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Author: Subject: Violuric acid salts (fantastic colors and variety)
vano
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[*] posted on 8-2-2021 at 15:12


Thank you



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Housane
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[*] posted on 9-2-2021 at 03:36


Ok thanks, where did you find your nitrite? As it is a explosives precursor here



Green QD's so far

Feel free to correct grammar or incorect knknowledge. We are all learning.
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RustyShackleford
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[*] posted on 9-2-2021 at 03:53


Quote: Originally posted by Housane  
Ok thanks, where did you find your nitrite? As it is a explosives precursor here

i purchased a pound of it from ebay in 2019, it was from britain so idk if youre correct, or maybe the laws have changed since then for nitrite
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artemov
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[*] posted on 10-2-2021 at 02:07


Quote: Originally posted by RustyShackleford  
if you want another route you can go from diethylmalonate via sodium metal and hydroxylamine.


Can you elaborate more on this, or can you point me to a resource or something? I have malonic acid and hydroxylamine hcl ...
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artemov
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[*] posted on 10-2-2021 at 02:09


Quote: Originally posted by Housane  
What amazing colours, I want to try and make sum but I can't find any sodium nitrite over here as it is a restricted chemical, could it be substuted for any easier to obtain chemicals here in the UK?


Do you have access to poppers? It's an alkyl nitrite, but I'm not sure how pure are commercial poppers.

[Edited on 10-2-2021 by artemov]
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h0lx
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[*] posted on 28-2-2021 at 00:50


Pyridinium violurate. Strangely in solution it's much like permanganate but the crystals are orange
https://imgur.com/gallery/xrDb5el
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Tsjerk
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[*] posted on 28-2-2021 at 02:29


Nice!

Can you embed the photos in your post? Otherwise the are lost when the link breaks.
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Amos
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[*] posted on 28-2-2021 at 09:22


I don't believe I've seen anyone post an aniline salt yet, that would be neat. Piperidine too if anyone has it.

Thanks a bunch for bringing this to everyone's attention, Mr. Gribble
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Boffis
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[*] posted on 28-2-2021 at 09:51


Aniline may not be a strong enough base but piperidine should form a salt
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RustyShackleford
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[*] posted on 28-2-2021 at 11:46


Quote: Originally posted by Amos  
I don't believe I've seen anyone post an aniline salt yet, that would be neat. Piperidine too if anyone has it.

Thanks a bunch for bringing this to everyone's attention, Mr. Gribble

I did make the aniline salt but it was kinda ugly, possibly due to decomposition impurity in the aniline. Its on page 2 of this thread.
As for piperidine, i do have some 200mg of the HCl salt, but the freebase smells so horrible (like rotten cum) i dont want to do it. Perhaps when ive built a fumehood.
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Bezaleel
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[*] posted on 6-3-2021 at 17:06


I received some violuric acid from RustyShackleford yesterday in order to test what colours its rare earth salts have - thanks!. It's already after midnight now, but I could not resists the temptation to do one test.

Violuric acid is sparingly soluble in cold water, but much better in hot water. I noticed a somewhat sweetish smell coming off the warm solution (~60C).

0.291g of violuric acid was dissolved in ~15ml warm water, giving a clear purple solution (the dry salt is off white). This was added to a solution of 0.229g EuCl3.6H2O in a few ml water, yielding an orange solution!

IMG_3529_adj.jpg - 286kB

The solution is evaporating in a desiccator over NaOH. I'm charging up my UV lamp batteries to see whether the solution still fluoresces. EuCl3 solution (as well as the solid compound) fluoresces with a reddish colour.
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RustyShackleford
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[*] posted on 7-3-2021 at 09:58


Remade the aniline violurate with distilled clean amine, its a very dark red.
Anthranilic acid violurate is a light orange.
Im planning to make some substituted anilines and try with those (N- acetyl, N-benzyl, N-benzylglycine)

IMG_20210307_185022.jpg - 1.1MB

Side note: i have noticed that the color of the salts seem to "develop" over time. Like for example the Ni salt i made is now a more consistent and nicer shade of green than it was when i initially made it. No good idea of what the cause is.

