Problem Negative peak in RI detection

Chromatography Forum: LC Archives: Problem Negative peak in RI detection
Top of pagePrevious messageNext messageBottom of pageLink to this message  By Pawel Palinkiewicz on Wednesday, May 29, 2002 - 12:44 am:

I have a problem with glucose/fructose/sucrose/sorbitol analysis.

HPLC: HP1050
Column: Alltech 700 CH Carbohydrate analysis
Detector: RI HP1057

Negative peak appears at 17 min. just before sorbitol ( it does not interfere with g/f/suc peak.

Since water is the eluent, I've injected three blanks 1.HPLC grade water 2.&3. water from two different deionizers. The negative peak appears on all the blanks, of the same size - additional but rather small negative peaks appeared for the first blanks earlier in the chromatogram.

I will be grateful for any hints and pointers to a solution.


One thing I am going to try is to separate the negative and sorbitol peaks, so thet I can do the sorbitol quantitation, but this is not a good solution.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By I.D. on Wednesday, May 29, 2002 - 04:35 am:

This could be a problem with deggasing. If you are using online vacuum deggaser - stop it and try again. Deggase samples/blanks.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Monday, June 3, 2002 - 09:23 am:

This question brings to mind a memory. Many years ago, I used RI a lot for determination of initiators in a polymer. The solvent was tetrahydrofuran and there was always a negative peak in th chromatograms. It did not seem to make a difference if we used new, old, stabilized, unstabilized, etc THF. We also got the peak just with solvent injection. I always assumed that it may have had to do with a side-effect of the injection (similar to a pressure peak in GC) or something like that. We could not do anying to change it, although the degassing should definitely be tried.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Thursday, June 6, 2002 - 08:30 am:

I've used the Bio-rad Aminex 87C column for a similar application with water as the mobile phase. I've seen a negative dip around 17 minutes due to low levels of methanol in the sample. Maybe you are picking up low levels of a solvent in your system or injector.


Top of pagePrevious messageNext messageBottom of pageLink to this message  By Anonymous on Tuesday, June 11, 2002 - 12:00 am:

Are u sure it is not a peak because of load-inject turning of injector?


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