Abstract：The import of zinc oxide (ZnO) enrichment can make up for the shortage of zinc mineral resources in China. The content of free ZnO should be higher than 50%. At present, the content of ZnO in ZnO enrichment is usually determined by YS/T 1171.10-2017 (Na2EDTA titration). However, this method is tedious and time-consuming. Two days are required to determine one sample, which cannot meet the requirements of faster customs clearance during the import of large quantities of ZnO enrichment.A determination method of free ZnO in ZnO enrichment by X-ray diffraction (XRD) standard curve was established. The constant value analysis of imported ZnO enrichment sample was conducted by YS/T 1171.10-2017. Then 15 samples with ZnO content gradient were selected as the calibration sample to prepare the standard curve between integral intensity and ZnO content using the strong diffraction line (101) as the measuring line. The standard curve showed good linearity. The content of ZnO in three imported ZnO enrichment samples was determined using the proposed standard curve method, full spectrum fitting method and chemical method, respectively. The found result of standard curve method was consistent with that of chemical method. The measured value of full spectrum fitting method had great difference with that of chemical method. Only 26 min was required to determine one sample for the proposed standard curve method, which could meet the detection requirements of faster customs clearance during the import of large quantities of ZnO enrichment.
[1] 姜澜,付高峰,王德全.选择性氯化焙烧脱除氧化锌烟尘中的氟氯[J].有色金属,2001,53(3):28-31. JIANG Lan,FU Gaofeng,WANG Dequan.Removal of F and Cl from zinc oxide dust using selective chlorination roasting process[J].Nonferrous Metals,2001,53(3):28-31. [2] 曾冠武.高炉瓦斯泥综合利用技术述评[J].化工环保,2015,35(3):279-283. ZENG Guanwu.Review on utilization technologies of blast-furnace gas sludge[J].Environmental Protection of Chemical Industry,2015,35(3):279-283. [3] 袁文辉,杨卜,李强.含锌烟尘回收利用研究进展[J].湿法冶金,2016,35(4):271-274. YUAN Wenhui,YANG Bo,LI Qiang.Research progress on recycling of zinc metallurgical furnace dust[J]. Hydrometallurgy of China,2016,35(4):271-274. [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 based 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α-Co的含量[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] 冉敬,郭创锋,杜谷,等.X射线衍射全谱图拟合法分析蓝晶石的矿物含量[J].岩矿测试,2019,38(6):660-667. RAN Jing,GUO Chuangfeng,DU Gu,et al.Quantitative analysis of mineral composition of kyanite by X-ray diffraction with rietveld refinement method[J]. Rock and Mineral Analysis,2019,38(6):660-667. [12] 唐梦奇,罗明贵,韦彦强,等.铜冶炼炉渣X射线衍射Rietveld全谱图拟合物相定量分析[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. [13] 吴景武,于泓锦,冯均利,等.粗制氧化锌的X射线衍射全谱图拟合定量相分析探讨[J].冶金分析,2018,38(9):14-19. WU Jingwu,YU Hongjin,FENG Junli,et al.Discussion on quantitative phase analysis of crude zinc oxide by X-ray diffraction full spectrum fitting[J]. Metallurgical Analysis,2018,38(9):14-19. [14] 房俊卓,张霞,徐崇福.实验条件对X射线衍射物相定量分析结果的影响[J].岩矿测试,2008,27(1):60-62. FANG Junzhuo,ZHANG Xia,XU Chongfu.Effect of experimental conditions on X-ray diffractometric quantitative phase analysis[J].Rock and Mineral Analysis,2008,27(1):60-62. [15] 迟广成,张泉,赵爱林,等.X射线粉晶衍射仪定量测量海泡石矿样的实验条件[J].岩矿测试,2012,31(2):282-286. CHI Guangcheng,ZHANG Quan,ZHAO Ailin,et al.Experimental conditions of X-ray powder diffraction for sepiolite measurement[J].Rock and Mineral Analysis,2012,31(2):282-286.
