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目的:建立石墨炉原子吸收光谱法同时测定尿中铅(浓度变化范围大)的检测方法。方法:应用动态三磁场塞曼校正技术的石墨炉原子吸收光谱仪,通过磁场优化,采用氯化钯作基体改进剂,在283.3 nm波长下进行测定。结果:采用动态3-磁场模式测定时,还可同时得到2-磁场模式的数据和校正曲线,2-磁场标准曲线段(0.0μg/L~80.0μg/L):y=0.0048x+0.0145,r=0.9997;3-磁场标准曲线段(80.0μg/L~600.0μg/L):y=0.0013x+0.0308,r=0.9998;最低检出浓度2.0μg/L;回收率94.6%~104.8%;RSD为0.60%~3.72%。结论:该方法保持两种磁场模式的优点:检出限低、快速(样品无需再稀释)、准确、线性范围宽(0.0μg/L~600.0μg/L);可应用于职业接触和非职业接触尿中铅的同时测定,低浓度采用灵敏度较高的2-磁场模式数据处理,高浓度可采用线性范围宽的3-磁场模式计算。
Objective: To establish a method for the simultaneous determination of lead (concentration range) in urine by graphite furnace atomic absorption spectrometry. Methods: Graphite furnace atomic absorption spectrometer with dynamic three-magnetic Zeeman correction was adopted. The magnetic field was optimized and Palladium Chloride was used as the matrix modifier to measure at 283.3 nm. Results: The 2-magnetic field data and calibration curves were obtained simultaneously with the dynamic 3-magnetic field measurement. The 2-magnetic field curve (0.0μg / L ~ 80.0μg / L) r = 0.9997; 3-magnetic field standard curve segment (80.0μg / L ~ 600.0μg / L): y = 0.0013x + 0.0308, r = 0.9998; the lowest detection concentration was 2.0μg / L; the recovery was 94.6% ~ 104.8% RSD 0.60% ~ 3.72%. Conclusion: This method maintains the advantages of two magnetic field modes: low detection limit, fast (no need to dilute the sample), accurate, wide linear range (0.0μg / L ~ 600.0μg / L); can be applied to occupational exposure and non-occupational Contact with urine lead at the same time determination, low concentration of high sensitivity using 2-magnetic field mode data processing, high concentrations can be linear range of 3-magnetic field mode calculation.