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Natural Science Forum / Chemistry / Organic Synthesis / August 2003



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GC help!

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Richard Guy - 11 Jul 2003 20:28 GMT
Hello,

For three days now I've been struggling to separate the enantiomers of
cryptone (4-isopropylcyclohexenone) using a chiral column on our HP
5890 Series II GC. No matter what conditions I try, the enantiomers
won't separate, the best I get is a broad (rather than sharp) peak.

I would be very grateful for any assistance anyone could provide me
with. I have been unable to track down GC conditions for this
molecule, and there is no GC knowledge base in my department.

Thanks in advance,

Richard
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Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

Mark Thorson - 14 Jul 2003 17:47 GMT
> I would be very grateful for any assistance anyone could provide me
> with. I have been unable to track down GC conditions for this
> molecule, and there is no GC knowledge base in my department.

Go here:

http://www.chromforum.com/

They have a discussion forum for GC.  Lots of knowledgable
people use it.  They also have a forum for HPLC.

It is a commercial web site, but it doesn't require cookies
or registering.  You can even post to the discussion groups
without doing any of that.  It's run by a trade magazine,
which doesn't show favoritism to particular vendors.

There are representatives of vendors who monitor the
discussion groups who will often recommend their own
products, but a lot of these guys are also great sources
of information.

There's almost no editing or moderation of the postings
made to the groups.  The only example I can think of
is a certain crackpot who is carrying on a personal war
against his former employer, a Japanese instrument
manufacturer.  :-)

I think you're much more likely to get a useful answer
there, than in sci.chem.  But there's no reason not to
use both.

Signature

Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

EdiSon - 15 Jul 2003 16:45 GMT
> Hello,

> For three days now I've been struggling to separate the enantiomers of
> cryptone (4-isopropylcyclohexenone) using a chiral column on our HP
> 5890 Series II GC. No matter what conditions I try, the enantiomers
> won't separate, the best I get is a broad (rather than sharp) peak.

> I would be very grateful for any assistance anyone could provide me
> with. I have been unable to track down GC conditions for this
> molecule, and there is no GC knowledge base in my department.

> Thanks in advance,

> Richard

Uncle Al can help. His email is: organiker@lycos.com

Signature

Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

Andrew P - 18 Jul 2003 15:16 GMT
> Hello,

> For three days now I've been struggling to separate the enantiomers of
> cryptone (4-isopropylcyclohexenone) using a chiral column on our HP
> 5890 Series II GC. No matter what conditions I try, the enantiomers
> won't separate, the best I get is a broad (rather than sharp) peak.

> I would be very grateful for any assistance anyone could provide me
> with. I have been unable to track down GC conditions for this
> molecule, and there is no GC knowledge base in my department.

> Thanks in advance,

> Richard

Has the technique worked previously for this compound or are you using are
you porting an existing method and hoping it will owrk in this instance?
try tweaking the conditions such as oven temp, ramp rates etc. Also how old
is the column, can you bake it to recover some lost active sites on the
stationary phase.

Andy

Signature

Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

Richard Guy - 09 Aug 2003 15:19 GMT
> Has the technique worked previously for this compound or are you using are
> you porting an existing method and hoping it will owrk in this instance?
[quoted text clipped - 3 lines]
>
> Andy

Thanks for all the help. In the end I got some flow rate values from
Agilent, but they were similar to the flow rates on our GC. So I
decided that the column just wouldn't separate the enantiomers of this
compound (the column is OK, it separates other peoples' enantiomers
fine).

I have had more success with HPLC.

Richard
Signature

Paul J. Franklin(moderator - sci.chem.organic.synthesis)
http://organicworldwide.net/sci.chem.organic.synthesis
Georgia State University <chepjf@panther.gsu.edu>
Atlanta, GA

 
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