Gunderson E C, Anderson C C
SRI International, Menlo Park, CA 94025.
Am Ind Hyg Assoc J. 1988 Oct;49(10):531-8. doi: 10.1080/15298668891380178.
A method has been developed and validated for monitoring worker exposure to airborne m-phenylenediamine (MPDA) and 4,4'-methylenedianiline (MDA) in an epoxy resin manufacturing operation. Aerosol and vapor MPDA and MDA are collected on an acid-coated, glass-fiber filter to stabilize them as their amine salts. The amines are extracted from the filter with a mixture of acetonitrile in aqueous base and then treated with acetic anhydride to form the diacetamide derivatives. Studies were performed on the acetylation reaction to establish sample work-up conditions. The derivatives are analyzed by high performance liquid chromatography with UV detection. The method was tested for precision and accuracy using the National Institute for Occupational Safety and Health (NIOSH) criteria for a valid industrial hygiene method. The method may be used with confidence to measure from 0.90 to 755 micrograms of MPDA and/or 0.36 to 55 micrograms of MDA in a total air volume of 200 to 630 L, sampling at a rate of 1.5 to 2.0 L/min. Collected samples remain stable on filters for at least 1 week before analysis. The method will not suffer from interference from high relative humidity or other process volatiles, including diglycidyl ether of bisphenyl A and bis(2,3-epoxycyclopentyl) ether. Test atmospheres of the process materials were prepared in the laboratory for validation of the overall sampling and analytical method. This method can be applied to most aromatic amines and is recommended for monitoring both ambient and workplace air.
已开发并验证了一种用于监测环氧树脂制造作业中工人对空气中间苯二胺(MPDA)和4,4'-亚甲基二苯胺(MDA)暴露情况的方法。气溶胶态和蒸汽态的MPDA和MDA被收集在涂有酸的玻璃纤维滤纸上,以将它们稳定为胺盐形式。胺类物质用乙腈与碱性水溶液的混合物从滤纸上萃取出来,然后用乙酸酐处理以形成二乙酰酰胺衍生物。对乙酰化反应进行了研究,以确定样品处理条件。衍生物通过带紫外检测的高效液相色谱法进行分析。使用美国国家职业安全与健康研究所(NIOSH)关于有效工业卫生方法的标准对该方法的精密度和准确度进行了测试。该方法可放心用于在200至630升的总空气体积中,以1.5至2.0升/分钟的采样速率测量0.90至755微克的MPDA和/或0.36至55微克的MDA。收集的样品在分析前在滤纸上至少可稳定保存1周。该方法不会受到高相对湿度或其他工艺挥发物(包括双酚A二缩水甘油醚和双(2,3-环氧环戊基)醚)的干扰。在实验室中制备了工艺材料的测试气氛,以验证整个采样和分析方法。该方法可应用于大多数芳香胺,推荐用于监测环境空气和工作场所空气。