| Pages:
1
2
3 |
ManyInterests
National Hazard
Posts: 838
Registered: 19-5-2019
Member Is Offline
|
|
ammonium nitrate from cold packs trouble
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
National Hazard
Posts: 838
Registered: 19-5-2019
Member Is Offline
|
|
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
National Hazard
Posts: 799
Registered: 22-12-2021
Member Is Offline
Mood: indisposition to activity
|
|
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]
"You can't do that" - challenge accepted
|
|
|
karolus28
Hazard to Self
Posts: 51
Registered: 14-4-2019
Location: EU's Brazil
Member Is Offline
Mood: zgrzyt
|
|
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
Hi, please read about exif data.
|
|
|
Rainwater
National Hazard
Posts: 799
Registered: 22-12-2021
Member Is Offline
Mood: indisposition to activity
|
|
Heating ammonia nitrate will not create ammonia gas. Sorry. I need to research before I post. It will generate NOx 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
"You can't do that" - challenge accepted
|
|
|
ManyInterests
National Hazard
Posts: 838
Registered: 19-5-2019
Member Is Offline
|
|
| 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.
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
National Hazard
Posts: 838
Registered: 19-5-2019
Member Is Offline
|
|
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
National Hazard
Posts: 799
Registered: 22-12-2021
Member Is Offline
Mood: indisposition to activity
|
|
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
"You can't do that" - challenge accepted
|
|
|
ManyInterests
National Hazard
Posts: 838
Registered: 19-5-2019
Member Is Offline
|
|
| Quote: | 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
| 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
National Hazard
Posts: 799
Registered: 22-12-2021
Member Is Offline
Mood: indisposition to activity
|
|
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
XyNO3 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.
"You can't do that" - challenge accepted
|
|
|
ManyInterests
National Hazard
Posts: 838
Registered: 19-5-2019
Member Is Offline
|
|
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
International Hazard
Posts: 1114
Registered: 29-9-2019
Member Is Offline
Mood: Festive
|
|
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
National Hazard
Posts: 799
Registered: 22-12-2021
Member Is Offline
Mood: indisposition to activity
|
|
Maybe. If the reaction is not violent then leave the copper in the solution, the liquid should turn blue/ blue green
"You can't do that" - challenge accepted
|
|
|
Rainwater
National Hazard
Posts: 799
Registered: 22-12-2021
Member Is Offline
Mood: indisposition to activity
|
|
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
"You can't do that" - challenge accepted
|
|
|
ManyInterests
National Hazard
Posts: 838
Registered: 19-5-2019
Member Is Offline
|
|
Quote: Originally posted by B(a)P  |
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.
|
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
National Hazard
Posts: 799
Registered: 22-12-2021
Member Is Offline
Mood: indisposition to activity
|
|
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
"You can't do that" - challenge accepted
|
|
|
ManyInterests
National Hazard
Posts: 838
Registered: 19-5-2019
Member Is Offline
|
|
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
International Hazard
Posts: 1114
Registered: 29-9-2019
Member Is Offline
Mood: Festive
|
|
| 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
National Hazard
Posts: 838
Registered: 19-5-2019
Member Is Offline
|
|
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
International Hazard
Posts: 1114
Registered: 29-9-2019
Member Is Offline
Mood: Festive
|
|
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
National Hazard
Posts: 838
Registered: 19-5-2019
Member Is Offline
|
|
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
National Hazard
Posts: 838
Registered: 19-5-2019
Member Is Offline
|
|
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
International Hazard
Posts: 1114
Registered: 29-9-2019
Member Is Offline
Mood: Festive
|
|
Sorry to hear that!
Best of luck with the ammonium chloride.
|
|
|
DocX
Hazard to Others
Posts: 179
Registered: 22-10-2015
Member Is Offline
Mood: No Mood
|
|
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
National Hazard
Posts: 838
Registered: 19-5-2019
Member Is Offline
|
|
| 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.
|
|
|
| Pages:
1
2
3 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
