Sciencemadness Discussion Board - ammonium nitrate from cold packs trouble

ammonium nitrate from cold packs trouble

ManyInterests - 19-6-2022 at 12:41

I am posting it in this forum because every time I ask a question of this nature it always ends up here!

Anyway some background information: I ordered some cold packs that contain only ammonium nitrate and water (as opposed to calcium ammonium nitrate which I normally do) from this Amazon.ca seller.

shorturl.at/aivJW

and this is a link to the product page on the manufacturer's website: https://www.primacaremedical.com/product/instant-cold-pack/

They clearly state that it is only ammonium nitrate and water. Commenters on the amazon page also stated that they did use it to make thermite, so I am confident that it is ammonium nitrate.

I followed the process as described by the Canadian Chemist here: https://www.youtube.com/watch?v=lYUdHEW2T2s

It is an elementary process. I just dissolved several packs in an excess of water (more than he said in the video) and waited a while for everything to settle down. What happened is that the insoluble filler all pooled at the bottom while the the remaining liquid remained crystal clear. I vacuum filtered the liquid and discarded the filler. After this I waited another couple of hours just to make absolutely sure that everything in my flask is settled. The liquid was slightly murky and off-white, and I poured it all into my glass lasagna pan that I use only for chemistry and I put it in my oven at 88 to 100 degrees Celsius for around 15 hours for everything to evaporate the water and dry everything.

In the end it resembled the same thing that the Canadian Chemist had in his video. I let it cool down and ground up some in my coffee grinder, after which I added sugar to it (50/50 ratio) and tried to burn it.

But no burn happened. It formed some blisters as a result of the heat and blackness, but no fire like potassium nitrate or my chlorate mixtures when I add sugar to them and burn.

I need to mention that in Canada, Ammonium nitrate with a nitrogen content above 28% is restricted. So this is not the 34-0-0 fertilizer grade that many are familiar with. I do not know the exact percentage of nitrogen in it, but if the CAN is any indicator, it might be around 20% or 15% at the lowest. The Canadian Chemist used cold packs he got from the US, but I am not sure if cold-pack grade ammonium nitrate is the same as fertilizer grade

Is my end product still ammonium nitrate? Can I still use it for things like making nitric acid and as a means of turning sodium perchlorate into ammonium perchlorate?

Is there any other test I can do?

ManyInterests - 19-6-2022 at 12:55

I should mention that I did two such processes in the past two days. I started the 2nd before the first one fully dried. I still have the powder from both synthesis in case I need to do something to salvage this. This is a lot of nitrate salt and I really want to put it to good use.

Rainwater - 19-6-2022 at 13:13

I would suggest you test for nitrates and chlorides.
https://en.m.wikipedia.org/wiki/Nitrate_test

test for ammonia by thermal decomposition. When you heat it, you will smell it.
Actually heating an unknown compound then taking a wiff is a good way to die.

Heat it in an apparatus then force the gas over a solution of HCl. If you see a white percipitate, then that is a positive test for ammonia.
NH4 + HCl gass mixing

Did you happen to measure the temperature change as the sample dissolved?
I can't remember which gets colder. ammonia chloride or ammonia nitrate.
Whichever it is, with a large excess of the salt. Will freeze the water before it is completely dissolved.

If the reagents for the nitrate test or chloride test are unavailable. I recommend measuring the solubility of the sample

NH4NO3 150 g/100 ml (20 °C)

ClH4N 294 g/L (0 °C)
383.0 g/L (25 °C)

P.S. if your going to make/use nitrates. I highly recommend the nitric acid thread. 5 stars. Will be reading again

[Edited on 19-6-2022 by Rainwater]

karolus28 - 19-6-2022 at 13:32

maybe mix a bit of it with a little excess of sulfuric acid(drain cleaner should work too)? It should fume and smell like nitric acid

Rainwater - 19-6-2022 at 13:37

Heating ammonia nitrate will not create ammonia gas. Sorry. I need to research before I post. It will generate NO_x and N₂.
Not sure what the best test for ammonia is.

