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1.
锆和铪的化学性质非常相似,要用简便方法分离这两个元素是困难的,用化学方法测定微量锆和铪也是困难的。Kouimtzis和Brookes曾经在这方面做了一些工作,在他们工作的基础上,我们确立了实验条件并应用于化探标些中锆、铪的测定。 相似文献
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3.
锆和铪的化学性质非常相似,要用简便方法分离这两个元素是困难的,用化学方法测定微量锆和铪也是困难的。Kouimtzis和Brookes曾经在这方面做了一些工作,在他们工作的基础上,我们确立了实验条件并应用于化探标些中锆、铪的测定。 实验部分 (一)仪器和试剂 相似文献
4.
本文介绍了一种快速离子交换分离—ICP-AES法同时测定岩石中微量锆、铪、铌和钽等元素的新方法。样品经碱熔、浸取、过滤,其沉淀连同滤纸放回原烧杯,加入H~+型阳离子交换树脂和少量酒石酸溶液。基体元素(Fe~(3+),Al~(3+),Ca~(2+),Mg~(2+)等)被树脂吸附,锆、铪、铌和钽与酒石酸形成稳定络合物存留在溶液中,经干过滤后,用ICP-AES方法直接测定。欲测元素的样品分析实际检出限分别为:Zr0.2ppm。Hf、Nb、Ta均为0.4ppm。实践证明,本方法不仅步骤简单,分析速度快,而且分析结果或靠,精密度和准确度良好。 相似文献
5.
ICP－AES 法测定地质样品中微量锆、 铪的研究 总被引：2，自引：0，他引：2
摘 要 在2％酒石酸介质中用阳离子交换树脂吸附干扰元素以 ICP-AES 法分别在
343∙823nm 和264∙141nm 直接测定地质样品中的微量锆和铪。锆的检出限为0∙5×10
－6 铪
为0∙4×10
－6 。此方法简单、快速应用于地球化学标准样品中锆和铪的分析取得了满意
的结果。 相似文献
6.
金橙G螯合形成树脂分离富集地质样品中微量贵金属研究Ⅱ——… 总被引：1，自引：0，他引：1
主要报道了用金橙Ｇ螯合负载形成树脂分离富集成地质样品贵金属Ｒｈ的方法，在最佳试验条件下Ｒｈ的回收率可达９５％～１０５％之间，其相对标准偏差为４．４９％，百分相对误差较小，为－２．４％方法无系统误差；用硫脲洗脱，该负载形成树脂不被破坏，重复使用５次，树脂均未见异常，均能定量回收，回收率在９８．５％～１０４％之间，符合要求说明，这种负载形成树脂也较稳定，也可用于实际地质样品中微量贵金属的分离富集。 相似文献
7.
HQS螯合形成纤维在分离富集痕量元素中的应用 总被引：2，自引：1，他引：2
8-羟基喹啉-5磺酸(HQS)螯合形成纤维制备容易,可用于痕量元素的分离富集。与相应的离子交换树脂相比,该纤维具有交换速率快、易洗脱等特点。经研究和改进,本文提出采用HQS整合形成纤维分离富集—火焰原子吸收光谱测定天然水中痕量Cu、Pb、Ni、Cd和Mn等元素的分析方法。方法的精密度和准确度较好。 相似文献
8.
主要报道了用金橙Ｇ螯合负载形成树脂分离富集地质样品中贵金属Ｒｈ的方法。在最佳试验条件下Ｒｈ的回收率可达９５％～１０５％之间；其相对标准偏差为４．４９％；百分相对误差较小，为－２．４％；方法无系统误差；用硫脲洗脱，该负载形成树脂不被破坏，重复使用５次，树脂均未见异常，均能定量回收，回收率在９８．５％～１０４％之间，符合要求。说明，这种负载形成树脂也较稳定，也可用于实际地质样品中微量贵金属的分离富集 相似文献
9.
P350反相色层分离岩石中痕量锆和铪及其测定 总被引：3，自引：0，他引：3
本文系统地研究了用P_(360)(甲基膦酸二甲庚脂)作固定相,聚二乙烯苯吸附树脂作为载体,锆与铪的反相色层行为及锆和铪反相色层的盐析剂效应。提出了连续反相色层分离锆、铪新方法。并应用于岩石中痕量锆和铪的测定。 相似文献
10.
