Abstract:A cheap, rapid and sensitive method for the determination of trace amount of lead in water samples by graphite furnace absorption spectrometry coupled with online flow injection preconcentration with ammonium pyrrolidine dithiocarboxylate chelating cellulose (CC-APDC) was developed. There were six steps in the preconcentration of flow injection: first, 0.15 mL nitric acid was used for a complete elution,which exceeded the volume of the graphite tube, so the 40 mL solution was removed before eluting. Secondly, 40 mL maximum concentration elution solution was added to GFAAS by fixed volume sampling to improve the accuracy. In addition, traditional stopping gas measurement was substituted with small flow gas atomization (30 mL·min-1,preconcention for 1 min) during the removal of high memory effect for ashing stage in graphite furnace, which develops tail-out phenomenon and makes blank value low and steady. Various parameters affecting the adsorption and elution, such as pH of the solution, eluent concentration, sample flow rate etc, were optimized. If miniflow in atomization step was used, the memory effect in the determination of lead by GFAAS could be removed. The CC-APDC was used for preparation and preconcentration. A good precision (RSD=1.4%, n=10), high enrichment factor (15) and sample throughput (50 h) with detection limit 0.12 μg·L-1 were obtained. This method has been successfully applied to the water sample for lead determination with a recovery of 95%-105%.
陈中兰. 螯合棉纤维预富集流动注射在线测定痕量铅[J]. 光谱学与光谱分析, 2007, 27(06): 1243-1245.
CHEN Zhong-lan. Determination of Lead with GFAAS Using Online Flow Injection. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2007, 27(06): 1243-1245.
[1] Welz B, Yin X, Sper Ling M. Anal. Chim. Acta,1992,261:477. [2] Sper Ling M, Yin X, Welz B. Analyst, 1992, 117: 629. [3] ZHANG Yuan, LUO Wen-hong, LI Hui(张 源, 罗文鸿, 李 慧). Spectroscopy and Spectral Analysis(光谱学与光谱分析),2006,26(7):1349. [4] SUN Han-wen, WEN Xiao-hua, LIANG Shu-xuan(孙汉文,温晓华,梁淑轩). Spectroscopy and Spectral Analysis(光谱学与光谱分析),2006,26(5):950. [5] ZHANG Han-ping, ZHAO Qiu-xiang, ZHANG Xue-rong(张汉萍,赵秋香,张雪容). Physical Testing and Chemical Analysis,Part B: Chemical Analysis(理化检验-化学分册),2006,42(9):705. [6] FAN Chun-lei, LIANG Zhen-yi(范春蕾,梁振益). Chemical Analysis and Meterage(化学分析计量),2006,15(2):30. [7] LIAN Hong-fang(连红芳). Shanxi Chemical Industry(山西化工),2005,25(3):21. [8] CHEN Zhong-lan,WANG Mo-hui(陈中兰, 汪模辉). Chinese Journal of Analytical Chemistry(分析化学),1997, 25(6):714. [9] CHEN Zhong-lan(陈中兰). Spectroscopy and Spectral Analysis(光谱学与光谱分析),1998,18(15):601. [10] CHEN Zhong-lan(陈中兰). Spectroscopy and Spectral Analysis(光谱学与光谱分析),2002, 22(5):865. [11] CHEN Zhong-lan(陈中兰). Chemical Journal of Chinese Universities(高等学校化学学报),1999,20(5):198. [12] CHEN Zhong-lan, WANG Mo-hui, SU Qing-ping(陈中兰, 汪模辉, 苏庆平). Acta Polymerica Sinica(高分子学报),1998, (3):368. [13] WANG Ge-hui, SONG Zhan-qian(王格慧,宋湛谦). Chinese Journal of Applied Chemistry(应用化学),2001,18(10):831. [14] CHEN Zhong-lan(陈中兰). Chinese Journal of Applied Chemistry(应用化学),2002,19(11):1098. [15] CHEN Zhong-lan, CHEN Long-sheng(陈中兰,陈龙生). Ion Exchang and Adsorption(离子交换与吸附),2002,18(5):464.