LIU Xiao-xiao,SONG Zhi-feng,CHEN Guan-ning,et al.Establishment of Determination Method of Lead,Cadmium and Chromium in Soil by High Pressure Tank DigestionAAS Method[J].HEILONGJIANG AGRICULTURAL SCIENCES,2018,(11):85-89.[doi:10.11942j.issn1002-2767.2018.11.0085]
基于高压罐消解AAS法土壤中铅、镉、铬测定方法的建立
- Title:
- Establishment of Determination Method of Lead,Cadmium and Chromium in Soil by High Pressure Tank DigestionAAS Method
- Keywords:
- soil; lead; chromium; cadmium; atomic absorption spectrometry; high pressure tank digestion
- 文献标志码:
- A
- 摘要:
- 为建立高准确度、高灵敏度且稳定好的土壤重金属检测方法，建立了高压罐消解及原子吸收光谱法(AAS)测定土壤样品中铅、镉、铬3种元素的方法。通过对高压罐消解前处理条件的优化，确定了最适前处理方法。结果表明：高压罐消解的最佳方案为混酸体积比为浓硝酸∶氢氟酸∶高氯酸=2∶1∶1、消解温度为180 ℃、消解时间为7 h；通过对所建立的方法进行方法学考察发现，3个元素的线性达到0.999 3~0.999 9；检出限为0.009~0.740 μg?g-1；日内精密度RSD为1.74%~2.52%；日间精密度RSD为2.49%~2.99%；重现性RSD为1.83%~2.51%；稳定性RSD为1.83%~2.73%；加标回收率达到93.96%~95.05%。通过以上研究，该方法稳定性好、灵敏度高、准确性高。
- Abstract:
- In order to establish a high accuracy,high sensitivity and stable method for detecting heavy metals in soil,a method for determination of lead,cadmium and chromium in soil samples by high pressure tank digestion and atomic absorption spectrometry(AAS) was established.The optimum pretreatment method was determined by optimizing the pretreatment condition of the pressure tank.The results showed that the best solution for the digestion of high-pressure tanks was: mixed acid volume ratio was concentrated nitric acid∶hydrofluoric acid∶perchloric acid=2∶1∶1,digestion temperature was 180 ℃,digestion time was 7 h; Through the methodological investigation of the established method,the results showed that the linearity of the three elements reaches 0.9993-0.9999; The detection limit was 0.009-0.740 μg?g-1; The daily precision RSD was 1.74%-2.52%; Daytime precision RSD was 2.49%- 2.99%; The reproducibility RSD was 1.83%-2.51%; Stability RSD was 1.83%-2.73%; The standard recovery rate reached 93.96%-95.05%.Through the above research,the method had good stability,high sensitivity and high accuracy.
参考文献/References:
［1］陈冠宁,宋志峰,魏春雁.重金属检测技术研究进展及其在农产品检测中的应用[J].吉林农业科学,2012,37(6):61-63,71.[2]韩颖.原子吸收法测定污灌土中的重金属含量[J].山西农经，2017(4):76-77.[3]朱良漪，孙亦梁，陈耕燕.分析仪器手册[M].北京：化学工业出版社，1997:318-328.[4]宋伟，张志，郑平，等.土壤中砷、汞、铅、镉、铬测定方法的研究[J].安徽农业科学，2011,39（34）：21001-21002,21054.[5]朱颜苹,段桂玲,元学红.原子吸收分光光度法测定土壤中的重金属[J].绿色科技，2012(7):175-176.
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备注/Memo
收稿日期：2018-07-12