摘要
建立了火焰原子吸收光谱法测定高铼酸、高铼酸铵、铼粉中痕量钠的方法,对样品的预处理和测定钠的条件进行了研究。结果表明：水溶解法、硝酸溶解法或硝酸-硫酸溶解法溶解样品完全,测得钠的结果吻合;于选定条件下,钠的测定浓度在0.020 0~0.500 0μg/mL范围内线性良好;测定高铼酸、高铼酸铵和铼粉样品中0.27~0.47mg/L、0.000047%~0.00048%和0.000040%~0.00049%的钠含量,检出限、相对标准偏差（RSD,n=7）、加标回收率分别为高铼酸3×10-4μg/mL、6%~10%、98%~102%,高铼酸铵3×10-4μg/mL、8%~9%、96%~102%和铼粉3×10-4μg/mL、5%~9%、96%~103%。方法结果准确、分析快速、操作简便,应用于实际的样品分析,结果满意。
A method for the determination of trace sodium in perrhenic acid,ammonium perrhenate and rhenium powder by flame atomic absorption spectrometry was proposed.Samples pretreatment and experimental conditions for sodium analysis were researched.The results indicated that analytical results by water dissolving method were in good accord with those obtained by nitric acid dissolution method and nitric acid-sulphuric acid dissolution methods.Sodium concentration had a good linear relationship in the range of 0.020 0~0.500 0μg/mL under the optimized conditions.The concentration ranges for perrhenic acid,ammonium perrhenate and rhenium powde were 0.27~0.47 mg/L,0.000047% ~0.00048% and0.000040%~0.00049%,respectively.The detection limits,relative standard deviations（RSDs,n=7）and recoveries for sodium were 3×10-4μg/mL,6%~10% and 98%~102%（perrhenic acid）,3×10-4μg/mL,8%~9% and 96%~102%（ammonium perrhenate）and 3×10-4μg/mL,5%~9% and 96%~103%（rhenium powde）,respectively.The proposed method is accurate,rapid and convenient,and has been applied to the determination of trace sodium in actual sample with satisfactory results.
出处
《中国无机分析化学》
CAS
2015年第4期60-64,共5页
Chinese Journal of Inorganic Analytical Chemistry
基金
云南铜业股份有限公司基金项目(2014JK003
2014JK005
2014JK006)
贵研资源(易门)有限公司横向合作基金项目(GYZY-2014-001)资助
关键词
钠
痕量
铼产品
火焰原子吸收光谱法
sodium
trace
rhenium products
flame atomic absorption spectrometry
