Literature review on the application of X-ray fluorescence spectrometry in phosphate ore analysis
LI Song1, LI Xiaoli2, WANG Yimin*1, DENG Saiwen1, WANG Yiya1
1. National Research Center of Geoanalysis,Beijing 100037,China; 2. Institute of Geophysical and Geochemical Exploration,Chinese Academy of Geological Sciences, Langfang 065000,China
Abstract：At present,X-ray fluorescence spectrometry(XRF) has become one of the most important methods for phosphate ore analysis. In this paper, total 33 periodical articles on phosphate ore analysis by XRF from the introduction of XRF to 2022 were collected. Among them, 15 papers were related to fusion sample preparation,12 papers were related to pressed powder pellet sample preparation, 2 papers were review articles, 1 paper was about the development of reference materials, and 3 papers were focused on the application of XRF for the chemical composition determination in mineralogy and process mineralogy. This paper introduced the basic conditions for the analysis of phosphate ore composition in China, including monographs, reference materials, standard methods and related review literatures. The contents and main points of 27 periodical articles, including analytical instrument, sample preparation method, calibration and calibration method, component determination and main component measurement precision, were briefly introduced in the form of list. The typical and representative literatures were reviewed according to the sample preparation method. Moreover, the problems in the use of existing standard substances and standard methods were also summarized. Finally, the selection of sample preparation method, the influence of sample granularity and future development of XRF for phosphate ore analysis were discussed. Total 53 referenced were cited in this paper.
李松, 李小莉, 王毅民, 邓赛文, 王祎亚. X射线荧光光谱在磷矿石分析中的应用文献评介[J]. 冶金分析, 2023, 43(10): 19-28.
LI Song, LI Xiaoli, WANG Yimin, DENG Saiwen, WANG Yiya. Literature review on the application of X-ray fluorescence spectrometry in phosphate ore analysis. , 2023, 43(10): 19-28.
[1] 尹丽文.我国磷矿资源开发利用现状及对有关问题的建议[J].国土资源情报,2004(10):37-39. YIN Liwen.Current status of development and utilization of phosphate ore resources and suggestions on relevant problems[J].Land and Resources Information,2004(10):37-39. [2] 张卫峰,马文奇,张福锁,等.中国、美国、摩洛哥磷矿资源优势及开发战略比较分析[J].自然资源学报,2005,20(3):378-386. ZHANG Weifeng,MA Wenqi,ZHANG Fusuo,et al.Comparative analysis of the superiority of China's phosphate rock and development strategies with that of the United States and Morocco[J].Journal of Natural Resources,2005,20(3):378-386. [3] 柳正.我国磷矿资源的开发利用现状及发展战略[J].