摘要：用裂解同时烷基化气相色谱-质谱联用技术（SPM-GC-MS）对不同类型的醇酸树脂进行分析研究，将衍生化试剂四甲基氢氧化胺与样品同时裂解，经高效毛细管气相色谱分离，质谱鉴定，可区分醇酸树脂中的多元醇、多元酸、植物油类型，由此对改性醇酸树脂作结构鉴定。与直接裂解-气相色谱-质谱联用技术比较，具有样品前处理快速、简单，用量少，灵敏度高，定性准确，谱图直观等特点。
Abstract:Several types of alkyd resins have been analyzed by simultaneous pyrolysis methylation gas chromatography -mass spectrometry (SPM-GC-MS). The samples were mixed with tetramethylammonium hydroxide, and the process included simultaneous pyrolysis derivatization and mass spectrometry determination. SPM-GC-MS conditions: a vertical microfurnace-type pyrolyzer was directly attached to a gas chromatograph-mass spectrometer. About 20 μg of the mixed alkyd resin sample was introduced into the center of the pyrolyzer at 450 ℃ under the flow of helium carrier gas. The inlet mode was split with an injection interval of 10 s and the inlet pressure was 82.7 kPa. The gas chromatograph was fitted with a fused-silica capillary column ( SE-54 30 m×0.25 mm i.d.×0.25 μm).Temperature program settings were: initial temperature,40 ℃, hold 2 min; increase at 6 ℃.min-1 to 220 ℃, hold 14 min; increase at 10 ℃.min-1 to 280 ℃, hold 8 min. All pyrolysis products referred to were identified by mass spectrometry. The temperature of the ion source was 210 ℃ and that of the transfer line was 250 ℃. The technique could give additional information about the composition of the dibasic acids, polyols, six types of drying oils , and modified alkyd resins. This method is sensitive, accurate, convenient, and involves minimal sample manipulation.
作者简介：曹京宜(1972-)，女，硕士研究生，工程师，电话：(010)66975477。
曹京宜(海军舰船维修研究所， 北京 100072)
付大海(海军舰船维修研究所， 北京 100072)
张峰(海军舰船维修研究所， 北京 100072)
梁栋(海军舰船维修研究所， 北京 100072)
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原载于《色谱》2000 Vol.18 No.5 P.390-393
http://www.chinainfo.gov.cn/periodical/sp/sp2000/0005/0005ml.htm
作者：
2007-5-18