粉末压片-X射线荧光光谱法测定深海富铁粘土中主次量组分  

Determination of major and minor components in abyssal iron-rich clay by X-ray fluorescence spectrometry with pressed powder pellet

作　　者：李强[1] 张学华[1] LI Qiang;ZHANG Xue-hua(Guangzhou Marine Geological Survey,Guangzhou 510760,China)

机构地区：[1]广州海洋地质调查局,广东广州510760

出　　处：《冶金分析》2018年第4期57-62,共6页Metallurgical Analysis

摘　　要：富铁粘土赋存于深海大洋的某些区域,目前缺乏富铁粘土相关标准物质和分析方法,实验利用台式X射线荧光光谱仪(XRF)结合压片法制样现场快速测定深海富铁粘土样品中的Na_2O、MgO、Al_2O_3、SiO_2、P_2O_5、K_2O、CaO、TiO_2、Mn、Fe、Cu、Zn、V、Sr、Zr、Ba、Pb和Y等组分。优化选择压力30t和保压35s的制样条件;采用多金属结核和富钴结壳、深海及近海沉积物国家标准物质以及定值深海富铁粘土样品绘制校准曲线,解决了缺少富铁粘土标准物质的问题。对18个组分的测量条件进行了优化,使用经验系数法校正了主要成分SiO_2、CaO、Fe和Mn的基体效应。方法的检出限为3.67~1 172μg/g。精密度试验结果表明,各组分测定值的相对标准偏差(RSD,n=7)在0.3%~2.2%之间。方法用于实际样品的分析,其分析结果与实验室采用其他方法的测定结果吻合,能够满足野外现场富铁粘土样品中多种组分同时快速分析的要求。The iron-rich clay exists in some regions of deep sea and ocean.At present,there are no related standard substances and analysis method for iron-rich clay.The contents of Na 2O,MgO,Al 2O 3,SiO 2,P 2O 5,K 2O,CaO,TiO 2,Mn,Fe,Cu,Zn,V,Sr,Zr,Ba,Pb and Y in abyssal iron-rich clay sample were rapidly determined in site using desktop X-ray fluorescence spectrometer through sample prepare by pressed powder pellet.The optimum conditions for sample preparation were as follows:the pressure was 30 t and the pressing time was 35 s.The calibration curves were prepared by national standard substances of polymetallic nodule and cobalt-rich crust,deep sea and hemipelagic sediments as well as certified deep sea iron-rich clay samples,solving the problem of lack of iron-rich clay standard substances.The measurement conditions of 18 components were optimized.The matrix effect of major components including SiO 2,CaO,Fe and Mn was corrected by empirical coefficient method.The detection limit was 3.67-1 172μg/g.The results of precision test showed that the relative standard deviations(RSD,n=7)were between 0.3%and 2.2%for determination results of each component.The proposed method was applied for the analysis of actual samples.The found results were consistent with those obtained by other methods in laboratory.The proposed method could meet the requirements of simultaneous and rapid analysis of multiple components in iron-rich clay samples in field.

关 键 词：X射线荧光光谱仪 深海富铁粘土 主次量组分 粉末压片 

分 类 号：O657.34[理学—分析化学]