vano
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Ozone. Very easy
1)Barium peroxide synthesis. Precipitation from aqueous solutions of salts with concentrated hydrogen peroxide in an alkaline medium. With water forms
crystalline hydrates BaO2 • 8H2O and BaO2 • H2O.
BaCl2 + H2O2 + 2NH4•H2O + 6H2O = BaO2 • 8H2O + 2NH4Cl
2)Reacts with concentrated sulfuric acid to form barium sulfate , ozone and water :
3BaO2 + 3H2SO4(conc.) = 3H2O + 3BaSO4 + O3
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unionised
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What is the yield like?
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vano
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I do not have that information. Where I saw it was not written. I want to make Diiodosyl sulfate, so it's convenient for me.
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RustyShackleford
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https://sites.google.com/site/unusualchemistry/ozone
Seems to only form ca 2% concentration of ozone in the gas that evolves, kinda crap IMO.
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symboom
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there may be chemical ozone production methods that produce a higher amount of ozone
"Another method of generating ozone is decomposition of various highly oxidized or peroxide compounds in acidic solution. An example is decomposition
of barium peroxide in sulfuric acid. Alternately, you can use potassium permanganate and mid-strength (50-80%) sulfuric acid. The resulting
permanganic acid decomposes, liberating ozone."
Source http://www.sciencemadness.org/smwiki/index.php/Ozone
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RustyShackleford
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From the research ive done this evening i dont see it as viable at all to produce chemically. I found one reference stating the maximum amount of
ozone they were able to get from 20g of BaO2 was 14mg. Seems faaaar better to run even the worst chinese generator you can get.
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vano
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I will get it from potassium Permanganate. I have a lot of both compounds. Anyone know What is the yield like?
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Sulaiman
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I have been mixing KMnO4 and H2SO4 a few times recently,
and I rarely smell ozone,
so I'm fairly sure the yield is very low.
(I used to 'play' with high voltages a lot and I easily recognise the smell)
CAUTION : Hobby Chemist, not Professional or even Amateur
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vano
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I too think it is not a good idea. Using many substances to make diiodosyl sulfate would be necessary and foolish.
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symboom
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Found this gem of a video electrolysis of sulfuric acid to for ozone
https://youtu.be/Jrd_qQWl8b0
Also here is some interesting information on the SOLUBILITY of ozone.
Ozone is a colourless or pale blue gas, slightly soluble in water and much more soluble in inert non-polar solvents such as carbon tetrachloride or
fluorocarbons (makes me think of fluoroethane refrigerant) in which it forms a blue solution.
[Edited on 5-1-2021 by symboom]
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vano
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Thank you symboom. I want to make such a big ones. How do you think I should replace carbon. Because I do not have a long electrode. And to increase
the voltage? Up to 20 volts. Because I will have to use a laptop charger. What do you think?
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teodor
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@vano In the old soviet children book "занимательные опыты по химии, Алексинский" there is a method K2S2O8 or
(NH4)2S2O8 + H2SO4 or HNO3 (conc). which produces enough O3 in a beaker (from 2-3 "pinches" of the salt) to bleach a textile.
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vano
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Thank you teodor. I know this reaction, but I did not think it would release enough ozone. Now I have thought and I would rather build a hight voltage
ozone generator and have it permanently than use substances constantly. I really want the above sulfate. It is a very rare and beautiful compound.
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Bedlasky
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Vano: If you want to make iodosyl sulfate, you don't need ozone. Just HIO3 and conc. H2SO4 (HIO3 can be make from I2, HNO3 and H2O2 or from BaIO3 and
H2SO4). Look at page 332:
http://library.sciencemadness.org/library/books/brauer_ocr.p...
HIO3 preparation is on page 316.
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woelen
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If you have I2O5, then things are simple. Add I2, I2O5 and concentrated H2SO4 to each other and gently heat. I2O5 can be made from HIO3 by carefully
heating it. It splits off H2O. Do not overheat, because then it decomposes to I2 and O2.
