高效液相色谱法测定聚氨酯胶黏剂施工后2种二异氰酸酯类化合物的释放量  

HPLC Determination of Emission Quantity of 2Diisocyanates in Polyurethane Adhesives after Application

作　　者：强音[1] 咸洋[2] 邵敏[1] 顾中怡[1] 金樱华[1] 程欲晓[1] QIANG Yin;XIAN Yang;SHAO Min;GU Zhongyi;JIN Yinghua;CHENG Yuxiao(Shanghai Entry-Exit Inspection and Quarantine Bureau,Shanghai 200135,China;Shanghai Research Institute of Materials,Shanghai 200437,China)

机构地区：[1]上海出入境检验检疫局,上海200135 [2]上海材料研究所,上海200437

出　　处：《理化检验（化学分册）》2018年第8期906-910,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家质检总局科技专项(2017IK159;2017IK229);国家质检总局公益性行业科研专项(201510203-04)

摘　　要：采用高效液相色谱法测定聚氨酯胶黏剂施工后2种二异氰酸酯类化合物(2,6-甲苯二异氰酸酯和六亚甲基二异氰酸酯)的释放量。聚氨酯胶黏剂样品涂覆于玻璃板上,置于气候箱中,用含1-(2-甲氧基苯基)哌嗪的玻璃纤维滤膜采样,取出滤膜放于瓶中,加入0.2mol·L^(-1 )1-(2-甲氧基苯基)哌嗪甲苯溶液、乙酸乙酯和乙酸酐。采用Hypersil ODS色谱柱为分离柱,以乙腈与pH6.0的乙酸-乙酸钠缓冲溶液以体积比33∶67组成的混合液为流动相,在检测波长242nm处进行测定。2,6-甲苯二异氰酸酯和六亚甲基二异氰酸酯的质量浓度均在20.0mg·L^(-1)以内与其对应的峰面积呈线性关系,检出限(3S/N)依次为0.020,0.040mg·L^(-1)。加标回收率为81.4%~101%,测定值的相对标准偏差(n=6)为1.1%~6.6%。HPLC was applied to the determination of emission quantity of 2 diisocyanates, i.e. 2,6-TDI andHDI in polyurethane adhesives after application. The sample of polyurethane adhesive was spread on a glass plate, which was then put into the environmental chamber. Glass fiber filter membranes impregnated with 1-2MP were used for air sampling. The filter membranes were removed and put in a bottle. 0. 2 mol·L^-1 1-2MP toluene solution, ethyl acetate and acetic anhydride were added in the bottle. Hypersil ODS chromatographic column was used as stationary phase, and a mixture of acetonitrile and acetic acid-sodium acetate buffer solution of pH 6. 0 （33q-67） was used as mobile phase. Detection at 242 nm was adopted in the determination. Linear relationships between values of peak area and mass concentration of 2, 6-TDI and HDI were kept in the same range within 20. 0 mg·L^-1 , with detection limits（3S/N）of 0. 020, 0. 040 mg·L^-1 , respectively. Values of recovery found by standard addition method were in the range of 81.4%--101%, and values of RSDs （n= 6） were in the range of 1.1%-6.6% .

关 键 词：高效液相色谱法 聚氨酯胶黏剂 二异氰酸酯 释放量 

分 类 号：O652.63[理学—分析化学]