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作 者:喻旭东 张莉丽 陈坤锋 项毅 罗晟 朱日龙[1] YU Xudong;ZHANG Lili;CHEN Kunfeng;XIANG Yi;LUO Sheng;ZHU Rilong(College of Chemistry and Chemical Engineering,Hunan University,Changsha 410014,China;Yiyang Institute of Metrology,Yiyang413000,China;Changde Institute of Metrology,Changde 415000,China)
机构地区:[1]湖南大学化学化工学院,长沙410082 [2]益阳市计量测试检定所,湖南益阳413000 [3]常德市计量测试检定所,湖南常德415000
出 处:《化学分析计量》2020年第1期103-107,共5页Chemical Analysis And Meterage
基 金:中央高校基本科研业务费(531118010314);河南省土壤重金属污染监测与修复重点实验室重点开放课题(2017206);国家重大科学仪器设备开发专项(2014YQ06077307);环保公益性行业科研重大专项(201309050)
摘 要:对不同的样品消解方法及电感耦合等离子体质谱、电感耦合等离子体原子发射光谱、石墨炉原子吸收光谱法测定土壤中铅的测定结果进行比对。采用电热板、微波及水浴3种加热方式,选择硝酸、氢氟酸、双氧水、王水、高氯酸、盐酸的不同组合进行土壤样品消解,通过分析测定值的精密度和准确度,考察消解体系对电感耦合等离子体质谱、电感耦合等离子体发射光谱、石墨炉原子吸收光谱法测定结果的影响。结果表明采用电感耦合等离子体质谱法测定土壤中的铅,最适宜的消解体系是硝酸-氢氟酸-高氯酸(微波加热),采用电感耦合等离子体原子发射光谱法测定最适宜的消解体系是硝酸(电热板加热),采用石墨炉原子吸收光谱法测定最适宜的消解体系是硝酸-盐酸-高氯酸(微波加热)。电感耦合等离子体质谱法的精密度和准确度优于另外两种方法。The detection results were compared from vary sample treatment methods and different analysis method of ICP-MS,ICP-AES and GFC-AAS.With three heating modes on soil digestion including electrothermal plate heating,microwave heating and water bath heating,and different combinations of six kinds of digestion reagents such as nitric acid,hydrofluoric acid,hydrogen peroxide,aqua regia,perchloric acid and hydrochloric acid,the effect of the analysis method of ICP-MS,ICP-AES and GFC-AAS on the detection results was investigated by evaluating the precision and accuracy of the experimental results.The results showed that the most suitable digestion system for determination of lead in soil by ICP-MS was nitric acid-hydrofluoric acid-perchloric acid(heated by microwave),the most suitable digestion system for determination of lead by ICP-AES was nitric acid(heated by electrothermal plate),and the most appropriate digestion system for detection of lead by GFC-AAS was nitric acid-hydrochloric acid-perchloric acid(heated by microwave).The precision and accuracy of inductively coupled plasma mass spectrometry is better than that of graphite furnace atomic absorption spectrometry and inductively coupled plasma atomic emission spectrometry.
关 键 词:精密度 准确度 土壤 铅 电感耦合等离子体质谱法 电感耦合等离子体原子发射光谱法 石墨炉原子吸收光谱法 消解体系
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