摘要
提出了氢化物发生-原子荧光光谱法测定载金炭中砷的含量。采用硝酸和高氯酸分解载金炭样品，在盐酸（10＋90）溶液中加入溶于5g·L-1氢氧化钾溶液中的20g·L-1硼氢化钾溶液使与溶液中砷（11I）离子反应生成氢化物。分析中采用载气及屏蔽气的流量依次为300mL·min-1及900mL·min-1。试样溶液中加入硫脲抗坏血酸混合溶液作为还原剂。于仪器中引入取样量为1．0mL的试样溶液，按选定的工作条件操作。砷（UI）的质量浓度在120μg·L-1以内与其对应的荧光强度呈线性关系，方法的检出限（3s）为0．05μg·L-1。对10及80μg·L-1砷标准溶液连续进样11次，测定值的相对标准偏差分别为1．29／6和1．0％。应用此法对载金炭样品进行分析，测得砷的回收率在92．8％～101．9％之间。
HC-AFS was applied to the determination of arsenic in gold-loaded carbon. Sample was dissolved with HNO3 and HClO4, and hydride of As（UI） was generated from HC1 （10＋90） solution by reacting with 20 g ·L-1 KBH4 solution （dissolved in 5 g ·L-1 KOH solution）. Flow-rates of 300 mL · min-1 for carrier gas and 900 mL · min-1 for shielding gas were taken in the analysis. Mixed solution of thiourea and ascorbic acid was added to the water sample as reductant. One mL of sample solution was introduced and operated under the prescribed working condition of the instrument. Linear relationship between the fluorescence intensity and mass concentration of As（N） was found in the range within 120μg·L-1, with detection limit （3S/N） of 0. 05μg·L-1. Tests for precision were performed with 10 μg·L-1 and 80 μg·L-1 of As by addition of standard solution, values of RSD＇s （n=11） found were 1.2% and 1.0% respectively. The proposed method was applied to the analysis of samples of gold-loaded carbon, giving values of recovery in the range of 92.8%- 101.9%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2011年第9期1046-1048,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
