Headspace diluent contamination

[kmiller@insysrx.com]

Hello All,

I am having an issue keeping my diluent (used for headspace analysis of solvents) from getting contaminated with solvent fumes from our production lab. We recently ordered a new bottle and opened and aliquoted it under inert conditions. I opened one of the aliquotes in the lab to prepare my standards and samples and it was enough time to absorb/adsorb solvent fumes.
The levels are low, however, i would like my blank to look to like a blank.

Does anyone else have this problem or perhaps any good suggestions?

I am using N-Methyl-2-pyrrolidone (NMP).

Thanks.

[chromatographer1]

A purge box is one solution.

Preparing the standards outside of your lab is another solution.

I had methanol and acetonitrile and aromatics atmospheric contamination in my urban, downtown lab next to an LC lab.

Tolerate the contamination or get away from it. A purge box was an easy and doable solution.

Rod

[Peter Apps]

Some of the contaminants might be stuck on the glassware, rather than getting into the solvent direct from the atmosphere. Try baking off the glassware at 200 C or above for a few hours and using it immediately it has cooled to room temp.

Peter

[krickos]

Agree with Peter.

Also, some labs has specail preparation rooms that sheilded physically/ventilation wise from the rest of the lab to minimize contamination.

Depening on how big the problem is and what finances you have, you can pick different solutions.

[kmiller@insysrx.com]

A closed off area would be nice, but not do-able in our current available space. Other labs in our facility would be worse.

The contaminants probably are sticking to the glassware; I will try baking & see if we have a glove bag for my prep.

I appreciate yall’s suggestions.

Thanks!

[chromatographer1]

A useable purge box at Walmart may cost you $8-$12. A few feet of tygon tubing, a few dollars.

Do whatever your imagination leads you.

best wishes,

Rod