As Elemental Analysis is an indicator of purity, samples submitted for analysis need to have been purified and be free from contaminents such as solvents, as the presence of any contaminants will affect the composition of gases produced during the pyrolysis.
This page provides some information on preparation methods for different types of samples. In all cases a minimum of 10 mg is required for analysis, although ideally 50-100 mg should be provided to enable the service technicians to easily prepare the samples for analysis. Samples should be submitted in narrow sample vials, as used for mass spectrometry.
Solid samples can be analysed for CHN with additional options to record oxygen or halogens (Note: F can only be analysed if >1%).
Prior to submission, solids should be recrystallised and thoroughly dried to remove any residual solvent. Solids need to be free flowing powders which are easy to weigh out. Samples may need grinding to break up larger crystal forms (eg long needles) prior to submission. Alternatively samples can be redissolved in solvent and rotary evaporated to give a powder.
Thorough drying of samples is essential. Samples should be placed on a high vacuum line to remove any residual solvent prior to submission.
Liquid samples can be analysed for CHN only.
It is possible to analyse volatile samples, but this should be clearly indicated on the submission form. Liquids should be distilled prior to submission to ensure they are sufficiently purified before analysis.