丁二酮肟分光光度法测定富铼渣中铼  

Determination of rhenium in rhenium-rich slag by dimethylglyoxime spectrophotometry

作　　者：史谊峰[1] 郑文英[1] 房勇[1] 李君[1] 唐慧[1] 朱利亚 

机构地区：[1]云南铜业股份有限公司,云南昆明650102 [2]贵研资源(易门)有限公司稀贵金属综合利用新技术国家重点实验室,云南昆明650106

出　　处：《冶金分析》2015年第12期68-72,共5页Metallurgical Analysis

基　　金：云南铜业股份有限公司基金资助项目(2014JK003;2014JK005;2014JK006);贵研资源(易门)有限公司横向合作基金资助项目(GYZY-2014-001);云南省地方标准制(修)订基金资助项目(DBZD 052-2015)

摘　　要：称取0.20g样品于高铝坩埚中,置于马弗炉中升温至250℃,恒温30min以驱除硫和砷,再加入3.5g过氧化钠于730℃熔解7min,以水浸出熔融物后,加热微沸约5min以促进过氧化钠产生的过氧化氢分解完全,加水定容后,过滤,加入1滴对硝基酚溶液,滴加盐酸（1＋6）至溶液黄色刚褪去（pH≈1）,加水至20mL,再加入5mL 400g/L柠檬酸溶液、5mL盐酸（1＋3）、5mL 10g/L丁二酮肟乙醇溶液、5mL 250g/L氯化亚锡溶液进行显色测定,建立了丁二酮肟分光光度法测定富铼渣中铼含量的方法。实验表明：铼的质量浓度在100-600μg/100mL范围内与其吸光度符合比尔定律,方法检出限为11.3μg/mL。干扰试验表明样品中共存离子不干扰测定。将方法用于两个富铼渣管理样品及两个实际样品中铼的测定,测定值与参考值相符,相对标准偏差（RSD,n=22）为0.69%-1.1%,回收率为99%-100%。After 0.20 g of sample was transferred into high-aluminum crucible,the crucible was put into muffle furnace at 250℃for 30 min to remove sulfur and arsenic.Then,3.5g of sodium peroxide was added,and they were fused at730℃for 7min.The melt was leached with water,and the solution was heated to slight boiling for about 5min to accelerate the complete decomposition of hydrogen peroxide generated from sodium peroxide.Then,the solution was diluted to the constant volume followed by filtration.One drop of paranitrophenol solution was added and hydrochloric acid（1＋6）was dripped into solution until the yellow color just disappeared（pH≈1）.The solution was diluted to 20 mL.Then,5mL of 400g/L citric acid solution,5mL of hydrochloric acid（1＋6）,5mL of 10g/L dimethylglyoxime ethanol solution and 5mL of 250g/L stannous chloride solution were added for coloring.Consequently,a method was established for determination of rhenium in rhenium-rich slag by dimethylglyoxime spectrophotometry.The experiments showed that Beer＇s law was obeyed for rhenium in mass fraction range of 100-600μg/100 mL with absorbance.The detection limit of method was 11.3μg/mL.The interference test indicated that the coexisting ions in sample had no interference with the determination.The proposed method was applied to the determination of rhenium in two rhenium-rich slag control samples and two actual samples.The results were basically consistent with the reference values.The relative standard deviations（RSD,n=22）were in range of 0.69%-1.1%,and the recoveries were between99%and 100%.

关 键 词：铼 富铼渣 丁二酮肟 分光光度法 

分 类 号：X833[环境科学与工程—环境工程] O657.3[理学—分析化学]