X射线荧光光谱法测定粗氢氧化钴中钴、锰、铜的含量

Determination of Cobalt,Manganese and Copper in Crude Cobalt Hydroxide by X-ray Fluorescence Spectrometry

为了加快进口粗氢氧化钴的通关时效,缓解买卖双方的贸易纠纷,需要一种准确快速的获得粗氢氧化钴中钴、锰、铜含量的检测方法,采用高温熔融制成玻璃片的前处理方式,通过X射线荧光光谱法测定粗氢氧化钴中钴、锰、铜的含量。重点考察混合熔剂、试样与熔剂稀释比、熔融温度、熔融时间、氧化剂、内标物等影响因素。通过一系列实验获得的最佳条件为以氧化镱为内标物,以四硼酸锂-偏硼酸锂(质量百分比1∶1)为混合熔剂,试样与熔剂稀释比为1∶30,硝酸锂(220 g/L)为氧化剂,溴化锂(600 g/L)为脱模剂,在1050℃下熔融6 min制成试样片,并且采用高纯物质人工配制校准标准样品制定标准曲线。实验结果表明,钴、锰和铜的测定范围(质量分数)分别为10%~60%,0.1%~12%,0.1%~12%,方法具有较好的准确度和精密度,能快速、准确测定粗氢氧化钴中钴、锰、铜的含量,并且应用于实际粗氢氧化钴样品的检测,取得了满意的结果。

In order to speed up the time of customs clearance of imported crude cobalt hydroxide and ease the trade disputes between the buyer and the seller,it is needed to accurately and quickly obtain the content of cobalt,manganese and copper in crude cobalt hydroxide.So a method for determination of cobalt,manganese and copper in crude cobalt hydroxide by X-ray fluorescence spectrometry was developed.At the same time,the pretreatment method of high temperature melting is used to make glass sheets.Several influencing factors were investigated,including the mixed flux,the dilution ratio between sample and flux,the melting temperature and time,the oxidant,and the internal standard substance.It was found that the sample could be well prepared under the following conditions:ytterbium oxide as internal standard substance,Na_(2)B_(4)O_(7)-Li_(2)B_(4)O_(7)(m∶m=1∶1)as mixed flux,dilution ratio between sample and flux was 1∶30,LiNO_(3)(220 g/L)as oxidant,LiBr(600 g/L)as release agent,melting at 1050℃for 6 min to make sample sheet.The calibration standard samples were manually prepared with high purity materials to make standard curves.The experimental results show that the determination range(mass fraction)of cobalt,manganese and copper is 10%-60%,0.1%-12%,0.1%-12%,respectively.The method has good accuracy and precision,can quickly and accurately determine the content of cobalt,manganese and copper in crude cobalt hydroxide.It has been applied to the detection of practical crude cobalt hydroxide samples with satisfactory results.