• 中文核心期刊
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镍矿石和镍精矿标准物质研制

Preparation and Certification of Nickel Ore and Nickel Concentrate Reference Materials

  • 摘要: 我国镍矿石与镍精矿标准物质较少,镍矿石成分分析标准物质仅有1个,镍含量较高(4.33%),当前已有的标准物质基本用尽,且国际上尚没有镍精矿标准物质。本文研制了3个镍矿石标准物质(GNi-1、GNi-2、GNi-3)和2个镍精矿标准物质(GNi-4和GNi-5)。标准物质候选物采自吉林省红旗岭镍矿,将样品粉碎至粒度小于0.074 mm,针对样品硫化物含量较高的特点,在样品加工过程中采用低温和球磨机中充满氩气的保存方法,防止加工过程中产生热量导致硫化物发生氧化,提高样品长期稳定性。采用X射线荧光光谱和电感耦合等离子体发射光谱法(ICP-AES)对样品的均匀性进行检验,F的实测值小于临界值,相对标准偏差较小,样品均匀性良好;两年内4次测定的分析结果无方向性变化趋势,统计计算结果显示稳定性良好。19家实验室对此批标准物质进行联合定值,Ni采用经典分光光度法、容量法与重量法测定,微量元素采用ICP-AES和电感耦合等离子体质谱(ICP-MS)等技术测定,依照ISO导则35和国家一级标准物质研制规范,3个镍矿石标准物质给出了Ni、Cu、S等23种组分的标准值与不确定度;2个镍精矿标准物质的19种组分给出标准值与不确定度,4种组分给出参考值。镍矿石标准物质中镍的含量分别为0.11%、0.33%、1.02%;镍精矿标准物质中镍的含量分别为5.93%、9.01%,形成一个从边界品位、工业品位至镍精矿较为完整的含量系列,能够满足镍矿勘查和选冶对标准物质的需求。

     

    Abstract: The only available nickel ore reference material in China, which has a Ni content of 4.33%, is currently out of stock. Therefore, three nickel ore reference materials (GNi-1, GNi-2 and GNi-3) and two nickel concentrate reference materials (GNi-4 and GNi-5) have been developed and are described in this paper. The samples of nickel ore and nickel concentrate were collected from the Hongqiling Nickel deposit in Jilin province. The samples were crushed and sieved to less than 20 mesh and ground for 48 hours in a high alumina ball mill, which was filled with Ar gas in order to avoid oxidization of the sulfide, until the particles were less than 0.074 mm. The samples are stored at temperatures below 8℃. The homogeneity was tested by WD-XRF and ICP-AES, and the relative standard deviation was less than 1.0%. The F-test result, which was less than the threshold value, showed that all five samples were homogeneous. Good stability was verified by repeating the analysis four times within two years without any changes. Nineteen laboratories were involved in the inter-laboratory programme and provided 2002 values for 23 oxides and elements. Classical chemical methods such as Spectrophotometry, Volumetry and Gravimetric Analysis, were taken as the dominant methods in the determination of Ni, Cu and major oxides (SiO2, S, and Al2O3 etc). Minor and trace elements were determined by ICP-AES, ICP-MS and AAS. The estimation of certified values and uncertainty conform to ISO guide 35 and Technical Norms of Primary Reference Materials. 23 components of nickel ore were characterised as certified values. Ni concentrations for GNi-1, GNi-2 and GNi-3 were 0.11%, 0.33% and 1.02%, respectively. 19 components of nickel concentrates were characterized as certified values, 4 components were taken as reference values. Ni concentrations for GNi-4 and GNi-5 were 5.93% and 9.01%. The Ni concentrations which were selected from cut-off grade to industrial grade, have a good range and meet the requirements as the reference materials for nickel exploration and metallurgy.

     

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