For the analysis of the most commonly encountered phthalates by gas chromatography-mass spectrometry
(GC-MS), absorption of phthalates from the laboratory air on the outer wall of the syringe needle is shown to
be an important contribution to the blank problems. It was investigated for programmed temperature
vaporizing (PTV) injection. Cleaning of the needle in automated injection is of modest efficiency, since the
needle cannot be immersed deeply enough. Two approaches were studied to minimize transfer into the
column: (i) cleaning of the needle in the injector prior to splitless injection by inserting the needle in split
mode while the precolumn is backflushed, which presupposes a high injector temperature to be efficient; (ii)
injection under conditions minimizing thermal desorption from the needle wall, i.e. fast injection at low
injector temperature (e.g. 40 °C). Both approaches resulted in blank levels of around 0.1 pg for diisobutyl
phthalate (DIBP) and dibutyl phthalate (DBP), and of around 1 pg for di(2-ethylhexyl) phthalate (DEHP).
They could be useful tools in existing or future methods for the analysis of phthalates or other compounds
causing blank problems through contamination of the laboratory air.
