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1.
高级变质岩中Zr、Hf、Nb、Ta的ICP-MS准确分析 总被引：15，自引：0，他引：15
采用高压密闭溶样ICP－MS研究了片麻岩、榴辉岩等高级变质岩中Nb、Ta、Zr、Hf准确分析方法。实验表明：在温度为190℃时,溶样时间大于36h,Nb、Ta、Zr、Hf可完全溶解,而获得准确的分析结果。但Nb、Ta在稀硝酸介质中的不稳定性会导致分析结果的误差,采用0．1％HF介质的“F^-基体”匹配,可保持Nb、Ta长时间的稳定性。所建立的高压密闭溶样ICP－MS分析方法用于苏鲁－大别地区片麻岩、榴辉岩等高级变质岩的分析,经与XRF及碱熔融ICP－MS方法对比,分析结果具有良好的一致性。 相似文献
2.
BPR螯合树脂分离偶氮胂Ⅲ光度法测定岩石中微量锆（铪） 总被引：2，自引：0，他引：2
在酒石酸介质中,BPR螯合树脂可选择性地吸附Zr、Hf、Nb、Ta而与岩石中常见的伴生元素如Fe、Al、Ca、Mg、Cu、Pb、Cd、Co等以及U、Th、Sc等微量元素分离。Zr、Hf、Nb、Ta均可被2-4mol/LHCI溶液洗脱。在此基础上提出了一个测定岩石中微量Zr(Hf)的新方法。 相似文献
3.
封闭压力酸溶-盐酸提取-电感耦合等离子体质谱法测定地质样品中的多元素 总被引：10，自引：8，他引：2
高温、高压封闭压力酸溶可有效分解岩石、土壤、沉积物等地质样品,采用电感耦合等离子体质谱法(ICP-MS)进行测定,大部分元素可得到满意的回收率;但Zr、Hf、REEs、Rb、Th、U等元素用硝酸复溶困难,测定结果不准确。本文对传统的封闭压力酸溶方法进行改进,用盐酸复溶提取代替硝酸复溶提取,ICP-MS法测定岩石、土壤、沉积物等国家一级标准物质中Li、Be、Cr、Mn、Co、Ni、Cu、Zn、Ga、Rb、Sr、Mo、Cd、In、Cs、Ba、Ti、Zr、Nb、Sn、Sb、W、Hf、Ta、Tl、Pb、Bi、Th、U以及稀土元素(REEs)等46个元素。将原方法中的称样量25 mg加大至100 mg,溶样时间由12 h延长至48 h,有效地解决了取样代表性及HNO3复溶提取时Rb、Sr、REEs等元素测定结果偏低的问题。分析结果表明,除元素As和V在电感耦合等离子体质谱测定中存在Cl的干扰不能准确测定之外,其他44个元素的测定值与标准值基本一致。改进后的方法测定下限为0.01～0.85μg/g,精密度(RSD,n=10)为0.73%～13.1%,准确度小于<10%。方法准确、可靠,适用于各种不同种类地质样品的分析。 相似文献
4.
等离子体质谱法测定岩石中的锆、铪、铌、钽 总被引：8，自引：0，他引：8
本文建立了用HF、HNO3 在高压釜内溶解样品 ,准确测定花岗岩样品中Nb、Ta、Zr、Hf的ICP MS分析方法。分析结果与推荐值的偏差在 5 %以内。该方法具有简单、准确、测定元素多的特点。本文还对高压釜酸溶和碱熔方法进行了对比实验。 相似文献
5.
本方法系利用热化学试剂CdCl_2 AgCl在室电极内与岩石中的难挥发元素Nb、Ta、W、Hf发生化学反应,形成易挥发氯化物的办法,使这些元素的直接测定下限降低到ppm级(Nb、W—5ppm;Ta、Hf—8ppm)。测定的相对标准偏差,当浓度为50ppm时,不超过9％。鉴于Nb、Ta、Hf的矿物较其氧化物更难于被氯化的事实,标准样品应采用有正确分析结果的天然样品。 相似文献
6.