花岗岩锆石中铪的地球化学研究 总被引：5，自引：0，他引：5
花岗岩锆石中铪的电子探针分析结果表明,花岗质岩浆中含量很低的铪以完全类质同象形式置换锆而大量富集在锆石中。因此,通过对花岗岩锆石中铪含量的分析研究可以反映出花岗质岩浆结晶过程中锆/铪值的演化规律、铪的地球化学行为特征及其花岗岩成因探讨中的应用意义。 相似文献
11.
We have developed a rapid and accurate method to determine Zr, Nb, Hf and Ta (denoted as HFSE) in geological samples by inductively coupled plasma-mass spectrometry fitted with a flow injection system (FI-ICP-MS). The method involves sample decomposition by HF followed by HF dissolution of HFSE coprecipitated with insoluble M and Ca fluoride residues formed during the initial HF attack. This HF solution was directly nebulized into an ICP mass spectrometer. An external calibration curve method and an isotope dilution method (ID) were applied for the determination of Nb and Ta, and of Zr and Hf, respectively. Recovery yields of HFSE were > 96% for peridotite, basalt and andesite compositions, apart from Zr and Hf for peridotite (> 85%). No matrix effects for either signal intensities of HFSE or isotope ratios of Zr and Hf were observed in basalt, andesite and peridotite solutions down to a dilution factor of 100. Detection limits in silicate rocks were 40, 2, 1 and 0.1 ng g-1 for Zr, Nb, Hf and Ta, respectively. This technique required only 0.1 ml of sample solution, and thus is suitable for analysing small and/or precious samples such as meteorites, mantle peridotites and their mineral separates. We also present newly determined data for the Zr, Nb, Hf and Ta concentrations in USGS silicate reference materials DTS-1, PCC-1, BCR-1, BHVO-1 and AGV-1, GSJ reference materials JB-1, -2, -3, JA-1, -2 and -3, and the Smithsonian reference Allende powder. 相似文献
12.
丹宁棉分离富集—发射光谱法同时测定地质样品中微量铌钽锆铪 总被引：1，自引：1，他引：1
采用丹宁棉对地质样品溶液中的铌、钽、锆、铪进行分离富集，将写信后的丹宁棉在600℃灼烧30min，灰分用发射光谱法同时测定四元素。检出限与通常的发射光谱法相比降低约2个数量级，经国家级标准物质检验，结果与标准值相符，精密度试验，各元素的RSD（n＝20）为2.6％－7.9％。 相似文献
13.
Analysis of geologic reference materials for REE and HFSE by inductively coupled plasma-mass spectrometry (ICP-MS) 总被引：1，自引：0，他引：1
I. V. Nikolaeva S. V. Palesskii O. A. Koz’menko G. N. Anoshin 《Geochemistry International》2008,46(10):1016-1022
A variant of the ICP-MS technique was developed for the analysis of geological materials for REE and HFSE (Zr, Nb, Hf, and Ta) and is illustrated by analyzing geological reference materials (GRM) of various composition. The chemical preparation of the samples, including their sintering/fusing with highly purified Li metaborate and the stabilization of the solution, ensures the complete transfer of the elements to be analyzed into solution. The use of an ELEMENT high-sensitivity mass spectrometer with an U-5000AT+ ultrasonic nebulizer made it possible to improve the detection limits of REE and HFSE. A combination of an external calibration with internal standard for the calculation of the concentrations allowed us to take into account the effect of the matrix and variations in the plasma parameters on the analytical signal. The accuracy of the method is illustrated by the comparison of the results obtained on the most reliably certified GRM with the values assumed for them. The relative standard deviation of the analysis amounts to 2–5% on average, depending on the concentrations. 相似文献
14.
