It was put in the freezer and it became like this, is it useful or is it damaged?
It was put in the freezer and it became like this, is it useful or is it damaged?
which one?
drained thoroughly.
Pour 30 ml of water into the flask, insert a thermometer into the left throat of the flask, insert a reflux condenser into the central throat, and insert a dropping funnel with 110 ml of 14% P2NP (it is phenylnitropropene; 1-phenyl-2-methyl-2-nitroethylene) solution into the right throat.
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
Maybe the reason that you dried it. Learn this method.
I will change the method and try again. If I manage to find the reason for our problem, I will let you know.Hi,
I`ve got the same problem, except that I have tried at least 6 times. No reaction. If I let it run as long as there is any activity then the Al turns blackish colour and it is greatly reduced in volume, after adding the P2NP/GAC/IPA it `freezes` with some yellow-white precipitate. Warming, even near boiling does not help. If I run the Amalgam until everything floats and most of the bubbling subsides, I get no reaction at all. Now I have a lot of P2NP to recrystallize. Perhaps we are using the wrong foil?
Hello.
I performed the reaction on a smaller scale - 1g of P2NP.
When the aluminium started to break down into smaller pieces(due to stirring), I drained it, then proceeded to add 2ml of cold distilled water. The solution of P2NP was added. Reaction began instantly. No further problems were encountered. The final product came out looking great.
It was put in the freezer and it became like this, is it useful or is it damaged?
In a very small scale it would be possible yes.I have a condenser and a flask like this, is it suitable for this synthesis process?
I think 5g P2NP and 6g Alu foil, 50ml IPA and 25 ml glacial acetic acid are to much for a 250ml Flask, try 500-1000ml, or with a smaller 1g P2NP scale.5gm P2nP Can mode
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
1) Make sure that you use aluminum foil with no other elements in it.Hi,
I`ve got the same problem, except that I have tried at least 6 times. No reaction. If I let it run as long as there is any activity then the Al turns blackish colour and it is greatly reduced in volume, after adding the P2NP/GAC/IPA it `freezes` with some yellow-white precipitate. Warming, even near boiling does not help. If I run the Amalgam until everything floats and most of the bubbling subsides, I get no reaction at all. Now I have a lot of P2NP to recrystallize. Perhaps we are using the wrong foil?
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