氢化物原子荧光法测定水砷的分析质量控制

Analytical quality control of determination of arsenic in water by hydride generation atomic fluorescence spectrometry

目的 分析氢化物原子荧光法测定水砷的质量控制并进行误差预测,提高实验室水砷检测能力和质量控制能力,确保检测数据的准确性和可靠性.方法 按水质分析中评价微量元素精密度和准确度的分析质量控制工作程序,用氢化物原子荧光法（GB/T5750.5-2006）对空白溶液（3％盐酸溶液）、2种标准溶液（0.1C、0.9C砷标准溶液,C为分析方法测定范围的上限,本实验C为20.0 μg/L）、天然水样、加标水样（5.0 μg/L）中砷含量进行测定.结果 5种试样的批内、批间变异分析,差异无统计学意义（F＜F0.05,P均＞ 0.05）,每种试样的总标准差（S）小于其测定浓度的5％,总平均回收率可信限（R/d）为0.99.能力验证样品实验室内的随机误差（ZWAs）为1.04、实验室间的系统误差（ZBAs）为1.12.质控考核结果为满意.结论 采用精密度和准确度的分析质量控制工作程序对氢化物原子荧光法测定水中砷进行分析质量控制,保证实验结果误差在可控制的范围内,获得高度可信的分析结果.

Objective To implement analytical quality control（AQC） and predict analysis error of arsenic determination in water by hydride generation atomic fluorescence spectrometry,enhancing the technical level of testing arsenic and lab quality control capability,and to ensure the accuracy and reliability of test data.Methods According to the AQC procedure of water quality analysis for evaluating precision and accuracy of trace elements,arsenic content was measured in a blank solution（3% hydrochloric acid solution）,two kinds of standard solution （0.1C,0.9C arsenic standard solution,the C was the upper limit of measuring scope of the analytical method,and in this experiment the C was 20.0 μg/L）,natural water sample and standard quality control sample（5.0 μg/L） with hydride generation atomic fluorescence spectrometry corresponding to GB/T 5750.5-2006.Results Of the five kinds of intra-samples and inter-assay,the difference was not significant statistically （F 〈 F0.05,all P 〉 0.05）.Total standard deviation （St） of every solution was less than 5% of the concentration,the confidence limit of total average rate of recovery（R/d =0.99） was in a allowable range.The proficiency of testing samples were ZWAs =1.04 and ZBAs =1.12.The blind sample testing result was satisfactory.Conclusions Arsenic in water is determined by hydride generation atomic fluorescence spectrometry,and the analytical quality control is adopted by precision-bias analysis and accuracy quality control procedure.Ensuring that the error results are in a controlled range and highly reliable analytical results are obtainable.