中国非金属矿工业导刊,2006(1):21-23. LIU Zheng.Present exploitation situation of China phosphorus resources and its development[J].China Non-metallic Mining Industry Herald,2006(1):21-23. [4] 任清宇,姚金蕊.中国磷矿资源的特点与开发策略[J].矿业快报,2006(2):1-4. REN Qingyu,YAO Jinrui.Characteristics and development strategies of phosphorite resources in China[J].Express Information of Mining Industry,2006(2):1-4. [5] 李家熙,朱玉伦.现代岩矿分析技术格局与展望[J].岩矿测试,1990,9(1):1-8. LI Jiaxi,ZHU Yulun.The prospect and new system of rock and mineral analysis[J].Rock and Mineral Analysis,1990,9(1):1-8. [6] 王毅民,王晓红,高玉淑.地质分析的历史发展与当今热点[J].分析化学,2001,29(7):845-851. WANG Yimin,WANG Xiaohong,GAO Yushu.The review and prospect on geoanalysis[J].Chinese Journal of Analytical Chemistry,2001,29(7):845-851. [7] 邓赛文,王祎亚,王毅民.中国磷矿石分析文献评介[J].岩矿测试,2011,30(3):384-390. DENG Saiwen,WANG Yiya,WANG Yimin.A review on literatures of phosphate ores analysis in China[J].Rock and Mineral Analysis,2011,30(3):384-390. [8] 王祎亚,邓赛文,王毅民,等.磷矿石分析方法评述[J].冶金分析,2013,33(4):26-34. WANG Yiya,DENG Saiwen,WANG Yimin,et al.Review on analytical methods of phosphate ores[J].Metal-lurgical Analysis,2013,33(4):26-34. [9] 湖南省矿产测试利用研究所.磷矿石分析[M].北京:地质出版社,1995:1-476. [10] 岩石矿物分析编委会.岩石矿物分析:第2分册[M].4版.北京:地质出版社,2011:206-262. [11] 王毅民,顾铁新,王晓红,等.实用地质分析标准物质手册(汉-英对照)[M].2版.北京:地质出版社,2013:589. [12] 曾美云,刘金,邵鑫,等.磷矿石化学成分分析标准物质研制[J].岩矿测试,2017,36(6):633-640. ZENG Meiyun,LIU Jin,SHAO Xin,et al.Preparation of phosphate ore reference materials for chemical composition analysis[J].Rock and Mineral Analysis,2017,36(6):633-640. [13] 国家标准总局.GB/T 1868—1980～GB/T 1881—1980磷矿石和磷精矿统一分析方法[S].北京:中国标准出版社,1980. [14] 国家技术监督局.GB/T 1868—1995 磷矿石和磷精矿采样与样品制备及化学分析方法[S].北京:中国标准出版社,1996. [15] 中华人民共和国国家质量监督检验检疫总局. SN/T 1097—2002 出口磷矿石中五氧化二磷、氧化钙、三氧化二铁、氧化铝、氧化镁、二氧化硅和氧化钾的X-射线荧光光谱法测定方法[S].北京:中国标准出版社,2002. [16] 云南省质量技术监督局.DB53/T 574—2014 磷矿石 磷、镁、铁、铝、硅、钙、钾、钠氧化物含量的测定 波长色散X射线荧光光谱法[S].北京:人民交通出版社,2014. [17] 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. GB/T 35996—2018 磷矿石和磷精矿中八种元素含量的快速测定 X射线荧光光谱法[S].北京:中国标准出版社,2018. [18] 陈梅玲.荧光X光谱技术在矿石分析中的应用[J].研究与探索,1985(2):57-60. CHEN Meiling.Application of fluorescence X spectroscopy in ore analysis[J]. Research and Exploration,1985(2):57-60. [19] 茅祖兴.磷矿石的X射线荧光光谱分析[J].分析化学,1988,16(10):909-911. MAO Zuxing.Analysis of phosphate ore by X-ray fluorescence spectrometry[J].Chinese Journal of Analytical Chemistry,1988,16(10):909-911. [20] 王毅民,贺中央.磷矿石中主要和次要组分的X射线荧光光谱分析[J].分析化学,1989,17(1):87-90. WANG Yimin,HE Zhongyang.Determination of multielements in phosphate ore by XRF[J].Chinese Journal of Analytical Chemistry,1989,17(1):87-90. [21] 杨发景,李张胜.X荧光分析技术在磷矿分析中的应用[J].云南化工,1992(2):34-35. YANG Fajing,LI Zhangsheng.Application of X fluorescence analysis in phosphorore analysis[J].Yunnan Chemical Technology,1992(2):34-35. [22] 杨丽萍.X-ray荧光光谱法在磷肥生产原料分析中的应用[J].