Development and validation of an automated static headspace gas chromatography-mass spectrometry (SHS-GC-MS) method for monitoring the formation of ethyl methane sulfonate from ethanol and methane sulfonic acid.
An automated sample preparation and analysis procedure was developed to monitor the formation of ethyl methane sulfonate from reaction mixtures containing ethanol and methane sulfonic acid. The system is based on a liquid handling robot combined with a static headspace module. The formed ethyl methane sulfonate is analysed after derivatisation with pentafluorothiophenol using static headspace-gas chromatography-mass spectrometry (SHS-GC-MS). Using the automated reaction-derivatisation-headspace GC-MS system, the formation of ethyl methane sulfonate can be monitored in different reaction mixtures under different reaction conditions, including temperature, water content and pH. Excellent linearity, repeatability and robustness were obtained, allowing the system to be used in kinetic studies.
Jacq
Karine
K
Research Institute for Chromatography, Pres. Kennedypark 26, B-8500, Kortrijk, Belgium.
Delaney
Ed
E
Teasdale
Andrew
A
Eyley
Steve
S
Taylor-Worth
Karen
K
Lipczynski
Andrew
A
Reif
Van D
VD
Elder
David P
DP
Facchine
Kevin L
KL
Golec
Simon
S
Oestrich
Rolf Schulte
RS
Sandra
Pat
P
David
Frank
F
D000431:Ethanol / Q000737:chemistry*; D005020:Ethyl Methanesulfonate / Q000138:chemical synthesis* / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D008698:Mesylates / Q000737:chemistry*; D015394:Molecular Structure; D012015:Reference Standards; D015203:Reproducibility of Results; D012371:Robotics / Q000379:methods; D013696:Temperature; D013997:Time Factors
D008698:Mesylates; C045880:methanesulfonic acid; D000431:Ethanol; D005020:Ethyl Methanesulfonate