Sciencemadness Discussion Board - Ammonium Nitrate Source

Ammonium Nitrate Source

Murexide - 7-3-2020 at 01:33

I've noticed that ammonium nitrate has recently become (more or less) impossible to obtain even in small quantities (100g ish) though it was widely used in the past as a fertiliser. Not available at hardware shops, banned for sale on ebay etc... can't locate a source anywhere. Ironically, I may actually be able to obtain conc. HNO3 and NH3...which can be used to make ammonium nitrate although it would seem extremely wasteful.

What has your experience been on this, especially within oz?

tahallium - 7-3-2020 at 06:54

Ummm I think you can react ozone with ammonia but you need ozone
You can make ozone by adding sulfuric acid to potassium permanganate but be careful cuz manganese heptoxide and ozone are extremely explosive and poisonous

B(a)P - 7-3-2020 at 11:24

I can't find an Australian source either. I make mine from calcium nitrate and ammonium sulphate, both sourced from Bunnings.

Murexide - 7-3-2020 at 12:59

Calcium sulfate precipitate is very difficult to remove though. It forms an unfilterable slurry that clogs everything, and it doesn’t even fully ppt so what filtrate you get will be contaminated

B(a)P - 7-3-2020 at 16:22

Calcium sulfate has a very low solubility in water. I set up a large gravity filtration overnight and it works fine. One recrystalisation gets it pure enough for my needs.

draculic acid69 - 7-3-2020 at 19:32

Quote: Originally posted by Murexide

Calcium sulfate precipitate is very difficult to remove though. It forms an unfilterable slurry that clogs everything, and it doesn’t even fully ppt so what filtrate you get will be contaminated

Filter thru a t shirt first to remove the bulk then filter as usual or let as much settle out as possible first so u can decant it.

Murexide - 7-3-2020 at 20:03

I suspect the the slurry would pass right through the t-shirt, though I haven't tried.

Might give it a go sometime.

Wow, just looked up solubility. You can get 580g/100 mL to dissolve, so only a 20% loss on recrystallisation. Not bad.

Deathunter88 - 7-3-2020 at 20:32

https://www.ebay.com/itm/Cardinal-Health-KWIK-KOLD-Instant-C...

Didn't see you were oz, but similar story probably.

[Edited on 8-3-2020 by Deathunter88]

Murexide - 8-3-2020 at 00:52

It's actually rather difficult to find ammonium nitrate based cold packs here.

They're all urea.

B(a)P - 8-3-2020 at 01:46

Quote: Originally posted by Murexide

It's actually rather difficult to find ammonium nitrate based cold packs here.

They're all urea.

Yep exactly, this is why i use the double displacement of the two fertilisers. Use a slight excess of calcium nitrate then wash your first lot of ammonium nitrate crystals with ethanol to get rid of any excess calcium nitrate.

Murexide - 8-3-2020 at 02:20

Wow, the solubility difference between calcium nitrate and ammonium sulfate in etoh is impresssive. Probably calcium complexing with ethanol?

This makes me think, what are the chances of recrystallisation in ethanol solvent working to eliminate the calcium nitrate?

Calcium sulfate fully insoluble in ethanol so hot filtration may be an option.

https://en.crystalls.info/Solubility_curve Looks promising

Murexide - 8-3-2020 at 02:23

Side note, what product do you source your calcium nitrate from in Bunnings? I can’t seem to find it.

Murexide - 8-3-2020 at 02:26

Also after filtration, do you just let evaporate to obtain product?

B(a)P - 8-3-2020 at 11:16

Part B of this https://www.bunnings.com.au/manutec-600g-hydrangea-pink-fert...
After filtering off the calcium sulphate I boil it down to about 10 or 20 percent of the original volume allow to cool then filter off the ammonium nitrate crystals, wash with ethanol, then perform a recrystalisation. I spread the crystals out on a ceramic dish then seal in a tub with a jar of anhydrous magnesium sulphate for drying.

Are you in Sydney? Since I made my last lot I have also found a reliable potassium nitrate source.

[Edited on 8-3-2020 by B(a)P]

Murexide - 9-3-2020 at 02:53

Wow never realised the multipart fertilisers were anything but homogonised mixes!

I'll give the procedure a go when I get some time.

Yeah I'm in Sydney too.

I have a reliable online source of KNO3, although not an OTC.

draculic acid69 - 9-3-2020 at 04:20

Quote: Originally posted by Murexide

Side note, what product do you source your calcium nitrate from in Bunnings? I can’t seem to find it.

Calcium nitrate is also part b of powdered hydroponic nutrient from Bunnings as well.

