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Author: Subject: What the hell is in my cold packs?!?!
Luftwaffe
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[*] posted on 19-11-2011 at 17:59
What the hell is in my cold packs?!?!


So I decided to purify my AN I got from instant cold packs and something and I was suprised at how pure they looked.

The cold pack consisted of bright white prills of ammonium nitrate (stated on the box) with some anti caking that I can filter out after a few passes through paper towel. So I dissolved about 220g in 400ml of water and filtered. the solution turned slightly brown when I dissolved the prills but just a faint tint. I proceeded to then boil down the solution to less than 100ml of water and as the solution got to boiling it went crystal clear. So I left it to boil for an hour and came back to find it boiled down to a little less than 100ml. it was very lightly bubbling making a foam like substance and was DARK BROWN and when I swirled the beaker around it would foam alot then settle down.

So I ask, what the hell is in my AN cold packs to make such a distasteful looking solution, and should I be worried about anything harmful coming out of it? I avoided smelling any fumes outside, but it has the smell of, well, fertilizer in a hardware store which isnt hard to believe since they probably pack up a bit from the fertilizer buisness to make the packs.

I also experienced something odd in my nitrations using the cold pack AN, when I dissolved the AN in the sulfuric acid, it turned red, and not brown from what I've seen other nitration mixtures with AN. The nitration yielded some product, but less than 20% of expected. I attributed it to the large amount of water in the prills to begin with which I tested after my nitration results, but I wonder now if it is the contaminants that are killing my yields.

Any input would be greatly appreciated.

Update: so I boiled it down to the point where it solidified in my beaker when I cooled it down. There should still be water in there, just stuck in the crystals. Anyways, there are veins of dark grey in the solid mass. Just more data to figure out what it is...

[Edited on 20-11-2011 by Luftwaffe]

[Edited on 20-11-2011 by Luftwaffe]
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bonelesss
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mad.gif posted on 20-11-2011 at 01:58


In Eu area instant cold packs no longer contain AN. Some stupid law back in 2006. Now packs contain usually Nirtrogenous salts or Carbamide. But thats just my quess based on this Eu-law information.

Still some packs has text which say containing Ammonium Nitrate and Water. I buy entire box and inside was printed paper informing even packs has text AN and Water they containing Nitrogenous salts

[Edited on 20-11-2011 by bonelesss]
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unionised
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[*] posted on 20-11-2011 at 05:12


AN is a nitrogenous salt.
What law was it? I'd like to see if there's a loophole, but actually I don't think any such law exists.
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hiperion42
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[*] posted on 20-11-2011 at 05:13







.....ejuu....................................................................Ffg..............................g.............
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Steve_hi
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[*] posted on 20-11-2011 at 06:34


If it's what i had in mine there is calcium carbonate in it I had the same brown foamy gook on top of my slurry too I ladeled it off and threw it out I let it settle down and then let it flow through a tap to not get the gunk mixed in again

[img]C:\Users\Steve\Pictures\2011-11-20 nov_20_2011\Nov_20_2011 002-8.jpg[/img]
Home made sep funnel for large quantities
I got a 25Kg bag of fertilizer for 20$ way cheaper than cold packs
Nov_20_2011 002-8.jpg - 47kB

[Edited on 20-11-2011 by Steve_hi]
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bonelesss
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[*] posted on 20-11-2011 at 08:46


unionised : Im 100% sure that law thing.
http://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri=CELEX:...

Somewhere here it is told,and I contact local instant cold pack manufactuter and he told me same thing.
one reason was some people keep instant cold packs their first-aid packs and when they go to airport they get troubles in customs and so on

shopkeepers can sell their stock out if they had earlier manufactured packs so you can still find some

google 2006/1907

[Edited on 20-11-2011 by bonelesss]
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watson.fawkes
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[*] posted on 20-11-2011 at 15:55


Quote: Originally posted by bonelesss  
unionised : Im 100% sure that law thing.
http://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri=CELEX:...
A little searching yield the fact that ammonium nitrate was not in the original legislation (as cited) but rather added afterwards to Annex I in 2008. I can't figure out exactly how to cite the definitive version of this, but it comes right up if you search their web site for the CAS number 6484-52-2 of ammonium nitrate.
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Luftwaffe
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[*] posted on 20-11-2011 at 15:55


So after searching heavily through sciencemadness there was a similar problem ( http://www.sciencemadness.org/talk/viewthread.php?tid=16126 ) with another type of fertilizer (Ammonium Sulphate) which had contaminants that could not be removed which would react at about 106C to form an even darker solution which occured in my situation. I think this cold pack brand is a lost cause, what looked to be very pure AN was just massively contaminated AN with white contaminants that turn brown when you dissolve and boil them...