IMG_20210307_191532.jpg - 363kB

[Edited on 7-3-2021 by RustyShackleford]
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Bezaleel
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[*] posted on 12-3-2021 at 14:38


Adding violuric acid to solutions of rare earth chlorides proved not a good idea. I had hoped to evaporate the HCl in solution over NaOH in a desiccator and obtain the rare earth violurates, but this did not happen. Instead, the Eu-violurate shown in my 7 March post lost its colour and a creme coloured solid was obtained.

So I continued to combine carbonates and hydroxides with violuric acid instead of chlorides. Sm2(CO3)3 gave a deep red solution which on drying gave red-brown granular crystals. I assumed the carbonate to be a 2.5 hydrate as posted here (bottom of page 8), but seeing I have some Sm-carbonate coloured residue, my carbonate may just have been dry.

Pr(OH)3 also gave a deep red solution. Pr(OH)3 was added in excess and intensely stirred for 15 minutes on a 70C hotplate. The solution was then filtered using a fine fritte. It's is now drying in a desiccator over NaOH.

Li2CO3 gave a strongly permanganate coloured solution, which on drying gives an intense almost fluorescent pink solid.

IMG_3562.JPG - 414kB IMG_3578.JPG - 329kB IMG_3555.JPG - 332kB

Edit: fixed link

[Edited on 12-3-2021 by Bezaleel]
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RustyShackleford
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[*] posted on 12-3-2021 at 14:54


@Bezaleel
Wow that lithium salt looks amazing!
I have also noticed that its not really possible to make the violurate from strong acid salts of the metal, unless the metal violurate is quite insoluble. The technique i have been using for almost all of the salts i made is to make the carbonate or hydroxide of the metal, adding water + stoiciometric violuric acid, and evaporating that with the hotplate on 120C in a 50ml beaker. For ~0.2g violuric + corresponding metal carbonate/hydroxide ive been using 10-15ml of water. If you get a crummy looking product i have found that washing the salt w some acetone helps.
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Bezaleel
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[*] posted on 12-3-2021 at 15:30


So we ended up using the same method, apart from the use of a desiccator vs. a hotplate to evaporate the solution. I was not sure whether the violurate would stand temperatures over 100C, so I chose low pressure over temperature.

It seems like all the rare earths form red-brown compounds, so it may be more interesting to make a few non-rare earth ones instead. I can choose from indium, bismuth, antimony, vanadyl, maybe uranyl, rhenium, chromium, molybdenum, tungsten, and diethylamine. Of molybdenum, tungsten, and rhenium I don't expect much, but you never know, of course. (Other rare earth choices would be erbium, dysprosium, neodymium, holmium, lanthanum (~95%), and gadolinium.)

Please let me know your preferences.

Doe anyone know whether cyanuric acid could be used to make violuric acid from in a home lab?
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[*] posted on 12-3-2021 at 16:04


Vacuum is better, i just dont have a pump good enough for that.
I would like to see all of those done, but if i had to pick a few i think uranyl>rhenium>indium.
A full rare earth series would be very cool, but ofc thats a lot of work.
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[*] posted on 16-3-2021 at 11:27


Updates

Samarium
I redissolved the Sm violurate and filtered off the undissolved carbonate, obtaining a warm clear solution. As it cooled down, a beige film formed on the flask. The solution was poured off and dried in a desiccator over NaOH, forming a deep red solid.

IMG_3616.JPG - 324kB IMG_3629.JPG - 420kB

Praseodymium
A new sample was made using Pr(OH)3. The hydroxide was stirred powerfully with demiwater, filtered again and then used. 0.300g of violuric acid was added to an excess of Pr(OH)3 and the undissolved hydroxide filtered off. When left to crystallise over NaOH, an orange-yellow film formed on the walls of the beaker and after everything had dried up completely, a mix of dark red and yellow-orange crystals had formed. As far as possible, the dark crystals were separated and the rest was redissolved - the yellow crystals did not dissolve on heating, but the red ones did. The solution is now crystallising again.