贵州化工,1997(4):37-40. YANG Liping.Application of X-ray fluorescence spectrometry method in raw materials analysis of phosphate fertilizer production[J].Guizhou Chemical Industry,1997(4):37-40. [23] 程雪刚,吴扬,何学忠,等.X荧光光谱法测定磷矿石中化学成分的研究[J].现代商检科技,1998,8(2): 27-29. CHENG Xuegang,WU Yang,HE Xuezhong,et al.Study on the chemical composition of phosphate ore by X-fluorescence spectrometry[J].Modern Commodity Inspection Sciecnce and Technique,1998,8(2):27-29. [24] 杨发景,汤光中,段棋仁,等.X射线荧光光谱标准添加法测定磷矿、磷肥中Mn、Cu、Zn、Mo、Pb等微量元素[J].广西化工,2000(S1):161-164. YANG Fajing,TANG Guangzhong,DUAN Qiren,et al.XRF spectrometry determination of Mn,Cu,Zn,Mo,Pb trace elements in phosphatic ore and phosphate ferlilizer[J].Guangxi Chemical Industry,2000(S1):161-164. [25] 张万平,李张胜,席涛.压片法X-射线荧光光谱测定磷铁[J].云南化工,2001(2):30-32. ZHANG Wanping,LI Zhangsheng,XI Tao.Phosphoiron analysis by X-ray fluorescence spectroscopy with pressed powder pellet[J].Yunnan Chemical Technology,2001(2):30-32. [26] WANG Xiaohong,LI Guohui,ZHANG Qin,et al.Determination of major,minor and trace elements in seamount phosphorite by XRF[J].Geostandards and Geoanalytical Research,2004,28(1):81-88. [27] 李张胜. X射线荧光光谱法定量测定湿法磷酸中主次成分[J].云南化工,2006(5):71-73. LI Zhangsheng.Quantitative analysis of main and impurity element in wet phosphoric acid by XRFA[J].Yun-nan Chemical Technology,2006(5):71-73. [28] 王宁伟,朱登峻,朱金连,等.X-射线荧光光谱法测定磷矿石中五氧化二磷、氧化钙、三氧化二铁、氧化铝、氧化镁和二氧化硅[J].冶金分析,2006,26(6):65-67. WANG Ningwei,ZHU Dengjun,ZHU Jinlian,et al.Determination of P2O5,CaO,Fe2O3,Al2O3,MgO and SiO2 in phosphorus rock by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2006,26(6):65-67. [29] 冯晓军,叶罕章.X射线荧光光谱快速分析浮选磷矿中的P2O5和MgO[J].磷肥与复肥,2009,24(2):65-66. FENG Xiaojun,YE Hanzhang.Rapid analysis on P2O5 and MgO in phosphate floatation by using X-ray fluorescence spectrometer[J].Phosphate & Compound Fertilizer,2009,24(2):65-66. [30] 李红叶,许海娥,李小莉,等.熔融制片-X射线荧光光谱法测定磷矿石中主次量组分[J].岩矿测试,2009,28(4):379-381. LI Hongye,XU Haie,LI Xiaoli,et al.Determination of major and minor components in phosphate ores by X-ray fluorescence spectrometry with fused bead sample preparation[J].Rock and Mineral Analysis,2009,28(4):379-381. [31] 叶罕章,冯晓军,张江坤,等.X 射线荧光光谱法测定磷矿中Na 元素的重叠校正[J].广东化工,2009,36(12):159-160. YE Hanzhang,FENG Xiaojun,ZHANG Jiangkun,et al.Determination of overlap correction of natrium element in phosphorus ore by X-ray fluorescence spectrometry [J].Guangdong Chemistry Industry,2009,36(12):159-160. [32] 杨润泉.X射线荧光光谱仪无标样分析测定磷矿浮选样品组成[J].磷肥与复肥,2010,25(4):70-72. YANG Runquan.Determination of sample composition by X-ray fluorescence spectrometer analysis without standard sample in phosphate floatation[J].Phosphate & Compound Fertilizer,2010,25(4):70-72. [33] 叶罕章,陈晶亮,李平芬,等.X射线荧光光谱法测定浮选磷矿中的主次组分[J].