Abstract：In China′s export supervision, the mixed ore with talc content higher than 50% should be managed as talc, and the export license system is implemented. At present, the detection of talc only includes the determination of magnesium and silicon contents, which cannot meet the quantitative analysis requirements of talc. Therefore, the method for the quantitative determination of talc in talc mixed ore by X-ray diffraction (XRD) Rietveld full spectrum fitting was established. Pure samples of talc powder, dolomite, calcite, quartz, cristobalite, rutile and other samples were screened from daily test samples by XRD. A series of mixture system with different ratios were prepared using the above samples as standard samples. The content of talc in the prepared mixture system was investigated by XRD combined with Rietveld full spectrum fitting. The different between the fitting values and the talc contents in the known mixture system ranged from -0.9% to 0.3%, which meant that the results were close. Therefore, it was feasible to detect talc content in talc mixed ore by XRD combined with Rietveld full spectrum fitting. The proposed method was applied to the detection of some talc mixed ore exported through Guangzhou Port in recent years. The samples with low, medium and high talc content were selected for the standard addition experiments. It was found that the recoveries were between 90% and 120%. In addition, the selected samples with medium gradient were used for precision tests. The relative standard deviation (RSD, n=10) of determination results was 0.94%, which could meet the requirements in YB/T 56320-2006. The proposed method could meet the export supervision requirements of talc ore.
[1] 中华人民共和国商务部,中华人民共和国海关总署公告 2008年第27号[EB/OL].[2008-4-16]. http://www.mofcom.gov.cn/swfgzc/article.shtml?id=20080405503160. [2] 刘茜,孙杨,苏丹.电感耦合等离子体原子发射光谱法测定滑石中MgO含量[J].湖南有色金属,2018,34(4):76-77. LIU Qian,SUN Yang,SU Dan.Determination of MgO content in talc by inductively coupled plasma atomic emission spectrometry[J].Hunan Nonferrous Metals,2018,34(4):76-77. [3] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.SN/T 2949—2011 出口滑石中二氧化硅、三氧化二铁、三氧化二铝、氧化钙、氧化镁的测定X射线荧光光谱法[S].北京:中国标准出版社,2011. [4] 薛雍,江向峰,钟玉峰.标准曲线法X射线粉晶衍射直接分析滑石中微量石棉[J].岩矿测试,2010,29(3):322-324. XUE Yong,JIANG Xiangfeng,ZHONG Yufeng.Quantitative determination of trace asbestos in talcum by X-ray powder diffraction with external standardization[J].Rock and Mineral Analysis,2010,29(3):322-324. [5] 李丹凤,朱健萍,卢日刚.粉末X射线衍射法测定甘氨酸原料药中α晶型的含量[J].中国药师,2018,21(10):1759-1761. LI Danfeng,ZHU Jianping,LU Rigang.Determination of crystal type α in glycine by powder X-ray diffraction[J].China Pharmscist,2018,21(10):1759-1761. [6] 候冬.XRD测定熟料中玻璃体含量[J].水泥工程,2018(4):18-20. HOU Dong.Measure the content of vitreous in clinker by XRD[J].Cement Engineering,2018(4):18-20. [7] 罗宇宏,萧丽芳,郑国华.等.X-射线衍射内标法测定滑石粉中的温石棉[J].