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high cell current

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

3 posts Page 1 of 1
Hello,

After hours with our HPLC system, in the corresponding manuals and on the internet, I give up. After around 1 month of daily but not intensive use, the pressure and the cell current started to increase and the baseline became noisy.
I first changed the mobile phase for a fresh one. No improvement.
We changed the pre-column, and now the pressure is "normal". (yeah)
I cleaned, then polished the reference and working electrode and coated the reference electrode with its reference electrode solution.
I paid attention to bubbles and not to tight too strong the bolts when I reassembled the flow cell.
I checked bubbles everywhere t is visible on the system.
I performed an electrochemical cleaning of the working electrode by applying pulses of +1 to -1V during 10 min (I know I should have tried this before polishing)
I added more EDTA (it is now 0.1g/L, around 0.2mM) into the mobile phase.
But nothing had neither a positive nor a negative effect.

The screen displays an Icell = +66 nA!!!
(other settings are range NA, Eox=+0.65V, range 20 nA, Offset 0%, Filt. 2s)

The noise of the baseline is of course a problem (I would say it is a regular noise, but the baseline drifts up from time to time) but my concern is more the high cell current. I could not find anything about this issue on the internet whereas I have a list of potential causes of the noise and possible solutions.

Does anyone know? Could anyone explain me a bit about it: what can cause the Icell to increase (decrease?), what can I do to correct it?

Thanks a lot in advance for any information, I feel so alone!

Hi,

Do you use post column addition of NaOH?
If so, try to replace your NaOH, this can cause a lot of noise.
Also check if your components of your mobile phase are fresh.
You changed anything? eg switch from reagent supplier, other water source, ...?

Best regards

Ace

Hi Ace,

Thanks for your answer!
No, I do not use post-column addition of NaOH.
And I also did not change any reagent...
Today we cleaned the mobile-phase uptake frit, the column and the flow cell and I filtered the mobile phase. I cannot say much about the baseline, as I left it was not stabilised, but the cell current was still very high!
I plan to give a try again with polishing again the reference electrode but if it does not work we will try UV detection.
Or do you have other suggestion?

Best,
3 posts Page 1 of 1

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