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Same Vial, Different Area Counts

Posted: Thu Jan 15, 2015 1:47 pm
by Kidkudi
Hello,

I have noticed an issue at my institute where a sample is run as part of a bracketing standard USP test method that yields areas low enough to generate a failing result. However, if the same sample prep is run on the same system (either a new vial is prepared or the same vial is used) with the same column, mobile phase, standards etc. the sample passes with expected area counts.

The system consists of an auto-injector, heated mobile phase, column heater and refractive index detector. The retention times of all standards and samples were very consistent and the area counts of the failing samples and the standards had very little variation (probably around 0.2% RSD).

My question is: why would the sample areas be low enough to give a failing result while in a subsequent run the area count for the sample is high enough that it would pass on the second analysis?

During first run, sample areas are low and fail. During second run, sample areas are high and sample passes. Nothing is changed from run 1 to run 2 (same column, mobile phase, detector, system, vials, etc.). Why does this happen?

Re: Same Vial, Different Area Counts

Posted: Fri Jan 16, 2015 6:20 am
by Gerhard Kratz
And what is your question?????

Re: Same Vial, Different Area Counts

Posted: Fri Feb 06, 2015 9:05 am
by danko
Kidkudi, What do you mean saying "run 1 and run 2"
Injection 1 and injection 2?

Re: Same Vial, Different Area Counts

Posted: Sat Feb 07, 2015 1:28 am
by tom jupille
Is this a consistent problem or did it happen only once?

Re: Same Vial, Different Area Counts

Posted: Thu Apr 02, 2015 6:05 am
by Alfred88
Hi,
I just want to throw in some simple things to check.
1/ Voltage supplied to UVD
2/ Lamp age of UVD
3/ Vial caps are pre-cut (have slit).

Good luck

Re: Same Vial, Different Area Counts

Posted: Thu Apr 02, 2015 8:15 am
by kubowicz.tomasz
Hi,
I just want to throw in some simple things to check.
1/ Voltage supplied to UVD
2/ Lamp age of UVD
3/ Vial caps are pre-cut (have slit).

Good luck
LC has RI detector

Re: Same Vial, Different Area Counts

Posted: Fri Apr 03, 2015 10:37 am
by dblux_
The original post is old enough to think that the person is no more interested in getting help, especially bearing in mind he or she was a "one time visitor".