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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。
Objective To establish a simple and practical method to eliminate the interference and improve the precision and accuracy of blood lead determination, and to reduce the troubles caused by the long service life of the instrument, so as to provide a reference for the grassroots experimenters to improve the quality of detection. Methods High density graphite tube coated with molybdenum was used to reduce the background absorption of deuterium lamp. The quality control method of determination of blood lead by 0.1% palladium chloride + 0.1% Triton X-100 + 0.1% nitric acid was used as matrix modifier. feasibility. Results The relative standard deviation of determination of blood lead was improved from 1.1% to 8.2% with the recovery of 97.8% ~ 101.8%. The paired t test showed that the RSD value (t = 2.635, P <0.05) The method has good precision; in the detection of 300 blood lead samples in 2012 and 2013, the above-mentioned improved graphite furnace atomic absorption spectrophotometry has good linearity in the range of 0-80 μg / L with a correlation coefficient of 0.999 , The relative deviation of parallel double samples was 0.5% -7.6%. Two batches of freeze-dried bovine lead and cadmium (GBW 09139h, GBW 09140h) were used to simulate the blind sample test. The lead test results were 118.5 and 316.8μg / L, Certificate given range. Conclusion The use of molybdenum-coated high-density graphite tube with 0.1% palladium chloride + 0.1% Triton X-100 + 0.1% nitric acid as a matrix modifier can effectively improve the precision and accuracy of the instrument, and is highly practical and practical. It is a worthwhile promotion test method.