发射光谱法测定乳浊料中的锆和铪

Determination of Trace Zirconium and Hafniumin Sample by Atomic Emission Spectrometry

研究了用碳粉和二氧化钛作缓冲剂同时测定乳浊料中的锆和铪的发射光谱法,选择钛作内标线,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、准确的特点。对测定条件、干扰因素进行了研究,从而建立测定锆和铪的新方法。锆和铪的分析线分别为3273和2866nm,内标线选择为钛的3088nm线,锆和铪的线性范围分别为0～050%和0～025%。锆和铪的检测限分别为0001%和0010%,其回收率为9667%～1050%,当n=9时,锆的RSD为361%;铪的RSD为482%;用于样品的测定取得了满意的结果。

This paper describes the determination of trace Zr and Hf in the sample using carbon powder and titanium oxide as the buffer by Atomic Emission Spectrometry (AES). Titanium was selected for the internal standard line. Sample separation and chemical treatment were not required. The sample was directly loaded into an ordinary electrode. The method is simple, rapid and accurate. The conditions for the determination, and the factors of influence have been studied. A new method has been developed for the determination of zirconium and hafnium. The analytical lines of Zr and Hf were 327.3 and 286.6 nm respectively. The internal standard line of Ti was 308.8 nm. The linear range of the determination of Zr and Hf was 0-0.50% and 0-0.25% respectively. The detection limit of Zr and Hf was 0.0010% and 0.010% respectively. The range of the recovery of zirconium and hafnium was 96.67%-105.0%. The results for these elements in standard sample are in agreement with certified values with a precision of 3.61% RSD for Zr (n = 9), and 4.82% RSD for Hf (n = 9). The method has been applied to the determination of Zr and Hf with satisfactory results.