溶剂解吸-气相色谱法测定工作场所空气中二亚乙基三胺

目的建立工作场所空气中二亚乙基三胺的溶剂解吸-气相色谱检测方法。方法使用碱性硅胶管采样,用0.2 mol/L盐酸甲醇溶液解吸,离心后取上清液与0.3 mol/L氢氧化钾甲醇溶液中和,经5%-苯基-甲基聚硅氧烷(HP-5)毛细管色谱柱(25 m×0.32 mm×0.52 mm)分离,氢火焰离子化检测器测定。结果该方法检出限为0.49μg/mL,定量限为1.64μg/mL,定量测定范围为1.64~233.80μg/mL,最低定量检出浓度为0.22 mg/m^3(以采集7.5 L空气样品计);方法的重现性好,相对标准偏差为1.4%~3.3%,平均解吸效率为90.8%,平均采样效率为93.2%;200 mg碱性硅胶的穿透容量大于7.1 mg,样品在室温下至少可保存15 d;空气中共存的乙二胺、三亚乙基四胺、四亚乙基五胺在本法条件下不干扰测定。结论该方法检出浓度低、准确度高、精密度好,适用于工作场所空气中二亚乙基三胺的测定。

Determination of diethylenetriamine in workplace air by solvent desorption-gas chromatography

OBJECTIVE To establish solvent desorption gas chromatograph method for diethylenetriamine determination in workplace air. METHODS Diethylenetriamine in workplace air was collected with alkaline silicone tube, and desorbed with 0.2 mol/L methanol solution of hydrochloric acid. After centrifugation, the supernatant neutralized with 0.3 mol/L methanol solution of potassium hydroxide, was separated with 5%-phenyl-methyl polysiloxane(HP-5)(25 m×0.32 mm×0.52 mm)and measured with flame ionization detector. RESULTS Detection limit of the method was 0.49 μg/mL,quantification limit of the method was 1.64 μg/mL, quantitative determination range of method was 1.64-233.80 μg/mL,and the minimum quantitative determination concentration was 0.22 mg/m^3(based on 7.5 L sample). The method had a good reproducibility, the relative standard deviation was 1.4%-3.3%, the average of desorption efficiency was 90.8%, and the average of sampling efficiency was 93.2%. The penetrating capacity of 200 mg alkaline silicone was over than 7.1 mg, and the samples at room temperature could be preserved for 15 days at least. Ethylenediamine, triethylenetetramine or tetraethylenepentamine coexisted in the air did not interfere during the determination of diethylenetriamine. CONCLUSION The method with low determination concentration, high accuracy and precision, is feasible for determination of diethylenetriamine in workplace air.