HPLC Determination of Emission Quantity of 2 Diisocyanates in Polyurethane Adhesives after Application
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0.2 mol·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pH 6.0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242 nm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20.0 mg·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0.020,0.040 mg·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%。
Abstract
HPLC was applied to the determination of emission quantity of 2 diisocyanates, i.e. 2,6-TDI and HDI 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 (33+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%.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201808008
所属栏目 工作简报
基金项目 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)
收稿日期 2017/10/27
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备注强音,工程师,研究方向为进出口涂料、胶黏剂有害物质检验及标准化
引用该论文: QIANG Yin,XIAN Yang,SHAO Min,GU Zhongyi,JIN Yinghua,CHENG Yuxiao. HPLC Determination of Emission Quantity of 2 Diisocyanates in Polyurethane Adhesives after Application[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(8): 906~910
强音,咸洋,邵敏,顾中怡,金樱华,程欲晓. 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[J]. 理化检验-化学分册, 2018, 54(8): 906~910
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参考文献
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【2】GBZ/T 160.67-2004工业场所空气有害物质测定异氰酸酯类化合物[S].
【3】宫经会.工作场所空气中甲苯二异氰酸酯(TDI)采集与测定方法的研究[J].长江大学学报(自然科学版), 2011,8(5):14-15.
【4】郭新东,冼燕萍,杜志峰,等.气相色谱法快速测定食品用胶粘剂中9种有毒物质[J].现代食品科技, 2008,24(9):937-939.
【5】向仲朝,先德强,刘鹏程,等.空气中甲苯二异氰酸酯的高效液相色谱测定法[J].环境与健康杂志, 2011,28(11):1002-1003.
【6】栾杨,李翎,王晓芸,等.车间空气中2,4-二异氰酸甲苯酯的高效液相色谱测定法[J].中华劳动卫生职业病杂志, 1999,17(5):302-303.
【7】崔强,宋景平,刘浏,等.空气中TDI的滤膜采集和HPLC测定法的实验研究[J].职业与健康, 2005,21(12):1957-1958.
【8】MOLANDER P, HANGLAND K, FLADSETH G, et al. Determination of 1-(2-methoxyphenyl) piperazine derivatives of isocyanates at low concentrations by temperature-programmed miniaturized liquid chromatography[J]. Journal of Chromatography A, 2000,892:67-74.
【9】MATTSSON C, LINDH C H, TINNERBERG H. Underestimation of toluene diisocyanate concentration using long-term sampling with 1-(2-methoxyphenyl) piperazine impregnated filters[J]. International Journal of Hygiene and Environmental Health, 2008,211:458-462.
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