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Author: Subject: Sodium Nitroprusside Synthesis
Doped-Al2O3-fusion
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[*] posted on 11-4-2019 at 07:21
Sodium Nitroprusside Synthesis


I performed two attempts at synthesizing sodium nitroprusside recently. My first attempt was mostly failure with a minuscule yield. It was soon lost to acts of frustration during the recrystallizing procedure to purify.

The second attempt I performed a full sized batch according to a procedure I followed from the 1800s or something. These were in my book, horrible inaccurate and vague instructions. So, I split the batch into several equal portions to experiment with modifications to the procedures in the next steps. Two of these separated batches were complete failures, but yesterday I found the forgotten third flask which I had placed off to the side in the dark to avoid light decomposition.

I treated this batch through several filtrations and careful evaporation yesterday and through the night last night. To my excitement I come down to my office finding this. Crystals!!!

This is a huge win for me since I had so many frustrations trying to get a successful run. I'm going through some hard times in my personal life right now, so finding something as simple as a crystallized solution of a substance I've been struggling to successfully synthesize brings a bit of much needed happiness.

I will attempt to recreate the steps I performed in a "How-to" post later on.

Success.JPG - 268kB




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[*] posted on 11-4-2019 at 10:24


I've got the dried crystals. The yield is approximately 30% which is a lot better than my first attempt yield of less than 15%

I'm also noting that the successful batch measures at approximately 8 pH.

dry.JPG - 136kB




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Boffis
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[*] posted on 12-4-2019 at 09:32


Nice looking product there D.A.F.. I look forward to reading your experimental write-up. What do you intend to do with it? It has some really interesting properties because the -NO group is quite laibile and easily replaced by ammonia, amines etc. I think that the nitroprussides are the most interesting of the iron cyanide complexes.
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[*] posted on 3-6-2019 at 16:22


Nice! Would like to see your write up as well.



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Boffis
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[*] posted on 4-6-2019 at 01:58


@ DAF. just out of a matter of interest which method are you using, the nitric acid oxidation of ferrocyanide or the sodium nitrite-barium displacement technique?
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[*] posted on 23-9-2019 at 22:27


Quote: Originally posted by Boffis  
Nice looking product there D.A.F.. I look forward to reading your experimental write-up. What do you intend to do with it? It has some really interesting properties because the -NO group is quite laibile and easily replaced by ammonia, amines etc. I think that the nitroprussides are the most interesting of the iron cyanide complexes.


It's been a while since I last checked this thread out.--sorry for the delay.

I really don't know what I'll ever do with the sodium nitroprusside other than admire what little I have stored away at the moment. I know it won't hang around forever and honestly, I should check on it to see how it's holding up. I plan on revisiting this experiment sometime again in the future and I will definitely write up a detailed summary. I want to have a better yield and I'm hoping that will happen on the next attempt.

I'll get the last set of notes I made and post them if it will be too much longer.--says me many months later...

I used the the nitric acid oxidation of ferrocyanide technique both times.

[Edited on 24-9-2019 by Doped-Al2O3-fusion]




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