火焰原子吸收光谱法测定工作场所空气中铅和锰及其无机化合物的前处理方法改进  

IImprovement of pretreatment method for detection of lead, manganese and their inorganic compounds in the air of workplace by flame atomic absorption spectrometry

作　　者：杨展鸿 吴川[1] 罗晓婷[1] 董明[1] 张爱华[1] 吴邦华[1] YANG Zhanhong;WU Chuang;LUO Xiaoting;DONG Ming;ZHANG Aihua;WU Banghua(Guangdong Province Hospital for Occupational Disease Prevention and Treatment,Guangdong Provincial Key Laboratory of Occupational Disease Prevention and Treatment,Guangdong 510300,China)

机构地区：[1]广东省职业病防治院毒化监测所,广东省职业病防治重点实验室,广东广州510300

出　　处：《中国职业医学》2020年第5期582-585,共4页China Occupational Medicine

基　　金：广东省职业病防治重点实验室(2017B030314152);广东省化学中毒与核辐射突发事件医学救援应急技术研究中心(2016A020224005)。

摘　　要：目的改进火焰原子吸收光谱法测定工作场所空气样品中铅和锰及其无机化合物的前处理方法。方法微孔滤膜样品用浓度为1.0~2.0 mol/L的硝酸溶液20.0 mL消解后,于石墨电热板中140~160℃消化至0.5~1.0 mL,冷却后定容至10.0mL,采用火焰原子吸收光谱法测定。结果铅在质量浓度为0.10~3.00 mg/L时线性关系良好,相关系数为0.999 5,检出限和定量下限分别为0.03、0.10 mg/L(分别以3、10倍标准差计),最低检出浓度为0.004 mg/m3,最低定量浓度为0.010 mg/m3(以采集75 L空气计算);锰在质量浓度为0.05~3.00 mg/L时线性关系良好,相关系数为0.999 8,检出限和定量下限分别为0.02、0.05 mg/L(分别以3、10倍标准差计),最低检出浓度为0.002 mg/m3,最低定量浓度为0.007 mg/m3(以采集75 L空气计算);铅和锰的加标回收率为97.8%~99.6%,批内、批间相对标准偏差分别为0.4%~2.0%和0.4%~1.7%。结论本前处理改进方法操作简便,试剂用量少,消解温度低,精密度和准确度高,适合推广使用。Objective To improve the pretreatment method for the detection of lead, manganese and their inorganic compounds in workplace air samples by flame atomic absorption spectrometry. Methods In this method, 20.0 mL of 1.0-2.0 mol/L nitric acid solution was used as the digestion solution to digest the microporous membrane sample at 140-160 ℃ to a volume of 0.5-1.0 mL. Samples were cooled and fixed to 10 mL and detected by flame atomic absorption spectrometry method. Results The lead detection had a good linear relationship in the range of 0.10-3.00 mg/L. The correlation coefficient was 0.999 5, the detection limit and the lower limit of quantification were 0.03 and 0.10 mg/L respectively(calculated by 3 and 10 times of standard deviation respectively). The minimum detection concentration was 0.004 mg/m^3, and the minimum quantitative concentration was 0.010 mg/m^3(collected by 75 L air calculation). The manganese detection had a good linear relationship in the range of 0.05-3.00 mg/L mass concentration. The correlation coefficient was 0.999 8, the detection limit and the lower limit of quantification were 0.015 and 0.05 mg/L respectively(calculated by 3 and 10 times of standard deviation respectively), the minimum detection concentration was 0.002 mg/m^3, and the minimum quantitative concentration was 0.007 mg/m^3(based on collection 75 L air calculation). The recovery rate of standard addition was 97.8%-99.6%, and the relative standard deviation within and between run were 0.4%-2.0% and 0.4%-1.7% respectively. Conclusion The method is simple, the reagent consumption is small, the digestion temperature is low, the precision and accuracy are high. This method is suitable for widespread use.

关 键 词：前处理 酸消解 铅 锰 火焰原子吸收光谱法 工作场所 空气 

分 类 号：R134.4[医药卫生—劳动卫生]