Organic sulfurs in refrigerant gases - any methods available?

Chromatography Forum: GC Archives: Organic sulfurs in refrigerant gases - any methods available?
Top of pagePrevious messageNext messageBottom of pageLink to this message  By Paul on Wednesday, February 27, 2002 - 07:17 am:

I'm looking to develop a GC method to study the level of in-process sulfur contaminants in a fluorinated alkane stream. I have a Varian 3600 GC, P-FPD and DB-5 column and am experiencing sensitivity/reproducibility problems. Any one know of a better method/choice of GC column etc
Regards
Paul


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Rod on Wednesday, February 27, 2002 - 09:57 am:

Which of the sulfur compounds do you measure and at what levels?

Can you be more specific about the halogenated hydrocarbon content?

Can you do multidimensional chromatography? Do you have a 10 port injection valve installed?

I could give you a method for sulfurs up to a certain carbon number but I need to know the stream composition and/or if you need to know the individual sulfur components to determine the final analytical column needed.

Rodney George
Senior Research Chemist
Gas Separations Research
Supelco
595 North Harrison Road
Bellefonte, PA 16823


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Paul on Thursday, June 6, 2002 - 02:23 am:

Rod
apologies that I took so long getting back in touch. I typically see about 7 or 8 sulfur species, most of which are too low in concentration to determine their identities by GC-MS. I have however identified diethyldisulfide, ethanethiol and a chlorinated thiophene. The trouble is I only 'see' them after boiling off about 100g of trifluoroethane (R143a)and then purging the headspace of the test tube through a 6 port valve and onto the column (splitless). This is surprisingly reproducible but, I believe, low in efficiency. Any thoughts on improving this? I have tried a sample preconcentrator (Varian) but only managed to massively overload the column (and P-FPD) with R143a!


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