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  

Determination of fifteen major,minor and micro components in coral reef sample by X-ray fluorescence spectrometry with fusion sample preparation

作　　者：李强[1,2] 雷知生[1,2] 张学华[1,2] 杨天邦 黄雪华[1,2] LI Qiang;LEI Zhisheng;ZHANG Xuehua;YANG Tianbang;HUANG Xuehua(Guangzhou Marine Geological Survey,Guangzhou 510760,China;National Engineering Research Center of Gas Hydrate Exploration and Development,Guangzhou 511458,China)

机构地区：[1]广州海洋地质调查局,广东广州510760 [2]天然气水合物勘查开发国家工程研究中心,广东广州511458

出　　处：《冶金分析》2022年第11期30-36,共7页Metallurgical Analysis

基　　金：南方海洋科学与工程广东省实验室(广州)人才团队引进重大专项(GML2019ZD0506)。

摘　　要：珊瑚礁样品中SiO_(2)、Al_(2)O_(3)、Fe_(2)O_(3)、Na_(2)O、K_(2)O、MnO、TiO_(2)和P_(2)O_(5)等低含量组分的测试通常需要采用不同的方法和仪器,难以满足批量样品测试的需求。实验以Li_(2)B_(4)O_(7)-LiBO_(2)-LiF为熔剂,采用高温熔融制样,建立X射线荧光光谱法(XRF)测定珊瑚礁样品中SiO_(2)、Al_(2)O_(3)、Fe_(2)O_(3)、MgO、CaO、Na_(2)O、K_(2)O、MnO、TiO_(2)、P_(2)O_(5)、SO_(3)、Sr、Zr、Ba和Cr含量的方法。对熔融制样条件进行了优化,其中脱模剂LiBr饱和溶液最佳用量为150μL。选取岩石、碳酸盐岩石、水系沉积物国家标准物质以及在标准物质中加入Sr标准溶液的方式建立校准样品系列,Sr和Zr采用经验系数法和康普顿散射线内标法校正基体效应,其他组分采用理论α系数校正基体效应,有效克服了基体效应的影响。结果表明,各组分测定值的相对标准偏差(RSD,n=7)为0.25%~19.5%。方法用于珊瑚礁实际样品分析,其分析结果与采用化学湿法的测定结果吻合,各组分的相对误差绝对值为0~28.86%。The determination of low content components in coral reef samples,such as SiO_(2),Al2O_(3),Fe_(2)O_(3),Na_(2)O,K_(2)O,MnO,TiO_(2),and P_(2)O_(5),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 Li_(2)B_(4)O_(7)-LiBO_(2)-LiF mixture as the flux.A method for the determination of SiO_(2),Al2O_(3),Fe_(2)O_(3),MgO,CaO,Na_(2)O,K_(2)O,MnO,TiO_(2),P_(2)O_(5),SO_(3),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 150μL.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 theoreticalαinfluence 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%.

关 键 词：珊瑚礁 主次量组分 微量组分 X射线荧光光谱法(XRF) 熔融制样 

分 类 号：O657.34[理学—分析化学]