Determination of fifteen major, minor and micro components in coral reef sample by X-ray fluorescence spectrometry with fusion sample preparation
LI Qiang1,2, LEI Zhisheng1,2, ZHANG Xuehua1,2, YANG Tianbang1,2, HUANG Xuehua1,2
1. Guangzhou Marine Geological Survey, Guangzhou 510760, China; 2. National Engineering Research Center of Gas Hydrate Exploration and Development, Guangzhou 511458, China
Abstract：The determination of low content components in coral reef samples, such as SiO2, Al2O3, Fe2O3, Na2O, K2O, MnO, TiO2, and P2O5, usually requires different methods and instruments, which is difficult to meet the requirements of batch detection.The samples were prepared by high temperature fusion using Li2B4O7-LiBO2-LiF mixture as the flux. A method for the determination of SiO2, Al2O3, Fe2O3, MgO, CaO, Na2O, K2O, MnO, TiO2, P2O5, SO3, Sr, Zr, Ba and Cr in coral reef samples by X-ray fluorescence spectrometry (XRF) was established. The fusion sample preparation conditions were optimized, the optimum amount of release reagent (LiBr saturated solution) was 150 μL. The calibration curves were established using the certified reference materials of rocks, carbonate rocks and stream sediments, as well as the artificially synthesized samples by mixing certified reference materials and Sr standard solution. The empirical coefficient method and Compton scattering internal standard method were used to correct the matrix effect for Sr and Zr, and the theoretical α influence coefficient method was used to correct the matrix effect for other components, which effectively overcome the influence of matrix effect. The results showed that the relative standard deviations (RSD, n=7) of determination results were between 0.25% and 19.5%. The proposed method was applied to the analysis of actual coral reef samples, and the found results were consistent with those obtained by wet chemical methods. The absolute value of relative errors of components were 0-28.86%.
李强, 雷知生, 张学华, 杨天邦, 黄雪华. 熔融制样-X射线荧光光谱法测定珊瑚礁样品中15种主次和微量组分[J]. 冶金分析, 2022, 42(11): 30-36.
LI Qiang, LEI Zhisheng, ZHANG Xuehua, YANG Tianbang, HUANG Xuehua. Determination of fifteen major, minor and micro components in coral reef sample by X-ray fluorescence spectrometry with fusion sample preparation. , 2022, 42(11): 30-36.
[1] 王瑞,余克服,王英辉,等.珊瑚礁的成岩作用[J].地球科学进展,2017,32(3):221-233. WANG Rui,YU Kefu,WANG Yinghui,et al.The diagenesis of coral reefs[J].Advances in Earth Science,2017,32(3):221-233. [2] 修淳,罗威,杨红君,等.西沙石岛西科1井生物礁碳酸盐岩地球化学特征[J].地球科学(中国地质大学学报), 2015,40(4):645-652. XIU Chun,LUO Wei,YANG Hongjun,et al.Geochemical characteristics of reef carbonate rocks in well Xike-1 of Shidao island,Xisha area[J].Earth Science(Journal of China University of Geoscience),2015,40(4):645-652. [3] 王子玉,范玉蝶,徐秋阳,等.南海海域珊瑚礁元素分析试验研究[J].海洋技术学报,2019,38(3):64-69. WANG Ziyu,FAN Yudie,XU Qiuyang,et al.Analysis of coral reef elements in the South China Sea and its instruction significance[J].Journal of Ocean Technology,2019,38(3):64-69. [4] 喻德科.西沙群岛石珊瑚中钙、铝、硅、磷、铁和锶的X-射线荧光光谱测定[J].分析化学,1991,19(1):126. YU Deke.Determination of calcium,aluminum,silicon,phosphorus,iron and strontium of stone coral in Paracel Islands by X-ray fluorescence spectrometry[J].Chinese Journal of Analytical Chemistry,1991,19(1):126. [5] 林学辉,刘昌岭.单道扫描电感耦合等离子体发射光谱法测定珊瑚礁中主量和微量元素[J].岩矿测试,2003,22(3):225-227. LIN Xuehui,LIU Changling.Determination of major and trace elements in coral accumulation samples by sequential ICP-AES[J].Rock and Mineral Analysis,2003,22(3):225-227. [6] 马兵兵.电位滴定法测定石灰石中钙和镁含量[J].理化检验(化学分册),2012,48(12):1492-1493. MA Bingbing.Determination of calcium and magnesium in limestone by potentiometric titration[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2012,48(12):1492-1493. [7] 韩晓.EDTA络合滴定法快速测定矿石中钙、镁[J].