Boc anhydride by gc

Chromatography Forum: GC Archives: Boc anhydride by gc
Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Wednesday, October 15, 2003 - 09:36 pm:

hai,
in the analysis of di-tertiary butyl dicarbonate by gc i got problems with injector temperature.
i used hp1 capillary column and various inj. temp.
from 80 to 150 C.
any one could provide details about this.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Thursday, October 16, 2003 - 05:16 am:

What problems are you having, could you provide some details?


Top of pagePrevious messageNext messageBottom of pageLink to this message  By vijayaragavan on Thursday, October 16, 2003 - 06:01 am:

hai,
sample - ditertiarybutyl dicarbonate
melting point - 30C BoilingPoint - 57C at vaccum
column: hp1-(30mX0.32mmX0.25)
oven 40C-10C/MIN.-100C -20C/MIN - 240C. INJECTOR 75C TO 225C (VARIOUS ATTEMPTS)
DETECTOR 250C - FID
FLOW 1.0mL/MIN. - direct injection - neat sample

ABOVE 100C INJECTOR TEMP. two broad peaks with less separation at 6.8 and one which tails at 9.8 min. (with less reproduceable results)

oven 60C - 10C/min - 120C - 20C/min. - 240C, at 75C injector temp. one broad peak at 5.3 min and one which talis at 8.3 min. (with less reproduceable results)

does FID will really works for this sample but we don't have no option

or on column injection will help sorry this too not available.

or dervatisation will give some reasonable solution.

please help me this sample is so important to us


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Thursday, October 16, 2003 - 06:15 am:

My guess is you are dealing with a temperature sensitive compound that is unstable. On cold column injection (0.53mm id column or precolumn?) may be necessary. How about NMR to look for impurities?


Top of pagePrevious messageNext messageBottom of pageLink to this message  By vijayaragavan on Thursday, October 16, 2003 - 10:23 pm:

hi,
you can verify any of the msds for the stability it should be stored below 0C. self life is 2 years. NMR (H) won't work. i asked for C13 results. if you heat in a vial bubbles are coming out. i guess CO2 & CO are coming out. but the sample doesn't contain t-butanol.
almost all lit. survey speaks about gc analysis.
one tells for titration method.
i really wondering where i am lacking.


Add a Message


This is a private posting area. A valid username and password combination is required to post messages to this discussion.
Username:  
Password: