CAJ | 학술논문

使用电感耦合等离子原子发射光谱(ICP-AES)研究了贵金属铑和NaBH_4在酸性水溶液中的化学蒸气发生反应的条件,并测定了有机合成催化剂中的铑.研究结果表明: 在NaBH_4和样品溶液流速为2 mL/min、废液排放流速为6 mL/min的条件下的最佳蒸气发生条件为:载气流速0.4 L/min、HNO_3浓度为1.0 mol/L、NaBH_4浓度为1.2%(m/V).研究中获得的铑化学蒸气进样效率是常规的气动雾化进样效率的2.7倍;检出限是6.9 μg/L, 略优于气动雾化法;线性范围20～1500 μg/L;线性相关系数是0.9986;RSD是1.6%.样品分析加标回收率分别是94%和97%.用本法测得的样品值与原子吸收法的测得值吻合很好.
사용전감우합등리자원자발사광보(ICP-AES)연구료귀금속로화NaBH_4재산성수용액중적화학증기발생반응적조건,병측정료유궤합성최화제중적로.연구결과표명: 재NaBH_4화양품용액류속위2 mL/min、폐액배방류속위6 mL/min적조건하적최가증기발생조건위:재기류속0.4 L/min、HNO_3농도위1.0 mol/L、NaBH_4농도위1.2%(m/V).연구중획득적로화학증기진양효솔시상규적기동무화진양효솔적2.7배;검출한시6.9 μg/L, 략우우기동무화법;선성범위20～1500 μg/L;선성상관계수시0.9986;RSD시1.6%.양품분석가표회수솔분별시94%화97%.용본법측득적양품치여원자흡수법적측득치문합흔호.
An inductively coupled plasma atomic emission spectrometry(ICP-AES) combined with a boron hydride vapour generation device was used for the determination of rhodium in waste catalyst. When the flow rate of sample and sodium borohydride solution was 2 mL/min, waste rate was 6 mL/min, the optimum conditions were as follows: 0.4 L/min of carrier rate, 1.0 mol/L of acidity of nitric acid for vapor generation and concentration of sodium borohydride 1.2(m/V). The study showed that a two-fold increase in the efficiency of rhodium was achieved as compared to nebulization. The detection limit was 6.9 μg/L, which is slight better than that of with nebulization. The linear range for rhodium was 20-1500 μg/L with a correlation coefficient of 0.9986. The mean recovery of sample analysis was 95.5%. Excellent agreement was found between the present method and FAAS.