I am going to rerun a scanning electrochemical microscopy . It is from CH instrument. I can make a nice CV of the ferrocincarboxylic acid as the mediator with both the UME and the substrate electrode (Pt 25 uM). but when I want to record the probe approach curve it doers not work. in CV the current is in the order of nA .In probe approach curve during the quiet time the current is in the same order but when it want to start the current jump to 10-7 A. and I have no point recorded. Any advice and guide is very welcome.
Thank you for explaining your experimental setup. I have a couple observations regarding to what you send:
1.- I think you should improve the response of your microelectrode. It must show a steady state current (related to your mediator oxidation) when you run the CV. In order to achieve that, I will suggest to check that your microelectrode tip is clean and it has the right geometry (disc), with a good RG value. Also, I would suggest to change your potential range from -0 V to +0. 6V.
Here is a link that shows a good example of CV for the mediator that you are using:
2.-You may change some parameters for the approach curve, for instance:
Probe E(V) to 0.6
Max Incr(um) to 1 or 2
Withdraw distance (um) to 100 or 200.
Being further from the substrate and having a smaller step size might let you see the approach curve with more points, and thus with a better resolution to detect additional issues, if any.
I really hope that everything goes well. Kind regards.
I tried every parameter but it did not help me. To observe the problem which I am facing I recorded a video . Please see the current manitude at quiet time and after it. is it possible to observe such a big jump just in the beggining of the scan. (scan was only in Z direction). Because I have never had the oppurtunity to attend in any training course for this instrument and it was not being used for some years I am afraid that there is something wrong with it .
I put the tip far from the substrate (very far) and I did it manually it means I used the XZY control and put the tip by pressing Z up and when it was very far from the substrate I started the scan. Any way I tried different positions of Z but they all had the same problem
Why don´t you try to test the equipment with a well known system (Pt substrate in KCl solution for instance)? This would be in order to discard problems with the SECM. By the way, What is your subtrate?