工作场所空气中1,6-己二异氰酸酯和异氟尔酮二异氰酸酯的高效液相色谱同时测定法

Simultaneous determination of 1,6-hexamethylene diisocyanate and isophorone diisocyanate in air of workplaces by HPLC

目的建立同时检测工作场所空气中1,6-己二异氰酸酯(HDI)和异氟尔酮二异氰酸酯(IPDI)的高效液相色谱(HPLC)方法。方法工作场所空气中HDI和IPDI用浸渍了1-(2-吡啶基)哌嗪(1-2PP)的玻璃纤维滤纸采集,用流动相洗脱后上机分析,以保留时间定性、以对应峰面积定量。结果 HDI和IPDI可以在HPLC中完全分离,且在0.005~2.0 mg/L范围内线性相关系数分别是0.999 93和0.999 98,检出限HDI为0.000 5 mg/L,IPDI为0.000 6 mg/L,对应于15 L采样体积的最低检出浓度均为0.002 mg/m3;采样效率分别为97.6%和98.5%;在0~4℃冰箱中样品至少可保存14天。结论本方法采样方便,操作简单,精密度高,可以用于工作场所空气中HDI和IPDI的同时测定。

[Objective] To establish a method based on the high performance liquid chromatography（HPLC） for detection simultaneously of 1,6-Hexamethylene diisocyanate（HDI） and isophorone diisocyanate（IPDI） in the air of workplaces.[Methods] Samples in the air of workplaces which contained HDI and IPDI were collected with glass fiber filter papers impregnated with 1-（2-pyridyl） piperazine（1-2 PP） and eluted by using mobile phase solution, than analyzed by HPLC. The qualitative identification of the target compounds was given according to the retention times and the quantitative measurements to be achieved by the corresponding peak area. [Results] HDI and IPDI can be completely separated in the HPLC graph, and in the concentration range of 0.005-2.0 mg/L both have good linearity with correlation coefficient 0.999 93 and 0.999 98 respectively. The detection limit of HDI is 0.000 5 mg/L and which of IPDI is 0.000 6 mg/L, which gives out the minimum detectable concentration 0.002 mg/m3 corresponds to the sampled air volume of 15 L. The sampling efficiency is 97.6% and98.5% respectively. The samples can be stored for at least 14 d in 0-4 ℃ refrigerator. [Conclusion] This method has the advantages of convenient to sampling, easy to operate and high precision, and it is valid to be applied to simultaneously detecting of HDI and IPDI in the air of workplaces.