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激光诱导击穿光谱法测定铅泥废渣中的铅含量

Determination of Pb in Waste Lead Mud by Laser Induced Breakdown Spectroscopy
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摘要 铅泥废渣样品经105℃烘干3h,并研磨至通过0.075mm筛。称取此样品与石墨按1∶4~1∶29的质量比混合,两者的总质量为3.00g,充分混匀后压制成直径为30 mm,厚度为3mm的圆片,采用激光诱导击穿光谱法(LIBS)测定其中铅含量。选择铅的灵敏谱线405.78nm为分析线,仪器的采样门宽和延迟时间依次选为5.5,4.0μs。铅的拟合线性关系在10 000μg·g^(-1)以下,方法的检出限为345.2μg·g^(-1)。对同一样品用电感耦合等离子体原子发射光谱法测定其中铅含量并与LIBS结果进行比较。结果表明:两种方法的结果之间存在一定误差,当铅从约9 000μg·g^(-1)降低至约1 500μg·g^(-1)时,其相对误差从约1.3%增加至约15%,平均相对误差为6.80%。 The sample of waste lead mud was dried at 105 ℃ for 3 h and pulverized to pass through sieve with mesh of 0. 075 mm Portions of the pulverized sampIe were taken to mix thoroughly with graphite powder in the mass ratios from 1 to 4 to 1 to 29 to give total mass of 3.00 g for each portion. The mixtures were pressed and separated to give sample discs having 30 mm in diameter and 3 mm in thickness; and lead content of each disc was determined by laser induced breakdown spectroscopy (LIBS). The sensitive spectral line of 405.78 nm of lead was chosen as the analytical spectral line, and the width of sampling inlet and the delay time were chosen at 5.5, 4. 0μs respectively. Fitting linear relationship for Pb was found in the range within 10 000μg · g^-1. Value of detection limit found was 345.2 μg · g^-1. ICP AES was applied to determine lead in a same sample as a check for the LIBS determination. It was shown by the comparative study that obvious deviations were observed between the results of LIBS and ICP-AES, showing an increase of relative deviation from ca. 1. 3% to ca. 15% as the lead content decreases from ca. 9 000μg · g^-1 to ca. 1 500 μg · g^-1, giving an average relative deviation of 6.80%.
出处 《理化检验(化学分册)》 CAS CSCD 北大核心 2017年第2期196-200,共5页 Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词 激光诱导击穿光谱法 铅泥废渣 Laser induced breakdown spectroscopy Lead Waste lead mud
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