  王龙山 《岩矿测试》2011,30(1):7-11
对电感耦合等离子体质谱法同时测定铜矿石、铅矿石和锌矿石中镓、铟、铊、钨和钼量时,基体效应和主量元素铜、铅、锌对测量的干扰情况及可能的消除方法进行试验,结果表明,溶液中共存小于200μg/mL锌对上述微量元素的测量没有干扰;溶液中共存大于50μg/mL的铜对镓、铟、铊、钨、钼的测量有负干扰,共存大于100μg/mL铅对钨的测量有正干扰,对钼的测量有负干扰,采用钪、铼、镧混合内标或基体匹配可以消除这些干扰;溶液中共存大于20μg/mL的铅对铊的测量有正干扰,选择203Tl为测量质量数,可使耐受铅的干扰浓度提高到50μg/mL,铅对铊测量的干扰可以采用校正系数法或基体匹配进行校正或消除。  相似文献   

13.
A suite of elements(Ag,Au,Ba,Bi,Cd,Co,Cr,Cu,Ga,Hf,Hg,Mn,Mo,Ni,Pb,Rb,Sb,Se, Sr,Te and Zn),total organic carbon(TOC)and pH were analyzed in stream sediment and tailing samples from Um Shashoba area,in order to evaluate Au placer and the sediments being impacted by old mining activities.Analytical results were examined using statistical,graphical and mapping methods.In spite of the results revealing that Au and most of the elements in sediments were in general significantly lower than those in tailing,Au wa...  相似文献   

14.
With the aim of better understanding geochemistry of coal, 71 Late Permian whole-seam coal channel samples from western Guizhou Province, Southwest China were studied and 57 elements in them were determined. The contents of Al, Ca, Co, Cr, Cu, Fe, Ga, Hf, K, Li, Mn, Mo, Nb, Ni, Sn, Ta, Ti, Th, U, V, Zr, and REEs in the Late Permian coals from western Guizhou Province are higher than the arithmetic means for the corresponding elements in the US coals, whereas As, Ba, Br, F, Hg, P, Se, and Tl are lower. Compared to common Chinese coals, the contents of Co, Cr, Cu, Ga, Hf, Li, Mn, Mo, Ni, Sc, Sn, Ti, U, V, Zn, and Zr in western Guizhou coals are higher, and As, F, Hg, Rb, Sb, Tl, and W are lower. Five groups of elements may be classified according to their mode of occurrence in coal: The first two, Group A, Tm–Yb–Lu–Y–Er–Ho–Dy–Tb–Ce–La–Nd–Pr–Gd–Sm, and Group B, As–Sr–K–Rb–Ba–F–Ash–Si–Sn–Ga–Hf–Al–Ta–Zr–Be–Th–Na, have high positive correlation coefficients with ash yield and they show mainly inorganic affinity. Some elements from Group B, such as Ba, Be, Ga, Hf, and Th, are also characterized by significant aluminosilicate affinity. In addition, arsenic also exhibits high sulfide affinity (rS–Fe>0.5). The elements, which have negative or lower positive correlation coefficients with ash yield (with exceptions of Bi, Cs, Nb, Mn, Se, and Ti), are grouped in other four associations: Group C, Cr–V–Mo–U–Cd–Tl; Group D, Hg–Li–Sc–Ti–Eu–Nb–Cs–W; Group E, Bi–Sb; and Group F, Co–Ni–Cu–Pb–Zn–Mg–Se–Ca–Mn–S–Fe. The correlation coefficients of some elements, including Co, Cr, Cu, Fe, Hg, Li, Mo, Ni, P, S, Sc, U, V, and Zn, with ash yield are below the statistically significant value. Only Cr and Cu are negatively correlated to ash yield (−0.07 and −0.01, respectively), showing intermediate (organic and inorganic) affinity. Manganese and Fe are characterized by carbonate affinity probably due to high content of epigenetic veined ankerite in some coals. Phosphorus has low correlation coefficients with any other elements and is not included in these six associations. There are five possible genetic types of enrichment of elements in coal from western Guizhou Province: source rock, volcanic ash, low-temperature hydrothermal fluid, groundwater, and magmatic hydrothermal inputs.  相似文献   

15.
Mass fractions of S, Cu, Se, Mo, Ag, Cd, In, Te, Ba, Sm, W and Tl were determined by isotope dilution sector field ICP‐MS in the same sample aliquot of reference materials using HF‐HNO3 digestion in PFA beakers in pressure bombs and glassy carbon vessels in a high‐pressure asher (HPA‐S) for comparison. Additionally, Bi was determined by internal standardisation relative to Tl. Because isobaric and oxide interferences pose problems for many of these elements, efficient chromatographic separation methods in combination with an Aridus desolvator were employed to minimise interference effects. Repeated digestion and measurement of geological reference materials (BHVO‐1, BHVO‐2, SCo‐1, MAG‐1, MRG‐1 and UB‐N) gave results with < 5% relative intermediate precision (1s) for most elements, except Bi. Replicates of NIST SRM 612 glass digested on a hot plate were analysed by the same methods, and the results agree with reference values mostly within 2% relative deviation. Data for the carbonaceous chondrites Allende, Murchison, Orgueil and Ivuna are also reported. Digestion in a HPA‐S was as efficient as in pressure bombs, but some elements displayed higher blank levels following HPA‐S treatment. Pressure bomb digestion yielded precise data for volatile S, Se and Te, but may result in high blanks for W.  相似文献   

