基于高压罐消解/AAS法土壤中铅、镉、铬测定方法的建立  

Establishment of Determination Method of Lead,Cadmium and Chromium in Soil by High Pressure Tank Digestion/AAS Method

作　　者：刘笑笑[1] 宋志峰[1] 陈冠宁[2] 魏春雁[1] LIU Xiao-xiao;SONG Zhi-feng;CHEN Guan-ning;WEI Chun-yan(Institute of Agricultural Quality Standards and Testing Technology,Risk Assessment Lab of Agri-products Quality and Safety（Changchun）,Agriculture Ministry of P.R.C,Changchun 130033,China;Jilin Province Chinese Medicine Research Institute,Changchun 130021,China)

机构地区：[1]吉林省农业科学院农业质量标准与检测技术研究所/农业部农产品质量安全风险评估实验室,吉林长春130033 [2]吉林省中医中药研究院,吉林长春130021

出　　处：《黑龙江农业科学》2018年第11期85-89,共5页Heilongjiang Agricultural Sciences

基　　金：吉林省财政厅公益性科研院所行业科研资助项目(2010-2011);吉林省农业科技创新工程资助项目(CXGC2017TD011;CXGC2017ZY038)

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7h;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0.009～0.740μg·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。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.

关 键 词：土壤 铅 铬 镉 原子吸收光谱法 高压罐消解 

分 类 号：O657.31[理学—分析化学] X833[理学—化学]