B(a)P - 9-3-2020 at 10:37

Quote: Originally posted by Murexide

Wow never realised the multipart fertilisers were anything but homogonised mixes!

I'll give the procedure a go when I get some time.

Yeah I'm in Sydney too.

I have a reliable online source of KNO3, although not an OTC.

These guys sell fertilizer grade KNO3. Looks like they also sell calcium nitrate in larger volumes than Bunnings do. https://www.petandgarden.com.au/

Nonexistent - 1-4-2020 at 06:59

We need a Bunnings tips and tricks thread I think. Damned panic buyers getting all the metho (etho) and IPA. Was glad to get some acetone and cooper sulphate today, although everything seems to be running thin.

CouchHatter - 1-4-2020 at 08:38

The new marijuana supply shops everywhere around here are good for something after all! I recently got some potassium nitrate for $2/lb. Some of them sell it for quite a lot more though. And I don't know how many plant supply stores you have down there, or if potassium nitrate would even be useful to you.

The replies to this thread mention Australian law concerning these chemicals... Good luck!

dicyanin - 1-4-2020 at 14:50

Years ago I have seen it available at a ceramics supply house in 1kg bags. I don't know what use it has there, and this was before 2014, back when bags of sodium chlorate were still sold as herbicide and 60% nitric acid solutions could be bought off the shelf. Today both, at least here, cannot be sold to private individuals anymore. At one point even 30% hydrogen peroxide was banned but luckily they came back from that.

B(a)P - 1-4-2020 at 16:06

Quote: Originally posted by Nonexistent

It is annoying not being able to source ethanol. I am currently running a fermentation for the purpose of restocking my ethanol supplies.
I was in Bunnings a couple of weekends ago and strolled by the place where ethanol usually sits in the hope that some may have come back in stock. As I walked past another customer experiencing the same disappointment as me said to the person standing next to them, 'I think mineral turpentine is just a brand of methylated spirits, let's grab 4 of those'.

draculic acid69 - 1-4-2020 at 16:53

Quote: Originally posted by Nonexistent

We need a Bunnings tips and tricks thread I think. Damned panic buyers getting all the metho (etho) and IPA. Was glad to get some acetone and cooper sulphate today, although everything seems to be running thin.[/rquote

Iso costs like $54 a litre from bunnings.its definitely a bad source for isopropyl alcohol.

draculic acid69 - 1-4-2020 at 16:58

It is annoying not being able to source ethanol. I am currently running a fermentation for the purpose of restocking my ethanol supplies.
I was in Bunnings a couple of weekends ago and strolled by the place where ethanol usually sits in the hope that some may have come back in stock. As I walked past another customer experiencing the same disappointment as me said to the person standing next to them, 'I think mineral turpentine is just a brand of methylated spirits, let's grab 4 of those'.

[/rquote]

Idiots.

Lion850 - 2-4-2020 at 04:30

Science Essentials was selling 2.5 liter of 96% LR ethanol for around $70 a week ago. Maybe they still have stock.

RogueRose - 2-4-2020 at 04:44

Quote: Originally posted by Lion850

Science Essentials was selling 2.5 liter of 96% LR ethanol for around $70 a week ago. Maybe they still have stock.

Man you can buy 50lbs of sugar and get about 4.5 gals of 100% ethanol for less than the $70, if you have the time.

dicyanin - 2-4-2020 at 17:32

I usually buy ethanol denatured with 5% diethyl ether through the pharmacy. 20 euros for a gallon.

FranzAnton - 8-5-2020 at 05:27

Oxidation of NH3 with Ozone

hm, the idea sounds good, because ozone can be created also from air and electricity ... but I fear that there are also a lot of side reaction? Is the reaction save? Can the mixture of NH3 gas and O3 gas ( on top of the liquid layer) explode?
Do you have more detailed information? Yield would also interestin.

[Edited on 8-5-2020 by FranzAnton]

dicyanin - 24-9-2020 at 23:09

Quote: Originally posted by RogueRose

Quote: Originally posted by Lion850

Science Essentials was selling 2.5 liter of 96% LR ethanol for around $70 a week ago. Maybe they still have stock.

Man you can buy 50lbs of sugar and get about 4.5 gals of 100% ethanol for less than the $70, if you have the time.

I just ordered some turbo-yeast, it can take up to 18% ethanol. There are instructions on the package: dissolve 8 kg sugar in 8 liter boiling water, and dilute this to 25 liter volume. Then, after cooling to room temperature, the contents of the package are added, and after 7 days of fermenting the result should be a solution of ethanol around 18%.

edit: maybe it's a good idea to add a few grams of diammonium phosphate as a free nitrogen source, as is generally done for wine. Maybe along with a few grams of yeast extract and a multivitamin tablet? Probably not really necessary.

