氢化物-原子荧光光谱法测定高纯铅中微量锡  

DETERMINATION OF TIN IN PURE LEAD METAL BY HYDRIDE GENERATION ATOMIC FLUORESCENCE SPECTROMETRY

作　　者：冯先进[1] 王肇中[1] 卓毓瑞 师世龙 符斌[1] 

机构地区：[1]北京矿冶研究总院,北京100044 [2]中金岭南铅锌分公司韶关冶炼厂,广东韶关512000

出　　处：《有色金属》2001年第4期91-94,共4页Nonferrous Metals

摘　　要：在试验基础上 ,研究高纯铅中微量锡的氢化物 -原子荧光光谱简便、快速测定方法。最佳仪器条件和最佳测定条件为 :负高压 30 0V ;测定灯电流 80mA ;原子化器温度为 2 0 0℃ ;载气流量和屏蔽气流量分别为 40 0mL/min和 80 0mL/min;1.5 %硫酸介质 ;5g/L硫脲和 5 g/L抗坏血酸。试样采用硫酸溶解 ,加热冒干硫酸烟后 ,在 1.5 %硫酸介质中进行测定。锡的检测限为 0 40ng/mL ,检出限小于 1μg/g ,样品加标回收率在 86 %～ 10 7%之间 ,对含锡 2 .5 μg/g样品的测量精密度RSD为 9.2 %。A simple and rapid method for the determination of trace amount of tin in pure lead metal by spiccato flow hydride generation atomic fluorescence spectrometry (HG AFS) is described. Optimum instrumental and analytical conditions for determining the tin are: PMT 300V;lamp current 80mA;atomizer temperature 200℃;400 and 800 mL/min flow rate of carrier gas and shield gas respectively;1.5%sulfuric acid medium;5g/L thiourea +5g/L ascorbic acid. The sample is dissolved in sulfuric acid solution and dried by evaporating on an electrothermal plate, then determined in 1.5% sulfuric acid medium. The detection limits for tin is 0.40ng/mL (3σ). Less than 1μg/g of tin in sample can be determined accurately. The analytical result is accordant with the certificate value. The recoveries of standard addition for tin are between 86% and 107%. The RSD for the determination of 2.5 μg/g sample is 9.2%. The procedure has been applied to the determination of trace amount of tin in pure lead metal and in lead ingot samples.

关 键 词：氢化物-原子荧光光谱法 高纯铅 锡 测定 

分 类 号：TG146.12[一般工业技术—材料科学与工程] O657.31[金属学及工艺—金属材料]