摘要
建立了反相高效液相色谱法测定固化剂中游离MDI含量的方法。以异丙醇为衍生剂进行柱前衍生化,选用Waters XTerra C18,5μm,3.9mm×150mm色谱柱,乙腈—水为流动相,V(乙腈)∶V(水)=50∶50,检测波长为254nm。在5～50μg/mL范围内,4,4'-MDI、2,4'-MDI的回归方程相关系数均大于0.999,固化剂中4,4'-MDI、2,4'-MDI添加回收率在102.3%～109.9%。按样品测定方法平行测定5次,2,4'-MDI、4,4'-MDI峰面积的相对标准偏差(RSD)分别为0.74%、0.49%。该法测定固化剂中游离MDI具有良好的准确性和精密度。
A method of reversed-phase HPLC determining free-MDI in curing agent products is established. The method is carried out under the follow chromatographic conditions：Isopropyl alcohol as pre-column derivatizing agent,column of Waters XTerra C18,5 μm and 3.9 mm×150 mm,the ratio of the two mobile phases （acetonitrile and water） being 1：1,and the wavelength of ultraviolet detection being 254 nm. In the range of 5～50 μg/mL,the correlation coefficients of regression equations of 4,4＇-MDI and 2,4＇-MDI are all more than 0.999. The recoveries of 4,4＇-MDI and 2,4＇-MDI in curing agent are in 102.3%～ 109.9%. The RSDs of peak areas of 2,4＇-MDI and 4,4＇-MDI in 5 parallel experiments by sample determination method are 0.74% and 0.49% respectively. Determination of free-MDI in curing agent by this method has good accuracy and reproducibility.
出处
《中国涂料》
CAS
2010年第10期53-55,共3页
China Coatings
关键词
高效液相
游离MDI
固化剂
异丙醇
衍生剂
HPLC； free-MDI； curing agent； isopropyl alcohol； derivatizing reagent；
