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Herr Haber
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See my signature ? Look for the whole text, it's a 2 minutes gem and very related to what I read here 
The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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ManyInterests
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Yes. I remember that right now. So no, there was no reaction, because it was not nitric acid.
I will continue to attempt to make ammonium nitrate, I hope that adding an excess of 6% ammonia solution (it is ammonia and water, nothing else) and
see if I can turn calcium-ammonium nitrate into ammonium nitrate.
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Rainwater
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You can bubble ammonia gas through dilute nitric acid.
An ice bath would be needed. And the acid.
"You can't do that" - challenge accepted
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Quote: Originally posted by ManyInterests  |
Thanks for your concern about it. But what was the brand you used? I have a link in my opening comment to show what brand I was trying to work with.
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No, sorry, the cold packs had been emptied to a suitable large container ages ago, so I don't have the brand. But I'm still not sure they're not at
least partially ammonium nitrate, I just think there might be urea in there. Enough to screw up my attempts to make tannerite from them.
So what I needed was a way to ascertain if there were contamination. I guess you could use the same method to find out if yours are urea too.
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ManyInterests
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OK, so I decided to do one thing. I did realize that I did want to make sodium nitrate as well. So I got a lot of (proven) cold packs that I can turn
into sodium nitrate with the addition of sodium bicarbonate into the CAN mixture. However before opening those, I decided to give those (alleged)
ammonium nitrate cold packs one last chance to redeem themselves. I followed Canadian Chemist's instructions on the process and added an excess of
water (to make sure everything is dissolved) and added the required amount of baking soda... upon adding the baking soda, the solution did fizz. Not
as vigorously as in the video, but that could be because the solution was more dilute as I added more water.
After mixing quite strongly by hand. I did smell the faint smell of ammonia coming out, which means a reaction is happening. I then put it on my
heating mantle and boiled off most of the water (until no more ammonia was produced) and stirred occasionally. Now I put the leftover slush in my
glass lasagana pan and am drying it in the oven. AS I smelt no ammonia I do believe there is no danger of poisonous gasses.
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arkoma
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Slightly off topic, but DEF fluid is distilled water and urea. A lot of urea, that crystalizes beautifly when you dry out the solution. As every
modern diesel truck requires DEF, it's OTC everywhere and fairly inexpensive.
Edit--BEAUTIFULLY, d'oh!!
[Edited on 6-26-2022 by arkoma]
"We believe the knowledge and cultural heritage of mankind should be accessible to all people around the world, regardless of their wealth, social
status, nationality, citizenship, etc" z-lib
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ManyInterests
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What is DEF fluid?
At any rate, my experiment was a success! I got me some sodium nitrate! 170 grams of it from 190 grams starting! I'll be making more of these.
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| Quote: Originally posted by ManyInterests | What is DEF fluid?
At any rate, my experiment was a success! I got me some sodium nitrate! 170 grams of it from 190 grams starting! I'll be making more of these.
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He just told you? It's called AdBlue in many countries. You buy it at the gas station. It's urea in water. You put it in cars with Diesel engines.
To continue this OT theme: urea is also available as Intensive Care Foot Baths. Pure, fine urea.
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ManyInterests
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Urea is good. But they have urea cold packs cheaply available as well where I live. I just purified 400 grams of urea a while ago.
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Rainwater
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| Quote: Originally posted by ManyInterests | | Urea is good. But they have urea cold packs cheaply available as well where I live. I just purified 400 grams of urea a while ago.
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Def fluid comes in 2.5 gallon containers. About $25 here.
32.5% urea. Yielding about 3 kilos when dried.
"You can't do that" - challenge accepted
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And if it's sodium nitrate you want, and you're in Europe, there's always https://www.pyrogarage.pl/en/category/chemicals/oxidizers/
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ManyInterests
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Except I live in Canada. Nitrates are a bit more restricted here. Ditto for chlorates. If I could buy the chlorates and perchlorates and nitrates and
all that stuff off the shelf I would do it. But as it stands I need to make them myself.
Calcium-ammonium nitrate cold packs are commonly available where I live. They're my only source of nitrates. I made a lot of potassium nitrate and
looks like I'll be making sodium nitrate for good measure.
I will have an abundance of nitric acid which will allow me to make ammonium nitrate for whatever I need my adding ammonia solution to it and making
very pure ammonium nitrate crystals.
The sodium nitrate synthesis did prove that the cold packs I bought ARE worth something. I could turn them into potassium nitrate I believe. But I got
enough potassium nitrate.
One thing I do want to make is sodium nitrite for a possible DDNP synthesis.
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B(a)P
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I tried some experimentation over the weekend adding ammonium sulfate to potassium nitrate in an attempt to isolate ammonium nitrate, though this is
the potassium salt it is still applicable to CAN.
100 g of ammonium sulfate and 153 g of potassium nitrate was weighed out and and placed in a 600 ml beaker. To this 150 ml of distilled water was
added then placed on the hot plate with stirring.
Almost immediately a cloudy white precipitate started to form (potassium sulfate).
The mixture was heated until the potassium nitrate and ammonium sulfate had dissolved and to the point that a faint ammonia odour could be detected.
The mixture was removed from the heat and return to room temperature. Solid potassium sulfate was then filtered off, but at this point the solution
still contained about 10 g/100 ml water of potassium sulfate.
