Chromatography Forum

Hi to every body,
i have some analysis on packed GC column and i want to confirm the compounds eluting on packed column with GC mass. I have Agilent 59873 and 5975 MS detector.
can anybody help me to do the Mass analysis with packed column.
though i know this technique is very usefull in early 60-70's and right now this techniques is not available but still i want to do this mass analysis.
help me to do mass analysis with packed column.

sample is gaseous highly reactive and corrosive and not possible to analyze on capillary column.

MS will only handle a couple on ml per minute so if you cannot use a smaller diameter column you will have to split your sample or use a jet separator (does anyone still make one ?) Can you not buy a suitable packed capillary column ?

Actually no one is preparing the capillary column consisting of G-30 as stationary phase. if anyone is capable to provide me the capillary column containing G-30 stationary phase i am ready to but the capillary column.
I am also looking for jet separator but still i can't able to find out the supplier for jet separator.
if anybody can provide me the jet separator then also i am ready to buy.

thanks and hope some one help me to do this kind of Job.

Fitting a jet separator to either of the MSs that you have might be quite difficult. I would be reluctant to put a corrosive sample in an MS anyway.

Peter

The question here is really the concentration. If it is high enough, then a splitter consisting of a length of 0.1 column to MS with a different length of 0.53 to vent would probably do what you want it to do. If the concentration is high enough.

As for the jet separator, I would contact SGE since they were the ones who made them in the past. They might still be able to make you one of the metal ones they brought out many years ago.

Best regards,

AICMM

Thanks a lot,
Actually the sample is sulfur tetra fluoride and i want to quantify one of the impurity SO2F2 and on many column i tried and found this impurity is coeluting with sulfur tetra fluoride peak.
both have the boiling point is -38°C and -44°C. If i can separate these two peaks by suitable capillary column then we can do it on sulfur detector (PFPD) also.
though this separation is very difficul due to high content of Sulfur tetrafluoride(99.0%) and SO2F2(0.10 to 1.0%).
if any body can suggest a capillary column which can work for these separation then please suggest.

thanks for continuous support.

Chandresh,

Out of curiosity, what packed columns have you tried? Which have had no success??

I will ping a buddy and see what he has to say about this application. He is not so old and very wise in the ways of
funky gas separations.

Best regards,

AICMM

Thanks AICMM,
actually i got one reference for the above separation which says
Tetra glyme ( USP Phase G-30) on 35-60 mesh Sodium fluoride

Or

Tetramethylene sulfone on 35 to 60 mesh sodium fluoride.

6ft x ¼ or 1/6 or 1/8 inch or1/16 inch narrower diameter

actually in my samples follwoing impurities are present:
SF4 main component. CF4, S2F6,SO2F2, SOF2, SF6 and HF (hydrogen Fluoride)

due to presence of HF and all other corrosive gases any stationary phase of capillary column is not suitable.
but in that case my focus is only on SF4 and the minor component SO2F2 which are not separable on the capillary column at this level.
Sodium fluoride is used to take care of HF.
now in a days nobody is ready to make this kind of packed column also so we are trying to focus on prepare this column and analysing the samples. but how we can ensure that the peak is pure.

with regards