摘要
建立了毛细管气相色谱氢火焰离子化法检测涂料中13种二异氰酸酯的方法。样品乙酸乙酯溶解提取并过滤,经过0.45μm过滤膜进一步净化。使用中等极性的色谱柱Rtx-1701(14%-氰丙基苯基-86%-二甲基硅氧烷,30m×0.25mm,1μm),在梯度升温条件下,对标准溶液和样品中的二异氰酸酯进行分离。本方法对二异氰酸酯类单体的检出限为0.05～10mg/kg。加标回收率为56%～104%。RSD为1.2%～6.1%。本方法相对简单而且快速,适用于油漆涂料中二异氰酸酯类化合物的高通量快速检测。
A method for simultaneous determination of 13 diisocyanates in polyurethane paint by GC（gas chromatography） has been developed.The target determining materials cover not only the diisocyanates which cited and banned in OSHA articles,European directives and State standards,but also the diisocyanates which could be potentially used in industry in the future.The testing sample was obtained by dissolving liquid polyurethane in ethyl acetate,extracting by filtration,and followed by further purification by adopting the 0.45 μm membrane to filtration.A stationary phase of crossbond 14% -cyanopropylphenyl-86% -dimethyl polysiloxane painted inside the capillary（Rtx -1701,30 m×0.25 mm ID×1 μm df） was adopted to separate the 13 diisocyanates.With the temperature program,the qualitative analysis was performed by retention time,and quantitative analysis was conducted by the resulted peak areas coupled with internal standard method.System-atical research demonstrated that the limit of detection for each diisocyanates was different,which ranged from 0.05 to 10 mg/kg.The recoveries located at 56% -104%,as well as the RSD ranged from 1.2 to 6.1%.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2010年第9期1337-1341,共5页
Chinese Journal of Analytical Chemistry