I do know that
Ammonia and magnesium nitrates are used for several different cold packs. As is ammonia chloride

ManyInterests - 19-6-2022 at 13:54

Quote:

test for ammonia by thermal decomposition. When you heat it, you will smell it.
Actually heating an unknown compound then taking a wiff is a good way to die.

Well it isn't an unknown compound. It's not like it's a big mystery. The package says ammonium nitrate and water. I did get a super cheap teflon pan to use for chemistry, so I guess I can use that.

But no smell happened in my oven whatsoever when I put the tray in to both evaporate the water and dry everything. How hot do I have to heat it to smell anything?

I also cooked chicken wings for dinner last night after I dried the first batch. I'm still here and there was nothing unusual about the taste of the chicken.

Quote:

https://youtube.com/shorts/ldHBp3hBof8?feature=share

That's a really cool video, but I don't have the appartus to perform that test. So I'll have to find another way.

Quote:

Did you happen to measure the temperature change as the sample dissolved?
I can't remember which gets colder. ammonia chloride or ammonia nitrate.
Whichever it is, with a large excess of the salt. Will freeze the water before it is completely dissolved.

It's a cold pack. It got REALLY cold, I mean freezing cold, when I added the room temperature water. I did not measure how cold it got, but the water did not freeze, no. Why do you suspect there is ammonia chloride in it? It isn't mentioned anywhere by the manufacturer.

Quote:

maybe mix a bit of it with a little excess of sulfuric acid(drain cleaner should work too)? It should fume and smell like nitric acid

I did think about that. I think I'll do it. I wasn't sure what would happen. I will definitely be doing it on my balcony since nitric acid fumes are horrific and I don't want to do anything other than a confirmation of it.

ManyInterests - 19-6-2022 at 14:25

OK so I mixed 10 grams of my (possibly) ammonium nitrate salt to 60 ml of purified sulfuric acid. There was no exothermic reaction and no strong odor of anything. It may have been nitric acid. But my experience of potassium nitrate in sulfuric acid produced a LOT of fumes even with a small quantity like that.

I did try to take a whiff of pure sulfuric acid, but I didn't get the spiciness of sniffing the small container that I made

Maybe it did smell of nitric acid, but I really had to put my nose uncomfortably close to the whole thing.

Rainwater - 19-6-2022 at 14:55

Quote: Originally posted by ManyInterests

Well it isn't an unknown compound. It's not like it's a big mystery.

Your experiment didnt produce the expected results.

Dont trust the lables. Manufacturers lie. They sold you a cold pack, not ammonia nitrate. They are pre packaging an endothermic reaction.
If you do some simple test you can prove what compound you have. For sugar rockets i think the preferred mixture is 2 parts oxidized to 1 part fuel. Might give better results. I like powdered sugar myself

ManyInterests - 19-6-2022 at 15:04

Quote:

Isn't it illegal to lie about the contents of your product? It is possible that they are lying and can get away with it... because I mean, cold packs aren't normally intended to be used to get the nitrate salt for use in making energetics or home chemistry.

But the highest rated comment on the amazon page did say that the guy using it said 'it's perfect for tannerite'. It has to contain ammonium nitrate to make that.

Is it possible to make ammonium nitrate by dissolving the CAN (Calcium-Ammonium Nitrate) in 6% ammonia solution? What if I dissolve the current stuff I have in ammonia solution? Do you think that might work?

Rainwater - 19-6-2022 at 15:18

Take your compound + sulfuric acid solution and place a few drops onto some copper metal. If there is no reaction occurs you do not have a X_yNO₃ salt.

If you have silver or lead nitrate, make a small solution, .5g to 100ml water.
Make the same solution with your compound. Mix them together. If a white(silver) or gray(lead) precipitate forms you have a chloride salt.
The video referenced mentions a melting point. Very useful information if you have the abilty to measure it.

If you want to make ammonia nitrate, i suggest ice cold nitric acid and a solution of ammonia. If candy rockets are what your wanting to study then ammonia is the best to use but any nitrate salt will work.

