王丽雅, 袁金华, 孔璐. 建立浓盐酸超声提取-原子荧光光谱法测定大气PM2.5中锡及其化合物水平[J]. 环境与职业医学, 2022, 39(4): 453-458. DOI: 10.11836/JEOM21372
引用本文: 王丽雅, 袁金华, 孔璐. 建立浓盐酸超声提取-原子荧光光谱法测定大气PM2.5中锡及其化合物水平[J]. 环境与职业医学, 2022, 39(4): 453-458. DOI: 10.11836/JEOM21372
WANG Liya, YUAN Jinhua, KONG Lu. Determination of tin and its compounds in ambient PM2.5 by atomic fluorescence spectrometry after ultrasonic extraction with concentrated hydrochloric acid[J]. Journal of Environmental and Occupational Medicine, 2022, 39(4): 453-458. DOI: 10.11836/JEOM21372
Citation: WANG Liya, YUAN Jinhua, KONG Lu. Determination of tin and its compounds in ambient PM2.5 by atomic fluorescence spectrometry after ultrasonic extraction with concentrated hydrochloric acid[J]. Journal of Environmental and Occupational Medicine, 2022, 39(4): 453-458. DOI: 10.11836/JEOM21372

建立浓盐酸超声提取-原子荧光光谱法测定大气PM2.5中锡及其化合物水平

Determination of tin and its compounds in ambient PM2.5 by atomic fluorescence spectrometry after ultrasonic extraction with concentrated hydrochloric acid

  • 摘要: 背景 锡及其化合物会对人体的呼吸系统、神经系统造成严重危害,但目前对于大气PM2.5中的锡尚缺乏相应的国家标准检测方法。

    目的 建立浓盐酸超声浸提-原子荧光光谱法测定大气PM2.5中的锡及其化合物水平的方法。

    方法 恒速抽取定量体积空气通过具有一定切割特性的采样器,使大气PM2.5被截留在石英滤膜上。通过选择浸提溶剂,比较浸提温度和时间,调整样品待测液酸度,优化样品的前处理过程,建立测定PM2.5中锡及其化合物的原子荧光方法,得到线性、检出限、定量下限等性能指标。采用空白石英滤膜加标回收试验评价方法的准确度和精密度,采用城市颗粒物标准样品加标回收进行干扰试验。将本实验建立的方法和《空气污染(雾霾)对人群健康影响监测与防护手册(2020)》(简称《手册》)的方法应用于实际样品的检测并比较结果。

    结果 采用浓盐酸作为浸提溶剂,浸提时反应温度越高,反应时间越长,则回收率越高,因此选择70 ℃水浴超声浸提3 h。本法锡检测范围为5.00~50.00 μg·L−1,线性相关系数≥0.999,检出限为0.27 μg·L−1;定量检出下限为0.90 μg·L−1(按采样体积144 m3计算,样品最低检出量为1.25 ng·m−3)。本法空白滤膜加标回收率94.1%~97.5%,相对标准偏差≤3.2%;城市颗粒物样品加标回收率93.5%~103.0%,相对标准偏差≤2.1%,即PM2.5共存成分均不影响锡的测定。选取PM2.5监测的10份石英滤膜样品,本方法(浓盐酸浸提)的锡测定结果高于《手册》的方法(硝酸浸提),其差值的均数加减标准差为(3.61±0.54)ng·m−3t=21.303,P<0.05)。

    结论 采用浓盐酸超声浸提-原子荧光光谱法测定PM2.5石英滤膜中的锡及其化合物,方法操作简单,精密度高,适用于实验室大批量PM2.5样品中锡及其化合物的测定。

     

    Abstract: Background Tin and its compounds can cause serious harm to human respiratory system and nervous system, but there is no corresponding national standard method for the determination of tin in PM2.5.

    Objective To establish a method for the determination of tin and its compounds in PM2.5 by atomic fluorescence spectrometry (AFS) after ultrasonic extraction with concentrated hydrochloric acid.

    Methods We extracted a fixed volume of air at a constant speed through a sampler with preset cutting characteristics to trap PM2.5 in the ambient air on quartz filter membranes. By selecting extraction solvent, comparing extraction temperature and time, and adjusting the acidity of solution to be measured, the sample pretreatment process was optimized, and a method for the determination of tin and its compounds in PM2.5 by AFS was proposed, and its performance indexes such as linearity, detection limit, and lower limit of quantification were obtained. The accuracy and precision of the method were evaluated by the standard addition recovery test with blank quartz filter membranes, and the interference test was carried out by adding standard urban particulate samples. The proposed method and the method recommended by the “Handbook on Monitoring and Protection of Air Pollution (Haze) Effects on Population Health (2020)” (the Handbook) were applied to actual samples, and the results were compared.

    Results This experiment used concentrated hydrochloric acid as the extraction solvent. The higher the reaction temperature and the longer the reaction time, the higher the recovery rate. Therefore, 70 ℃ water bath ultrasonic extraction for 3 h was selected. In terms of the proposed method, the linear range of detection was from 5.00 μg·L−1 to 50.00 μg·L−1, with a correlation coefficient ≥0.999 and a detection limit of 0.27 μg·L−1. When the quantitative detection of the lower limit was 0.90 μg·L−1, and the sampling volume was 144 m3, the limit of quantification was 1.25 ng·m−3. The recovery rate of standard addition of blank quartz filter membranes was 94.1%-97.5%, with a relative standard deviation ≤3.2%; the recovery rate of standard addition of standard urban particulate matter samples was 93.5%-103.0%, and the relative standard deviation was ≤2.1%, indicating that coexisting components in PM2.5 samples would not affect the determination of tin. For the 10 quartz filter membrane samples of PM2.5 monitoring, the results of tin by the established method (extraction with concentrated hydrochloric acid) were higher than those of the Handbook recommended method (extraction with nitric acid), and the difference is (3.61±0.54) ng·m−3(t=21.303, P<0.05).

    Conclusion The established method for the determination of tin and its compounds in PM2.5 by AFS after ultrasonic extraction with concentrated hydrochloric acid is simple, accurate, and suitable for laboratory determination of tin and its compounds in large quantities of PM2.5 samples.

     

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