建立了萃取镉的乙醇-硫酸铵双水相体系。以火焰原子吸收光谱法(FAAS)为检测手段,研究了乙醇-硫酸铵双水相萃取镉的主要影响因素,并且利用FT—IR光谱,对其萃取机理进行了初步的探讨。实验结果表明,Cd^2+与I^-、结晶紫在pH5.0~6.0的乙醇-硫酸铵双水相体系中形成稳定的紫色络合物,在最佳萃取条件下,镉能很好地与其他常见的金属离子分离,萃取率达到100%。该方法测定镉的线性范围为0~0.50μg/mL,相关线性系数为0.9993,方法检出限为0.012μg/mL。用于环境水样中镉量的测定,相对标准偏差为为2.8%~3.6%,加标回收率大于95%。
The ethanol-ammonium sulfate two-phase extraction system for cadmium was developed. The main influencing factors for the extraction of cadmium by ethanol-ammonium sulfate two-phase system were investigated with flame atomic absorption spectrometry (FAAS). Moreover, the extraction mechanism was preliminarily discussed by Fourier transform infrared spectrometry (FT-IR). The results showed that Cd^2+ could form stable purple complex with I and crystal violet in ethanol-ammonium sulfate two-phase system at pH 5.0--6.0. Under the optimal extraction conditions, cadmium could be well separated from other common metal ions. The extraction rate was up to 100 %. The linear range of calibration curve was 0--0.50 μg/mL, with the linear correlation coefficient of 0. 999 3 and the detection limit of 0. 012 μg/mL. The proposed method was applied to the determination of cadmium in environmental water samples. The relative standard deviations (RSD) were 2. 8 %- 3.6 % ,and the recoveries were higher than 95%.