IMG_3608.JPG - 354kB IMG_3631.JPG - 382kB IMG_3646.JPG - 366kB

A comparison between the Sm and Pr salts is in the last picture. It looks like the colour of the compounds is mainly caused by interactions inside the violuric acid ligand and not so much by the metal-ligand interactions. In particular the weak green of the Pr forbidden transitions seems to be retained, and causes a minor difference in colour of the salt as compared to Sm.

IMG_3643_adj2.JPG - 312kB

Indium
0.096g of indium were dissolved in 10% HCl. This took a long time, although the acid was heated to near boiling. The indium was precipitated with ammonia solution and the supernatant liquid pipetted off 3 times. 300mg of violuric acid were added. The solution turned purple immediately, which suggests that not all of the ammonium had been removed, although the pH of the solution with the In(OH)3 was 8.
On heating hardly any of the precipitate dissolved. The beaker was covered with cling film and put on a stirrer at 1200 rpm and heated at 70C plate temperature and stirred for 1 hour. Still much In(OH)3 remained undissolved, but the mix had obtained a colour resembling molybdenum blue.

IMG_3603_adj_detail.JPG - 163kB IMG_3623.JPG - 283kB IMG_3626_adj.JPG - 277kB

It seems that indium is chemically too basic to easily form a salt with violuric acid. My estimate is that this will count all the more for Re, Mo and W. I decided that I will not make the uranyl salt, because of the precautions necessary to safely work with it. I consider cerium, which is interesting because it is a coloured RE and also has a stable +IV oxidation state, and aluminium.
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DraconicAcid
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[*] posted on 16-3-2021 at 12:32


So violuric acid is made from barbituic acid....I wonder if something similar could be made from Meldrum's acid (which seems easier to make than barbituic).
https://en.wikipedia.org/wiki/Meldrum%27s_acid




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[*] posted on 16-3-2021 at 19:01


Quote: Originally posted by DraconicAcid  
So violuric acid is made from barbituic acid....I wonder if something similar could be made from Meldrum's acid (which seems easier to make than barbituic).
https://en.wikipedia.org/wiki/Meldrum%27s_acid
I think it should be possible! Meldrum’s acid is a very nice compound. I’ve worked with it a couple of times and it loves to undergo those sort of reactions. Without the nitrogens though, it may not have the same interesting coordination properties. It’s also not the most stable thing since it’s a geminal bis-lactone. Still, definitely worth a try.



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RustyShackleford
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[*] posted on 17-3-2021 at 06:44


Shame that the indium didnt form a solid, the solution looks real nice though. Also im quite suprised the Sm and Pr are so similar in color, from all the other salts i woulve expected a bigger differece. They both look quite nice though, thank you for taking the time to produce the salts and post pictures!
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[*] posted on 17-3-2021 at 10:55


I follow this thread with much interest. Sadly up to now I did not manage to find any precursors to make violuric acid in Australia. And local prices I was quoted for violuric acid is astronomical.
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[*] posted on 17-3-2021 at 12:48


Depending on what other basic chemicals you have access to (ie nitric acid) you can prepare violuric acid from bird shit!

Guano -> uric acid -> alloxan -> alloxan-5-oxime (violuric acid)

The first step is the most difficult and complex because of the need to filter intensely alkaline solutions that result from the extraction of guano with caustic soda
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[*] posted on 27-3-2021 at 03:55


Hi. RustyShackleford gave me violuric acid and will make some violurates. Today i made scandium violurate, i used scandium carbonate. Nice yellow- brown colour.

received_912623242885571.jpeg - 176kB
received_247565420429893.jpeg - 123kB




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[*] posted on 27-3-2021 at 04:40


Quote: Originally posted by vano  
Hi. RustyShackleford gave me violuric acid and will make some violurates. Today i made scandium violurate, i used scandium carbonate. Nice yellow- brown colour.

Very nice! Thats the first yellow violurate salt i believe
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[*] posted on 27-3-2021 at 04:50


Thanks. This is indium violurate. Brown- dark red colour. I used indium carbonate. Carbonates are better.


PicsArt_03-27-04.48.31.jpg - 237kB

[Edited on 27-3-2021 by vano]




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