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机构地区:[1]北京市通州区疾病预防控制中心,北京101100 [2]河北医科大学,河北石家庄050017
出 处:《现代预防医学》2018年第1期106-108,112,共4页Modern Preventive Medicine
摘 要:目的研究石墨炉原子吸收法测定尿铅的影响因素。方法比较5种基体改进剂的效果并选择最佳基体改进剂及其用量;优化石墨炉的升温程序;对标准加入法与外标法及尿样的稀释比例对尿铅测定的影响进行探讨。结果基体改进剂及其用量、灰化温度、原子化温度、尿样稀释及标准曲线中加入正常人尿与否对尿铅的测定影响较大。比较5种基体改进剂的效果,最佳基体改进剂及用量为5μl 5g/L磷酸二氢铵-1g/L硝酸钯。优化石墨炉升温程序,最佳灰化温度为1 200℃,最佳原子化温度为1 600℃,在灰化之前通入空气,有利于清除尿样中的有机物。在标准曲线中加入正常人尿,测定1∶1稀释尿样加标回收率和尿铅参考物,加标回收率在95.3%-112.7%之间,尿铅参考物测定值在标准值范围内。结论石墨炉原子吸收法测尿铅,采用5μl 5g/L磷酸二氢铵-1g/L硝酸钯基体改进剂,最佳灰化温度1 200℃,最佳原子化温度1 600℃,在灰化之前通入空气,采用加入正常人尿的标准加入曲线测定1∶1稀释尿样,可得到更加准确的尿铅测定结果。Objective To study the factors affecting the determination of urine lead by graphite furnace atomic absorption spectrometry. Methods The effects of 5 kinds of matrix modifiers were compared, and the best matrix modifiers and their dosage were selected. The heating program of graphite furnace was optimized, and the influence of standard addition method, external standard method and the urine dilution ratio on urine lead determination were discussed. Results The effects of matrix modifier and its dosage, the ashing temperature, the atomization temperature, the dilution ratio of urine and whether adding normal human urine or not were greatly affected. The effect of the 5 matrix modifiers were compared, and the best matrix modifier were ammonium dihydrogen phosphate and palladium nitrate with the dose of 5uL 5g/L and - lg/L respectively. The temperature programmed by graphite furnace was optimized. The best ashing temperature was 1200℃, and the best atomization temperature was 1600℃. Adding air before the ashing was beneficial to remove the organic matter in the urine. Normal human urine was added to the standard curve, and the recoveries of the urine samples diluted 1 time and the reference material of urine lead were measured. The recovery rate of the added standard was between 95.3% -112.7% and the urine lead reference value was within the standard range. Conclusion When measuring the urine lead,using 5uL 5g/L ammonium dihydrogen phosphate - lg/L palladium nitrate matrix modifier, setting the optimum ashing temperature of 1200 and the optimum atomization temperature of 1600, adding air before the ashing, and adding 1:1 diluted normal human, can obtain more accurate results of urine lead determination.
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