研究表明,当In的共存量大于或等于400倍Cd量时,石墨炉原子吸收光谱(GFAAS)法直接测定Cd的误差≥+5%.采用强酸阳离子交换纤维柱,控制试液流速为0.6 mL/min进行交换,用相同流速的1.2 mol/L HNO_3淋洗交换柱,Cd从纤维柱上首先被洗脱而使之与In达到分离,有效地消除了In对Cd的测定干扰.In与Cd质量比(m_(In):m_(Cd))在100:1～1 000 000:1之间,经过纤维柱分离,GFAAS测定Cd的检出限(3S)为1.5×10~(-5)μg/mL,线性范围为5.0×10~(-5)～1.0×10~(-2)μg/mL;加标回收率为98%～102%,RSD(n=6)为0.8%～1.5%.测定金属铟和硫酸铟中Cd的含量分别为17.6 μg/g和1.86μg/g,加标平均回收率分别为100%和99%,RSD(n=6)分别为2.0%和2.3%.
The research showed that when coexistent amount of indium was greater than or equal to 400 times of cadmium, the relative error of direct determination cadmium by graphite furnace atomic absorption spectrometry (GFAAS) was greater than or equal to +5%. In the paper, a strong acid cation exchange fiber column was used to eliminate interference in the determination of cadmium. Test solution was fed into the column at a flow rate of 0.6 mL/min to perform exchange; then the adsorption column was leached with 1.2 mol/L HNO_3 at the same flow rate; and cadmium eluted at first was separated from indium. When the mass ratio of indium to cadmium (m_(In):m_(Cd)) was between 100 : 1 to 1 000 000 : 1, the detection limit(3S) of Cd by GFAAS was 1.5×10~(-5) μg/mL after the separation by the fiber column. The linear range was from 5.0× 10~(-5)μg/mL to 1.0×10~(-2)μg/mL; the recoveries were in the range of 98% -102%; and RSD (n = 6) were 0.8% -1.5%. Determination result of cadmium in metallic indium and indium sulfate was 17.6 μg/g and 1.86 μg/g, respectively. The average recovery of standard addition was 100% and 99%, and RSD (n=6) was 2.0% and 2.3%.
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