广州化学,2019,44(4):45-50. LUO Yuhong,XIAO Lifang,ZHENG Guohua,et al.Quantitative analysis of chrysotile in talc by X-ray diffraction internal standard method[J].Guangzhou Chemistry,2019,44(4):45-50. [8] 许聚良,陈汀水.一种基于晶体结构数据建立XRD内标法定量相分析标准曲线库的方法[J].理化检验(物理分册),2016,52(3):164-167. XU Juliang,CHEN Tingshui.A method of establishing standard curves database for quantitative phase analysis by XRD internal standard method on crystal structure data[J].Physical Testing and Chemical Analysis(Part A:Physical Testing),2016,52(3):164-167. [9] 谢梦雨,戴苏云,沈晓敏,等.X-射线粉末衍射K值法测定钴粉中的α-Co含量[J].南京师大学报(自然科学版),2017,40(4):93-97. XIE Mengyu,DAI Suyun,SHEN Xiaomin,et al.Quantification of α-Co in cobalt using K-value method of PXRD [J].Journal of Nanjing Normal University(Natural Science Edition),2017,40(4):93-97. [10] 唐梦奇,黎香荣,刘国文,等.X射线衍射K值法测定氧化铁皮中游离α-SiO2的含量[J].岩矿测试,2015,34(5):565-569. TANG Mengqi,LI Xiangrong,LIU Guowen,et al.Determination of free α-SiO2 content in mill scale by X-ray diffraction K value method[J].Rock and Mineral Analysis,2015,34(5):565-569. [11] 曾令民,杨喜英,王力珩.等.X射线衍射里特沃尔德全谱拟合测定粉尘中游离的SiO2[J].分析化学,2008,36(5):599-603. ZENG Lingmin,YANG Xiying,WANG Liheng,et al.Determination of weight concentration of free silicon dioxide for dust using X-ray diffraction technique and Rietveld refinement method[J].Chinese Journal of Analytical Chemistry,2008,36(5):599-603. [12] 宓小川,刘莲君.热轧板氧化皮Rietveld全谱拟合定量分析[J].物理测试,2008,26(2):31-34. MI Xiaochuan,LIU Lianjun.Quantitative analysis of scale on hot-rolled plate by Rietveld method[J].Physics Examination and Testing,2008,26(2):31-34. [13] 王锐,周敬,李文竹,等.Rietveld精修定量分析钢中残余奥氏体[J].物理测试,2008,26(4):46-48. WANG Rui,ZHOU Jing,LI Wenzhu,et al.Rietveld full patern fitting method for quantitative phase analysis of austenite in steel[J].Physics Examination and Testing,2008,26(4):46-48. [14] 曾令民,汪万林,陆美文.X射线全谱拟合定量相分析铁矿石[J].广西科学院学报,2010,26(3):291-294. ZENG Lingmin,WANG Wanlin,LU Meiwen.X-ray quantitative analysis of iron ore using Rietveld refinement method[J].Journal of Guangxi Academy of Sciences,2010,26(3):291-294. [15] 曾超,何维.赤泥物相的X射线粉末衍射Rietveld法定量分析研究[J].冶金分析,2014,34(8):1-6. ZENG Chao,HE Wei.Study on quantitative phase analyses of red mud by Rietveld method from X-ray powder diffraction[J].Metallurgical Analysis,2014,34(8):1-6. [16] 李昆,王文宝.云母矿粉中游离二氧化硅含量的快速测定[J].分析仪器,2014(2):43-46. LI Kun,WANG Wenbao.Quick determination of free silica in mica powder[J].Analytical Instrumentation,2014(2):43-46. [17] 王培铭,赵丕琪,刘贤萍.基于Rietveld精修法的水泥熟料物相定量分析[J].建筑材料学报,2015,18(4):692-698. WANG Peiming,ZHAO Piqi,LIU Xianping.Quantitative analysis of cement clinker by Rietveld refinement method[J].Journal of Building Materials,2015,18(4):692-698. [18] 唐梦奇,罗明贵,韦彦强.等.铜冶炼炉渣的X射线衍射Rietveld全谱拟合物相定量分析[J].冶金分析,2016,36(11):11-16. TANG Mengqi,LUO Minggui,WEI Yanqiang,et al.Quantitative analysis of phases in copper smelting slag by Rietveld full spectrum fitting of X-ray diffraction[J].Metallurgical Analysis,2016,36(11):11-16. [19] 国家能源局,石油地质勘探专业标准化委员会.SY/T 5163—2018 沉积岩中黏土矿物和常见非粘土矿物X射线衍射分析方法[S].北京:石油工业出版社,2018.
