Hello.
I have a problem with this reaction. I tried performing it twice. I am using lab grade reagents and lab glassware. I scaled down the reagents proportionally, because I use a 1l flask. The issue appears when i try to reduce the P2NP using aluminium amalgam.
I prepare the solution of P2NP, heating it just enought to dissolve the crystals.
I use a coffee grinder to grind the aluminium into little globs - as written in the
Aluminium amalgam (Al/Hg) summary.
After adding HgCl2, I pour in 0,5l of cold distilled water. 10 minutes later the reaction begins.
The first time I waited until no more small bubbles were forming and all of the aluminium was floating, the water - cloudy gray. I rinsed it twice with little cold distilled water, drained thoroughly. I added the P2NP solution, no reaction took place. I noticed the P2NP partly crystallized. I tried starting the reaction with heat, but to no avail.
The second time I drained the water from the amalgam when lots of small bubbles appeared and most of the aluminium had surfaced, the water was cloudy gray. Once again - I rinsed it twice with little cold distilled water, drained thoroughly. After the addition of P2NP the result was identical as the first attempt. Heating the mixture did not help.
What am I doing wrong? What should I change? Do you have any suggestions?
Any help will be greatly appreciated