Determination of trace lead by catalytic kinetic spectrophotometry based on fading of methyl green oxidized by potassium bromate
ZHANG Yue, LIU Bin*, YANG Huixi, DU Yanping, CHANG Wei
Xi'an Key Laboratory of Textile Chemical Engineering Auxiliaries, School of Environmental and Chemical Engineering, Xi'an Polytechnic University, Xi'an 710600, China
Abstract:In the medium of hydrochloric acid, the oxidant of potassium bromate could oxidize methyl green to fade and decrease its absorbance. Lead ions could catalyze the reaction. Based on this, a determination of trace lead was established by catalytic kinetic spectrophotometry based on the fading reaction of methyl green oxidized by potassium bromate. Two stoppered glass colorimetric tubes of the same specification were taken. One was added with 2.1 mL methyl green solution, 1.0 mL hydrochloric acid, 0.9 mL potassium bromate solution, and a certain amount of lead standard solution, the other was a blank control without lead solution. After reacting in a boiling water bath at 100 ℃ for 10 min, the absorbance of the catalytic system (with lead) and the non-catalytic reaction system (without lead) at the maximum wavelength of 631 nm were determined with an ultraviolet-visible spectrophotometer, and the difference in absorbance was calculated. The results showed that, the lead mass concentration within the range of 0.004-0.12 μg/mL had a good linear relationship with the difference in absorbance, and the correlation coefficient was r=0.999 7. The rate constant of the catalytic reaction was 3.5×10-1 s-1, the apparent activation energy was 11.99 kJ/mol; the limit of detection for the method was 2.8×10-3 μg/mL, and the limit of quantification was 9.5×10-3 μg/mL. The experimental method was applied to the determination of lead in domestic sewage and wastewater of printing and dyeing. The relative standard deviation (RSDs, n=6) of the results were 1.6%-3.6%. The results are basically consistent with atomic absorption spectrometry, and the recoveries were 95%-108%.
张悦, 刘斌, 杨荟茜, 杜燕萍, 常薇. 溴酸钾氧化甲基绿褪色催化动力学光度法测定痕量铅[J]. 冶金分析, 2021, 41(9): 91-95.
ZHANG Yue, LIU Bin, YANG Huixi, DU Yanping, CHANG Wei. Determination of trace lead by catalytic kinetic spectrophotometry based on fading of methyl green oxidized by potassium bromate. , 2021, 41(9): 91-95.
[1] 吴世杰.几种金属基电极制备及在重金属检测中的应用研究[D].济南:山东师范大学,2013. [2] ZHOU Q X,LEI M,LIU Y L,et al.Simultaneous determination of cadmium, lead and mercury ions at trace level by magnetic solid phase extraction with Fe@Ag@Dimercaptobenzene coupled to high performance liquid chromate-graphy[J].Talanta,2017,175:194-199. [3] 马建宏,李阳.石墨炉原子吸收光谱法测定土壤中重金属铅、镉的方法改进[J].理化检验(化学分册),2020,56(1): 94-96. MA Jianhong,LI Yang.An improved method for the determination of lead and cadmium in soil by graphite furnace atomic absorption spectrometry[J].Physical Testing and Chemical Analysis (Part B: Chemical Analysis),2020,56(1): 94-96. [4] RACHA A,MOUNIR A.Determination of trace lead and cadmium in canned soft drinks in Syria[J].Journal of Pharmacy and Bioallied Science,2020,12(3):344-350. [5] 王红专,于红林.