农田土壤中重金属含量测定及其不确定度评估.docVIP

农田土壤中重金属含量测定及其不确定度评估 　　摘要: 利用微波消解-火焰原子吸收光谱法测定农田土壤中的铅、铬、铜和锌含量,并对测量结果不确定度来源进行了分析,分析得知不确定度来源主要包括样品的称量,重复性测量,标准溶液的配制,曲线拟合,样品的定容.通过建立数学模型计算出各不确定度分量,总结出标准物质不确定度,重复性测量不确定度占较大比例,并提出了减小不确定度的建议. 　　? 　　关键词: 微波消解；火焰原子吸收光谱法；土壤；不确定度 ? 　　中图分类号:O 657.31 　　 文献标志码:A文章编号:1672-8513(2012)02-0101-03 　　?? 　　Determination of Pb, Cr, Cu and Zn in Farmland Soil and ?Assessment of the Uncertainty of Analytical Results 　　 　　YANG Xin?zhou, ZHANG Gong?xin, LI Xue?sen, MU Huai?xue, YAO Fu?quan, HU Qiu?fen 　　? 　　（Key Laboratory of Ethnic Medicine Resource Chemistry, State Ethnic Affairs Commission and Ministry of? Education of China, Yunnan University of Nationalities, Kunming 650031, China） 　　 　　Abstract: The method of Microwave Digestion and Flame Atomic Absorption Spectrometry for the determination of the trace amount of Pb, Cr, Cu and Zn in farmland soil was established, and the uncertainty sources of the measurement results were analyzed. According to the analytical results, the uncertainty sources include the samples size, the repeatability of measurement, the preparation of standard liquid, the carve fitting, and the sample volume. These components of uncertainty were calculated by the mathematical mode. The results showed that the uncertainty of standard substance and the repeatability of measurement were the main source. Some suggestions for reducing the uncertainty were also given. 　　? 　　Key words: microwave-digestion; flame atomic absorption spectrometry; farmland soil; uncertainty 　　 　　不确定度是判断检测结果可靠程度和客观性的依据,是评定一个分析方法可行性的依据.对测量结果进行不确定度评定也是中国实验室国家认可委(CNAL)认可准则对实验室的要求??［1-3］?.目前不确定度已经大量用于评估检测方法,被许多计量单位、监测单位和实验室使用.土壤无机污染物中以重金属比较突出,主要是由于重金属不能为土壤微生物所分解,而易于积累,转化为毒性更大的甲基化合物,甚至有的通过食物链以有害浓度在人体内蓄积,严重危害人体健康??［4］?.因而测定农田土壤中的重金属含量及其对测定结果的不确定度分析具有重要的意义.因此笔者利用微波消解-火焰原子吸收光谱法测定农田土壤中铅、铬、铜和锌的含量,并对测量结果的不确定来源进行了详细的分析和评定.? 　　1 实验部分? 　　1.1 主要仪器和试剂? 　　AA6300原子吸收分光光度计(日本岛津公司)；铅、铬、铜和锌空心阴极灯；DKQ-3型智能控温电加热器,WX-4000微波消解仪(上海屹尧分析仪器有限公司)；电子分析天平（北京赛多利斯天平有限公司）；移液管、容量瓶：均为A级,均用20%的硝酸溶液浸泡48?h以上.? 　　铅、