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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
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将偏硼酸锂与四硼酸锂混合熔剂高温熔融伟晶岩样品形成的玻璃,于硝酸、盐酸、氢氟酸的混合液中进行快速消解后,采用电感耦合等离子体质谱仪测定了其中的Ga、Sr、Th、U和稀土元素。方法检出限为0.03～0.91μg/g,相对标准偏差（RSD）优于5%。经国家标准物质验证,待测元素的测定值与推荐值的相对误差在0.07%～25%之间,满足地质矿产行业标准（DZ/T0130—2006）中的相对误差允许限要求。将本方法应用于实际样品分析,分析结果与酸溶法结果基本一致。该方法从前处理到上机测试能在48 h内完成,极大地提高了分析效率,适用于包括伟晶岩在内的地质样品中稀土、铀、钍、镓、锶元素含量的快速测定。 相似文献
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X射线荧光光谱法(XRF)已经应用于石膏等非金属矿物的测定,但由于石膏标准物质匮乏、硫含量较高且在高温易挥发损失,给测定带来了一定困难。本文采用石膏标准物质、高纯硫酸钙和其他国家一级标准物质(土壤、水系沉积物、碳酸盐)配制人工标准物质拟合校准曲线,优化稀释比、熔矿温度等熔融制样条件,用理论α系数校正基体效应,建立了采用XRF同时测定石膏矿中10个主次量元素(硅铝铁钙镁钾钠钛硫锶)的分析方法。样品与四硼酸锂-偏硼酸锂熔剂的稀释比为1∶9,在1050℃温度下样品熔融完全。方法检出限为4~135μg/g,精密度(RSD,n=12)小于3.0%。本方法配制的人工校准样品加强了样品基体的适应性,使用的四硼酸锂-偏硼酸锂熔剂在样品熔融过程中可有效地结合硫,抑制了硫的挥发损失,适用于批量分析硫含量高达12.60%~51.91%的实际石膏矿物。 相似文献
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钨钼矿石是重要的战略性矿产资源,中国是钨钼矿的产出和消费大国,准确、高效地分析钨钼及其共伴生的有益有害元素含量对钨钼矿的矿床评价和综合利用有重要意义。钨钼矿石中钨钼及伴生元素的分析目前主要采用酸溶和碱熔方式消解样品,酸溶方式在处理高钨钼样品时无法克服水解问题,过氧化钠、氢氧化钠等碱熔方式通常会引入大量碱金属,不能完成钾钠的测定。本文建立了一种偏硼酸锂熔融,盐酸-酒石酸超声浸取,电感耦合等离子体发射光谱(ICP-OES)同时测定钨钼矿石中钨钼铜铅锌铝铁钙镁钛锰钾钠的方法。利用偏硼酸锂熔融的强解离作用使样品完全分解,溶液除硼锂外不引入其他金属元素,在盐酸提取液中加入酒石酸络合能够有效抑制钨钼水解,经超声浸取加快了熔块溶解。实验优化了各元素的分析谱线和观测方式,对熔剂用量以及仪器条件进行对比实验以获得最佳条件,采用基体匹配法绘制标准曲线消除了基体效应的影响。标准曲线线性相关系数均大于0.9990,方法检出限为1.34～46.2μg/g,标准物质测定结果的相对误差为0.14%～8.7%,相对标准偏差(RSD,n=10)为1.4%～7.6%。该方法能够准确、高效地完成钨钼矿石样品中多元素的同时测定。 相似文献
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广泛赋存在花岗伟晶岩和热液石英脉中的铍矿石是铍最重要的矿物载体,目前铍矿石系统分析仍以传统化学法为主,影响分析效率,亟待开发一种简单高效的铍矿石中多元素分析方法。本文建立了一种基于偏硼酸锂熔融-电感耦合等离子体发射光谱(ICP-OES)测定铍矿石中铍及主量元素的定量分析方法,使用4∶1熔剂-样品比,950℃下熔融15min后,通过超声提取制备溶液。偏硼酸锂熔融法能有效地分解铍矿石中的氧化物,克服了传统酸溶或碱熔无法检测硅、钠、钾等元素的局限。本方法通过校准曲线与样品基体匹配,加入铕作内标等措施消除基体效应,实现了各元素(以氧化物计)低至0.003%～0.2%的检出限,满足铍精矿质量检测需求。对绿柱石、香花石、日光榴石样品(BeO含量范围为0.14%～13.33%)测定的相对标准偏差(RSD)小于6.83%,与混合酸酸溶分析方法的测定值相对偏差为0.06%～21.28%。通过标准物质GBW07150、GBW07151和GBW07183验证,本方法精密度和准确度均符合地质矿产实验室测试质量管理规范,适用于多种类型铍矿石样品中铍及主量元素的快速连续分析。 相似文献
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用偏硼酸锂熔样ICP-AES法测定岩石中Si、Zr等12个元素 总被引：5，自引：0，他引：5
本方法采用偏硼酸锂分解样品，电感耦合等离子体发射光谱法测量，在同一份溶液中可以测定硅、钠、铝、钙、镁、铁、钛、锰、钡、锶、钒、锆等元素。通过对国家标准物质测定，其准确度、精密度能满足岩石样品中定量分析要求。 相似文献
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较低稀释比熔融制样X射线荧光光谱法分析铬铁矿 总被引：3，自引：3，他引：0
铬铁矿属难熔矿物,目前对铬铁矿的分析以化学分析为主,方法成熟,但操作麻烦且步骤繁琐;而应用X射线荧光光谱法进行分析测定,一般都采用较高稀释比熔融制样,不利于低含量元素的测定。本文选用四硼酸锂+偏硼酸锂作为混合熔剂,与样品以20:1的稀释比熔融制样,利用波长色散X射线荧光光谱测定铬铁矿中多种元素(Cr、Si、Al、TFe、Mg、Ca、Mn)的方法。采用多种铬铁矿标准物质和人工配制标准物质制作工作曲线,理论α系数及康普顿散射内标法校正元素间的吸收-增强效应,方法精密度(RSD,n=10)为0.2%~5.3%。方法检出限低,如锰元素的检出限可低至60 μg/g;镁元素的检出限为225 μg/g,比文献采用高稀释比XRF测定的方法检出限(250 μg/g)要低。本方法通过选择有效的熔剂和较低的稀释比解决了铬铁矿的制样问题,熔剂的用量减少,称样量增加,提高了低含量元素分析的准确度,相应地降低了分析成本。 相似文献
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铝土矿中主成分的X射线荧光光谱分析 总被引：1，自引：1，他引：0
利用X射线荧光光谱法测定铝土矿中主成分A l2O3、SiO2、Fe2O3、TiO2。采用四硼酸锂-偏硼酸锂作熔剂,溴化锂作脱模剂,国产高频熔样炉高温熔融制备玻璃圆片,以标准物质制作校准曲线进行测定,并与化学法进行对照,结果基本一致。方法操作简单、快速,准确度和精密度均达到国家标准方法规定的要求,已用于实际生产中。 相似文献