[Edited on 25-9-2020 by dicyanin]

Fyndium - 24-9-2020 at 23:20

Purify you ethanol from car wiper fluid. At here it contains ethanol that distills over at 77-78C with short path column and MEK which seems to be get rid of using 20g/L of NaOH upon distillation. It is excessive to make it from scratch if you aren't intending to drink it.

But, how about using ammonium sulfate and calcium nitrate to obtain ammonium nitrate? It will precipitate into calcium sulfate and what does not settle, could be vacuum filtered to clear out? You can also use sand filter like I did to filter a really nasty, glue-like sludge. It didn't even take that long to get 20 liters of diluted liquor through a bucket into which I made holes, put cloth, about 10cm of sand and another cloth. I presume you use water as solvent.

[Edited on 25-9-2020 by Fyndium]

arkoma - 25-9-2020 at 19:30

Probably won't help you Ozzies, but Tannerite is pure, DRY NH₄NO₃, and at least here (Arkansas) Academy sports has shelves full of it. As a bonus, there is a packet of Aluminum powder with it (dunno the mesh, but its fine a hell).

Now a response to the off topic thought further up:

Quote: Originally posted by dicyanin

Quote: Originally posted by RogueRose

Quote: Originally posted by Lion850

Science Essentials was selling 2.5 liter of 96% LR ethanol for around $70 a week ago. Maybe they still have stock.

Man you can buy 50lbs of sugar and get about 4.5 gals of 100% ethanol for less than the $70, if you have the time.

I, umm, have a bit of experience in this area (Officer, it's HAND SANITIZER, not moonshine!).

My preferred yeast is this. It needs absolutely NOTHING except sugar and water. The yeast nutrient is already in there. Half a bag (25lb) of sugar poured is a five gallon bucket and the bucket filled about three inches from top with water. Usually use boiling water for the first gallon or two and stir to dissolve the sugar. Check temp before pitching yeast (45C or lower). Snap on lid with fermentation lock. Sucker will be BUMPING within hours. Let sit at least til no more bubbling through lock. Distill and keep fraction >100C. Distill again and keep fraction >82C or so. Yield about 2 litres of around 90% EtOH.

For "medicinal" purposes, the product is good first go round (will be about 120 proof, buy a hydrometer!) and is extra "medicinal" after a soak in a jar with whisky barrel chips. I use a 2l erlenmeyer (dedicated), a claisen adapter packed with copper gauze (genuine Chore Boy, not the 3M crap, it has some daggum coating on it) and a still head and a graham condenser. The copper catches the stinky sulfur compounds. I know the graham condenser ain't a favorite here, but i LOVE mine.

[Edited on 9-26-2020 by arkoma]

symboom - 26-9-2020 at 09:59

Calcium nitrate and ammonium sulfate should work to make ammonium nitrate

unionised - 26-9-2020 at 11:34

Quote: Originally posted by symboom

Calcium nitrate and ammonium sulfate should work to make ammonium nitrate

It does, but the sludge of calcium sulphate is a pig to deal with.

Fyndium - 27-9-2020 at 01:21

I have heard so. Apparently I have experience on similar matter as I recovered some soluble compounds from some fertilizer and filtering the sludge was terrible using plain sand, but resulted in clear solution anyway.

GammaFunction - 5-10-2020 at 15:50

Quote: Originally posted by B(a)P

I am currently running a fermentation for the purpose of restocking my ethanol supplie

Why not start with bottom-shelf vodka and distill to 96% (and then sieves if needed).

In US, 1.75l of 40% vodka is as low as $13, and will distill to 0.7l of ethanol. And it's much more convenient distilling from 40% than sub-20%.

B(a)P - 5-10-2020 at 16:47

Quote: Originally posted by GammaFunction

Quote: Originally posted by B(a)P

I am currently running a fermentation for the purpose of restocking my ethanol supplie

It is a bit different here in Australia you would struggle to get a 0.7 L bottle of 40% for less than $25. For $10 I can get enough sugar to make around 3 L of ethanol. I also enjoy and am well set up for the fermenting and distillation.