ManyInterests - 19-6-2022 at 15:35

I have copper tape (it is electrically conductive and it is copper, so I used it) and here is what happened to it. I dipped the part that changed color into the solution.

I did see some change. But is that the reaction you are talking about?

B(a)P - 19-6-2022 at 15:37

Quote: Originally posted by ManyInterests

Commenters on the amazon page also stated that they did use it to make thermite, so I am confident that it is ammonium nitrate.

Do you mean tannerite?

Try making a solution of your compound in just enough water to dissolve it. Then add sodium hydroxide (do this in a well ventilated space). If your compound contains ammonia then ammonia gas will be released.

It is odd that you get no noticeable warming or nitric acid fumes when you add sulfuric acid. Is your sulfuric acid concentrated? Try again with the sulfuric acid and add some copper. If nitrate ions are present you will see a strong reaction with lots of NOx produced, again do this in a well ventilated space.

Rainwater - 19-6-2022 at 15:38

Maybe. If the reaction is not violent then leave the copper in the solution, the liquid should turn blue/ blue green

Rainwater - 19-6-2022 at 15:51

https://youtube.com/shorts/lpn_LdXg39Q?feature=share
This color. Give me a minute and ill do the nitrate salt + sulfuric acid + copper reaction for you

ManyInterests - 19-6-2022 at 16:09

Quote: Originally posted by B(a)P

Quote: Originally posted by ManyInterests

Commenters on the amazon page also stated that they did use it to make thermite, so I am confident that it is ammonium nitrate.

Yes Tannerite, my apologies.

My sulfuric acid is quite concentrated. Albeit maybe not 98%. The reason why is my mantle started to have problems after a previous acid spill on it and wasn't heating as it was previously. But I am confident is more than 93% as I started with around 550ml or 540ml drain opener + 35ml of 33% H2O2 to clean it. It didn't reach a rolling boil as it did previously, but I did see small bits of white fumes come out after I heated it at max (normally I get it to a rolling boil and I see plenty of white fumes). I ended up with around 515ml of end product

However it is still a thick, syrupy acid. So I assume it is quite concentrated. I have other acid that I know is more concentrated.

But it is very strong sulfuric acid. It should react well with a nitrate salt. I could test it with some potassium nitrate that I do have (plenty of, too!).

I will try the sodium hydroxide thing you mentioned.

Rainwater - 19-6-2022 at 16:16

H2so4 + kno3 + copper
https://youtu.be/zHGPSgm5Swk
As you can see. Very reactive. Its about 27c outside today

Sugar + kno3
Uploading .......
As you can see I didn't mix the sugar very well. Best to suspend both in an ethanol mix and let it air dry for a truly powerful reaction.
https://youtu.be/J76h9MDq4Xk

ManyInterests - 19-6-2022 at 16:34

I know how sugar and KNO3 burn. I always do that to test every batch. Purple flames are beautiful!

Also I did not see the reaction with the copper...

Quote:

Try making a solution of your compound in just enough water to dissolve it. Then add sodium hydroxide (do this in a well ventilated space). If your compound contains ammonia then ammonia gas will be released.

Winner! Winner! Chicken Dinner! I smell ammonia.

I confirmed that the smell IS ammonia by opening my 28% solution bottle and having my olfactory system being assulted by a POWERFUL smell of ammonia. I'll be OK, but holy shit. I will never forgot the smell of ammonia ever again.

So it's confirmed. dissolving the stuff in just enough water and adding sodium hydroxide (I put in a sprinkle but did not measure the amount) will absolutely yield ammonia.

So does this mean that I do have ammonium nitrate? Maybe one that doesn't burn, but I can use to make ammonium perchlorate?

B(a)P - 19-6-2022 at 16:47

Quote: Originally posted by ManyInterests

Also I did not see the reaction with the copper...

So it's confirmed. dissolving the stuff in just enough water and adding sodium hydroxide (I put in a sprinkle but did not measure the amount) will absolutely yield ammonia.

So does this mean that I do have ammonium nitrate? Maybe one that doesn't burn, but I can use to make ammonium perchlorate?

