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.
By Anonymous on Thursday, October 16, 2003 - 05:16 am:
What problems are you having, could you provide some details?
By vijayaragavan on Thursday, October 16, 2003 - 06:01 am:
sample - ditertiarybutyl dicarbonate
melting point - 30°C BoilingPoint - 57°C at vaccum
oven 40°C-10°C/MIN.-100°C -20°C/MIN - 240°C. INJECTOR 75°C TO 225°C (VARIOUS ATTEMPTS)
DETECTOR 250°C - FID
FLOW 1.0mL/MIN. - direct injection - neat sample
ABOVE 100°C INJECTOR TEMP. two broad peaks with less separation at 6.8 and one which tails at 9.8 min. (with less reproduceable results)
oven 60°C - 10°C/min - 120°C - 20°C/min. - 240°C, at 75°C 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
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?
By vijayaragavan on Thursday, October 16, 2003 - 10:23 pm:
you can verify any of the msds for the stability it should be stored below 0°C. 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.