氢化物发生—原子荧光光谱法测定地质样品中的锑(Ⅲ)和锑(Ⅴ)

THE DETERMINATION OF ANTIMONY(Ⅲ) AND ANTOMONY(Ⅴ) IN GEOLOGICAL SAMPLES BY HYDRIDE GENERATION-ATOMIC FLUORESCENCE SPECTROMETRY

提出了一种氢化物发生—原子荧光光谱法测定地质样品(水系沉积物)中Sb(Ⅲ)和Sb(Ⅴ)的方法。选取4.8 mol/L HCl为提取剂,采用超声波辅助提取,以6 g/mL柠檬酸钠作为Sb(V)的掩蔽剂,在0.24 mol/L的HCl介质中选择性测定Sb(Ⅲ),用差减法求得Sb(Ⅴ)。Sb(Ⅲ)的方法检出限为0.075×10-6,Sb(Ⅴ)的方法检出限为0.097×10-6。对40 ng/mL的Sb(Ⅲ)和Sb(Ⅴ)分别连续测定11次,得到相对标准偏差分别为1.1%和0.64%。应用该方法对地质样品中的Sb(Ⅲ)和Sb(Ⅴ)进行分析测定,并与王水溶解值相比较,该方法测定的总Sb提取率在80%以上,Sb(Ⅲ)和Sb(Ⅴ)的加标回收率分别为83%～107%和98%～114%。

A method for the determination of antimony （Ⅲ） and ANTOMONY （Ⅴ） in geological samples （ stream sediments） by hydride generation-atomic fluorescence spectrometry was developed in the paper. 4.8 mol/L HCI could be used as the extractant with ultrasonic-assisted extraction. In the medium of 0.24 moL/L hydrochloric acid, antimony （Ⅲ ） could be alternatively determined with 6 g/mE sodium citrate as the masking agent for Sb （Ⅴ）. Then antimony （Ⅴ） could be figured out by the subtraction method. The detection limit of the method was 0. 075 ×10 -6 for Sb （ Ⅲ） and 0.097 × 10 -6 for Sh （Ⅴ）, and the relative standard deviation was 1.1% arid 0.04% （ n = 11 ） for 40 ng/mL Sb （ Ⅲ ） and 40 ng/mL Sb（Ⅴ） standard solution. The proposed method was applied to the determination of antimony （ Ⅲ） and antimony （Ⅴ） in geological samples, and a comparison between the extraction results and the aqua regia dissolution results shows that the extraction rate of antimony was higher than 80%, the recoveries were in the ranges of 83% - 107% and 98% - 114% for Sb （Ⅲ） and Sb （Ⅴ） respectively.