[Structure determination of alkyd resins by simultaneous pyrolysis methylation gas chromatography-mass spectometry].
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 ug of the mixed alkyd resin sample was introduced into the center of the pyrolyzer at 450 degrees C 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 x0.25 mm i.d. x 0.25 um). Temperature program settings were: initial temperature, 40 degrees C, hold 2 min; increase at 6 degrees C min 1 to 220 degrees C, hold 14 min; increase at 10 degrees C min 1 to 280 degrees C, hold 8 min. All pyrolysis products referred to were identified by mass spectrometry. The temperature of the ion source was 210 degrees C and that of the transfer line was 250 degrees C. The technique could give additional information about the composition of the dibasic acids, polyols, six types of drying oils, and modified alkyd resins. The method is sensitive, accurate, convenient, and involves minimal sample manipulation.
Cao
J Y
JY
Fu
D H
DH
Zhang
F
F
Liang
D
D