Analysis of Lead in Unknown Samples Based on the Standard Addition Method Using Laser Induced Breakdown Spectroscopy
FANG Li1, ZHAO Nan-jing1, MENG De-shuo1, YUAN Jing2, TANG Jie2, WANG Yin1, YU Yang1, MA Ming-jun1, HU Li1, ZHANG Da-hai1, XIAO Xue1, WANG Yu1, LIU Jian-guo1, LIU Wen-qing1
1. Anhui Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Key Laboratory of Environmental Optics and Technology, Hefei 230031, China 2. Yangzhou Environmental Monitoring Center, Yangzhou 225007, China
Abstract：The standard addition method with laser induced breakdown spectroscopy was used to analyze an unknown sample taken from a lead battery factory. the matrix influence on the results was effectively avoided when the external or internal standard method was used, and the pretreatment of samples was simple and quick. The Nd∶YAG pulse laser with wavelength 1 064 nm was used as the excitation source. The echelle spectroscopy with high resolution and wide spectral range was used as the spectral separation device, and the intensified charge coupled device (ICCD) as the spectral detection device in the experiment. The characteristic line at 405.78 nm was chosen as the analysis line to measure Pb concentration. FeⅠ: 404.58 line was chosen as the internal standard. Pre-experiment was carried out to confirm the appropriate condition. Under the laser energy of 128.5 mJ, the delay time of 2.5 μs, and the gate width of 3 μs, it was determined that with the addition of Pb to the sample in the range of 0 and 25 000 mg·kg-1, there wasn’t self-absorption. There was a good linear relationship between the intensity of the spectral line of 405.78 nm and the addition of Pb. The appropriate concentration of Pb added into the sample for analysis was determined by this series of samples. On this basis, four samples were prepared with three parallel samples for each sample in order to verify the repeatability and reliability of the method, i.e. 5 000, 10 000, 15 000, 20 000 mg·kg-1 Pb was added into the original sample. The results were compared with the result of ICP-MS. The twelve samples’ relative errors were between -24.6% and 17.6%. The average result was 43 069 mg·kg-1 with the relative error -2.44%.
方 丽1，赵南京1，孟德硕1，袁 静2，汤 洁2，王 寅1，余 洋1，马明俊1，胡 丽1，张大海1，肖 雪1，王 煜1，刘建国1，刘文清1 . 激光诱导击穿光谱结合标准加入法定量分析未知样品中铅含量 [J]. 光谱学与光谱分析, 2015, 35(01): 208-211.
FANG Li1, ZHAO Nan-jing1, MENG De-shuo1, YUAN Jing2, TANG Jie2, WANG Yin1, YU Yang1, MA Ming-jun1, HU Li1, ZHANG Da-hai1, XIAO Xue1, WANG Yu1, LIU Jian-guo1, LIU Wen-qing1 . Analysis of Lead in Unknown Samples Based on the Standard Addition Method Using Laser Induced Breakdown Spectroscopy . SPECTROSCOPY AND SPECTRAL ANALYSIS, 2015, 35(01): 208-211.
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