ANALYSIS OF A MIXTURE OF LINEAR AND CYCLIC SILOXANES BY CRYO-GAS CHROMATOGRAPHY FOURIER-TRANSFORM INFRARED-SPECTROSCOPY AND GAS-CHROMATOGRAPHY MASS-SPECTROMETRY

被引:21
作者
WACHHOLZ, S [1 ]
KEIDEL, F [1 ]
JUST, U [1 ]
GEISSLER, H [1 ]
KAPPLER, K [1 ]
机构
[1] TECH UNIV DRESDEN,D-01069 DRESDEN,GERMANY
关键词
D O I
10.1016/0021-9673(94)01115-U
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A mixture of linear and cyclic methylsiloxanes was analysed to characterize the different types of siloxane structures using gas chromatography (GC), mass spectrometry (MS) and Fourier transform infrared (FT-IR) spectroscopy. Siloxane structures are formed by hydrolysis of dimethyldichlorosilane under controlled conditions in technical applications. In the presence of methyltrichlorosilane or even trimethylchlorosilane, linear polydimethylsiloxanes and mono-, bi- or polycyclic methylsiloxanes are synthesized depending on the reaction conditions. The main structural units are (CH3)(3)SiO1/2, (CH3)(2)SiO and (CH3)SiO3/2. GC-MS may provide molecular mass information, but it is not able to identify isomeric structures, which are also formed in lower quantities by the mentioned reactions. Coupling GC with FT-IR enables the determination of group frequencies to assign specific structures. Thus, combination of GC with MS and FT-IR may be used in elucidating complex cyclosiloxane compounds. FT-IR measurements were performed with a Tracer unit.
引用
收藏
页码:89 / 99
页数:11
相关论文
共 14 条
[1]  
ALEXANDER G, 1974, CHROMATOGRAPHIA, V7, P190
[2]  
BOURNE S, 1990, ANAL CHEM, V62, P2449
[3]   COMPARISON OF GAS-CHROMATOGRAPHY FOURIER-TRANSFORM INFRARED SPECTROMETRIC GRAM-SCHMIDT RECONSTRUCTIONS FROM DIFFERENT INTERFEROMETERS [J].
BRISSEY, GM ;
HENRY, DE ;
GISS, GN ;
YANG, PW ;
GRIFFITHS, PR ;
WILKINS, CL .
ANALYTICAL CHEMISTRY, 1984, 56 (12) :2002-2006
[4]  
GARZO G, 1971, ACTA CHIM HUNG, V69, P273
[6]  
JANCKE H, 1973, Z CHEM, V13, P392
[7]   SPEKTROSKOPISCHE UNTERSUCHUNGEN AN SILICIUMVERBINDUNGEN .7. DIE SCHWINGUNGSSPEKTREN DER HOHEREN DIMETHYL-POLYSILOXAN-RINGE UND DIE STRUKTUR DES OKTAMETHYL-CYCLO-TETRASILOXANS [J].
KRIEGSMANN, H .
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE, 1959, 298 (3-4) :232-240
[8]  
KRIEGSMANN H, 1962, ADV MOL SPECTROSC, P999
[9]  
LIPP ED, 1991, ANAL CHEM SILICONES, P323
[10]   METHYLPOLYSILOXANES [J].
PATNODE, W ;
WILCOCK, DF .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1946, 68 (03) :358-363