阻抑动力学光度法测定水样中的痕量铅[J].河南化工,2016,33(7): 49-52. WANG Hongzhuan,YU Honglin.Determination of trace lead in water sample by inhibitory kinetic spectrophotometry[J].Henan Chemical,2016,33(7):49-52. [6] 李赵平.电感耦合等离子体质谱法测定食用植物油中铅、总砷含量不确定度评定[J].化学分析计量,2020,29(2):118-122. LI Zhaoping.Uncertainty evaluation of determination of lead and total arsenic in edible vegetable oil by inductively coupled plasma mass spectrometry[J].Chemical Analysis and Meterage,2020,29(2):118-122. [7] 王书民, 樊雪梅, 张晓晶, 等.催化动力学光度法测定锌尾矿中痕量铅[J].冶金分析,2013,33(6):42-46. WANG Shumin,FAN Xuemei,ZHANG Xiaojing,et al.Determination of trace lead in zinc tailings by catalytic kinetic spectrophotometry[J].Metallurgical Analysis,2013,33(6):42-46. [8] 孙仓.原子荧光光谱法与ICP-MS法测定水中总铅的比对研究[J].环境研究与监测,2020,33(3):12-15. SUN Cang.Comparative study on determination of total lead in water by atomic fluorescence spectrometry and ICP-MS[J].Environmental Research and Monitoring,2020,33(3):12-15. [9] 卢玉曦,栾锋,刘惠涛.双水杨醛邻苯二胺柱前衍生-高效液相色谱法测定茶叶中的Pb2+[J].色谱,2017,35(8):843-847. LU Yuxi,LUAN Feng,LIU Huitao.Determination of lead in tea leaves by precolumn derivatization of di-salicylaldehyde o-phenylenediamine with high-performance liquid chromatography[J].Chinese Journal of Chromatography,2017,35(8):843-847. [10] 王德利,毕洪梅,徐凤英,等.原子吸收分光光度法测定土壤Cd2+、Pb2+含量的研究[J]. 黑龙江八一农垦大学学报,2006,18(3): 83-85. WANG Deli,BI Hongmei,XU Fengying,et al.Determination of cadmium and lead in soil by atomic absorption spectrometry[J]. Journal of Heilongjiang Bayi Agricultural University, 2006, 18(3): 83-85. [11] 陆渤翰, 李庆乐, 朱薪宇, 等. D113树脂富集-电感耦合等离子体原子发射光谱法测定面制品中铝、镉、铅[J].化工时刊,2019,33(5) 2:10-13. LU Bohan,LI Qingle,ZHU Xinyu,et al.Determination of aluminum, cadmium and lead in flour products by inductively coupled plasma atomic emission spectrometry enriched with D113 resin[J].Chemical Industry Times,2019,33(5):10-13. [12] 林颂和.火焰原子吸收光度法测废水中的铅[J].科技与创新,2014(8): 20-23. LIN Songhe.Determination of lead in wastewater by flame atomic absorption spectrometry[J].Science and Technology & Innovation, 2014(8): 20-23. [13] 贾云海, 孙晓飞, 张帆.用相对标准偏差和相对极差及测量极值比例确定分析检出限和定量限[J].冶金分析, 2021, 41(1): 1-12. JIA Yunhai,SUN Xiaofei,ZHANG Fan.The limit of detection and limit of quantitation were determined by relative standard deviation, relative range and ratio of extreme value[J]. Metallurgical Analysis,2021,41(1):1-12. [14] 田久英, 卢菊生, 吴宏. 阻抑过氧化氢氧化偶氮胂I褪色动力学光度法测定痕量铅和镉[J].冶金分析,2008,23(3):64-67. TIAN Jiuying,LU Jusheng,WU Hong.Determination of trace lead and cadmium by kinetic spectrophotometry with inhibition of discoloration of arsenazo oxide I by hydrogen peroxide[J].Metallurgical Analysis,2008,23(3):64-67. [15] 刘石军, 涂嘉玲, 黄晓辉, 等. 锰矿区受污染水体处理方法研究[J].环境科学与技术,2017,40(S2):243-248. LIU Shijun, TU Jialing, HUANG Xiaohui, et al. Treatment of polluted water with a high concentration of manganese ion from manganese area[J].Environmental Science & Technology,2017,40(S2):243-248.