摘要
以DB1701P毛细管柱为分析柱,十四烷为内标物,建立了一套用于聚氨酯固化剂中游离六亚甲基二异氰酸酯(HDI)检测的气相色谱条件。通过对进样温度、气化室程序升温进行选择,分别对低浓度游离HDI样品(已知样品N75)和高浓度游离HDI样品(实验室制HDI缩二脲未知样)进行分析。实验结果得到已知样品变异系数为6.48%,未知样品变异系数为1.77%;同时对合成反应过程中的高游离HDI的检测也有很好的准确度和重现性。表明该方法既适用于检测聚氨酯固化剂产品中的低浓度(0.1%～2.0%)游离HDI含量,也适用于跟踪反应过程中高浓度(30%～90%)游离HDI含量变化,对于确定合成反应的终点和检测HDI缩二脲产品性能具有重要意义。
A method to determine unreacted hexamethylene diisocyanate （HDI） content in polyurethane curing agent was established by gas chromatography with DB1701P capillary column and tetradecane as the internal standard. Through the choice of the injection temperature and vaporizer temperature program,HDI samples in low concentration range （with known sample N75） and HDI samples in high concentration range （unknown sample prepared in lab with HDI biuret） were analyzed. The coefficients of variation of the known sample and unknown sample were 6.48% and 1.77%,respectively：and detection of high free HDI during the synthesis reaction also had good accuracy and reproducibility. The experimental results show this method can not only determine the content of free HDI with low concentration （0.1%～2.0%） in the polyurethane curing agent,but also track the content variation of free HDI with high concentration （30%～90%） during the reaction process of polyurethane curing agent. It plays an important role in determining the end point of synthesis process and detecting the properties of HDI biuret.
出处
《新型建筑材料》
北大核心
2011年第10期40-44,共5页
New Building Materials
基金
广东省教育部产学研结合重大科技专项项目(2010A09020039)
华南理工大学中央高校基本科研业务费资助重点项目(2009ZZ0062)
