Video-taped sample evaporation in hot chambers simulating gas chromatography split/splitless injectors. I. Thermospray injection.
The processes in devices imitating vaporising injectors were visualised and video-taped using perylene as a fluorescent marker for non-evaporated samples. The observations in the context of thermospray injection are summarised. Partial evaporation inside the needle turns the solvent into a propellant which nebulises the sample liquid at the needle exit. Evaporation in the vaporising chamber occurs from fine droplets suspended in the gas phase. Empty injector liners are best suited; packings with glass wool or obstacles in the liner, like the cup, have no significant effect on the process observed. Non-evaporated (matrix) material forms aerosol particles which may enter the column together with the vapours, but most of them are transferred to the liner wall. Since solute material may be carried along, this is a possible source of matrix effects.
Large volume splitless injection with concurrent solvent recondensation: keeping the sample in place in the hot vaporizing chamber.
An injector liner packed with a plug of glass wool is compared with a laminar and a mini laminar liner for large volume (20-50 microL) splitless injection with concurrent solvent recondensation (CSR-LV splitless injection). Videos from experiments with perylene solutions injected into imitation injectors show that glass wool perfectly arrested the sample liquid and kept it in place until the solvent had evaporated. The sample must be transferred from the needle to the glass wool as a band, avoiding 'thermospraying' by partial solvent evaporation inside the needle. The liquid contacted the liner wall when the band was directed towards it, but from there it was largely diverted to the glass wool. In the laminar liners, part of the liquid remained and evaporated at the entrance of the obstacle, while the other proceeded to the center cavity. Vapors formed in the center cavity drove liquid from the entrance of the obstacle upwards, but the importance of such problems could not be verified in the real injector. Some liquid split into small droplets broke through the obstacle and entered the column. Breakthrough through the laminar liners was confirmed by a chromatographic experiment. An improved design of a laminar liner for large volume injection is discussed as a promising alternative if glass wool causes problems originating from insufficient inertness.
Augusta Klumpke: pioneering female neurologist.
The latter part of the 19th century was an exciting period when women at last were succeeding in their battle to obtain their medical training and qualifications to practice in the UK, continental Europe and in the USA. Moreover, and perhaps not surprisingly, many of these determined and doughty pioneers showed themselves to be exceptionally able in their chosen specialities. Perhaps the best example of this was Augusta Klumpke (Figure 1), who became an outstanding neurologist in Paris. This year marks the 150th anniversary of her birth.