Considering the new regulations in Canada they couldn't get away with pure AN in cold packs, so instead of adding chalk they added some soluable gunk. I've bought a different brand which contains CAN, I will dissolve and filter to see if it comes clear.
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bonelesss
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[*] posted on 20-11-2011 at 23:52


watson.fawkes : ok. sorry.When i searched couple years a go and site was Finnish language and I use similar key words.my english isn`t so good so I couldn`t checked that, my bad sorry
Well in this country where I live (Finland)
I`ve contacted several cold pack sellers or manufacturers and everyone has told me same thing that eu-law.
Also I bought different cold pack`s and none of them contain pure AN anymore.Some has Carbamide or AN mixed chalk or limestone or something,and some packs contain clears prills but i am sure it`s not AN.
Luckily there is another source for AN than cold pack`s :D
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Luftwaffe
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[*] posted on 21-11-2011 at 01:18


Just cracked open a new bag of instant cold pack which contained brown prills. I did the standard dissolve it in water and filter the gunk to get a clear solution and in fact it came perfectly clear, crystal clear solution void of colour. Final test will be to boil it down to get the NH4NO3 back and hope it doesn't turn brown at some point! :D
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watson.fawkes
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[*] posted on 21-11-2011 at 05:44


Quote: Originally posted by bonelesss  
When i searched couple years a go and site was Finnish language and I use similar key words.my english isn`t so good so I couldn`t checked that, my bad sorry
You had the right law. The restriction on AN was later, so the full story has to include both. I someone would like to find the right way to bring up this citation, it would be useful as reference, as these kinds of chemical availability regulations have a tendency to recur.

It would also be amusing, as the commentary on why it should be regulated includes the phrase "accidental detonation", as if a bag of AN fertilizer will spontaneously go off in the warehouse. Is there even one known incident of this with AN fertilizer? Just because I've never heard of such a one doesn't mean it hasn't happened, though it does sound a little far-fetched.
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[*] posted on 21-11-2011 at 05:55


IIRC 5-10 years ago railroad cars full of AN detonated in north-korea when powerline dropped or something like that i cant remember accurately,but it devastated extensive area.

aah now i find it http://en.wikipedia.org/wiki/Ammonium_nitrate_disasters#Ryon...

Yes i know thats different thing but just jumped on my mind when you mentioned accidental ignition. :D

[Edited on 21-11-2011 by bonelesss]
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watson.fawkes
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[*] posted on 21-11-2011 at 06:10


Quote: Originally posted by bonelesss  
aah now i find it http://en.wikipedia.org/wiki/Ammonium_nitrate_disasters#Ryon...
Thank you for that. That whole page describes rather well the hazards. As the introduction states, it's either from detonation because an explosion, such as stray artillery shells (the first example), or from fire. Having admitted that there are hazards, it stills seems to me that this particular justification is a little overwrought, as AN just doesn't pose the same kind of hazard in small quantities, such as in consumer products.

Edit: Added a space after the quoted URL to deal with a defect in the board software.

[Edited on 21-11-2011 by watson.fawkes]
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fledarmus
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[*] posted on 21-11-2011 at 10:41


@watson.fawkes - I don't know about accidental detonation of AN fertilizers, but there has been some recent work studying self-sustaining decomposition of fertilizers. One interesting study here:

Edinburgh Fire Research Blog

related to a major cargo ship fire
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[*] posted on 21-11-2011 at 13:19


Well, the legislation seems pretty tight. However I don't think recrystallising AN would be too difficult
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Luftwaffe
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[*] posted on 21-11-2011 at 16:20


So I boiled down the clear solution and I couldn't be any happier! It remained crystal clear even to the point of melting (boiled a little too much) It may have decomposed a little as I smelled something sweet taking it off the hotplate. I poured it on some Al foil and it immediately turned solid. The solid has a slight yellow tint to it but I consider it a negligible contaminant but if anyone has some insights as to what it is, be my guest. Probably some clear soluable contaminants decomposing under the heat, nothing a recrystallization cant fix!

