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Alkylated PAH analysis

Posted: Fri Oct 27, 2006 5:02 pm
by Sean
I have a mixture of PAH in an alkane solution that I am having trouble separating with ordinary methods. Most of the PAH in this solution have a high degree of alkylation making them extremely difficult to resolve (there are a very large number of PAH, and they tend to coelute).

My understanding is that a normal phase column will separate PAH by ring number with little sensitivity towards the alkyl groups. So my plan is to use a normal phase column to fractionate the sample by ring number, then use a reverse phase column to analyze each fraction.

I plan to buy a cyanopropyl column for this purpose, but I am wondering if there is a stationary phase better suited for this purpose. Is there a column that is more sensitive to ring number and less to alkyl groups?

Thanks in advance.

Posted: Fri Oct 27, 2006 5:22 pm
by Uwe Neue
It is not normal phase per se that tends to separate the PAH according to ring number. You need an amino column to do that.

Posted: Fri Oct 27, 2006 6:11 pm
by Sean
It is not normal phase per se that tends to separate the PAH according to ring number. You need an amino column to do that.
Thanks for the clarification. I was aware that I needed a specific stationary phase, but I didn't make it clear in the post. I believe my choices are either a cyano or amino column.

I had heard that an amino column would be ideal, but I am also told that compounds with carbonyl groups (which are present in my sample) will bind permanantly to the stationary phase. Is this true?

Posted: Fri Oct 27, 2006 9:32 pm
by Uwe Neue
I am not aware that cyano columns do this group separation as well. I have some doubts though. Nitro-phases do this though via clear pi-pi interactions.

You are right that amino phases are prone to react with aldehydes and ketones. Since you have such things in your sample, the amino column is not a good idea.

I would go for the nitro-phase, but you may have to dig until you find a supplier. Check with Macherey-Nagel in Germany!

Posted: Mon Oct 30, 2006 10:54 am
by HW Mueller
How do phenyl phases or Hypercarb behave with PAH?

Posted: Mon Oct 30, 2006 9:37 pm
by Uwe Neue
Phenyl columns give more retention for pi acceptors, but I don't think that this will help here.