Blocked frit

Chromatography Forum: LC Archives: Blocked frit
Top of pagePrevious messageNext messageBottom of pageLink to this message  By Pål V. Hemmingsen on Tuesday, January 9, 2001 - 01:55 am:

Hi

I'm currently packing my own SEC columns using poly(styrene-divinylbenzene) particles. As columns I have used some old Waters styragel columns, with old frits which I have cleaned in methanol in an ultrasound bath. When I started I used rather tough packing conditions, and experienced peak doubling. This was probably caused by blocked frits from fragments of damaged column particles. Later I used a kinder packing method and made some satisfactory columns. However, I still have some problems on some columns with broad peaks and I wonder if some of the frits I have could still be blocked. Has anyone some suggestion on how to clean frits, blocked with poly(styrene-divylbenzene)? The frits seems to be metallic, the poresize I guess is 2 um, they are from Waters styragel HT 6E columns.

Best Regards

Pål V. Hemmingsen


Top of pagePrevious messageNext messageBottom of pageLink to this message  By bill tindall on Tuesday, January 9, 2001 - 09:02 am:

I have never tried to clean a frit so the following is a guess. Styrene divinylbenzene polymers can be analyzed by pyrolysis, that is they nearly quantitatively pyrolyze to monomers upon heating. Hence, it might be possible to remove this polymer from a frit by heating the frit to a few hundred degrees.

Alternatively,Waters might sell you some new frits.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Thursday, January 11, 2001 - 12:25 am:

Boil them in 50% nitric acid for at least 30mins.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Tuesday, February 6, 2001 - 07:25 am:

Try a cleaning with ultrasonic bath for 30 min
in 15% nitric acid.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Guido on Thursday, February 22, 2001 - 08:55 am:

Get some new spare frits on hand, don't waste your time and money with cleaning experiments!


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