地质样品中多种元素的分析,通常采用高压密封消解电感耦合等离子体质谱法(ICP-MS),而应用于测定地球化学样品中的V、Cr、Ni、Ge、As等元素,影响分析准确度的主要原因有:样品前处理方面,高压密封罐会释放Cr和Ni污染样品,同时Ge和As属于易挥发元素容易造成损失;质谱测定方面,多原子分子离子会产生干扰。本文针对两方面的干扰因素,对比了微波消解硝酸提取、微波消解王水提取、高压密封硝酸复溶、高压密封王水复溶四种前处理方法中待测元素的溶出效果以及污染或损失情况。结果表明,采用微波消解替代高压密封罐消解可消除引入的Cr、Ni污染,避免了Ge、As挥发损失,同时微波消解的时间短。而采用硝酸提取,由于避免了氯的引入,分析效果优于王水提取。且使用八极杆ICP-MS氦气碰撞模式消除了样品基体中的氯多原子分子离子干扰(如37Cl14N对51V干扰,35Cl16OH对52Cr干扰,35Cl37Cl对72Ge干扰以及40Ar35Cl对75As干扰等)。应用微波消解硝酸提取、ICP-MS测定岩石、水系沉积物和土壤国家标准物质,V、Cr、Ni、Ge、As的检出限分别为1.09、0.19、0.55、0.02、0.50μg/g,精密度(RSD)4%,而采用高压密封消解、ICPMS测定V、Cr、Ni的检出限为3.48、13.09、21.67μg/g(Ge和As由于挥发无法用此法检测)。运用微波消解硝酸提取-ICP-MS氦气碰撞模式测定地球化学样品中V、Cr、Ni、Ge、As,简化了分析流程,样品消解时间仅2 h,相比于高压密封方法(消解时间48 h)具有消解快速、多元素同时测定、检出限低的特点。 相似文献
7.
AG MP-1阴离子交换树脂元素分离方法再研究 总被引：2，自引：0，他引：2
目前不同实验室建立的用于MC-ICP-MS铜铁锌同位素测定的离子交换分离方法多适用于一般地质样品的Fe同位素高精度测定,而对于一些类似于白云鄂博Fe-Nb-REE矿床的特殊地质样品,这些分离方法的适用情况有待进一步研究。为研究REE、Nb、Ta、Co、Cu、W等元素是否能够和Fe有效分离,采用AG MP-1阴离子交换树脂,依次以6mol/L HCl和2 mol/L HCl为介质对这些元素进行淋洗,并利用ICP-AES和ICP-MS对淋洗液中的各元素含量进行测定。实验结果表明,在6 mol/L HCl介质条件下,运用AG MP-1树脂可以将REE、W与Fe有效地分离,能够将Nb、Ta的含量降低一个数量级;Fe、Co、Cu的淋洗行为和前人研究结果一致。 相似文献
8.
利用多接收电感耦合等离子体质谱仪测定Mg同位素比值时,样品溶液中的基质元素可影响Mg同位素比值的准确测定。根据白云鄂博样品富含REE、Nb、Fe(REE质量分数可达10%、Nb质量分数可达0.1%)等元素的特性,本研究在评估测试溶液中Nd(REE)、Mn元素质量比对Mg同位素比值影响的基础上,建立了适用于富含REE、Nb、Fe等元素的特殊样品中Mg同位素的化学纯化方法。研究表明,当m(Nd)/m(Mg)>0.2、m(Mn)/m(Mg)>0.2时,REE和Mn的存在明显影响Mg同位素测定值的准确性,应予以去除。所建纯化方法首先是利用AG MP-1阴离子交换树脂,以10mol/L HCl+0.001%H2O2溶液为上样介质和淋洗液,接取前2.5mL淋洗液,去除样品中Fe、Mn等杂质元素;然后利用AG50W-X12阳离子交换树脂,以2mol/L HCl为上样介质和淋洗液,去除REE、Nb等杂质元素。所建方法满足多接收器等离子体质谱进行高REE-Nb-Fe-Mn样品中Mg同位素测定的要求。 相似文献
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10.
ICP-AES由于具有灵敏度高、稳定性好、线性范围宽、化学干扰少、多元素同时测定等优点，已成为地球化学探矿的重要手段之一。但提升量和雾化效率方面受到溶液含盐量高及碱性溶液粘度大等因素的影响。因此，通常用硝酸、高氯酸分解试样用氢氟酸挥发除去大量硅后测定其他元素。锆属难溶元素，酸溶不能充分分解。故要测定硅和锆，不得不采用其他的分解手段。 相似文献
11.
Significance of Nb/Ta as an indicator of geochemical processes in the crust-mantle system 总被引：89，自引：0，他引：89
Trevor H. Green 《Chemical Geology》1995,120(3-4):347-359
A mantle value of 17.5 for Nb/Ta appears well established; less well established are crustal values of 11–12, although it appears that Nb/Ta for crustal-derived melts is less than mantle Nb/Ta, demonstrating fractionation of these two elements during crustal evolution, and suggesting that Nb/Ta variation may be indicative of a particular chemical process within the crust-mantle system.
