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Same Vial, Different Area Counts

Discussions about HPLC, CE, TLC, SFC, and other "liquid phase" separation techniques.

7 posts Page 1 of 1
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?
And what is your question?????
Gerhard Kratz, Kratz_Gerhard@web.de
Kidkudi, What do you mean saying "run 1 and run 2"
Injection 1 and injection 2?
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Dancho Dikov
Is this a consistent problem or did it happen only once?
-- Tom Jupille
LC Resources / Separation Science Associates
tjupille@lcresources.com
+ 1 (925) 297-5374
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
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
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".
7 posts Page 1 of 1

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