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Author: Subject: chloric acid solution becomes yellow ...produces a peculiar noise
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[*] posted on 25-4-2010 at 13:51
chloric acid solution becomes yellow ...produces a peculiar noise


Anyone up to trying this and reporting back?


Preparation of Perchloric Acid
Mon. Scient., XI 961
In:— The Journal of the Society of Chemical Industry
1 [4] 149. 29 April 1882

It is recommended that this acid should be prepared by the user
himself, the cost in this case being 20 to 25 francs per kilo.,
whereas the manufactures demand 90 francs per kilo. It can be
prepared in the following manner without the slightest danger.
[Forsooth!] Pure barium chlorate is dissolved in luke-warm water
and dilute sulphuric acid is added. The precipitate is allowed to
settle, and the clear liquid poured off, and the barium sulphate
thoroughly washed. The chloric acid solution becomes yellow, and
upon further evaporation produces a peculiar noise. The
liquid is divided into two parts, placed in two dishes, 19
centimeters in diameter and containing about 700 cubic
centimeters, and evaporated further until the liquid is quite
decolourised and thick white fumes are given off. In order to
lessen this unavoidable loss of perchloric acid the liquid can be
diluted from time to time with a little water. The colourless liquid
is then distilled in a retort heated on a sand bath and collected in
a long-necked receiver. The perchloric acid so obtained contains
traces of iron. From 4 kilos of barium chlorate, 1 kilo. of perchloric
acid of 45o B. is obtained. The barium chlorate occurs in
commerce, and costs 4 francs the kilo.—M.J.L.

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[*] posted on 25-4-2010 at 14:05


Heh. Pure barium chlorate, huh? The last time I heard, the only supplier left in the US who would sell to individuals required pickup at his location because shipping it was fraught with regulations and a few real hazards.

Even BaCl2 is hard to come by, though BaSO4 is easy and can be calcined to BaO if one is sufficiently extreme. BaClO3 from pharmaceutical sulfate should not be contaminated with iron, which difference might make the reactions not produce the mentioned sound. I believe that Fe+3 and Fe2O3 can be potent catalysts, though their interaction with ClO3 and friends I am utterly ignorant. Perhaps ceramic grade sulfate would be more correct to produce the 1882 item.

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[*] posted on 25-4-2010 at 17:29


Quote: Originally posted by densest  
Heh. Pure barium chlorate, huh? The last time I heard, the only supplier left in the US who would sell to individuals required pickup at his location because shipping it was fraught with regulations and a few real hazards.



This dobe the reason I have not attempted the experiment.
However, in the usual place you can occasionally find people
selling BaClO3 who do not know/care about hazmat shipping.

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[*] posted on 25-4-2010 at 21:45


Ceramics grade BaCO3. Sometimes this contains the sulfide, so do the next steps with good ventilation.

If all you have is tech HCl, dilute it to roughly 18-20 percent, and distill off the constant boiling hydrochloric acid. Use an antispray bulb, short column, or glass wool 'plug' to prevent spray droplets from carrying over iron into the distillate.

Dissolve BaCO3 in hydrochloric acid. Add a bit of HNO3, H2O2, or bubble Cl2 through the solution; in all cases to convert Fe(II) to Fe(III). Heat the solution, slowly add a paste of BaCO3 and DI water with good stirring until there is an obvious excess of the carbonate. Boil the solution for some minutes, Fe and Mn will precipitate out on the excess carbonate as hydroxides, hydrated oxides, or basic carbonates - darkening the white BaCO3 if there is more than a trace of Fe or Mn. Filter off the excess carbonate, test the filtrate for Fe and if tests positive repeat the oxidation/BaCO3/filter addition steps; otherwise crystallise BaCl2 out of the filtrate.

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[*] posted on 29-4-2010 at 10:56


Try calcium chlorate and oxalic acid. Caclium oxalate is around as insoluble as BaSO4.
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[*] posted on 29-4-2010 at 11:02


"produces a peculiar noise"
still wonder what this is xD




Don't stare at me making fumes... I'm just experimenting with some gas...
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[*] posted on 29-4-2010 at 11:09


Nitrogen triiodide crystals caught on the wall of the beaker crack and pop when you swirl the suspension of them. This is caused by the liquid that crashes the crystals against the wall. Probably something similar? I'd try it.
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