Chromatography Forum

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?

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

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.

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

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