应用柱前衍生-气相色谱法分离并测定了反应混合物中同存的季戊四醇(MPE)和双季戊四醇(DPE)、衍生化反应系在120 ℃加热的封闭试管中进行.将含有MPE及DPE的试样与甘露醇,4-二乙氨基吡啶及乙酸酐和吡啶的混合溶液置于此试管中,密封,加热并每隔10 min摇动溶液一次直至溶液成澄清液.此时MPE,DPE及甘露醇均生成乙酸酯衍生物,取此澄清溶液0.2 mL进行色谱分析,分离及测定时采用内装3% OV-17+3% XE-60及过180-150 μm 101AW-WS的不锈钢管(1 m× 3 mm)作色谱柱.应用此方法分析了不同含量的4个试样,所得结果的RSD值,测MPE时小于0.21%,测DPE时小于0.14%.测定值与标准值之间的偏差均小于0.7%.

Gas chromatography was applied to the separation and determination of pentaerythritol (MPE) and dipentaerythritol (DPE) in the reaction mixture by a precolumn derivatization process.Derivatization was carried out in a sealed reaction test tube at 120 ℃,by mixting the sample containing both MPE and DPE,mannitol 4-diethylaminopyridine and a mixed solution of ancetic anhydride and pyridine.Shake the reaction solution every 10 min until the solution turned to clear.0.21 mL of the clear solution containing the corresponding acetate derivatives was taken for GC analysis.A stainless steel chromatographic column (i.d.3 mm×1 m) filled with 3% OV-17+3% XE-60 and 101 AW-WS with graininese of 180-150 μm was used in the separation and determination.In its application to the analysis of 4 samples with different contents of MPE and DPE,RSD′s found were less than 0.21% for MPE and less than 0.14% for DPE,deviations of the determined values and the standard values were less than 0.7%.