发射光谱法同时测定钛基复合材料中的镍铁钼锰和硼的研究

Study on the Determinations of Ni,Fe,Mo,Mn and B in Ti/TiC Composite Material by Atomic Emission Spectrometry

研究了用碳粉、碳酸钙、氧化铜和氧化铍作缓冲剂同时测定钛基复合材料中的镍、铁、钼、锰和硼的发射光谱法,选择铍作内标线,不需分离、不需化学处理,直接压样于杯形的石墨电极中,具有简便、快速、准确。对测定条件、干扰因素进行了研究,从而建立测定镍、铁、钼、锰和硼的新方法。镍、铁、钼、锰和硼的分析线分别为300·36,248·33,315·82,260·57和249·68nm,内标线选择为铍的298·61nm,镍、铁、钼、锰和硼的线性范围分别为0·003%～0·30%;0·001%～0·20%;0·003%～0·30%;0·001%～0·20%;0·001%～0·20%。镍、铁、钼、锰和硼的检测限分别0·003%,0·001%,0·003%,0·001%,0·001%,其回收率在95·80%～104·8%范围内,当n=9时,相对标准偏差RSD均小于5%。用于样品的测定取得了满意的结果。

The present paper describes the determination of trace Ni, Fe, Mo , Mn and B in Ti/TiC composite material using carbon powder, calcium carbonate, cupric oxide and beryllium oxide as buffer by atomic emission spectrometry（ASE）. Be 298. 61 nm was selected as internal standard line. Sample separation and chemistry treatment were not requirel. The sample was directly loaded into ordinary electrode. The method is simple, rapid and accurate. The requirement of determination, and factors of influence were studied. A new method has developed for the determination of Ni, Fe, Mo, Mn and B. The analysis lines of Ni, Fe, Mo, Mn and B are 300. 36, 248. 33, 315.82, 260. 57 and 249. 68 nm respectively. The internal standard line of Be is 298. 61 nm. The linear ranges of the determination of Ni, Fe, Mo, Mn and B are 0. 003%-0. 30%, 0. 001%-0. 20%, 0. 003%- 0. 30%, 0. 001%-0. 20%, 0. 001%-0. 20% respectively. The detection limits of Ni, Fe, Mo, Mn and B are 0. 003% ; 0. 001%, 0. 003%, 0. 001% and 0. 001% respectively. The ranges of the recovery of Ni, Fe, Mo, Mn and B are 95.80%-104. 8%%, and the standard relative deviations（RSD） are less than 5.0%（n=9）. The method has been applied to the determination of Ni, Fe, Mo , Mn and B with satisfactory results.