Martin Bizzarro Joel A. Baker David Ulfbeck 《Geostandards and Geoanalytical Research》2003,27(2):133-145
A new digestion procedure and chemical separation technique has been developed for measurement of Lu/Hf and Hf isotope ratios that does not require high‐pressure bombs or use of HF or HClO4 acids. Samples are digested in dilute HCl or HNO3 after flux‐fusion at 110 0 °C in the presence of lithium metaborate. High field strength elements (HFSE) and rare earth elements (REE) are separated from this solution by co‐precipitation with iron hydroxide. The dissolved precipitate (in 2 mol l?1 HCl) is loaded directly onto a standard cation exchange column which separates remaining sample matrix from the heavy REE (Lu+Yb), and the middle‐light REE and HFSE (Hf). The middle‐light REE and individual HFSE are then separated (10.5, 9 and 6 mol l?1 HCl) using a miniaturized column containing TEVA spec resin which provides a REE‐, Ti‐ and Zr‐free Hf cut. This chemical separation scheme can also be readily adapted for isotopic analysis of the Sm‐Nd system and/or the other HFSE (Ti, Zr). Total procedural blanks for this technique are < 10 0 pg and < 2 pg for Hf and Lu, respectively, even when digesting large (0.5 g) samples. We present data from replicate digestions of international rock reference materials which demonstrate this technique routinely reproduces Lu/Hf ratios to < 0.2% (2s) and 176 Hf/177 Hf isotope ratios to < 30 ppm (2s). Moreover, the technique is matrix‐independent and has been successfully applied to analysis of diverse materials including basalts, meteorites, komatiites, kimberlites and carbonatites. The relative simplicity of this technique, coupled with the ease of digestion (and sample‐spike equilibration) of large difficult‐to‐dissolve samples, and the speed (2 days) with which samples can be digested and processed through the chemical separation scheme makes it an attractive new method for preparing samples for Lu‐Hf isotopic investigation. 相似文献
15.
对裂隙岩体的爆破破碎阻力特性进行了研究，提出了裂隙岩体爆破阻力矢量的概念和研究方法。以单元结构体作为主要研究对象，建立了爆破阻力矢量与岩体实际阻力矢量的关系模型。作为一种研究方法，它对裂隙岩体的爆破破碎的理论研究及施工技术的研究具有一定的实际意义。 相似文献
16.
Joy E. Reid Ingo Horn Henry P. Longerich Lance Forsythe George A. Jenner 《Geostandards and Geoanalytical Research》1999,23(2):149-155
Isotope dilution calibration has been applied to the determination of Zr and Hf in whole rocks by laser ablation (LA)-ICP-MS. Enriched isotopes were added during the preparation of flux-free, synthetic whole rock glasses and homogenised through a combination of grinding and fusion. This method avoids problems, such as solution instability and the chemical resistance of minerals such as zircon, inherent in acid digestion sample preparation. The use of isotope dilution removes the need for external calibration using certified reference material glasses such as NIST SRM 612 for which certified Zr and Hf values are not available. The precision of Zr and Hf determinations were found to be < 1% and 3.5% respectively, limited by Poisson counting statistics which contributed to 50% of the final precision of analysis. Measured values correlate closely with compiled literature values. 相似文献
17.
电感耦合等离子体质谱法(ICP-MS)测定水系沉积物中的铌钽锆铪 总被引：1，自引：0，他引：1
建立电感耦合等离子体质谱法(ICP-MS)测定水系沉积物中铌、钽、锆、铪四种元素的分析方法。将样品与氢氧化钠、过氧化钠混合物放入高温炉中,熔融分解完全,用热水提取,过滤后弃去滤液,将滤纸及沉淀用酒石酸-盐酸溶液溶解,稀释至刻度测定。方法检出限(3s)为:LD(Nb)=0.08μg/g,LD(Ta)=0.04μg/g,LD(Zr)=0.5μg/g,LD(Hf)=0.04μg/g,精密度(RSD%,n=6)为:0.84%~4.21%。该测定方法具有灵敏度高、精密度好、分析速度快、线性范围宽、操作性强等优势。采用该方法对国家一级标准物质进行测定表明,其结果与标准值吻合。此方法已在实际地质调查样品分析中得到应用。 相似文献
18.
