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Ionisation Techniques Ionisation is the first stage of the mass spectrometric process, and occurs in an ion source. The type of ionisation chosen for a particular analysis will be dictated by the hyphenated technique being used and the sample in question. Electron Ionisation This is the classical ionisation technique used in mass spectrometry, and is still used extensively today in GC-MS experiments. The sample is vaporised by heating it in a small cup on the end of a probe. Of course in GC-MS the sample is already vaporised by the GC process and this stage of the ionisation is not necessary. The probe reaches into a high vacuum ion source and the sample ionised by a stream of fairly high energy electrons (typically ~70eV) emanating from a tungsten or rhenium filament source. Although most are elastically scattered, some of these high energy electrons remove electrons from the sample atoms, resulting in a radical ion (M +• ) – usually termed the molecular ion. This ion gives the molecular weight of the compound (minus the mass of one electron). These ions are unstable due to the high internal energy attained from the ionisation process, and as a result some or all of these ions will spontaneously fragment to smaller ions and neutrals. All the ions formed are continuously removed from the ion source by a small repeller voltage. After leaving the source a potential difference (300- 10000V) applied across the focussing lenses accelerates the ions towards the ion source. EI spectra contain more information than any other ionisation technique due to the excessive fragmentation. This fragmentation occurs as around 20eV will typically be transferred to the analyte molecule, and as the typical ionisation energy for many organic molecules is ~15eV, 5eV is retained by the molecule as internal energy. The covalent bond strength in organic molecules is of the order of a few eV, resulting in an unstable molecular ion which will reduce its energy by fragmentation. In some cases the molecular ion is not observed as it is totally fragmented, which can make determination of molecular weight, and thus identification, difficult. However, the fragmentation can allow structure elucidation of an unknown, and as the spectra produced are highly reproducible EI lends itself very well to library matching. EI gives good linear response curves, making it suitable for use in quantitative analysis.

Ionisation Methods in Mass Spectrometry

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