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Author: Subject: Silver nitrate without NOx
BJ68
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[*] posted on 1-5-2018 at 23:53
Silver nitrate without NOx


50 g of metallic silver is added to 200 ml of 10.39% (m/v) nitric acid. The mixture is heated up (short before boiling) and 50% hydrogen peroxide (17 ml) is added over a 6-8 h period with a syringe pump.
After this time the mixture is cooled to RT and evaporated to get raw silver nitrate, which is melted to get pieces.
The pH goes up to 4, that means more or less the complete nitric acid is consumed and there is no liberation of NOx.

Literature: https://patentimages.storage.googleapis.com/pdfs/65897df1e37...


Results:

Left over Ag: 13.72 g

36.28 g Ag consumed, that equals 0.336 mol.

Theoretical yield (calculated from used silver): 57.13 g

Amount silver nitrate: 49.74 g which is 87.06 % of theory.

Reason for losses:

a) I got tiny silver nitrate particles, where I boiled down the soulution
b) At the first boil down trial (with out pictures): I used an oven @70°C and the silver nitrate crystals crawled up the porcelain dish, even outside. So I had to wash this dish and make a second try, now with smaller amounts.

Source (in German) with a few other trials:
http://illumina-chemie.de/silbernitrat-nach-ep0568259a1-t471...

Advantages: Diluted nitric acid can be used and no nitrogen oxides are liberated, so there is no fume hood necessary.

Pictures:

Silver metal:
Silber.jpg - 272kB

The reaction:
Reaktion.jpg - 39kB

Consumed hydrogen peroxide:
Wasserstoffperoxid.jpg - 34kB

End of reaction:
Ende-Reaktion.jpg - 41kB

Decay (Abklingen):
Abklingen.jpg - 48kB

pH-Measurement:
pH-Wert.jpg - 51kB

Rest of silver:
Auswaage.jpg - 47kB

Drying:
Trocken.jpg - 47kB

Melting:
Schmelzen.jpg - 52kB
Schmelzen-1.jpg - 47kB

Result:
Ergebnis.jpg - 43kB

Bj68
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VSEPR_VOID
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[*] posted on 2-5-2018 at 00:55


You should put this in the publication board. Good job.



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BJ68
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[*] posted on 2-5-2018 at 01:13


Quote: Originally posted by VSEPR_VOID  
You should put this in the publication board. Good job.



Okay, have overseen it....should I make a new topic or can a Admin move it?


Bj68
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woelen
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2-5-2018 at 01:22
BJ68
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[*] posted on 5-5-2018 at 10:08


Addition:

If somebody wants to play with different concentrations and parts "nitric acid"/"hydrogen peroxide":
Please read this:
http://hydrogen-peroxide.us/chemical-catalyst-decomposition/...
and be careful....

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[*] posted on 3-1-2019 at 12:40


i thought the pH measurement strip was a cigarette xd
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[*] posted on 25-3-2019 at 10:40


I think that it would have been better to use excess acid+peroxide as your silver nitrate looks to me to be quite impure - probably due to metallic siver
re-crystalisation will of course give purer silver nitrate
but it is best to start as pure as practical.




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[*] posted on 13-8-2019 at 00:12


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