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目的建立一次采样同时测定工作场所空气中磷酸和硫酸的方法。方法采用微孔滤膜进行采样,用超纯水浸泡后超声洗脱,用6.3 mmol/L Na HCO3/1.7 mmol/L Na CO3淋洗液,0.8 ml/min流速,经TSKgel Super IC-AZ阴离子色谱柱分离,电导检测器检测,以保留时间定性,峰面积定量。结果磷酸与硫酸在0~10.0 mg/L范围内均有良好的线性关系,相关系数均大于0.999(磷酸的相关系数r=0.999 7,硫酸的相关系数r=0.999 5),磷酸的最低检测浓度为0.027 mg/m3(以采集75 L空气样品计),精密度RSD在0.84%~2.11%之间,回收率97.9%~100%之间;硫酸的最低检测浓度为0.011 mg/m3(以采集75 L空气样品计),精密度RSD在0.67%~1.14%之间,回收率98.3%~99.9%之间。结论该方法操作简便,灵敏度高,一次采样能同时测定工作场所空气中磷酸和硫酸含量,适用于工作场所空气中磷酸和硫酸的测定。
OBJECTIVE To establish a method for the simultaneous determination of phosphoric acid and sulfuric acid in the workplace air samples. Methods The samples were collected with a microporous membrane filter and sonicated with ultrapure water. The supernatant was eluted with 6.3 mmol / L NaHC03 / 1.7 mmol / L Na CO3, 0.8 ml / min and TSKgel Super IC-AZ anion Column separation, conductivity detector detection, retention time qualitative, peak area quantitative. Results There was a good linear relationship between the concentration of phosphoric acid and sulfuric acid in the range of 0-10.0 mg / L, the correlation coefficient was greater than 0.999 (the correlation coefficient of phosphoric acid was r = 0.999 7, the correlation coefficient of sulfuric acid was r = 0.999 5) Was 0.027 mg / m3 (for 75 L air samples), the RSDs of precision were between 0.84% and 2.11%, and the recoveries were between 97.9% and 100%. The minimum detectable concentration of sulfuric acid was 0.011 mg / m3 75 L air sample meter), the RSD of precision was between 0.67% ~ 1.14% and the recovery rate was between 98.3% ~ 99.9%. Conclusion The method is simple, sensitive and can determine the content of phosphoric acid and sulfuric acid in the air at the same time in a single sampling. It is suitable for the determination of phosphoric acid and sulfuric acid in the air of workplace.