Experimental studies on silicate and carbonatitic liquids at high pressure indicate that, although silicate minerals such as garnet, amphibole and clinopyroxene do fractionate Nb and Ta, the partition coefficients (D's) for both elements are very low. Thus involvement of these minerals may explain relatively small changes in Nb/Ta, but appears inadequate to explain the crust-mantle variation. However, high-quality data for Nb, Ta may be used to provide information on mantle melting or metasomatic processes (e.g., amphibole in the source region decreases Nb/Ta in derived melts, while carbonatitic metasomatism will increase Nb/Ta in affected mantle). Titanate minerals have high D's for Nb and Ta, and do fractionate these elements (e.g., DNb/DTa rutile/liquid of 0.5–0.8), and their involvement in crystal fractionation would increase Nb/Ta in derivative liquids. In contrast, DNb/DTa for rutile/fluid is 1.25, so that rocks affected by fluid equilibrated with residual rutile will show a decrease in Nb/Ta
Some Archaean gneisses appear to have high Nb/Ta, and may be a complementary component to that part of the crust which has a relatively low Nb/Ta, such as crustal-derived magmas (e.g., A- ad I-type granites and silicic volcanics). Within the crustal system pegmatites are known to have extremely high and variable Nb, Ta contents, often with low Nb/Ta. A fluid is generally considered to be involved in the generation of these rocks. Thus it is possible that fluid/melt partitioning may be the key to fractionating Nb and Ta, with preference for Ta in the fluid, and enrichment of Ta relative to Nb into the mid-upper crustal system, as the crust evolved, through upward movement of fluid. 相似文献
12.
Nb,Ta的硅酸盐地球质量不平衡问题争论由来已久,备受关注。近年来研究发现,含金红石的榴辉岩Nb/Ta往往高于球粒陨石值(Nb/Ta=17.5),暗示其可能是平衡地球Nb亏损的独立储库。而洋壳玄武岩部分熔融实验表明Ta比Nb更倾向进入金红石晶格,这意味着作为俯冲洋壳部分熔融残留相的榴辉岩Nb/Ta不可能高于原岩。为了解释地质观察和实验结果之间的矛盾,系统分析了中国大陆科学钻探工程(CCSD)主孔、先导孔及附近地表榴辉岩的矿物微量元素。结果发现:榴辉岩中的Nb,Ta主要存在于金红石之中,其他矿物中含量极少;Nb,Ta之间存在着强烈分异(Nb/Ta=5.3～96.2),并总体上具有超球粒陨石的特征;韭闪石和多硅白云母的Nb/Ta平均分别为48.6,21.8,显示了很强的Nb,Ta分异能力;其他矿物如石榴石、绿辉石、绿帘石、磷灰石等的Nb、Ta含量及Nb/Ta都很低,对Nb-Ta分异不造成影响。认为导致Nb-Ta分异的不是金红石,而应出现在洋壳俯冲过程中金红石相出现之前的脱水和部分熔融阶段。富含Ti的角闪石(韭闪石)和白云母可能对Nb-Ta分异起到了决定性的作用。等金红石相出现之后,由于其对Nb,Ta的绝对控制作用,此前阶段的分异结果便被固定在金红石中而继承下来。因此,含金红石的榴辉岩常常表现出超球粒陨石Nb/Ta的特征,与金红石不能有效地分异Na,Ta的实验结果之间并不矛盾。在不均匀的上地幔中含金红石的榴辉岩是可能的超球粒陨石Nb/Ta储库之一。 相似文献
13.