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偏硼酸锂类熔剂，能够有效地分解硅酸盐岩石和太多数造岩矿物。样品分解后可以使用种种分析技术完成包括钾钠在内的元素定量分析，因此自C．O．英格梅尔斯(Ingamells)推荐偏硼酸锂作熔剂以来，已经在发射光谱和火焰光度法、原子吸收、比色 相似文献
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An Evaluation of Methods for the Chemical Decomposition of Geological Materials for Trace Element Determination using ICP-MS 总被引：3，自引：0，他引：3
Zongshou Yu Philip Robinson Peter McGoldrick 《Geostandards and Geoanalytical Research》2001,25(2-3):199-217
Complete dissolution is essential to obtain accurate analytical results using ICP-MS. In this study, decomposition techniques (i.e. acid digestions using Savillex Teflon vials, a high pressure digestion system and microwave oven, a combined lithium tetraborate fusion - HF/HNO3 acid decomposition and sodium peroxide sinter) for the total dissolution of different types of geological reference materials have been investigated. Savillex Teflon vial HF/HNO3 digestion is effective for basaltic samples. The high pressure HF/HClO4 digestion (PicoTrace TC-805 digestion system, Bovenden, Germany) allows dissolution of basalts and ironstones. Granites and magnetite-rich samples can be dissolved using a high pressure HF/H2 SO4 method. Geological samples cannot be effectively attacked by microwave acid digestion. A combined lithium tetraborate fusion - HF/HNO3 acid digestion method allows complete dissolution of many different types of geological materials; however, this method precludes the determination of volatile elements due to the high fusion temperature (1000 °C). A sodium peroxide sinter method at 480 °C has the potential for the rapid determination of Y, Sc and REE in different types of geological materials. However, the lack of ultra-pure reagents precludes the use of lithium tetraborate fusion and sodium peroxide sinter methods for the measurement of geological samples with low trace element abundances. 相似文献
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Chan‐Soo Park Hyung Seon Shin Haeyoung Oh Jong Hwa Moon Hana Cho Chang‐sik Cheong 《Geostandards and Geoanalytical Research》2013,37(3):361-368
We present a revised alkali fusion method for the determination of trace elements in geological samples. Our procedure is based on simple acid digestion of powdered low‐dilution (flux : sample ≈ 2 : 1) glass beads where large sample dilution demanded by high total dissolved solids, a main drawback of conventional alkali fusion, could be circumvented. Three geological reference materials (G‐3 granite, GSP‐2 granodiorite and SGD‐1a gabbro) decomposed by this technique and routine tabletop acid digestion were analysed for thirty trace elements using a quadrupole ICP‐MS. Results by conventional acid digestion distinctly showed poor recoveries of Zr, Hf and rare earth elements due to incomplete dissolution of resistant minerals. On the other hand, results obtained by our method were in reasonable agreement with reference data for most analytes, indicating that refractory minerals were efficiently dissolved and volatile loss was insignificant. 相似文献