It means you likely have an ammonium salt. It could also be that you have urea as it will also liberate ammonia when added to sodium hydroxide in solution.

If you add your compound to concentrated sulfuric acid then add a piece of copper and get no reaction, your compound is not a nitrate salt.

If you have some silver nitrate you can test for chloride ions as you may well have ammonium chloride. If you don't have silver nitrate then add a little of your compound to concentrated sulfuric acid, generate some more ammonia and waft it over the acid mix. If chloride is present it will be released as hydrogen chloride, which will react with ammonium to form ammonium chloride in the form of a white smoke.

ManyInterests - 19-6-2022 at 17:17

By compound you mean the water + salt + sodium hydroxide?

if that is the case, I will use some of my good stuff.

edit: If you mean just the salt and sulfuric acid, well I technically already did that, but I can try again and put in a copper penny.

[Edited on 20-6-2022 by ManyInterests]

B(a)P - 19-6-2022 at 18:12

Apologies for the confusion.
Let's break it down. You think you have ammonium nitrate, but you didn't get the reaction you expected when mixed with sugar and set on fire, so you need to do some tests to confirm what you have.

Firstly, does the suspected ammonium nitrate have ammonium ions, you tested for that by liberating ammonia from your solution of suspected ammonium nitrate by the addition of sodium hydroxide. However, a solution of urea will yield the same result and urea is often used in cold packs, so this is not definitely.

So the next thing to do is test for the nitrate. You tried this by adding concentrated sulfuric acid to your suspected ammonium nitrate and didn't get a definitive result (couldn't detect nitric acid odours). A better test for nitric acid is to add copper, as it reacts strongly with nitric acid. Have you tried adding copper to your suspected ammonium nitrate dissolved in concentrated sulfuric acid? If so, what did you observe?

If you have done the copper test and got no reaction you do not have a nitrate salt. If it isn't a nitrate it may be a chloride, so the tests I proposed in the last paragraph of my above post (provided below for clarity) were to test for chloride ions.

If you can't detect chloride ions then your suspected ammonium nitrate ids likely urea.

Quote:

If you have some silver nitrate you can test for chloride ions as you may well have ammonium chloride. If you don't have silver nitrate then add a little of your compound to concentrated sulfuric acid, generate some more ammonia and waft it over the acid mix. If chloride is present it will be released as hydrogen chloride, which will react with ammonium to form ammonium chloride in the form of a white smoke.

ManyInterests - 19-6-2022 at 19:16

Now you're talking my language!

OK so this time for the test. I got 12 grams of my compound and put around 90 ml of 98% sulfuric acid (I used the good stuff this time!) I stirred it with a long glass thermometer, and there was a temperature jump from 25C to 41C. I also did smell a noticable NO2 scent. It was not super strong (Thankfully) but it was there. After dissolving almost all of the compound (which was rocky and took a while to break up) I plopped a 1 cent coin in it and now am I watching what's happening. I see a reaction, I will monitor and report in another post (or editing of this post).

Edit: that 'reaction' was not what I thought it was. sorry, there was no reaction.

[Edited on 20-6-2022 by ManyInterests]

ManyInterests - 19-6-2022 at 19:22

OK so I am going to conclude that I was completely lied to by the manfucturer. The coin remains completely copper colored and has precisely no green morning or corrosion. This is not ammonium nitrate. Whatever it is.

I'm just going to dump whatever it is in the trash. I have no idea what it is and I don't need it and I don't want it. I feel like a sucker.

At any rate I ordered ammonium chloride from amazon. I will be using that in my ammonium perchlorate synthesis. I spent too much time on this already.

Thank you for all the help. You have been awesome.

[Edited on 20-6-2022 by ManyInterests]

B(a)P - 19-6-2022 at 20:02

Sorry to hear that!
Best of luck with the ammonium chloride.

DocX - 19-6-2022 at 23:38

It might very well be urea. It's what ammonium nitrate is usually replaced with. I have had the same problem and posted a thread recently about it: https://www.sciencemadness.org/whisper/viewthread.php?tid=15...

