摘要
本着减少环境污染、提高工作效率，建立了一种操作简单、准确测定硫磺中微量砷的微波消解．原子荧光．标准加入法。采用HNO，对硫磺进行微波消解，功率经过14min达到600W并保持20min；光电倍增管负高压为280V，灯电流为80mA，原子化器高度为8mm，载气流量为300mL／min，屏蔽气流量为800ml/min；采用标准加入法对样品中微量砷进行定量。结果表明，砷的线性范围为：0．25～15μg/L（r=0．9999），检出限为：0．03ug／L，加标平均回收率为99．6％（RSD≤1．8％）。与用于硫磺中砷含量测定的二乙基二硫代氨基甲酸银分光光度法（Ag．DDC）相比较．微波消解-原子荧光-标准加入法具有样品用量少、所需试剂种类少、无环境污染、操作简单、灵敏度高、测量数据准确等优点，适合硫磺中微量砷含量的检测。
With the purpose of environment pollution reducing,a rapid and accurate method for the deter- mination of micro arsenic in sulfur by microwave digestion-atomic fluorescence spectrophotometer-standard addition method has been established. The samples were processed by microwave digestion with HNO3 as digestion reagent,and the digestion power was risen to 600 W by 14 min ,and 600 W keeping 20 min. The detections were done at 280 V ,80 mA,8 mm,300 mL/min and 800 mL/min. The standard addition method was used for the quantitative detection of micro arsenic. The result showed that the linear range of arsenic was 0.25 - 15 μg/L （ r = 0.999 9 ）. The detection limit of arsenic was 0.03 μg/L. The average re- cover）, was 99.6% （ RSD ≤ 1.8% ）. Compared with Ag-DDC, microwave digestion-atomic fluorescence spectrophotometer-standard addition method is less samples and reagents, non pollution, easy operation, rapid, reproducible and accurate. It can be used for the determination of micro arsenic in sulfur.
出处
《应用化工》
CAS
CSCD
2013年第11期2108-2111,2114,共5页
Applied Chemical Industry
关键词
原子荧光法
微波消解
标准加入法
硫磺
砷
atomic fluorescence spectrophotometer
microwave digestion
standard addition method
sul-fur
arsenic
