I have a negative peak problem.

Chromatography Forum: LC Archives: I have a negative peak problem.
Top of pagePrevious messageNext messageBottom of pageLink to this message  By StephenLHardy on Friday, October 29, 1999 - 05:24 pm:

I am getting a negative peak immediately after the mineral oil peak. It is interfering with my integration. I am using DCM for my carrier solvent and I am using an infrared detector. This occurs even when I inject a blank sample. The mineral oil comes out at 16 minutes and the mineral oil peak does not return to baseline but goes immediately into a negative peak. What is causing this negative peak? I would appreciate any help you can give me. I have been trying to get this method working for 16 months.My supervisor is getting impatient. Help!


Top of pagePrevious messageNext messageBottom of pageLink to this message  By hinsbarlab on Tuesday, November 2, 1999 - 09:12 am:

What is the solvent the mineral oil is diluted in? What is your injection volume? What size and type of column? DCM = dichloromethane? What approaches have you tried to corrrect the problem already?


Top of pagePrevious messageNext messageBottom of pageLink to this message  By David Grant on Wednesday, November 24, 1999 - 07:51 am:

I have found that known analyte peaks are followed in some samples by a smallish neg peak, about 1/4 the size of the analyte peak. This happens about 5% of the time, sometimes to one of a series of replicates, sometimes to all. It seems sample specific, in other words, it does not happen to all the work done in a given morning. It fits no obvious pattern.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By anonymous on Wednesday, November 24, 1999 - 01:56 pm:

have you considered that the blending of your analyte with eluent (the tail) might cause a gradient with a lower IR absorbance than pure eluent (DCM). perhaps a change in eluent is called for?


Top of pagePrevious messageNext messageBottom of pageLink to this message  By ac on Tuesday, December 7, 1999 - 07:09 am:

Changing the brand/supplier for DCM may help.


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