论文部分内容阅读
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 established. The pretreatment of samples and the determination of sodium conditions were studied. The results showed that the dissolution of the sample by the water dissolution method, the nitric acid dissolution method or the nitric acid-sulfuric acid dissolution method was completely and the sodium results were in good agreement. Under the selected conditions, the sodium concentration was within the range of 0.020 0-0.500 0 μg / mL, The detection limits, relative standard deviations (RSDs, n = 7) for the sodium contents of 0.27 ~ 0.47mg / L, 0.000047% ~ 0.00048% and 0.000040% ~ 0.00049% of perrhenic acid, The recoveries of standard addition were 3 × 10-4 μg / mL, 6% -10%, 98% -102%, ammonium perrhenate 3 × 10-4 μg / mL, 8% -9%, 96% 102% and rhenium powder 3 × 10-4μg / mL, 5% ~ 9%, 96% ~ 103%. The method is accurate, rapid, easy to operate, and is applied to practical sample analysis with satisfactory results.