中国无机分析化学,2019,9(2):54-57. HAN Xiao.Rapid determination of calcium and magnesium in ore by EDTA complexometric titration[J].Chinese Journal of Inorganic Analytical Chemistry,2019,9(2):54-57. [8] 陈金凤,钟坚海,林亚妹,等.电感耦合等离子体原子发射光谱法同时测定石灰石和白云石中镁等6种元素含量[J].检验检疫学刊,2013,23(6):4-7. CHEN Jinfeng,ZHONG Jianhai,LIN Yamei,et al.Simultaneous determination of Mg,Si,Al,Fe,Mn and P in limestone and dolomite by inductively coupled plasma atomic emission spectrometry[J].Journal of Inspection and Quarantine,2013,23(6):4-7. [9] 国家市场监督管理总局,国家标准化管理委员会.GB/T 3286.10—2020石灰石及白云石化学分析方法 第10部分:二氧化钛含量的测定 二安替吡啉甲烷分光光度法[S].北京:中国标准出版社,2017. [10] 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 3286.6—2014 石灰石及白云石化学分析方法 第6部分:磷含量的测定 磷钼蓝分光光度法[S].北京:中国标准出版社,2017. [11] 马景治,刘恒杰,王峰.熔融制样-X 射线荧光光谱法测定地质样品中的主次成分[J].分析试验室,2016,35(11):1348-1352. MA Jingzhi,LIU Hengjie,WANG Feng.Simultaneous determination of major and minor components in geological sample by XRF with fusion sample preparation[J].Chinese Journal of Analysis Laboratory,2016,35(11):1348-1352. [12] 郑瑞娟,钟坚海,张艳燕,等.熔融制样-波长色散X射线荧光光谱法同时测定超基性岩中主、次及微量成分[J].分析试验室,2018,37(12):1411-1415. ZHENG Ruijuan,ZHONG Jianhai,ZHANG Yanyan,et al.Determination of major,minor and micro components in ultrabasic rocks by wavelength dispersive X-ray fluorescence spectrometry with fusion sample preparation[J].Chinese Journal of Analysis Laboratory,2018,37(12):1411-1415. [13] 乔蓉,郭钢.X射线荧光光谱法测定白云石、石灰石中氧化钙、氧化镁和二氧化硅[J].冶金分析,2014,34(1):75-78. QIAO Rong,GUO Gang.Determination of calcium oxide,magnesium oxide and silicon dioxide in dolomite and limestone by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2014,34(1):75-78. [14] 曲月华,王翠艳,王一凌,等.熔融制样-X射线荧光光谱法测定石灰石中5种组分[J].冶金分析,2013,33(12):29-33. QU Yuehua,WANG Cuiyan,WANG Yiling,et al.Determination of five components in limestone by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2013,33(12):29-33. [15] 褚宁,李卫刚,蒋晓光,等.熔融制样-波长色散X射线荧光光谱法测定石灰石中主次成分[J].冶金分析,2014,34(10):37-41. CHU Ning,LI Weigang,JIANG Xiaoguang,et al.Determination of major and minor components in limestone by wavelength dispersive X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2014,34(10):37-41. [16] 吕善胜,徐金龙,田琼,等.X射线荧光光谱法测定石灰石中多组分含量[J].冶金分析,2014,34(9):39-42. LÜ Shansheng,XU Jinlong,TIAN Qiong,et al.Determination of multi-components in limestone by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2014,34(9):39-42. [17] 张敏,陈赟,龚沂.熔融制样-X射线荧光光谱法测定石灰石和白云石中8种组分[J].冶金分析,2015,35(10):54-59. ZHANG Min,CHEN Yun,GONG Yi.Determination of eight components in limestone and dolomite by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2015,35(10):54-59. [18] 杨竞,张秀华,田志宏,等.熔融制样-X射线荧光光谱法测定菱镁矿和白云石中6种组分[J].冶金分析,2020,40(11):26-31. YANG Jing,ZHANG Xiuhua,TIAN Zhihong,et al.Determination of six components in magnesite and dolomite by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2020,40(11):26-31. [19] 杨忠梅,李静,张春花.熔融制样-X射线荧光光谱法测定轻烧白云石中主要成分[J].冶金分析,2020,40(7):82-86. YANG Zhongmei,LI Jing,ZHANG Chunhua.Determination of main components in light-burned dolomite by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2020,40(7):82-86. [20] 孙晓飞,文孟喜,杨丹丹.康普顿散射线结合经验系数法校正在X射线荧光光谱测定石灰石和白云石中的应用[J].冶金分析,2016,36(1):11-17. SUN Xiaofei,WEN Mengxi,YANG Dandan.Application of Compton scatter and empirical coefficient correction in X-ray fluorescence spectrometric determination of limestone and dolomite[J].Metallurgical Analysis,2016,36(1):11-17. [21] 钟坚海,陈金凤,张艳燕,等.熔片制样-X 射线荧光光谱法同时测定石灰石及白云石中主、次、微量成分[J].分析试验室,2016,35(7):826-830. ZHONG Jianhai, CHEN Jinfeng,ZHANG Yanyan,et al.Determination of major,minor and micro components in limestone and dolomite by X-ray fluorescence spectrometry with fusion sample preparation[J].Chinese Journal of Analysis Laboratory,2016,35(7):826-830.
