A low thermal mass fast gas chromatograph and its implementation in fast gas chromatography mass spectrometry with supersonic molecular beams

Alexander B. Fialkov, Mati Moragn, Aviv Amirav

Research output: Contribution to journalArticlepeer-review

Abstract

A new type of low thermal mass (LTM) fast gas chromatograph (GC) was designed and operated in combination with gas chromatography mass spectrometry (GC-MS) with supersonic molecular beams (SMB), including GC-MS-MS with SMB, thereby providing a novel combination with unique capabilities. The LTM fast GC is based on a short capillary column inserted inside a stainless steel tube that is resistively heated. It is located and mounted outside the standard GC oven on its available top detector port, while the capillary column is connected as usual to the standard GC injector and supersonic molecular beam interface transfer line. This new type of fast GC-MS with SMB enables less than 1min full range temperature programming and cooling down analysis cycle time. The operation of the fast GC-MS with SMB was explored and 1min full analysis cycle time of a mixture of 16 hydrocarbons in the C 10H 22 up to C 44H 90 range was achieved. The use of 35mL/min high column flow rate enabled the elution of C 44H 90 in less than 45s while the SMB interface enabled splitless acceptance of this high flow rate and the provision of dominant molecular ions. A novel compound 9-benzylazidanthracene was analyzed for its purity and a synthetic chemistry process was monitored for the optimization of the chemical reaction yield. Biodiesel was analyzed in jet fuel (by both GC-MS and GC-MS-MS) in under 1min as 5ppm fatty acid methyl esters. Authentic iprodion and cypermethrin pesticides were analyzed in grapes extract in both full scan mode and fast GC-MS-MS mode in under 1min cycle time and explosive mixture including TATP, TNT and RDX was analyzed in under 1min combined with exhibiting dominant molecular ion for TATP. Fast GC-MS with SMB is based on trading GC separation for speed of analysis while enhancing the separation power of the MS via the enhancement of the molecular ion in the electron ionization of cold molecules in the SMB. This paper further discusses several features of fast GC and fast GC-MS and the various trade-offs involved in having powerful and practical fast GC-MS.

Original languageEnglish
Pages (from-to)9375-9383
Number of pages9
JournalJournal of Chromatography A
Volume1218
Issue number52
DOIs
StatePublished - 30 Dec 2011

Keywords

  • Fast GC
  • Fast GC-MS
  • High throughput analysis
  • Low thermal mass
  • Supersonic molecular beams

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