Edit: It might have been the yellowish light coming from the walls and lights in the room reflecting off the smooth surface of the crystal. I crushed it up and it's white. :)

[Edited on 22-11-2011 by Luftwaffe]
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[*] posted on 25-12-2011 at 06:15


I think i had some insoluble hydroxide or basic oxide in my fertilizer. After filtering hot brownish solution and freeze-crystalising oversaturated soln of AN i got perfectly white crystals. Yet after many attempts to heat out N2O, even bubbling through water and washing the gas it smells like ammonia or something. The crystals are soluble and no reaction occurs when in water. Its driving me crazy, what the hell :mad:

Is this even possible or am i a catastrophe breaking all the rules of nature?
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[*] posted on 25-12-2011 at 07:16


was it CAN? If so you may have magnesium nitrate in your crystals, which will destabilise the ammonium every time the powder is wetted. See the end of Crows post on cold packs.
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[*] posted on 25-12-2011 at 10:21


Quote: Originally posted by bonelesss  
In Eu area instant cold packs no longer contain AN. Some stupid law back in 2006.


Quote:

...the Government of Canada has enacted the Restricted Components Regulations (“RCR”) which govern the sale of ammonium nitrate having a nitrogen concentration between 28% and 34%

The RCR attempt to prevent AN from being acquired for terrorist or criminal purposes as AN can, under certain circumstances, be used as an explosive. The RCR impose various security, inventory control, record keeping, and customer identification requirements upon each seller of AN.

AN has been the active ingredient in our company’s Instant Cold Packs (“Cold Products”) for some time. While the amount of AN in our Cold Products is small, we have decided to discontinue the use of AN in our Cold Products and use calcium ammonium nitrate in place of AN.

http://www.rapidaid.com/news/

I cannot believe how ignorant people can be. They hear about ammonium nitrate being used in a bomb and then become afraid someone someone will be able to make a bomb out of their cold packs. Ammonium nitrate is a relatively weak explosive compared to the others. It would take at least 100 cold packs to make a bomb with enough power to pose any significant threat. And the potential terrorist would need some other explosive to begin with just to be able to detonate the mass. Not only this, but the ammonium nitrate in cold packs is not even the ideal quality and grain shape to make a decent explosive. Many experimenters have commented that it is nearly impossible to get the AN from cold packs to detonate. The AN in the cold packs is also wet. It would all have to be carefully baked before it could even have the possibility of being used as an explosive.

And not only all this, but what do they replace the ammonium nitrate with? Calcium nitrate.

I do not know why stupid people are allowed to make stupid regulations. Trying to control every area of our lives. The governments are clearly not willing to change some of their other policies that are conducive to the growth of terrorism. (cannot elaborate since this is not a political forum and this thread is not the place for controversy). It seems inconsistent and unfair to blame the chemicals and put more regulations on products to try to solve the problem. All to often the government looks for simple solutions to complex problems by trying to just legislate them away through more rules or harsher punishments. This is just not effective.

Some people are even want to take away cold packs to stop illicit methamphetamine production!
http://www.medtox.com/Resources/Images/4824.pdf
Where will it stop! Are they just going to take away all chemicals?! Someone should put a stop to all this invassive regulation and chemical paranoia. Society is just going to have to accept that anyone could potentially make [small quantities of] explosives and illegal drugs.
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Neil
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[*] posted on 25-12-2011 at 10:51


Just wait till ya find out they have Urea in their sites. dun dun dun it can be used to make drugs and bombs...
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[*] posted on 25-12-2011 at 15:35


Quote: Originally posted by AndersHoveland  
I do not know why stupid people are allowed to make stupid regulations.
Because we elect them to public office.
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Alastair
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[*] posted on 25-12-2011 at 23:56


Quote: Originally posted by Neil  
was it CAN? If so you may have magnesium nitrate in your crystals, which will destabilise the ammonium every time the powder is wetted. See the end of Crows post on cold packs.


It was simple fertiliser, not CAN. I cant find the post you're reffering to. It is quite stable and nothing happens when wet. Do you mean when molten? I can already see a big problem purifying if its mixed with another nitrate -.-
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[*] posted on 26-12-2011 at 05:37


Hot and wet makes the reaction really noticeable. At RT the reaction is very slow.

It might now have been CAN but it sounds like it could have been similar given your description of it being brown. If there was added dolomite of calcium carbonate the formation of calcium/magnesium ammonium nitrate could have occurred.

Have you tried treating a small amount with NaCO3 and looking for a precipitate?

Wait a tick I missed something - do you mean decompose it to produce N2O?


Edit: If you are trying to decompose it by heating you are getting some NOx - it doesn't smell like ammonia to me, it smells more like Diesel exhaust without the soot and bleach over tones. Would you know the difference?

http://www.sciencemadness.org/talk/viewthread.php?tid=959

[Edited on 26-12-2011 by Neil]
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