HFSE systematics of rutile-bearing eclogites: New insights into subduction zone processes and implications for the earth’s HFSE budget 总被引：1，自引：0，他引：1
The depleted mantle and the continental crust are generally thought to balance the budget of refractory and lithophile elements of the Bulk Silicate Earth (BSE), resulting in complementary trace element patterns. However, the two high field strength elements (HFSE) niobium and tantalum appear to contradict this mass balance. All reservoirs of the silicate Earth exhibit subchondritic Nb/Ta ratios, possibly as a result of Nb depletion.In this study a series of nineteen orogenic MORB-type eclogites from different localities was analyzed to determine their HFSE concentrations and to contribute to the question of whether subducted oceanic crust could form a hidden reservoir to account for the mass imbalance of Nb/Ta between BSE and the chondritic reservoir. Concentrations of HFSE were analyzed with isotope dilution (ID) techniques. Additionally, LA-ICPMS analyses of clinopyroxene, garnet and rutile have been performed. Rutile is by far the major host for Nb and Ta in all analyzed eclogites. However, many rutiles revealed zoning in Nb/Ta ratios, with cores being higher than rims. Accordingly, in situ analyses of rutiles have to be evaluated carefully and rutile cores do not necessarily reflect a bulk rock Nb and Ta composition, although over 90% of these elements reside in rutile.The HFSE concentration data in bulk rocks show that the orogenic eclogites have subchondritic Nb/Ta ratios and near chondritic Zr/Hf ratios. The investigated eclogites show neither enrichment of Nb compared to similarly incompatible elements (e.g. La), nor fractionation of Nb/Ta ratios relative to MOR-basalts, the likely precursor of these rocks. This indicates that during the conversion of the oceanic crust to eclogites in most cases, (1) HFSE and REE have similar mobility on average, possibly because both element groups remain in the down going slab, and (2) no significant fractionation of Nb/Ta occurs in subducted oceanic crust. With an average Nb/Ta ratio of 14.2 ± 1.4 (2s.e.), the investigated eclogites cannot balance the differences between BSE and chondrite. Additionally, as their average Nb/Ta is indistinguishable from the Nb/Ta of MORB, they are also an unlikely candidate to balance the potentially small differences in Nb/Ta between the continental crust and the mantle. 相似文献
14.
In order to improve the geochemical research degree of Nb and Ta deposits in Nianzishan area, the authors conducted 1:10 000 soil geochemical survey to comprehensively analyze the characteristics of geochemical element content, single element exception and comprehensive anomaly in the study area. The results show that Nb, Ta and other elements in Nizishan area belong to high background field and are unevenly distributed in the soil, which may result in the local enrichment of ore deposits. By R-type clustering analysis, these 18 elements were divided into three groups of precious and non-ferrous metal elements, rare and rare earth elements, and dispersed elements, which reflects the clustering and combination characteristics of normal granite elements, indicating that Nb and Ta minerals are closely related to granite bodies. In the study area, 521 single element anomalies and 12 composite anomalies were identified. Among these anomalies, three composite anomalies, Nian-2012-Ht-2, Nian -2012-Ht-7 and Nian -2012-Ht-11, were the key anomalies with great metallogenic potential. Three low-grade Nb and Ta ore bodies and 11 Nb and Ta mineralized bodies were found in the Early Cretaceous alkaline granite and syenogranite after trenching and drilling engineering verification. 相似文献
15.
为提高碾子山地区铌、钽矿的地球化学特征研究程度,通过1:1 万土壤地球化学测量,对区内地球化学元素含量特征、单元素异常特征、综合异常特征等进行研究分析。结果表明: 碾子山地区Nb、Ta等元素在研究区位于高背景场,在土壤中分布不均,存在局部富集成矿的可能; R型聚类分析将18种元素分为贵金属、有色金属元素,稀有、稀土元素和分散元素3组,显示为正长花岗岩体元素聚类组合特征,表明铌、钽矿与花岗岩体关系密切; 研究区共圈出土壤单元素异常521处,综合异常12处,其中碾-2012-Ht-2、碾-2012-Ht-7和碾-2012-Ht-11 3处综合异常为重点异常,成矿潜力较大。经槽探及钻探工程验证,共发现铌、钽低品位矿体3条,铌、钽矿化体11条,呈脉状分布于早白垩世碱性花岗岩、正长花岗岩中。 相似文献
16.
