Page 1 of 1
P-Nitroaniline GC Method
Posted: Wed Jul 20, 2011 6:12 am
by S.M.PANDYA
Dear Experts
I am looking for GC method for P-Nitroaniline .
I tried with DB-624 & DB-5 capillary column but did not find satisfactory result .
Can anybody help in this . If possible send method alongwith chromatogram .
Thanks in advance
Re: P-Nitroaniline GC Method
Posted: Wed Jul 20, 2011 7:17 am
by chromatographer1
You must have an inert system, including the injection liner and detector parts up to the flame tip.
So.......... how old is your column? Injection liner?
Or you can derivatize the free base.
best wishes,
Rod
Re: P-Nitroaniline GC Method
Posted: Thu Jul 21, 2011 3:51 pm
by tlahren
Chromatographer1 is right. Most likely the column is not the issue (unless it's old). I used to run this compound as part of a semi-volatiles list and the chromatography was always less than great but the liner I used made the biggest difference as well as injection parameters. Using an inert Siltek deactivated liner will work great (w/o wool if your analysis doesn't need it). I would use a pulsed splitless injection @ 25 psi (~170 kPa) of no more than 0.75 min splittless time to start on a 30m × 0.25mm × 0.25µm DB-5 column. You also have to make sure that the column cut on the injector is perfect with no breaks or burrs. Use a magnifying glass to check. It makes a difference. Overall there are a lot of factors that will affect nitroaniline in the GC. Starting with a completely inert system is the best suggestion.