摘要
利用苯基三乙氧基硅烷的酸催化水解缩合反应合成了具有梯形结构的聚苯基硅倍半氧烷预聚体 ,再以其2 0 %～ 30 %的丙酮溶液对气相色谱用金属柱管进行遮盖性脱活 .预聚体涂层经溶剂挥发高温老化处理后获得了能耐 4 0 0℃高温的脱活涂层 .以甲醇、乙醇、异丙醇、叔丁醇为测试物 ,内径 2mm、长 3.0m、固定相为PorapackQ的填充聚四氟乙烯柱为预分离柱串接测试柱的方法对该涂层进行了评价 .结果表明 ,经该涂层处理的不锈钢柱管在115℃时对低级醇的吸附活性与PorapackQ柱的活性相近 ,活性明显降低 .涂层结构中含有的苯环和羟基等官能基 。
The coating material used as deactivating substance for stainless steel columns in gas chromatography has been prepared by dynamic processing of 30 % propanone solution of polyphenylsilsesquioxane(PPSQ) and aged at high temperature. This coating is thermal stable under 400 ℃ and solvent stable. The chromatagraphic behavior of said coating was studied by GC with a pre column of a 2 mm×3 m Teflon column packed with Parapack-Q and the test column under isothermal condition. The test mixture was a solution of methanol, ethanol, iso propanol and tert butanol in water with the concentration of 0.6 ng/mL. The experiment results indicate that the active sites on the inner surface of the stainless steel columns have been shield effectively by the coating. The inertness of the treated column is nearly the same as the pre column. The IR spectra indicated that there are phenyl and hydroxyl groups in the structure of the coating material, which can be used to improve the compatibility of other stationary phases with the inner surface of the stainless steel column and to supply active sides for preparing a bonded stationary phase.
出处
《分析测试技术与仪器》
CAS
2002年第1期10-14,共5页
Analysis and Testing Technology and Instruments
