石墨炉原子吸收光谱法测定玻璃器皿浸出的锑量

GFAAS Determination of Microamounts of Antimony Eroded from Glass Hollow Wares

用乙酸(4+96)浸泡玻璃器皿24 h±10 min,使锑离子从玻璃器皿样品中浸出。用石墨炉原子吸收光谱法测定所得溶液中锑量,测定中加入铜(Ⅱ)离子作基体改进剂并采用氘灯扣背景,在制作工作曲线及空白溶液时采用与试样处理匹配的方法抵消了由乙酸存在而引起的误差。对石墨炉的升温程序,特别是灰化温度和原子化温度做了试验并对相关条件予以优化。结果表明:在所测得的吸光度与锑(Ⅲ)的质量浓度在20μg·L-1以内呈线性关系,方法的检出限(3S/b)为0.483μg·L-1,锑的特征浓度为0.396 pg/1%。用标准加入法做了回收试验,测得回收率在93%～104%之间。

Sample of transparent glass hollow-ware was soaked in HOAc（4＋96） to dissolve antimony from the sample. GFAAS was used to determine the amount of antimony eroded from the hollow-ware within definite time of soaking. Cupric ion solution was added as matrix modifier and background correction with deuterium lamp was adopted in GFAAS determination. Matching method was used in preparation of calibration curve and blank solution to compensate the error arisen from the presence of acetic acid. Conditions of the temperature elevation program, especially the temperature for ashing and atomization, were tested and optimized. Linear relationship between values of absorbance and mass concentration of antimony was obtained in the range within 20 μg·L^-1. Detection limit （3S/b） and characterization concentration of the method found for antimony were 0. 483 μg ·L^-1 and 0. 396 pg/1% respectively. Test for recovery was made by standard addition method, and values of recovery found were in the range of 93%-104%.