I was unsure if there is urea contamination in my ammonium nitrate from cold packs, and I got the tip to dissolve a bit in water and add nitric acid. If a white precipitate appears, it will be urea nitrate.

ManyInterests - 20-6-2022 at 07:14

Quote: Originally posted by DocX

It might very well be urea. It's what ammonium nitrate is usually replaced with. I have had the same problem and posted a thread recently about it: https://www.sciencemadness.org/whisper/viewthread.php?tid=15...

I was unsure if there is urea contamination in my ammonium nitrate from cold packs, and I got the tip to dissolve a bit in water and add nitric acid. If a white precipitate appears, it will be urea nitrate.

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.

I will be needing urea, but I have 4 cold packs of urea from a proven brand. I will be using that.

Herr Haber - 20-6-2022 at 12:50

Quote: Originally posted by ManyInterests

Edit: that 'reaction' was not what I thought it was. sorry, there was no reaction.

[Edited on 20-6-2022 by ManyInterests]

See my signature ? Look for the whole text, it's a 2 minutes gem and very related to what I read here

ManyInterests - 20-6-2022 at 13:25

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.

Rainwater - 20-6-2022 at 15:59

You can bubble ammonia gas through dilute nitric acid.
An ice bath would be needed. And the acid.

DocX - 21-6-2022 at 11:30

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.
.

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.

ManyInterests - 25-6-2022 at 11:46

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.

arkoma - 26-6-2022 at 08:26

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]

ManyInterests - 26-6-2022 at 10:06

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.

DocX - 26-6-2022 at 10:17

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.

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.

ManyInterests - 26-6-2022 at 10:41

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.

Rainwater - 26-6-2022 at 11:46

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.

Def fluid comes in 2.5 gallon containers. About $25 here.
32.5% urea. Yielding about 3 kilos when dried.

DocX - 26-6-2022 at 13:34

And if it's sodium nitrate you want, and you're in Europe, there's always https://www.pyrogarage.pl/en/category/chemicals/oxidizers/

ManyInterests - 26-6-2022 at 15:22

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.

B(a)P - 26-6-2022 at 15:54

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.

ManyInterests - 26-6-2022 at 16:41

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.

DocX - 26-6-2022 at 21:04

And if it's sodium nitrate you want, and you're in Europe, there's always https://www.pyrogarage.pl/en/category/chemicals/oxidizers/

ManyInterests - 26-6-2022 at 21:22

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!

DocX - 27-6-2022 at 10:10

I made potassium perchlorate through double electrolysis of potassium chloride. First to potassium chlorate, then onwards to perchlorate. Verified by stability tests.

ManyInterests - 27-6-2022 at 16:33

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?

Rainwater - 27-6-2022 at 16:56

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.

ManyInterests - 27-6-2022 at 19:12

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.

Rainwater - 28-6-2022 at 01:23

Quote: Originally posted by ManyInterests

I ordered a 2x3 platinum anode. So at 6 square inches it is around 38.7 cm2

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.

ManyInterests - 28-6-2022 at 19:23

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.

B(a)P - 29-6-2022 at 17:21

Quote: Originally posted by ManyInterests

I think my original thermal decomposition failed because my chlorates were not pure enough.

What impurities are you proposing that would prevent the melting/thermal decomposition?

ManyInterests - 29-6-2022 at 19:51

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.

Fyndium - 29-6-2022 at 23:42

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.

ManyInterests - 1-7-2022 at 23:35

Quote:

Likely the best way to obtain higher purity AN is to get CAN and ammonium sulfate.

I'll keep that in mind. Because I will need a little ammonium nitrate for a few things.

At any rate, I am purifying my chlorates, and it seems that something went wrong with my synth. Because i am nowhere near purity. In fact, out of the remaining 405 grams of chlorates that I had left from my thermal composition exercises... turns out that I have over a hundred grams of chloride. I don't know how much since I am drying the left over salt and I am boiling off the methanol I used for the purification.

Like holy shit. I had no idea how little chlorate I actually made. Something is up with my electrolysis.