George Pavlovich Zaraisky Valentina Korzhinskaya Nataliya Kotova 《Mineralogy and Petrology》2010,99(3-4):287-300
It is well established that the fractionation of Li–F granitic magmas at depth leads to the accumulation of flux elements such as F and Li, and metal cations such as Ta and Nb in residual melts. However, it remains to be determined whether magmatic fractionation is sufficient to concentrate Nb and Ta into economically significant quantities, and what role hydrothermal–metasomatic processes play in the formation of such ore deposits. In the literature, reliable data about the solubility of Ta and Nb in hydrothermal solutions is missing or incomplete. This study provides a quantitative experimental estimation of the possible contribution from hydrothermal processes in Ta enrichment in cupolas of albitized and greisenized Li–F granite. Experimental studies of Ta2O5 and columbite–tantalite (Mn,Fe)(Nb,Ta)2O6 solubility were carried out in fluoride solutions consisting of HF, NaF, KF, and LiF. At low fluoride concentrations (0.01 and 0.1 m), Ta2O5 solubility at 550°C and 100 MPa under Co–CoO oxidizing conditions is low (near 10?5–10?4 m) in all fluoride solutions (HF, NaF, KF, LiF). At high fluoride concentrations (1 and 2 m) the highest Ta2O5 concentrations (10?1 m) were detected in HF solutions. In KF, NaF, and LiF solutions, the Ta2O5 solubility is also high (10?3–10?2 m). The dependence of columbite–tantalite (Nb2O5-59 wt. %, Ta2O5-18 wt. %) solubility as a function of solution composition, T, and P has also been investigated. Tantalum and Nb concentrations have the highest values in HF solutions at reduced conditions (up to 10?3 to 10?2 m Ta in 1 m HF). In 1 m NaF solutions, the concentrations of Nb and Ta are, respectively, 2.5 and 3 orders of magnitude less than those in the 1 m HF solutions. Solubility of Ta and Nb in KF solutions has intermediate values. It is established that in NaF and KF solutions the dependence of solubility on pressure is distinctly negative. The Nb and Ta contents increase with increasing concentrations of HF and KF in solution, however, they do not change with increasing NaF concentration. In NaHCO3, Na2CO3, and HCl solutions columbite–tantalite solubility is low. Even in 1 m chloride solutions the content is within the limits of 10?5 m for Nb and 10?6 to 10?8 m for Ta. We conclude that hydrothermal transport of Ta and Nb is possible only in concentrated fluoride solutions. 相似文献
17.
Statistical data on major, trace and rare-earth elements in wolframite from the quartz vein-and greisen-type tin deposits
in the Dupangling orefield reveal: (1) The components in wolframite can be divided into two relatively independent groups:
the WO3-Nb-Ta-Sc-REE group, in which WO3 is negatively correlated with the others and the FeO-MnO-Sn group, in which MnO is negatively correlated with the other two;
(2) In general, REE fractionation is not significant, reflected mainly by the separation of Eu from other REE’s. LREE and
HREE increase or decrease simultaneously, with HREE being more variable; (3) Nb, Ta, Sc, REE substitute for W, and Sn may
enter into wolframite lattice accompanied by Fe-Mn substitution; (4) In contrast to wolframite in quartz veins, which is poor
in REE, Nb, Ta and Sc and has highδ Eu values and LREE / HREE and Nb/Ta ratios, wolframite in greisen is rich in REE, Nb, Ta, Sc and has lowδ Eu values and LREE/HREE and Nb/Ta ratios; and (5) The contents and ratios of trace elements and REE partitioning parameters
of wolframite can be used as guide for prospecting. 相似文献
18.
铌、钽在氢氟酸介质中能够形成稳定的溶液,使用耐氢氟酸进样系统的电感耦合等离子体发射光谱(ICP-OES)有利于提高分析的准确性。本文采用模块化的小罐型、多罐体组合(70罐/组)酸溶罐体的微波消解溶样模式,结合ICP-OES仪器的耐氢氟酸进样系统,建立了测定铌钽矿中铌、钽的分析方法。本方法加快了酸溶的溶样速度,溶样时间从原来的48 h减少至1 h,且在氢氟酸介质中测定,避免了高含量铌、钽在低酸度介质中容易水解的影响。方法检出限为铌5.58 μg/g,钽5.87 μg/g。本方法应用于测定铌钽精矿(19%Nb2O5,27%Ta2O5)的分析结果与碱熔方法一致,能够测定Nb2O5含量在42 μg/g~19%和Ta2O5含量在86 μg/g~27%高低品位的铌钽矿,尤其对于铌、钽在百分含量以上的铌钽矿具有优势。 相似文献
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20.
Scheelite and rutile from several metaturbidite-hosted gold-bearing quartz vein deposits of the Meguma Terrane of Nova Scotia were analyzed for trace elements including rare earth elements, niobium and tantalum. Scheelites have high concentrations of Sr, Nb, Y and rare earth elements (REE) with bell-shaped chondrite-normalized REE patterns accompanied by both positive and negative Eu anomalies. They also have high Nb/Ta ratios (80–300). Three distinct trace element types of the scheelites are interpreted to reflect chemical differences in the pulses of hydrothermal fluids. Hydrothermal rutiles have high contents of W (up to 4.2 wt.% WO3), are rich in Ta compared to Nb and have a very low Nb/Ta ratio (~0.3). Hydrothermal fluids which produced both scheelite with a high Nb/Ta and rutile with a low Nb/Ta ratio are an efficient medium for fractionation of this ratio although these two minerals play an important role during the process. 相似文献