Cleanest Headspace Vials

[Charles A. Burger]

So I'm working with a Total Evaporation Technique Headspace method. It has become clear that Manufacturers are not very familiar with this technique because I am getting plenty of garbage in my chromatography.

One partial solution has been to bake out the vials at 240°C. This had helped, but I still do get extra peaks.

So has anyone else had dealings with this style of Headspace? If so, what vials and septum have you had the best luck with?

[gapeev]

How about
1. baking glass at ~500C
2. Incubating plastic parts in conc H2SO4+NaCr2O7 briefly

[MSCHemist]

Hmm I use total evaporative static headspace and don't have many issues. I see one or two triangular peaks occasionally (GC/MS no definative ID probably siloxane or similar) but otherwise pretty clean blanks (other than carryover up to 5% for polar compounds like small acids and alcohols). I use a Tekmar 7000 loop system and I reuse headspace vials. Nothing fancy just put them in my dishwasher. The 9ml vials are hard to get for that instrument. I use typical crimp caps.

[Charles A. Burger]

What is your volume into the headspace vial. For me its 5µl of STD or Sample into a 10 ml Headspace vial and cap.

[MSCHemist]

7.5ul aqueous solution into a 9.2ml headspace vial. Tekmar 7000 takes an odd size.