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洪飞, 刘耀华, 吕振生, 赵伟, 王卿, 张英明. 钛铁矿化学成分标准物质研制[J]. 岩矿测试, 2014, 33(1): 63-73.
引用本文: 洪飞, 刘耀华, 吕振生, 赵伟, 王卿, 张英明. 钛铁矿化学成分标准物质研制[J]. 岩矿测试, 2014, 33(1): 63-73.
Fei HONG, Yao-hua LIU, Zhen-sheng LV, Wei ZHAO, Qing WANG, Ying-ming ZHANG. Certified Reference Materials Preparation of Ilmenite Chemical Composition[J]. Rock and Mineral Analysis, 2014, 33(1): 63-73.
Citation: Fei HONG, Yao-hua LIU, Zhen-sheng LV, Wei ZHAO, Qing WANG, Ying-ming ZHANG. Certified Reference Materials Preparation of Ilmenite Chemical Composition[J]. Rock and Mineral Analysis, 2014, 33(1): 63-73.

钛铁矿化学成分标准物质研制

Certified Reference Materials Preparation of Ilmenite Chemical Composition

  • 摘要: 当前我国没有钛铁矿化学成分标准物质,只有与其相似的钒钛磁铁矿石标准物质,国外钛铁矿标准样品主要是钛铁矿精矿,不能有效地进行分析质量控制,因此迫切急需研制钛铁矿化学成分标准物质。本文研制了5个钛铁矿化学成分标准物质。样品采自山东省莒县棋山钛铁矿矿区、山东省沂水常庄钛铁矿矿区和河北省承德黑山钛铁矿矿区,采用流化床对撞式气流粉碎磨将样品细碎至粒度小于50 μm,混合均匀后进行均匀性和稳定性检验,代表性元素的电感耦合等离子体发射光谱和电感耦合等离子体质谱分析结果表明方差检验的F值小于临界值,样品均匀性良好;所检验的元素经18个月6次分析,均未发现统计学意义的明显变化,样品的短期和长期稳定性良好;烘样温度(20~60℃)对亚铁(FeO)的稳定性并无影响,亚铁不会发生氧化。选择11家具有资质的实验室,采取经典分析方法与现代仪器分析技术相结合的方式,选用两种以上不同原理的准确度高的可靠方法对该标准物质联合定值,依照JJF 1343—2012和一级标准物质技术规范,5个钛铁矿化学成分标准物质给出了46项组分(包括主量、痕量和全部稀土元素)的认定值和不确定度,TiO2的含量范围为2.97%~19.76%,TFe的含量范围为18.88%~51.30%,基本涵盖了我国钛铁矿成矿类型,能够满足钛铁矿勘查、评价和开发的需求。

     

    Abstract: At present, there are no ilmenite chemical composition certified reference materials, the closest being of vanadium-titanium magnetite ore composition. Internationally, ilmenite standards consist mainly of ilmenite concentrate, which is unsuitable for effective quality control. Therefore, there is an urgent need to develop ilmenite chemical composition reference materials. Five certified chemical composition reference materials of ilmenite were prepared by first collecting samples from Ju County and Yishui Changzhuang ilmenite mines in Shandong Province, and Chengde Montenegro ilmenite mine in Hebei Province. The samples were ground to a particle size of less than 50 μm by using an advanced jet mill, and then loaded in a coulter-mixing machine for thorough mixing. Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) and Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) were conducted for homogeneity and stability testing. For the homogeneity test, the variance test F value was less than the threshold, indicating a good homogeneity. After 18 months, six analysis results showed that no significant statistical changes were found in the elements and components. The results demonstrate that the samples have high uniformity and stability which meets the requirements for standard reference materials. Drying temperature (20-60℃) has no effect on the stability of FeO based on a ferrous experiment. According to JJF 1343—2012 and standard material specifications, 11 qualified laboratories were selected to give certified values and uncertainties of 46 elements, including major, trace and rare earth elements, by using the combination of classical methods and modern instrumental technologies. More than two kinds of methods with different principles were applied to yield accurate values. The content range of TiO2 was 2.97%-19.76%, and the content range of TFe was 18.88%-51.30%, which covered many variations of ilmenite ores in China. These reference materials meet the requirements of ilmenite exploration, evaluation and development demand.

     

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