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王干珍, 彭君, 李力, 秦毅, 曹健, 田宗平. 锰矿石成分分析标准物质研制[J]. 岩矿测试, 2022, 41(2): 314-323. DOI: 10.15898/j.cnki.11-2131/td.202104080051
引用本文: 王干珍, 彭君, 李力, 秦毅, 曹健, 田宗平. 锰矿石成分分析标准物质研制[J]. 岩矿测试, 2022, 41(2): 314-323. DOI: 10.15898/j.cnki.11-2131/td.202104080051
WANG Ganzhen, PENG Jun, LI Li, QIN Yi, CAO Jian, TIAN Zongping. Preparation of Standard Material for Composition Analysis of Manganese Ore[J]. Rock and Mineral Analysis, 2022, 41(2): 314-323. DOI: 10.15898/j.cnki.11-2131/td.202104080051
Citation: WANG Ganzhen, PENG Jun, LI Li, QIN Yi, CAO Jian, TIAN Zongping. Preparation of Standard Material for Composition Analysis of Manganese Ore[J]. Rock and Mineral Analysis, 2022, 41(2): 314-323. DOI: 10.15898/j.cnki.11-2131/td.202104080051

锰矿石成分分析标准物质研制

Preparation of Standard Material for Composition Analysis of Manganese Ore

  • 摘要: 锰矿中有毒有害元素对锰提纯工艺、生产环境和产品质量的影响,一直是困扰锰行业发展的技术难题,也是实验测试亟需解决的质量基础共性技术问题。目前,国内外现有的锰矿石成分分析标准物质共有10个,定值成分有Mn、Fe、Al2O3和SiO2等17种,均缺乏Cl、F、Pb、Cd、Co、Cr、Hg和As等有害成分的定值,从而无法满足锰提纯工艺研发、环境监测评估、锰矿进口监督、检测方法评价等需要。本文研制了2个锰矿石成分分析标准物质(GBW07139、GBW07140),候选物样品采自湖南省和新疆自治区的3个大型锰矿区,根据矿床类型采用单独或组合方式进行样品制备,样品全部通过97μm标准筛和均匀性初检,并分装为最小包装单元。通过对随机抽取的2×30瓶样品进行均匀性检验,F实测值均小于F0.05(29, 60)=1.59,且相对标准偏差为0.45%~6.44%,表明样品的均匀性好。在一年时间内进行长期和短期稳定性检验,采用线性模型/平均值一致性数据统计,未发现统计学意义的明显差异,表明样品的稳定性好。通过10家实验室对Mn、MnO2、SiO2、Al2O3、Fe、CaO、MgO、K2O、Na2O、TiO2、S、P、Cu、Co、Zn、Ni、Pb、Cd、Hg、Cr、As、Cl、F共23种成分进行协作定值,2个锰矿石成分分析标准物质中Mn质量分数分别为21.63%和41.55%,Cl质量分数为38×10-6和1214×10-6,Ni质量分数为1075×10-6和30.9×10-6,具有较宽泛的含量范围和代表性。该批锰矿石成分分析标准物质实现了锰矿石成分分析标准物质中Cl、F、Pb、Cd、Cr、Co、Hg和As成分的定值,适用于锰相关分析检测质量控制。

     

    Abstract:
    BACKGROUNDThe toxic and hazardous elements in manganese ore not only affect manganese purification, production environment and product quality, but have also always been a technical problem in the manganese industry and particularly in experimental testing. At present, there are a total of 10 existing manganese ore composition analysis standard materials in the world, all of which lack the certified values of harmful components such as Cl, F, Co, Cr, Hg and As. Therefore, they do not meet the needs of manganese purification research, environmental monitoring, manganese ore import and detection method research.
    OBJECTIVESTo prepare manganese ore composition analysis standard materials with quantitative values for Cl, F, As, Pb, Cd, Cr and Hg.
    METHODSTwo certified chemical composition reference materials of manganese ore (GBW07139, GBW07140) were prepared by collecting samples from 3 large-scale manganese mining areas in Hunan Province and Xinjiang Autonomous Region. According to the type of deposit, all the samples passed the 97μm standard sieve and the initial uniformity inspection, and were packed into the smallest packaging unit individually or in combination.
    RESULTSFor the uniformity test of randomly selected 2×30 bottles, the measured values of F were all less than F0.05(29, 60)=1.59, and the relative standard deviation was between 0.45% and 6.44%, indicating good uniformity of the samples. The long-term stability/short-term stability test was carried out within one year, and the linear model/average consistency data showed no significant difference, indicating good stability of samples. Ten laboratories participated in the collaborative certified value research, which included 23 components such as Mn, MnO2, SiO2, Al2O3, Fe, CaO, MgO, K2O, Na2O, TiO2, S, P, Cu, Co, Zn, Ni, Pb, Cd, Hg, Cr, As, Cl and F. In the two manganese ore composition analysis standard materials, the mass fractions of Mn were 21.63% and 41.55%, Cl were 38×10-6 and 1214×10-6, Ni were 1075×10-6 and 30.9×10-6, respectively.
    CONCLUSIONSThis batch of manganese ore composition analysis standard materials contain certified values of Cl, F, Pb, Cd, Cr, Co, Hg and As, and is suitable for quality control of manganese-related analysis and testing.

     

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