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目的建立工作场所空气中锆及其化合物的电感耦合等离子体-质谱测定方法。方法工作场所空气中样品用微孔滤膜采集后,水溶性锆化合物用浓度为2.0 mol/L的盐酸洗脱、硝酸消解,不溶性锆化合物用硫酸铵溶液消解处理,采用电感耦合等离子体-质谱法进行测定。结果本方法锆及其化合物在质量浓度为0.000~1.000mg/L时线性关系良好,相关系数为0.999 9,方法的检出限为0.1μg/L,最低检出浓度为0.07μg/m~3(以采集空气样品体积75 L计算)。对于水溶性锆化合物加标回收率为95.0%~98.8%,批内相对标准偏差(RSD)为2.0%~3.9%,批间RSD为2.8%~6.6%;对于不溶性锆化合物加标回收率为94.4%~98.7%,批内RSD为2.1%~4.2%,批间RSD为3.2%~4.7%。样品在室温下至少可保存30 d。结论本方法快速、灵敏、准确,适用于工作场所空气中锆及其化合物的测定。
Objective To establish an inductively coupled plasma-mass spectrometry method for the determination of zirconium and its compounds in workplace air. Methods After air samples were collected in the air at room temperature, the water-soluble zirconium compounds were eluted with hydrochloric acid at a concentration of 2.0 mol / L, nitric acid was digested and insoluble zirconium compounds were digested with ammonium sulfate solution. Inductively coupled plasma-mass spectrometry Method for determination. Results The calibration curve of zirconium and its compounds was good at a concentration of 0.000-1.000 mg / L with a correlation coefficient of 0.999 9. The detection limit was 0.1 μg / L and the lowest detection limit was 0.07 μg / m 3 (Based on the volume of collected air sample 75 L). The spiked recoveries of water-soluble zirconium compounds ranged from 95.0% to 98.8%. The relative standard deviations (RSDs) were within the range of 2.0% -3.9%, and the RSDs between batches were between 2.8% and 6.6%. The spiked recoveries of insoluble zirconium compounds were 94.4% -98.7%. The intra-assay RSD was 2.1% -4.2%, and the inter-assay RSD was 3.2% -4.7%. Samples can be stored at room temperature for at least 30 d. Conclusion The method is rapid, sensitive and accurate and is suitable for the determination of zirconium and its compounds in the air of workplace.