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Author: Subject: Gallium and mercury acetate from Peracid+element in GAA
TheVoid
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[*] posted on 9-5-2018 at 19:49
Gallium and mercury acetate from Peracid+element in GAA


I'm planning on trying the below procedure But i also wanted to try it using gallium could anyone tell me if it should work for gallium acetate.

I have experience handling these metal salts and have worked with peracids before

https://patents.google.com/patent/US2661360

Example I A peracetic acid solution was prepared by reacting 90% hydrogen peroxide with glacial acetic acid, the two reactants being used in a mole ratio of 1: 1.5 in the manner described by Greenspan in J. Am. Chem. Soc. 68, 907, using nitric acid as catalyst instead of the sulfuric acid catalyst described in that paper. The nitric acid was employed in an amount corresponding to 1% of total volume of reactants. The resulting peracetic acid 40% solution was then used in the preparation of mercuric acetate as follows.

In an all-glass apparatus consisting of a twoneck flask equipped with reflux condenser, to prevent evaporation losses, and stirrer were placed 24 g. of metallic mercury to which were added 48 ml. of glacial acetic acid. The mercury was slurried up in the acid by means of the stirrer and then there was added in one batch 18.8 g. of the above described peracetic acid solution, this amount corresponding to a 10% ex cess, calculated on a total active oxygen basis, over the stoichiometric amount required. Agitation of the reaction mixture was continued for approximately 12 hours at room temperature, after which time a copious amount of insoluble mercurous acetate had formed.

The flask with its contents was then heated on a waterbath until the precipitated, insoluble mercurous acetate was dissolved by transformation into soluble mercuric acetate. There was no trace of metallic mercury or other insoluble residue. The solution was then cooled to precipitate the mercuric acetate, which was recovered by filtering off the liquid phase.

The product analyzed 61.7% Hg. It was readily soluble in water. Total weight of mercuric acetate recovered was 37.8 g., indicating a practically theoretical yield.

Example II In another test preparation of mercuric acetate was carried out exactly as described in Example I, but very vigorous stirring was provided for by using a high efiiciency stirrer. Agitation of the reaction mixture was continued for 2 hours at room temperature. The flask with its contents was then brought to reflux temperature. After 15 minutes of refluxing, the precipitated, insoluble mercurous acetate had been completely dissolved by transformation into the soluble mercuric acetate. There was no trace of metallic mercury or other insoluble residue. The solution was then cooled to precipitate the mercuric acetate, which was recovered by filtering off the liquid phase.

The product obtained analyzed 61.4% Hg. It was readily soluble in water. Total weight of mercuric acetate recovered was 37.6 g., indicating a practically theoretical yield.

[Edited on 10-5-2018 by TheVoid]
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ninhydric1
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[*] posted on 9-5-2018 at 21:06


What are you planning to use these acetates for?



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TheVoid
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[*] posted on 9-5-2018 at 21:52


Quote: Originally posted by ninhydric1  
What are you planning to use these acetates for?


I have an amount of both elements on hand that i would like to consume in a fashion that might later be useful.

I also wanted to try an Al amalgam using gallium, and will probably run a mercury amalgam for comparison.

I don't see why it shouldn't work for gallium i was just wondering if anyone has a reason.
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ninhydric1
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[*] posted on 10-5-2018 at 07:14


It could be that the reaction is exceedingly slow with gallium. Gallium requires strong acids such as sulfuric and nitric acid to be dissolved, albeit slowly. Have you tried heating the gallium,/peracetic acid mixture for a few days?



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[*] posted on 10-5-2018 at 20:09


Quote: Originally posted by ninhydric1  
Have you tried heating the gallium,/peracetic acid mixture for a few days?


sorry I haven't actually tried to run the reaction yet i am still planning, that is a good idea though. I have a friend who specializes in this type of chemistry i will have to ask them.
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