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Author: Subject: Violuric acid salts (fantastic colors and variety)
vano
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[*] posted on 2-4-2021 at 01:43


Hi. These photos are better. Last one is new (cadmium violurate). Unfortunately the indium violurate powder was spilled. I have so little right now that it is nonsense to stuff it in a vial.

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Diachrynic
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[*] posted on 2-4-2021 at 04:22


Amazing work vano!

Haven't seen lead mentioned, so here is some. Made from about 0.11 g of the sodium salt (dihydrate) and about 0.17 g of lead acetate trihydrate, from mixing the two as solutions (added lead to the violurate). Instant precipitate from the warm solution, but no complete discoloration. Filtered, washing water was colorless. A portion was dried at about 180 °C on a hotplate.

Left is the tetra/pentahydrate (still a bit wet), right anhydrous
lead_violurate_tetra_or_pentahydrate.jpg - 2.3MB lead_violurate_anhydrous.jpg - 2.2MB

Didn't find much information, and some conflicting on the hydration. Can't access the original source so I'll attach the scifinder screenshots.

Screenshot 2021-04-02 095035.png - 66kB Screenshot 2021-04-02 095215.png - 71kB




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[*] posted on 2-4-2021 at 06:01


Thanks Diachrynic. Nice work.



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Diachrynic
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[*] posted on 2-4-2021 at 11:45


Yttrium is generally not very interesting, but it's violurate is brightly yellow.

I dissolved about 0.5-0.7 g of violuric acid monohydrate (mine was freshly made and still wet so I don't know exactly, it's an excess of over 3:1 to the yttrium used however) in 50 mL of boiling 95% ethanol - had some insoluble grey-brown stuff so I filtered that off. To that solution was added about 0.25 g of YCl3 (it should be noted that YCl3 is very hygroscopic and mine was slightly wet so this amount is also lower than I measured out here) in about 1 mL of water to the boiling ethanol solution while stirring. It turned yellow and after about a minute of strong stirring and boiling the solution became turbid, it was boiled for five minutes longer and left to cool until luke warm. The yellow precipitate was vacuum filtered off and washed with some 95% ethanol. The solution that passes through is slightly yellow and deposits only small amounts of additional precipitate with more yttrium chloride solution. The solid was then air dried. Yield was about 0.166 g. (Because this was all done a bit sloppy I didn't bother to calculate a % yield.)

[YVio2(H2O)2]Vio+6H2O.jpg - 2MB

The product is of the composition [Y(Vio)2(H2O)2]Vio · 6 H2O where HVio is violuric acid.

The preparation comes from Gad, A. A. M., Farag, I. S. A., & Awadallah, R. M. (1992). Synthesis and Characterisation of Scandium (III)-, Yttrium (III)-, and Lanthanum (III) Violurate Complexes. Crystal Research and Technology, 27(2), 201–210. doi:10.1002/crat.2170270210

Attachment: gad1992.pdf (421kB)
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[Edited on 2-4-2021 by Diachrynic]




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[*] posted on 2-4-2021 at 12:13


Nice. Now there are two yellow violurates Sc and Y. Where did you buy yttrium chloride?



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Diachrynic
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[*] posted on 2-4-2021 at 12:40


Quote: Originally posted by vano  
Where did you buy yttrium chloride?

I happened to get about 6 kg (it was one big solid brick) of it when it was supposed be disposed of, so I saved it from being just thrown out, I don't actually know where to buy it.

[Edited on 2-4-2021 by Diachrynic]




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[*] posted on 3-4-2021 at 00:52


6 kg is too much, good source. I too have bought solid brick chemicals very cheaply.



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Diachrynic
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[*] posted on 3-4-2021 at 13:25


I found no literature on bismuth violurate, so here is a small test tube scale experiment. It seems fairly soluble.

Some bismuth nitrate pentahydrate was dissolved in some water with some sulfuric acid (bismuth hydrolyses to basic salts with annoying ease...), to this some sodium violurate solution was added. The color turned orange. When acetic acid and sodium acetate were added, the color became purple. Whether this is because the sodium is competing with the bismuth or something else, I am not sure, the color is somewhat different from pure sodium violurate however, which is more purple. If anyone wants to prepare the solid, I would suggest using a bismuth oxide/hydroxide and the free acid since I didn't get precipitation.

IMG_20210403_112718.jpg - 2.3MB IMG_20210403_112934_1.jpg - 2MB




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[*] posted on 17-4-2021 at 16:48


ortho-toluidine violurate, this one I did as a proof of concept in a very small unmeasured scale, I will now make more to vial up.

o-toluidinevio.jpg - 1.3MB
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