冶金分析
冶金分析
야금분석
METALLURGICAL ANALYSIS
2010年
4期
9-13
,共5页
潘雪珍%龚琦%韦小玲%董兰芳%陈杰
潘雪珍%龔琦%韋小玲%董蘭芳%陳傑
반설진%공기%위소령%동란방%진걸
强酸阳离子交换纤维%铟%镉%石墨炉原子吸收光谱法
彊痠暘離子交換纖維%銦%鎘%石墨爐原子吸收光譜法
강산양리자교환섬유%인%력%석묵로원자흡수광보법
strong acid cation exchange fiber%indium%cadmium%graphite furnace atomic absorption spectrometry (GFAAS)
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%.
研究錶明,噹In的共存量大于或等于400倍Cd量時,石墨爐原子吸收光譜(GFAAS)法直接測定Cd的誤差≥+5%.採用彊痠暘離子交換纖維柱,控製試液流速為0.6 mL/min進行交換,用相同流速的1.2 mol/L HNO_3淋洗交換柱,Cd從纖維柱上首先被洗脫而使之與In達到分離,有效地消除瞭In對Cd的測定榦擾.In與Cd質量比(m_(In):m_(Cd))在100:1~1 000 000:1之間,經過纖維柱分離,GFAAS測定Cd的檢齣限(3S)為1.5×10~(-5)μg/mL,線性範圍為5.0×10~(-5)~1.0×10~(-2)μg/mL;加標迴收率為98%~102%,RSD(n=6)為0.8%~1.5%.測定金屬銦和硫痠銦中Cd的含量分彆為17.6 μg/g和1.86μg/g,加標平均迴收率分彆為100%和99%,RSD(n=6)分彆為2.0%和2.3%.
연구표명,당In적공존량대우혹등우400배Cd량시,석묵로원자흡수광보(GFAAS)법직접측정Cd적오차≥+5%.채용강산양리자교환섬유주,공제시액류속위0.6 mL/min진행교환,용상동류속적1.2 mol/L HNO_3림세교환주,Cd종섬유주상수선피세탈이사지여In체도분리,유효지소제료In대Cd적측정간우.In여Cd질량비(m_(In):m_(Cd))재100:1~1 000 000:1지간,경과섬유주분리,GFAAS측정Cd적검출한(3S)위1.5×10~(-5)μg/mL,선성범위위5.0×10~(-5)~1.0×10~(-2)μg/mL;가표회수솔위98%~102%,RSD(n=6)위0.8%~1.5%.측정금속인화류산인중Cd적함량분별위17.6 μg/g화1.86μg/g,가표평균회수솔분별위100%화99%,RSD(n=6)분별위2.0%화2.3%.
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%.