Analysis of Niobium-Tantalum Ore by X-Ray Fluorescence Spectrometry Combined with Low Dilution Fusion
摘 要
应用低稀释比,即低熔剂-样品质量比的方法熔融样品为X射线荧光光谱(XRFS)分析制备了测试样品,提出了铌钽原矿及精矿的XRFS分析方法。选择质量比为12比22的四硼酸锂和偏硼酸锂作为混合熔剂,熔剂与样品的质量比为4比1的条件下熔融矿样。应用TNRY-01C型全自动熔样机,并选择如下熔样条件:称取样品2.000 g及混合熔剂8.000 g,置于铂-金(质量比95:5)坩埚中,搅拌均匀,滴加饱和溴化锂溶液0.15 mL,于1 200℃熔融180 s,摆动240 s,静置20 s,待样片自然冷却后翻转,补加饱和溴化锂溶液0.05 mL,按上述条件重复熔融1次。此熔融方法对铌钽氧化物质量分数不小于0.01%的原矿和铌钽氧化物质量分数不小于60%的精矿均能很好熔化。若仅考虑铌、钽分析,熔融时间影响可予忽略,无需统一。对于一些难熔样品可适当延长熔融时间,但需注意补充溴化锂溶液。若需测定样品中碱金属及卤族元素,则需保持一致的熔融时间。上述操作中加入了复熔步骤是为了消除气泡,使样片表面光滑平整,并能保证样品熔化完全。在所测定的11项组分中,常量组分测定值的相对标准偏差(n=6)均小于1.0%,微量组分测定值的相对标准偏差(n=6)不超过4.0%。
Abstract
Low dilution fusion, i.e. fusion of sample with low mass ratio of flux to sample, was used as sample preparation for use in XRFS analysis of crude ore and concentrate containing niobium and tantalu. Optimum conditions for sample fusion were studied thoroughly and reported in detail. A mixture of lithium tetraborate and lithium metaborate in the mass ratio of 12 to 22 was used as flux. Mass ratio of the flux mixture to sample of 4 to 1 was taken for the fusion, and the optimum conditions were chosen as follows:2.000 g of the ore sample were mixed thoroughly with 8.000 g of the mixed flux in a Pt-Au (wPt:wAu=95:5) crucible. After addition of 0.15 mL of saturated lithium bromide solution, the fusion was carried out with TNRY-01C automatic sample fusion melter at 1 200℃ for 180 s, the crucible was swung for 240 s and then stayed for 20 s. When the melt was cooled down naturally, the melt disc of the sample was turned over and the fusion was repeated once under the same conditions described above, with a supplementary addition of 0.05 mL of saturated lithium bromide solution. By the above fusion process either the crude ore samples containing ≥ 0.01% of niobium tantalum oxide or the concentrate sample containing ≥ 60% of niobium tantalum oxide can all be well melted. In case only analysis of ores containing Nb and Ta is considered, effects of time of fusion can be ignored, but in case of some ore samples hard to melt, the fusion time can be prolonged, with attention to supplementary addition of LiBr solution. In case of analysis of ore samples containing alkali metals or halogens, definite and consistent time of fusion should be kept. The purpose of the re-fusion process mentioned above were ① to expel gas bubbles from the melt in order to keep a plain and smooth surface of the melt; and ② to ensure a complete melting of the sample. Precision of determination of the 11 components in the ore samples was tested, values of RSDs (n=6) <1.0% were found for the major components and ≤ 4.0% for those micro-components.
中图分类号 O657.34 DOI 10.11973/lhjy-hx201812009
所属栏目 工作简报
基金项目 国土资源部川西稀有金属矿集区技术经济评价项目(121201016000150017-6)
收稿日期 2018/2/5
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备注李可及,硕士研究生,主要从事X射线荧光光谱法及贵金属火试金方法分析,xorlarrin@163.com
引用该论文: LI Keji,ZHAO Chaohui. Analysis of Niobium-Tantalum Ore by X-Ray Fluorescence Spectrometry Combined with Low Dilution Fusion[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(12): 1410~1414
李可及,赵朝辉. 低稀释比熔融-X射线荧光光谱法分析铌钽矿石[J]. 理化检验-化学分册, 2018, 54(12): 1410~1414
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参考文献
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【2】EASTELL J, WILLIS J P. A low dilution fusion technique for the analysis of geological samples. 2-major and minor element analysis and the use of influence/alpha coefficients[J]. X-Ray Spectrometry, 1993,22(2):71-79.
【3】HE Z W, HUANG F, YU H M, et al. A flux-free fusion technique for rapid determination of major and trace elements in silicate rocks by LA-ICP-MS[J]. Geostandards and Geoanalytical Research, 2016,40(1):5-21.
【4】MALMQVIST J. Semi-low-dilution fusion technique for analysis of geological, environmental and production plant samples in ferrous and non-ferrous industries[J]. X-Ray Spectrometry, 1998,27(3):183-197.
【5】唐力君,罗立强,江葛.低稀释比制样技术与多类型地质样品X射线荧光分析方法研究[J].岩矿测试, 2001,20(4):253-256.
【6】ICHIKAWA S, ONUMA H, NAKAMURA T. Development of undersized (12.5 mm diameter) low-dilution glass beads for X-ray fluorescence determination of 34 components in 200 mg of igneous rock for applications with geochemical and archeological silicic samples[J]. X-Ray Spectrometry, 2016,45(1):34-37.
【7】秦光荣.铌钽溶液的性质及其反应特性[J].分析化学, 1978(6):474-480.
【8】岩石矿物分析编委会.岩石矿物分析:第三分册[M].4版.北京:地质出版社, 2011.
【9】马生凤,温宏利,李冰,等.微波消解-耐氢氟酸系统电感耦合等离子体发射光谱法测定铌钽矿中的铌和钽[J].岩矿测试, 2016,35(3):271-275.
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