@Bedlasky: Does Mixing H2SO4 with HIO3 really give iodosyl sulfate? In the latter compound, iodine is in oxidation state +3, while in HIO3 it is in
oxidation state +5. I have an old book on halogen chemistry, which mentions the iodosyl cation, which can be made from I2 and I2O5 and H2SO4. The I2O5
then oxidizes the I2 and you get "I2O3", which with the acid gives rise to formation of IO(+) and H2O, which is bound by excess H2SO4. Things work
even better if the acid contains some SO3. This only works when the acid is so strong that IO(+) is formed. I write "I2O3" between quotation marks,
because this compound does not really exist, and the redox reaction between I2O5 and I2 only proceeds if the iodine(III) is bound and taken away from
the reaction.
I'll try this reaction myself. I have I2O5 and I2. I'll give it a shot.
[Edited on 5-1-21 by woelen]
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Bedlasky
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Woelen: I never tried this, but I want to. Look in that book, there is description. During heating HIO3 decompose and O2 is released. I also have an
idea to use H[ICl4] instead of HIO3 - iodine is already in III oxidation state in this compound and HCl escape from solution, so this reaction don't
need strong heating. Your suggestion is better than using just HIO3 - I think that this reaction need lower temperature than decomposing HIO3.
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vano
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Thank you to everyone. Good book Bedlasky. @Woelen can you give me this old book about halogens?
Nitric acid often contaminates the product. Also diiodosyl sulfate forms yellow hygroscopic crystals. It dissolves and can be recrystallized in
concentrated sulfuric acid. I have never had contact with iodic acid. So how can it be separated from the solution in solid form? Plus the temperature
is noticeable. In short I will buy iodine tomorrow and try it. I will read the theoretical sources, but I would prefer someone to share his
experience with this particular reaction.
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woelen
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The book is not in digital form, I have the actual old book in paper form, so giving it is not possible. I however, can lookup the info on iodosyl and
give it here.
@Bedlasky: I'll have a look into the book you linked to. As I wrote, I can try this reaction. I even have some oleum (80 ml or so of 65% SO3 plus a
little quantity of 20% SO3), so if it does not work with H2SO4, I can try with a mix of H2SO4 and oleum on a small scale. I also have 'poor man's
oleum', which in some experiments shows reactions similar to true oleum (' poor man's oleum' is chlorosulfonic acid, SO2(OH)Cl, and is easier to
obtain than real oleum and MUCH cheaper).
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Bedlasky
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Vano: HIO3 preparation is described in Brauer, look on page 317.
Woelen: Chlorosulfonic acid is cheaper than oleum? I think that oleum is cheaper. When I saw price for chlorosulfonic acid, I thought that was insane.
I don't want to see price for oleum.
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Sulaiman
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As most sulphuric acid is made by the contact process,
at industrial scale, oleum should be not much different in cost to sulphuric acid (diluted oleum).
CAUTION : Hobby Chemist, not Professional or even Amateur
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woelen
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Chlorosulfonic acid is appr. 125 euros for me per 500 ml. I can buy that without issues.
Oleum 65% is appr. 600 euros for me per liter. The small quantity I have was a one-time purchase from a non-official source 
I also have 70 grams of pure SO3 for a very good price (I paid only 60 euros for it). Normally you would have to pay 250 euros per 100 gram or so.
[Edited on 20-10-21 by woelen]
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vano
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The life of a chemist in the Netherlands has been difficult. The compounds are very expensive. I will buy about 250-300 different substances for the
price of one liter of oleum. It 's just unbelievable. I wonder why it is so expensive. Is there a reason?
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woelen
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All chemicals are expensive where I live. Safety regulations, storage, transport regulations, handling and overseeing by all kinds of experts, they
all add up to the price. Industrial amounts still are cheap, but before you have a small quantity in your hands, prices have gone up by a factor of 10
to 100.
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vano
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I want to build a generator. To get sulfur trioxide from dioxide, with iron oxide catalyst and atmospheric oxygen, but I do not know how good the
catalyst is compared to platinum, vanadium oxide or sodium metavanadate.
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Bedlasky
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65% oleum is quite concentrated. What about 20%? This will be cheaper I suppose.
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