To remove the remainder of the potassium sulfate 40 ml of ethanol was slowly added. This appeared to drop out the remainder of the potassium sulfate,
though it also could have caused potassium nitrate, ammonium sulfate or some ammonium nitrate to come out of solution.
The solution was boiled down to about half of its volume then left to cool and some nice prismatic crystals formed.
The next step will be to reduce the volume of the solution further to get as much ammonium nitrate out as possible. After assessing the yield of both
potassium sulfate and ammonium nitrate a method will be devised to test for both potassium and sulfate contamination in the ammonium nitrate. More to
come.
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ManyInterests
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Thanks. That is useful information. Although I might be going for the nitric acid/ammonia solution method in the future. It is good to have this in
case I do want to try it.
BTW, can you take a peek at the other thread where I had issues with sodium perchlorate? I got a propane torch and it's been running for almost 2
hours. I do see some progress, but I want to make sure I am doing it all right.
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And if it's sodium nitrate you want, and you're in Europe, there's always https://www.pyrogarage.pl/en/category/chemicals/oxidizers/
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ManyInterests
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Well I am in Canada, not Europe. Nitrates are generally more restricted around here . Calcium ammonium nitrate is available OTC in cold packs. And
Westlab sells various other nitrates. But the big three (potassium, sodium, and ammonium nitrates) are restricted. For ammonium nitrate if its
nitrogen content is 28% or below, it can be sold OTC, but the stuff used in the lab generally cannot be obtained without some paperwork.
I think I will get some ammonium nitrate when I start making nitric acid again. I can easily make a few kilos of sodium nitrate with what I have as
well. Even more potassium nitrate as I still have a good supply of potassium chloride.
Right now I am trying to get a handle to make some perchlorates. It is driving me up the wall!
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I made potassium perchlorate through double electrolysis of potassium chloride. First to potassium chlorate, then onwards to perchlorate. Verified by
stability tests.
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ManyInterests
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Great. I do need a perchlorate of some kind to make ammonium perchlorate. I have ammonium chloride so that when I have sodium perchlorate I can do it
that way.
My crucible broke during my latest extraction attempt. I ordered another one (because I will need to make nitrites and other things requiring a
crucible). So thermal decomposition is out of the question at the moment. I've also tried so much with it that I've honestly given up.
I did order a platinum electrode (a legit platinum anode) for 36$ American. It should be at my place in two weeks or so.
I have a question: Can I use the platinum anode combined with a titanium cathode to make perchlorates directly from chlorides? I do have the sodium
chlorate with me (I will not throw them away. I worked too hard for them!) Once my platinum anode arrives, can I just dump my sodium chlorate in
solution and start electrolysis?
How much current do I need? I have a 5V 20A power supply (it delivers consistent 5 or 5.1V. The amperage is likely around 15 to 17.5 amps) is that
sufficient?
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Rainwater
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You need to limit the current to around 0.2 amps for each cm² of the platinum anode. You could push it to .25amps but the higher amps need temp and
ph control.
Lots of fake anodes.
If it is fake you will find out fast in your perchlorate cell.
You can test it with H2O2 solution. Exposure to platinum will cause the h2o2 to decompose.
"You can't do that" - challenge accepted
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ManyInterests
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I am acutely aware of the sheer number of frauds out there. I saw NurdRage's video on it. The company I bought from is this:
https://electrodesupply.com/platinum-electrodes/
I had a fellow chlorate/perchlorate maker vouch for them as being authentic. Though only time will tell. The anode should be at my place within two
weeks.
I ordered a 2x3 platinum anode. So at 6 square inches it is around 38.7 cm2 and that amounts to 7.74 amps at maximum without pH and temp control.
My DROK DC-DC buck converter maxes out at 5A, so I guess I can connect my main power supply to that and deliver the most that the DROK can pull. It'll
be slower I know, but safer on the anode. I want the perchlorates. If it takes an added day or three I can live with that.
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Rainwater
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https://www.sciencemadness.org/talk/viewthread.php?tid=22412
https://www.sciencemadness.org/whisper/viewthread.php?tid=15...
I would like to know which one of these answers is correct. A google of "calculate anode surface area" turns up a large debate with both sides
concluding that its best to pick the lower values to protect their expensive anodes
Dont forget, you can double your anode's reactive surface area by using both sides.
"You can't do that" - challenge accepted
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ManyInterests
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Thanks. But I had a very long conversation with a fellow sciencemadness electrolysis specialist and I learned a lot.
I think my original thermal decomposition failed because my chlorates were not pure enough. I learned that sodium chlorate is VERY soluble in methanol
while sodium chloride is not (51 grams vs 1.2 grams in 100 ml at 25C). I will be shopping for more methanol soon and do some purification.
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B(a)P
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What impurities are you proposing that would prevent the melting/thermal decomposition?
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ManyInterests
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I actually do not know. I was just told (by LL and others) that in order for the thermal decomposition to work well, it seems to be at least 95% pure.
It clearly wasn't.
For chlorate to perchlorate via electrolysis, I was told it needed to be even purer than that, like 99.5%
I am going to try to purify them, but only in preparation for the future. Since I have neither a crucible (it broke as I said) or the platinum anodes
yet.
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Fyndium
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Just for the record, urea should be available in pure form as garden fertilizer. It costs around 2$/kg. No need to buy AdBlue, although it remains a
viable source. Cold packs are likely very expensive way to obtain urea as such basic constituent.
Likely the best way to obtain higher purity AN is to get CAN and ammonium sulfate.
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