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Assessment of Dissolution of Silicate Rock Reference Materials with Ammonium Bifluoride and Nitric Acid in a Microwave Oven 总被引：1，自引：0，他引：1
Thais T. Magaldi Margareth S. Navarro Jacinta Enzweiler 《Geostandards and Geoanalytical Research》2019,43(1):189-208
The complete dissolution of representative test portions of powdered rock samples for the determination of the mass fractions of trace elements by ICP‐MS relies either on aggressive and time‐consuming acid digestions or fusion/sintering with appropriate fluxes. Here, we evaluate a microwave oven dissolution method that employs a solution of NH4HF2 and HNO3. The entire procedure occurs in a closed vessel system and takes up to 4 h. In hundreds of digestions, the precipitation of fluorides was never observed. Replicate decomposition of 100 mg of twenty‐one international reference materials (RMs) of igneous rocks, and also one of a shale presented mostly satisfactory recoveries of forty‐one trace elements. Important exceptions were Zr and Hf in G‐2 and GSP‐2 (mean recoveries of ca. 70%), although for four other felsic rock RMs, the digestion was complete. For ultramafic rock RMs, we present Cr results that indicate quantitative dissolution of Cr‐bearing phases. We discuss the findings and conclude that advances in sample preparation of geological materials for instrumental analysis would benefit from a better understanding of how specific characteristics, such as composition and crystallinity of certain minerals, may affect their reactivity. 相似文献
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The beryllium and zirconium contents of 45 geochemical reference samples have been determined by inductively coupled plasma after fusion of the samples with lithium metaborate and dissolution of the melt in dilute nitric acid. The method described here is rapid and sample preparation straightforward. Good agreement is shown with previously published results for these two elements. A correction has to be made for an interference due to vanadium in determining the beryllium content, and there is a slight interference due to yttrium in the determination of zirconium. The detection limit for beryllium is about 0.2 μg g-1 and for zirconium about 15 μg g-1 in the sample. 相似文献
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采用电感耦合等离子体发射光谱法（ICP-OES）测定铝土矿中的稀土氧化物时,酸溶往往造成溶样不彻底,高温碱熔时大量的熔剂会降低稀土元素的发射强度,同时由于稀土氧化物含量（0.0010%~0.050%）较低,存在铝、铁等基体干扰,难以准确测定。本文采用氢氧化钠熔融铝土矿样品,熔融物用热水浸取,三乙醇胺溶液掩蔽铝和铁,乙二胺四乙酸二钠溶液络合钙、镁等干扰元素,稀土氢氧化物留存于沉淀中,沉淀经盐酸溶解进入待测液,从而将稀土元素与熔剂和基体元素分离。实验结果表明：标准溶液无需基体匹配,各稀土氧化物标准曲线的线性相关系数均不小于0.9999,检出限在0.0002%~0.0015%之间;按照实验方法分析实际样品中稀土氧化物的含量,测定结果的相对标准偏差（RSD,n=6）为2.0%~4.6%,回收率为85.2%~104.4%。本方法与电感耦合等离子体质谱法（ICP-MS）相比,两种方法的测定结果无显著性差异。 相似文献
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Voltammetric Determination of High Field‐Strength Elements (Ti,Zr, Hf,Nb, Ta) in Geological Matrices 