磷肥与复肥,2010,25(6):67-68. YE Hanzhang,CHEN Jingliang,LI Pingfen,et al.Determinations of major and minor components in floatation phosphate by X-ray fluorescence spectrometer[J].Phosphate & Compound Fertilizer,2010,25(6):67-68. [34] 张江坤,张华,余慧茹.用X射线荧光光谱仪测定磷矿多元素分析熔片制样条件的选择[J].磷肥与复肥,2010,26(1):66-67. ZHANG Jiangkun,ZHANG Hua,YU Huiru.The selection on sampling condition of sheet-melting for phosphate rock multi-element analysis by X-ray fluorescence spectrometer[J].Phosphate & Compound Fertilizer,2010,26(1):66-67. [35] 彭桦,蒋正国,叶罕章,等.X射线荧光光谱仪测定磷矿石中P2O5基底滤纸制样条件研究[J].磷肥与复肥,2011,26(1):61,78. PENG Hua,JIANG Zhengguo,YE Hanzhang,et al.Study on thin sampling preparation on filter paper for determination of P2O5 in phosphate rock with X-ray fluorescence spectrometer[J].Phosphate & Compound Fertilizer,2011,26(1):61,78. [36] 李可及,易建春,潘钢.X射线荧光光谱法测定磷矿石中11种主次组分[J].冶金分析,2013,33(9):22-27. LI Keji,YI Jianchun,PAN Gang.Determination of eleven major and minor components in phosphate ores by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2013,33(9):22-27. [37] 王祎亚,许俊玉,詹秀春,等.较低稀释比熔片制样X射线荧光光谱法测定磷矿石中12种主次痕量组分[J].岩矿测试,2013,32(1):58-63. WANG Yiya,XU Junyu,ZHAN Xiuchun,et al.Determination of twelve major,minor and trace components in phosphate ores by X-ray fluorescence spectrometry with a lower-dilution ratio of fused bead sample preparation[J].Rock and Mineral Analysis,2013,32(1):58-63. [38] 张江坤,冯晓军,叶罕章,等.微波消解滤纸制样XRF法测定磷矿石中的多元素[J].磷肥与复肥,2013,28(4):74-75. ZHANG Jiangkun,FENG Xiaojun,YE Hanzhang,et al.Determination of multi elements in phosphate rock with microwave digestion and filter paper sample preparation by XRF method[J].Phosphate & Compound Fertilizer,2013,28(4):74-75. [39] 曾江萍,张莉娟,李小莉,等.超细粉末压片-X射线荧光光谱法测定磷矿石中12种组分[J].冶金分析,2015,35(7):37-43. ZENG Jiangping,ZHANG Lijuan,LI Xiaoli,et al.Determination of twelve components in phosphate ore by X-ray fluorescence spectrometry with ultra-fine powder tabletting[J].Metallurgical Analysis,2015,35(7):37-43. [40] 李张胜,杨春元,郑朝伟,等.凝胶制样X射线荧光光谱法测定湿法磷酸中P2O5、Fe2O3、Al2O3、SO3含量[J].磷肥与复肥,2016,31(9):42-44. LI Zhangsheng,YANG Chunyuan,ZHENG Chaowei,et al.Determination of P2O5,Fe2O3,Al2O3,SO3 content in wet-process phosphoric acid by gel sampling X-ray fluorescence spectrometer method[J].Phosphate & Compound Fertilizer,2016,31(9):42-44. [41] 冯晓军.X射线荧光光谱法测定沙特碳酸盐型磷块岩的主次组分[J].理化检验(化学分册),2017,53(3):350-354. FENG Xiaojun.Determination of major and minor components in Saudi carbonate-type phosphate blocks ore by X-ray fluorescence spectrometry[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2017,53(3):350-354. [42] 石友昌,李国会,李志雄,等.熔融制样-X射线荧光光谱法测定磷矿石中主次组分[J].