I'm analyzing Organic Impurities in Ethanol by GC/MS and having poor reproducibility. The ethanol samples are diluted to ~40% in water and injected using headspace technique. Sample is incubated at 65 degrees C and 1 mL is injected. Internal Standards are used. Reproducibility intermittently poor. Could this be an incubation issue?
Water might not be the best solvent to dilute the samples with in this case. Maybe an alternative solvent like toluene (the organic impurities may not be water soluble) and a different incubation temperature might be more appropriate.
Is your reproducibility poor after correction for your internal standards? If so, are the internal standards similar enough to your impurities?
Are you injecting split or splitless? 1 ml could be overflowing your liner giving you poor reproducibility
Can you tell what impurities your are looking for, your internal standards,, GC program, column type, etc.
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