预焙阳极微量元素XRF测定方法的研究  

Determination of Minor Elements in Prebaked Anode by X-ray Fluoresence Spectrometry

作　　者：马慧侠[1] 张爱芬[1] 李智慧[1] 

机构地区：[1]中国铝业股份有限公司郑州研究院,河南郑州450041

出　　处：《分析测试学报》2008年第9期998-1001,1004,共5页Journal of Instrumental Analysis

摘　　要：使用X射线荧光光谱法测定预焙阳极中的微量和痕量元素,以粉末压片法制样,选用瑞士R&D碳素公司的C-300系列标准样品,并用仪器软件Super Q中提供的飞利浦模式的经验系数(Classic)和铑(Rh)靶康普顿散射线内标法校正元素间的谱线重叠干扰和基体效应,通过充分研磨样品消除颗粒效应,使用Magix(PW2403)X射线荧光光谱仪对样品中的F、Na、Mg、Al、Si、P、S、Cl、K、Ca、Ba、Ti、V、Cr、Mn、Fe、Ni、Cu、Zn、Pb、Sr和Sn共22个元素进行测定,11次测定的相对标准偏差小于10%,多数元素的检出限小于1μg.g-1。用R&D标准样品的混合样验证,测量结果与标准值的误差在化学分析允许范围内。A method has been developed for the determination of minor and trace elements, viz. F, Na, Mg, Al, Si, P, S, Cl, K, Ca, Ba, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Pb, SrandSn in prebaked anode by X-ray fluorescence spectrometer （Magix PW2403 ） with pressed powder pellet sample preparation technique and C -300 serial standard samples（ Switzerland R ＆ D carbon company）. The interelement and matrix effects were corrected by using empirical alpha（a） coefficient program（Classic） provided by the Super Q software and by using RhK Compton scattered line as internal standard. The precision of the method has been examined by analyzing a prebaked anode standard sample 11 times. The relative standard deviations （RSD）obtained for those elements were less than 10%. The detection limits for most of the elements were less than 1 μg·g^-1. The accuracy of the method has been evaluated by analyzing four C - 300 standard reference samples （ Anode - mix 1 to 4） ; the discrepancies between the results obtained by the present method and the certified values were within the allowable range of chemical analysis.

关 键 词：X射线荧光光谱 经验系数 散射线内标法 预焙阳极 粉末压片法 

分 类 号：O657.34[理学—分析化学]