摘要
提出了用催化极谱法测定复杂物料中微量砷的含量。选择测定的溶液介质中含碲(Ⅳ)硫酸溶液5mL和150g.L-1碘化钾溶液5mL。仪器扫描速率为250mV.s-1,并采用二阶导数测定。试样(0.01~1.0g)用氯酸钾0.5g、氢氟酸5滴、硝酸5~10mL溶解,用蒸馏法分离其中的砷。砷的质量浓度在0.4mg·L-1以内与相应的峰电流呈线性关系。按此方法测定了12个矿样中砷含量,其测定值与已知值相符。方法的回收率在97%~100%之间,相对标准偏差(n=6)在2.3%~7.2%之间。
It was reported that micro-amount of arsenic in complex materials were determined by catalytic polarography in testing solution containing 5 mL of Te( Ⅳ)-H2 SO4 solution and 5 mL of 150 g · L^-1 of KI solution. Anodic scanning at the rate of 250 mV · s^1 and 2nd derivative of the measured polarographic wave were adopted in the determination. The sample (0. 01-1.0 g) was dissolved in KC103 (0. 5 g), HF (5 drops) and HNOa (5- 10 mL), and As ion was separated by distillation. Linear relationship between values of peak current and mass concentration of As was obtained in the range within 0.4 rag · L^-1. Twelve samples of ores were analyzed by the proposed method for their arsenic contents, giving results consistent with the known values. Values of recovery and RSDrs (n=6) found were in the ranges of 97%-100% and 2. 3%--7. 20%
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2012年第2期201-203,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词
蒸馏
催化极谱法
复杂物料
砷
Distillation
Catalytic polarography
Complex materials
Arsenic