16.
The water quality of the Vacacaí River was assessed at different sites in the period between winter 2005 and autumn 2006. All samples were analyzed for 52 elements (Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Th, Li, Be, Mg, Al, Ca, V, Cr, Mn, Fe, Ni, Co, Cu, Zn, Ga, As, Se, Rb, Sr, Ag, Cd, In, Cs, Ba, Tl, Pb, Bi, U, Na, K, Hg, B, Mo, Sn, Te, Ti), temperature, pH, ammonia, and alkalinity levels. Water from the Vacacaí River ranged from slightly acidic to alkaline. No difference was observed in the chemical composition at different sites of the Vacacaí River. Levels of Ba, Ca, Sr and Mg increase in the dry seasons and reach their highest concentrations in autumn; Be and U decrease in the dry season and reach their highest concentration in spring. Al, Fe, Cr, Ni, Th, U Mn, Ca and Mg are highly positively related, indicating a common origin. Se and Cu are probably from anthropogenic source, from the rice crops of the margins of the river. Waterborne Al and Fe levels were above the desirable level for drinking water at all sites during all seasons. These results demonstrate the need for constant monitoring of water parameters, which is crucial to ensure water quality for the population of this region.  相似文献   

17.
以河北开滦矿区晚古生代煤及其洗选产品为例,运用电感耦合等离子体质谱 (ICP-MS)和冷原子吸收光谱 (CV-AAS)方法对煤中主要微量有害元素 (包括 Be、 Cr、 Co、 Ni、 Cu、 Zn、 Ga、 As、 Se、 Mo、 Tl、 Pb、 Th、 U和 Hg)的含量及其在洗选过程中的迁移和分配特征进行了研究.通过对开滦矿区 10个矿井 47个煤层刻槽样品主要有害微量元素含量的统计,发现开滦矿区晚古生代煤中 Cr、 Ni、 Cu、 Zn、 Pb和 As富集.通过对原煤精煤中煤尾煤煤泥两套系列样品的分析,发现主要有害微量元素在精煤中都有不同程度的脱除,中煤中相对富集的元素有 Se和 Th,明显被脱除的元素有 Co和 Tl.除 Tl以外,尾煤中主要微量有害元素均有不同程度的富集,以 As的富集率最高,可达 34.4%, Hg的富集率最低,为 1.1%.煤泥中所有微量有害元素均相对富集,以 Hg的相对富集率最高,达 78.4%.因此,如果对尾煤和煤泥加以利用,需要特别关注 As和 Hg等微量有害元素对环境的影响.主要微量有害元素在洗选过程中的分配行为主要受控于它在煤中的赋存状态.  相似文献   

18.
By R-mode factor analysis and enrichment factor calculations, most of the elements in abyssal ferromanganese nodules and associated pelagic sediments (excluding common authigenic minerals like apatite, barite, opal and carbonates) are found to be preferentially concentrated in one of the following three major phases: aluminosilicates (e.g., Al, Si, Sc, Ga, Cr, Be, Na, K, Rb and Cs), Fe-oxides (e.g., Fe, P, S, V, Se, Te, As, B, Sn, U, Hg, Pb, Ti, Ge, Y, Zr, Nb, Pd, In, rare-earths, Hf, Th, Pa, Pu, Am, Ru and Bi), and Mn-oxides (e.g., Mn, Tl, Ag, Cd, Mg, Ca, Ba, Ra, Co, Ni, Cu, Zn, Mo, Sb and probably W). The specific association of elements with these three phases can be explained by the difference in chemical forms of elements in seawater and by fundamental differences in physicochemical properties (e.g., the pH of zero point of charge and dieletric constant) of these three phases.  相似文献   

19.
We used neutron activation analysis to determine ten trace elements retained in Abee (E4) samples heated at 400–1000°C for 1 week in a low-pressure (initially ~ 10?5atm H2) environment. Eight elements generally are lost progressively with increasing temperature although gas(es) evolved from the samples apparently affect retention of some elements. In the extreme, ‘open-system’ losses are: Se—23%, Cs—40%; Te—87%; Ag, Bi, In, Tl, Zn— ≥93%. Under these conditions Co is not lost; Ga is lost only at 1000°C. At 900°C elements are lost from Abee chips in the same relative order as from Abee powder but the loss is somewhat less facile. Three of the most mobile elements—Bi, In, Tl—are lost more readily from Abee than from Allende (C3), the only other primitive chondrite studied to date. Assuming that elemental loss is a kinetic process involving mobilization from spherical grains, Bi, In, Se, Tl and Zn have different activation energies at high and low temperatures either because each element was originally present in two different sites or each has more than one loss mechanism (diffusion or desorption) in different temperature ranges.Comparison of elemental abundance patterns, patterns of statistically-significant correlations, factor analysis results and two-element correlation diagrams indicate strong similarities between heated Abee and ‘as-received’ enstatite chondrites for mobile elements. These results are consistent with a two-stage evolutionary model for enstatite chondrites involving condensation of cosmochemically fractionated primitive nebular material and subsequent loss of mobile elements from parent material by metamorphism.  相似文献   

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