Why is the cyclic voltammetry of my ferrocene compound not showing a standard shape? I am trying to set-up a new cyclic voltammetry measurement station in my lab but the results are very poor. I am using the following parameters:

working electrode: platinum wire, 0.25mm diameter
counter electrode: platinum wire, 0.25mm diameter
reference electrode: none
solvent: acetonitrile
electrolyte: ferrocenecarboxaldehyde
support electrolyte: tetrabutylammonium hexafluorophosphate
scan rate: ~600mV/s


Platinum wires each have a submerged length of about 2mm to 5mm and are separated by about 2cm. I was previously using tetrabutylammonium iodide, but that is probably not a good support because the iodide ions will become iodine and forming a blocking layer on my electrode?

I also tried using graphite rods as the electrodes but obtained similar poor-looking CV shapes.



What should I change to obtain the standard CV shape of an outer-sphere redox species?
Without a proper reference electrode, knowing what potential your ferrocene/ferrocenium couple will show up is quite impossible. You should sweep a larger potential window, until the solvent breakdown potential on either end. 

As Michael Dryden suggested, you should sweep slower as well. That will help with the signal getting resolved easier.