Minimisation of artefact formation of dimethyl disulphide during sampling and analysis of methanethiol in air using solid sorbent materials

作者：Andersen Kristin Barkve; Hansen Michael Jorgen; Feilberg Anders^*

来源：Journal of Chromatography A, 2012, 1245: 24-31.

DOI：10.1016/j.chroma.2012.05.020

• Methanethiol
• Dimethyl disulphide
• PTR-MS
• TD-GC-MS
• Sorbent tubes

Methanethiol (MT) is a potent odorant that can be difficult to measure due to its high volatility and reactivity; it easily reacts to form dimethyl disulphide (DMDS) during sampling and/or analysis. This paper focuses on finding an optimal method for sampling and measuring MT with minimum artefact formation using sorbent materials and a thermal desorption-gas chromatography-mass spectrometry method (TD-GC-MS). Experiments were conducted to identify suitable sorbent materials and tubes for analysis. Breakthrough, desorption rate, the effects of storage and desorption temperatures were investigated and different drying methods were established with respect to quantitative sampling and formation of DMDS. Proton-transfer-reaction mass spectrometry (FTR-MS) was used in the development of the method and was an especially useful tool for determination of breakthrough. The results show that glass tubes packed with silica gel for pre-concentration of MT before analysis with TD-GC-MS give the best results. In addition, a combination of Tenax TA and carbonised molecular sieve or Tenax TA cooled to %26lt;0 degrees C gives acceptable results. 80 degrees C was found to be the optimal desorption temperature. For all the sampling methods tested, storage conditions were observed to be very critical for transformation of MT. Room temperature storage should be limited to few minutes and, in general, tubes should be kept at 0 degrees C or lower during storage.

• 出版日期2012-7-6