ManyInterests - 24-1-2023 at 21:42

I decided to resurrect this thread since I am having similar problems with nitrate synthesis but for entirely different reasons:

Firstly I am using this brand of calcium-ammonium nitrate as a starter.

http://www.formedica.com/en/hot-cold-compresses/instant-cold...

In the past I've used this brand extensively to make potassium nitrate, and to a large extent, it produces a working product and I've used it to make good nitric acid and other applications where potassium nitrate is needed (it is not 100% pure and isn't super fast burning, but I never found that to be a problem). I wish I knew what to do to get the purest possible product.

Now remember those cold packs that I opened the thread with? The primacare? I used them to make sodium nitrate, and while that sodium nitrate is far form perfect, it worked for almost everything as well, from picric acid synthesis to making nitric acid (I even made nitric acid with a specific gravity of 1.51, so WFNA or near it).

But when I switched to the formedica brand, I applied the same process as the primacare but I got different results. The burn rate for the sodium nitrate was a snail's pace, and while it did work for nitric acid, I feared that the product is not pure enough for use on its own where I just need sodium nitrate, like picric acid synthesis and such.

I followed Canadian Chemist's process for making sodium nitrate using calcium ammonium nitrate (after filtering out the impurities) and mixing in sodium bicarbonate.

I decided to try something different. I feared I was using too much sodium bicarbonate, so what I did is I weighted out 553.1 grams of CAN from cold packs, filtered out the insolubles, evaporated off all the water, and I ended up with around 418.28 grams of dry CAN, then I added 1.054x that amount in sodium bicarbonate to it (I was using a vast excess of water) and I boiled it. It seemed to work. It was producing a lot of ammonia gas and I boiled it until it reached a super saturation point (the beaker was bumping violently, so I stopped the heating and it cool) then I placed the entire amount in the oven for it to dry overnight and now I've ground up all the chunks into fine bits, dried it some more, then ground it up again (there is still a lot of moisture) and made it a fine powder and it is in the oven again.

I did do a burn test, but I didn't get much in terms of results, but those are the crude chunks that wouldn't grind down, so I guess I shouldn't expect much. I pray that the sodium nitrate I have in the final dry will work. If not, I will dissolve them all again in water and add a little more sodium bicarbonate. Maybe I didn't add enough for everything to react together?

I used a 1:1 ratio of nitrate and granulated sugar for the burn test. it was REALLY slow.

As for some notes: I did get ammonium nitrate cold packs from the US, so I should have some real ammonium nitrate after I filter those and dry them properly. I also did obtain a pound of ammonium sulfate, so I can do the synthesis of ammonium nitrate via CAN and ammonium sulfate.

Can anyone give me the stoichiometric amounts?

Rainwater - 25-1-2023 at 13:59

Quote: Originally posted by ManyInterests

Can anyone give me the stoichiometric amounts?

Nope. But i can help you work it out.
Do you have a set of equations for your procedure yet?
Get those and will balance everything and cross reference some literature

Here are some relevant links
http://www.sciencemadness.org/talk/viewthread.php?tid=159262...
http://www.sciencemadness.org/talk/viewthread.php?tid=59080#...
Looks like you been stuck on this for a while. Will get you sorted.

Have you tried thermal decomposition?
Pnta but will produce NO_x that can be turned into HNO3 and you can use that to make any salt you need

ManyInterests - 25-1-2023 at 17:37

Thanks, I am looking into those now.

for my sodium nitrate, my latest synthesis is a lot more successful than previous one. Better burn rate with visible golden flames. It should work for all that I need, but I would like a better handle on it for obvious reasons. One of the first things I made was potassium nitrate and that was actually quite successful, though it didn't burn at the same speed at commercially available potassium nitrate (which I cannot obtain in Canada, sadly).

Edit: Wow, those methods for gauging whether it is calcium nitrate, calcium-ammonium nitrate, and how much ammonium nitrate there might be in sound really fascinating, I will definitely be working on those soon.

[Edited on 26-1-2023 by ManyInterests]