涂钼高密石墨管在血铅测定中的应用

目的建立一种消除干扰及提高血铅测定精密度和准确度的简单实用的方法,减少仪器使用年代太长带来的困扰,为基层实验人员提高检测质量提供参考。方法使用高密石墨管涂钼的方法降低氘灯背景吸收,联合使用0.1%氯化钯＋0.1%Triton X-100＋0.1%硝酸作为基体改进剂,通过血铅测定的质量控制方法,确定方法的可行性。结果使用改良方法测定血铅的相对标准偏差为1.1%-8.2%,加标回收率为97.8%-101.8%,经方法配对t检验,对RSD值统计（t=2.635,P〈0.05）表明改良法有良好精密度;2012和2013年300份血铅样品检测中,采用的上述改良的石墨炉原子吸收分光光度法,血铅浓度在0-80μg/L范围内线性关系良好,相关系数达0.999以上,平行双样相对偏差为0.5%-7.6%,用两批冻干牛血铅镉（GBW 09139h,GBW 09140h）模拟盲样考核,铅的检测结果为118.5和316.8μg/L,结果在标准证书给定范围内。结论使用涂钼高密石墨管配合采用0.1%氯化钯＋0.1%Triton X-100＋0.1%硝酸作为基体改进剂能有效提高仪器的精密度和准确度,高效实用,是一种值得推广的检测方法。

Application of molybdenum-coated high-density graphite tube in the determination of lead in blood

Objective]To establish a simple and practical method which can eliminate interference and improve the precision and accuracy in determination of blood lead,reduce the instrument problems caused by long-term service,and provide a reference for basic level experimenters to improve detection quality.Methods]The molybdenum-coated high-density graphite tube was applied to reduce the deuterium lamp background absorption. The combination of 0. 1% palladium chloride,0. 1% Triton X-100 and 0. 1% nitrate was used as the matrix modifier. The feasibility of the method was determined by the quality control method in the determination of blood lead.Results]The relative standard deviation（ RSD） of blood lead determination by using the modified method was 1. 1%-8. 2%,and the recovery of standard addition was 97. 8%-101. 8%. The RSD values were analyzed the paired t test（ t =2. 635,P〈0. 05）,and the results showed that the modified method had a good precision. 300 samples were detected for the blood lead by this modified atomic absorption spectrophotometry during 2012-2013. The method showed a good linear relationship within the blood lead concentration of 0-80 μg / L,the correlation coefficient reached over 0. 999,and the relative deviation of parallel double sample was 0. 5%-7. 6%. Two batches of lyophilized bovine blood lead and cadmium standard material（ GBW 09139 h, GBW 09140 h） were adopted to simulate the blind sample test,and the lead content was 118. 5 μg / L and 316. 8 μg / L respectively,which the results were within the range of standard certificate.Conclusion]The molybdenum-coated high-density graphite tube combined with the matrix modifier of 0. 1% palladium chloride,0. 1% Triton X-100 and 0. 1% nitrate can effectively improve the precision and accuracy of the instrument,which is efficient and practical,and this detection method is worth popularizing.