《Chemical Geology》2007,236(1-2):13-26
We examined the coprecipitation behavior of Ti, Mo, Sn and Sb in Ca–Al–Mg fluorides under two different fluoride forming conditions: at < 70 °C in an ultrasonic bath (denoted as the ultrasonic method) and at 245 °C using a Teflon bomb (denoted as the bomb method). In the ultrasonic method, small amounts of Ti, Mo and Sn coprecipitation were observed with 100% Ca and 100% Mg fluorides. No coprecipitation of Ti, Mo, Sn and Sb in Ca–Al–Mg fluorides occurred when the sample was decomposed by the bomb method except for 100% Ca fluoride. Based on our coprecipitation observations, we have developed a simultaneous determination method for B, Ti, Zr, Nb, Mo, Sn, Sb, Hf and Ta by Q-pole type ICP-MS (ICP-QMS) and sector field type ICP-MS (ICP-SFMS). 9–50 mg of samples with Zr–Mo–Sn–Sb–Hf spikes were decomposed by HF using the bomb method and the ultrasonic method with B spike. The sample was then evaporated and re-dissolved into 0.5 mol l− 1 HF, followed by the removal of fluorides by centrifuging. B, Zr, Mo, Sn, Sb and Hf were measured by ID method. Nb and Ta were measured by the ID-internal standardization method, based on Nb/Mo and Ta/Mo ratios using ICP-QMS, for which pseudo-FI was developed and applied. When 100% recovery yields of Zr and Hf are expected, Nb/Zr and Ta/Hf ratios may also be used. Ti was determined by the ID-internal standardization method, based on the Ti/Nb ratio from ICP-SFMS. Only 0.053 ml sample solution was required for measurement of all 9 elements. Dilution factors of ≤ 340 were aspirated without matrix effects. To demonstrate the applicability of our method, 4 carbonaceous chondrites (Ivuna, Orgueil, Cold Bokkeveld and Allende) as well as GSJ and USGS silicate reference materials of basalts, andesites and peridotites were analyzed. Our analytical results are consistent with previous studies, and the mean reproducibility of each element is 1.0–4.6% for basalts and andesites, and 6.7–11% for peridotites except for TiO2. 相似文献
19.
敞开酸溶和偏硼酸锂碱熔ICP-MS法测定多金属矿中的稀土元素及铌钽锆铪 总被引：2，自引：2，他引：0
用电感耦合等离子体质谱法(ICP-MS)测定地质样品中的稀土及难熔元素,混合酸敞开酸溶法和碱熔融法是两种主要的溶样方法。但地质样品组分复杂,元素之间存在相互共生的现象,对于特殊元素、特殊样品用传统酸溶法会造成部分元素消解不完全,使测定结果不准确;而碱熔法的操作过程繁琐,且溶液盐度高,易产生基体干扰和堵塞仪器进样系统。本文改进了传统四酸和五酸体系,采用氢氟酸-硝酸-硫酸敞开酸溶体系,用国家一级标准物质制作标准曲线测定15种稀土元素,方法准确度(ΔlgC)为0.001～0.027。同时改进了偏硼酸锂碱熔法,样品用偏硼酸锂碱熔提取,加入氢氧化钠调节溶液至碱性条件,所测元素与偏硼酸锂共沉淀后过滤分离熔剂,再用硝酸复溶测定15种稀土元素及铌钽锆铪。两种溶样方法的测定值与认定值的相对误差为1.09%～9.30%。将混合酸敞开酸溶法测定稀土元素、偏硼酸锂碱熔法测定铌钽锆铪的结果与其他实验室密闭酸溶法相比,两组数据的相对偏差为0.13%～15.32%。本实验表明,混合酸敞开酸溶法适用于测定地质样品中的稀土元素,偏硼酸锂碱熔法不仅适用于测定地质样品中的稀土元素及铌钽锆铪,也适用于测定如古老高压变质岩石及铝含量高的样品中的铌钽锆铪。 相似文献
20.
Thomas Meisel Nina Schöner Vaida Paliulionyte Elisabeth Kahr 《Geostandards and Geoanalytical Research》2002,26(1):53-61
Data are reported for rare earth elements (REE), Y, Th, Zr, Hf, Nb and Ta in four geological reference materials using sodium peroxide (Na2 O2 ) sintering and inductively coupled plasma-mass spectrometry. The described procedure was used by students during their thesis work. A compilation of their reference material data acquired over one year of laboratory work demonstrates the ease and reliability of the method and the high reproducibility of the analytical results. Relative standard deviations of up to thirty six measurements of one reference material were lower than 5% for Y and the REE. Reproduciblities of Zr, Hf, Nb, Ta and Th were higher at between 5% and 10%, and can be attributed to the inhomogeneous distribution of zircon and other trace mineral phases and uncorrected drift effects. The concentration data are compared to reference and literature values and demonstrate that the procedure is also accurate. New data on G-3 show some systematic deviations from G-2, which are statistically significant. 相似文献