摘要
为解决酸溶法难以溶解铜精矿的弊端,提出了高温碱熔-电感耦合等离子体原子发射光谱法测定铜精矿中铬含量的方法。称取0.3000 g样品于铁坩埚中,覆盖3.0 g氢氧化钾在样品表面,于300℃加热至氢氧化钾呈流体状后,将铁坩埚放入(700±10)℃的马弗炉中熔融15 min,再加入20 mL盐酸,于300℃加热酸化5 min,冷却至室温,用水定容至200 mL。分取5 mL,加入5 mL盐酸,再用水定容至50 mL,摇匀,按照电感耦合等离子体原子发射光谱仪工作条件进行测定。结果表明:铬的质量浓度在2.00 mg·L^(-1)内与其对应的发射强度呈线性关系,检出限(3 s)为0.92 mg·kg^(-1);方法用于4种铜精矿样品分析,测定值的相对标准偏差(n=12)为3.4%~7.0%,并且测定值与其他CNAS认可实验室的基本一致。
In order to solve the problem that copper concentrate is difficult to be dissolved by acid dissolution method,a method for the determination of chromium in copper concentrate by inductively coupled plasma atomic emission spectrometry with high temperature alkali fusion was proposed.The sample(0.3000 g)was taken and placed into an iron crucible,and 3.0 g of potassium hydroxide was covered on the surface of the sample.After the potassium hydroxide was heated to a fluid shape at 300℃,the iron crucible was put into a muffle furnace at(700±10)℃to melt the sample for 15 min,and then 20 mL of hydrochloric acid was added.The mixture was heated at 300℃for 5 min for acidification.After the mixture was cooled to room temperature,its volume was made up to 200 mL with water.An aliquot(5 mL)was taken,and 5 mL of hydrochloric acid was added.The above mixed sdution was made its volume up to 50 mL.After shaking well,the solution obtained was determined according to the operating conditions of the inductively coupled plasma atomic emission spectrometer.It was shown that linear relationship between the mass concentration and the emission intensity of chromium was found within 2.00 mg·L^(-1),with detection limit(3 s)of 0.92 mg·kg^(-1).The method was applied to the analysis of 4 copper concentrate samples.RSDs(n=12)of the determined values were in the range of 3.4%-7.0%,and the determined results of this method were basically consistent with those of other laboratories accredited by CNAS.
作者
张凤云
蒋磊
肖素群
ZHANG Fengyun;JIANG Lei;XIAO Suqun(Guixi Smelter,Jiangxi Copper Corporation Limited.,Guixi 335424,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2024年第4期394-397,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词
铜精矿
铬
碱熔
电感耦合等离子体原子发射光谱法
copper concentrate
chromium
alkali fusion
inductively coupled plasma atomic emission spectrometry
