Application of Hand-held X-ray Fluorescence Spectrometer in the Exploration of Cobalt-rich Crust Resources
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摘要: 便携式X射线荧光光谱仪具有快速、无损分析的特点，本文重点研究了手持式X射线荧光光谱仪在富钴结壳碎块和浅钻岩心野外现场原位分析中的应用能力。采用压片法制样，以富钴结壳国家标准物质（GBW 07337~GBW 07339）和多金属结核国家标准物质（GBW 07249、GBW 07295和GBW 07296）作为校准样品，建立了手持式X射线荧光光谱仪测定富钴结壳样品的校准曲线。方法经国家标准物质GBW 07339验证，元素Mn、Fe、Co、Ni和Cu的精密度（RSD）在0.3%～3.0%之间，满足富钴结壳样品现场分析的要求。在海上资源勘查现场，应用手持式X射线荧光光谱仪对富钴结壳碎块和浅钻岩心原样进行了现场原位分析。富钴结壳碎块原样烘干后直接测试分析数据与实验室压片制样XRF分析数据对比表明，Mn、Fe、Co、Ni和Cu元素的测定值一致性良好；浅钻岩心的原位分析数据与实验室人工分层分析数据对比表明，各层位Mn、Fe、Co、Ni和Cu元素直接测试数据与实验室压片制样XRF分析数据分布趋势基本一致。实际应用研究表明，手持式X射线荧光光谱仪适合于现场原位分析，满足野外富钴结壳资源快速评价的要求，同时原位分析能更真实地反映原始富钴结壳岩心不同层位中各元素的变化特征，为进一步研究富钴结壳成矿机制提供更丰富的数据资料。
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关键词:
- 手持式X射线荧光光谱仪 /
- 富钴结壳资源勘查 /
- 原位分析
Abstract: A portable X-ray Fluorescence Spectrometer (XRF) can be used for field analysis with the advantages of rapidity and non-destruction; the applications of hand-held XRF in in-situ analysis of cobalt-rich crust chunks and core are described. The calibration curve for cobalt-rich crusts was established using national certified reference materials such as GBW 07337, GBW 07338 and GBW 07339. The proposed method has been validated by analyzing certified reference materials; the relative standard deviation was 0.3%-3.0%, which is appropriate for analysis of cobalt-rich crust in field. The hand-held XRF was utilized for in-situ analysis of cobalt-rich crust chunks and drilling core in marine exploration. A comparison of the results from in-situ analysis of dried crust chunks and those obtained from the hand-held XRF instrument after pressed powder sample preparation is presented, and good consistencies were found for the elements of interest. The data of in-situ analysis of crust core was evaluated by comparing with that obtained from laboratory testing after powder was layered artificially; the results based on two different methods indicate that distribution features of Mn, Fe, Co, Ni and Cu are similar. The methodology has been proved to be an effective method for in-situ analysis, which can meet the need of fast evaluation of cobalt-rich crusts resources, meanwhile, the proposed method, is appropriate for distribution research of Mn, Fe, Co, Ni and Cu in original cobalt-rich crust, which is helpful for the study of mineralization in different metallogenic stages of the crust. -
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表 1 各元素校准曲线
Table 1. Calibration curve of the elements
分析元素 校准方程 相关系数 R2 Mn y=0.9142 x+1.5633 0.9994 Fe y=1.0244 x-0.2017 0.9998 Co y=1.1543 x+0.1702 0.9896 Ni y=1.1011 x+0.0139 0.9991 Cu y=1.1144 x+0.0460 0.9981 
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表 2 方法精密度
Table 2. Precision tests of the method
元素 元素含量(%) RSD(%) 标准值 分次测定值 平均值 Mn 20.50 20.70 20.57 20.53 20.66 20.61 20.61 0.3 Fe 14.90 14.71 14.88 14.78 14.84 14.96 14.83 0.6 Co 0.56 0.57 0.56 0.56 0.56 0.57 0.56 1.0 Ni 0.40 0.39 0.40 0.40 0.42 0.41 0.40 2.8 Cu 0.15 0.15 0.15 0.15 014 0.15 0.15 3.0
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表 3 样品分析结果对比
Table 3. Comparison of analytical results with different methods
站位号 分析方式 元素含量(%) Mn Fe Co Ni Cu JQ-1 原样 22.25 8.38 0.39 0.55 0.17 烘干样 25.85 10.69 0.49 0.70 0.18 压片制样 26.19 10.81 0.51 0.75 0.17 JQ-2 原样 21.79 11.59 0.66 0.47 0.15 烘干样 26.46 14.23 0.77 0.59 0.17 压片制样 26.95 13.96 0.81 0.63 0.15 JQ-3 原样 20.08 15.66 0.42 0.29 0.12 烘干样 23.64 20.19 0.52 0.38 0.11 压片制样 23.41 20.25 0.55 0.41 0.11 JQ-4 原样 20.45 7.47 0.48 0.52 0.14 烘干样 23.18 10.51 0.58 0.69 0.13 压片制样 22.86 10.23 0.59 0.66 0.13
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