冶金分析,2017,37(10):53-58. SHI Youchang,LI Guohui,LI Zhixiong,et al.Determination of major and minor components in phosphate ore by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2017,37(10):53-58. [43] 刘朝竹,欧志兵,彭桦,等.X射线荧光光谱熔片法分析沙特阿拉伯乌木乌尔磷矿中主次元素[J].磷肥与复肥,2018,33(5):46-48. LIU Chaozhu,OU Zhibing,PENG Hua,et al.Main and secondary element analysis of Saudi Arabia ebonyur phosphorus ore by XRF melting glass plate method[J].Phosphate & Compound Fertilizer,2018,33(5):46-48. [44] 彭桦,罗昆义,张树洪,等.超细样品压片X射线荧光光谱分析沙特阿拉伯磷矿中多元素含量[J].磷肥与复肥,2018,33(7):39-42. PENG Hua,LUO Kunyi,ZHANG Shuhong,et al.Analysis of multi-elements in phosphorus rock of Saudi Arabia by XRF ultra-fine sample squash method[J].Phosphate & Compound Fertilizer,2018,33(7):39-42. [45] 王晓红,高玉淑,王毅民.超细地质标准物质及其应用[J].自然科学进展,2006,16(3):309-315. WANG Xiaohong,GAO Yushu,WANG Yimin.Ultrafine geological reference material and its application[J].Progress in Natrural Science,2006,16(3):309-315. [46] 王晓红,王毅民,高玉淑,等.地质标准物质粒度测量与表征实践[J].岩矿测试,2009,28(1):5-9. WANG Xiaohong,WANG Yimin,GAO Yushu,et al.Measurement and characterization of the particle size of geological reference materials[J].Rock and Mineral Analysis,2009,28(1):5-9. [47] 王毅民,高玉淑,王晓红.中国地质标准物质研制和标准方法制定的成果与思考[J].岩矿测试,2006,25(1):55-63. WANG Yimin,GAO Yushu,WANG Xiaohong.A review on study of geochemical reference materials and reference methods in China[J].Rock and Mineral Analysis,2006,25(1):55-63. [48] 王庆楠,狄敬如,何翀,等.墨西哥Sonora(索诺拉州)锌绿松石的矿物学及谱学特征[J].光谱学与光谱分析,2019,39(7):2059-2066. WANG Qingnan,DI Jingru,HE Chong,et al.Mineralogical and spectral characteristics of faustite from Sonora Mexico[J].Spectroscopy and Spectral Analysis,2019,39(7):2059-2066. [49] 曹阳阳,李智力,田承涛,等.云南某中低品位磷矿工艺矿物学研究[J].现代矿业,2022,38(6):191-194. CAO Yangyang,LI Zhili,TIAN Chengtao,et al.Study on process mineralogy of a medium and low grade phosphate ores in Yunnan province[J].Modern Mining,2022,38(6):191-194. [50] 徐伟,石波,田言,等.贵州某复杂难处理磷矿石工艺矿物学及浮选应用研究[J].化工矿物与加工,2022,51(6):12-16. XU Wei,SHI Bo,TIAN Yan,et al.Study on the process mineralogy and flotation behavior of a complex phosphate rock in Guizhou[J].Industrial Minerals and Processing,2022,51(6):12-16. [51] 张江坤,欧志兵,甘海轩,等.粉末压片-X射线荧光光谱法测定沙特某地区磷矿石中的氯[J].磷肥与复肥,2022,37(2):36-37,45. ZHANG Jiangkun,OU Zhibing,GAN Haixuan,et al.Determination of chlorine in phosphate rock in Sandu Arabia by powder tablet pressing and X-ray fluorescence spectrometry[J].Phosphate & Compound Fertilizer,2022,37(2):36-37,45. [52] 王毅民,王晓红.我国地质分析中X射线光谱技术的回顾与发展[J].岩矿测试,2000,19(4):275-285. WANG Yimin,WANG Xiaohong.The review and prospect on X-ray spectrometry in geoanalysis in China[J].Rock and Mineral Analysis,2000,19(4):275-285. [53] 刘咸德,王林.绿色分析化学技术的研究进展[J].岩矿测试,2000,19(4):268-274. LIU Xiande,WANG Lin.Research progress of green analytical chemistry[J].Rock and Mineral Analysis,2000,19(4):268-274.