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下载免费PDF全文 A voltammetric method for the determination of the high field‐strength elements Ti, Zr, Hf, Nb and Ta by adsorptive stripping of their tartrate complexes is presented. The applicability of the method to geological and metallurgical samples is illustrated by the analysis of certified reference materials (USGS BCR‐2 basalt, BCS‐CRM 388 zircon and Euronorm CRM 579‐1 ferroniobium). Suitable sample preparation techniques, involving fusion with LiBO2 and acidic and basic fluxes, followed by preliminary separation by anion chromatography are described. The method is rapid, affordable and environmentally friendly as it does not require problematic compounds such as hydrofluoric acid or toxic solvents and represents an alternative to more commonly used methods (AAS, ICP‐OES, ICP‐MS). 相似文献
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Shenyang Y. Zhang Hongluo L. Zhang Zhenhui Hou Dmitri A. Ionov Fang Huang 《Geostandards and Geoanalytical Research》2019,43(1):93-111
A rapid sample preparation procedure is described to determine trace element compositions of peridotites using LA‐ICP‐MS. Peridotite powders were fused with albite in a molybdenum–graphite assembly to obtain homogeneous glasses. Best conditions for the fusion procedure (heating at 1500–1550 °C for 10–15 min with a sample‐to‐flux ratio of 1:2) were constrained with melting experiments on two USGS reference materials, PCC‐1 and DTS‐2B. Mass fractions of first series transition elements, Ba and Pb, in quenched glasses of PCC‐1 and DTS‐2B are consistent with published data within 10% RSD. Three spinel peridotite xenoliths from eastern China were analysed following both our method and conventional solution ICP‐MS. Compared with solution ICP‐MS, the relative deviations of our method for most elements were within 10%, while for the REE, Ta, Pb, Th and U, the relative deviations were within 20%. In particular, volatile elements (e.g., Pb and Zn) are retained in the glass. Compared with conventional wet chemistry digestion, our method is faster. Additional advantages are complete sample fusion, especially useful for samples with acid‐resistant minerals (spinel and rutile), and long‐term conservation of glasses allowing unlimited repeated measurements with microbeam techniques. The same approach can be used for analyses of other mantle rocks, such as eclogites and pyroxenites. 相似文献
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Results are presented of the determination of Zr, Nb, Hf and Ta in 74 standard reference materials by inductively coupled plasma mass spectrometry (ICP-MS). Samples are decomposed by fusion with lithium metaborate and the analytes are separated prior to analysis by precipitation of their cupferrates. Calibration is made using synthetic solutions and internal standardization with Ru (for Zr and Nb) and Re (for Hf and Ta). Accuracy is assessed by comparison with recommended values and precision is evaluated by replicate analyses of five SRMs. 相似文献