Mateo_swe - 13-10-2020 at 11:15

I also have some experience making ethanol although it was some years ago now.
I also use similar turbo yeast packs, sugar and water, same procedure for the starting fermentation to around 16-18%.
I have this all stainless distill rig with built in heater that takes the whole pail about 20liter of fermented material.
On top of the boiler there is a 8-10cm diameter stainless pipe filled with rachig rings (cerapic pieces of thin tube) and at the top a thermometer and a small tube going down to a condenser.
This device automatically dials in showing about 79°C at the top thermometer and the distilled ethanol drips out.
There are cooling water to condenser and it also goes right through the distill column at 2 places.
I get about 92% raw ethanol out that i dilute to 40% and pour it through a plastic pipe filled with activated carbon.
After the activated carbon treatment its way better than store bought vodka.
One can get it to the degree that it taste like nothing, one just feels the warmth in the chest.
One should get good quality activated stone based carbon, the better quality of activated carbon the better vodka.
If one wants ethanol for lab use do the same but dilute the carbon treated ethanol to about 20% and distill again.
How to get rid of the last % is harder, it wont go better than about 95% by distillation but i guess you all know that here.
One can use molecular sieves and some other methods to get rid of the water.
A good, well designed distill rig gets you high% ethanol on the first run but it needs the carbon treatment or maybe a second distill also works removing the foul tasting impurities, i dont know as i use activated carbon method.
An all stainless distill rig is a bit expensive if you cant make it yourself but it will last you a lifetime.
The sad thing is my distill rig is at our summer house and havent been used for years now as vodka for drinking is less hassle to just go buy at the store.
I have had thoughts about fire it up again just to make som absolute ethanol for experiments.
Right now all ethanol and isopropanol is bought up by people scared of the covid virus.
Maybe some isopropanol can be found at the 3D-printer stores.
They use it in large amounts to rinse the resin of 3D-printed items (the resin type 3D-printers).

Fyndium - 23-10-2020 at 08:46

I was tinkering this because I have a bucket full of extract that I made years ago. It originates from otc lawn fertilizer that has NPK rating of 8-4-13, contains also Mg+S 2+8 and 6% of calcium. I deducted that the calcium is either in calcium ammonium nitrate, or then just plain old calcium carbonate. So, apparently it contains no urea whatsoever, which is an excellent thing. The MSDS states that it just contains plain 25% AN and some minor additives like copper sulfate, etc.

Thing is, I dissolved it in boiling water and filtered it through sand and recovered everything that dissolved, and dumped everything that does not. The mixture formed literally a glue-like paste, that stuck everywhere and was literally impossible to filter with anything that resembles paper, but it dripped through a sand filter quite decently, although I had to dilute and agitate it now and then. The resulting liquor was crystal clear, though, so it did the job well. I concentrated the liquor until it started to mush up, and upon cooling it formed a moist white mass.

I suppose that if there were any soluble sulfates, they turned out to ammonium sulfate, which is inert to H2SO4. This could be checked by adding magnesium sulfate (which I have at hand) and see if precipitate occurs. Dropping in carbonate might not be a good idea, because it could turn stuff into carbonates, that react with H2SO4, expending valuable acid. I was thinking that I could do a test in tube by adding soluble sulfates and carbonates and see if precipitation occurs in attempt to determine what it contains and in which ratio. If I had Ca nitrate at hand, I would prefer it, because it would churn the ammonium sulfate and drop it out. Ammonium sulfate is inert to SA, so it only affects when determining the need for SA.

What would be the best net reaction to minimize the expenditure of sulfuric acid in order to extract all nitrates in form of nitric acid? I was thinking of starting the reaction with initial charge, and dropping in sulfuric acid as it proceeds, and when no more HNO3 appears, stop addition?

[Edited on 23-10-2020 by Fyndium]

njl - 23-10-2020 at 09:32

It is important to know what exactly you're dealing with before you try to isolate and nitrate. If I understand, you have a mass of water-soluble white solid. Why don't you try heating a small quantity to decomposition, maybe you could get an idea of actual nitrate concentration based on NOx evolution.

It sounds like you have in solution:
Ammonium nitrate
Ammonium sulfate
Potassium sulfate
Potassium nitrate

And possibly some soluble calcium and magnesium salts. Does that sound right?

Fyndium - 23-10-2020 at 10:22

The MSDS states only ammonium nitrate as the ingredient at 25%, and everything else is a wild-card.

Could it be better to make a microscale distillation with H2SO4 to figure out how much HNO3 it can output? Prior, dry the ingredients to eliminate all excess water and check the gravity of the resulting liquid. Estimating NOx fumes seems to be difficult from my point of expertise.

Anything that does not react with acid and or does not form volatiles that can affect HNO3, is ok with me.

[Edited on 23-10-2020 by Fyndium]

MadHatter - 23-10-2020 at 12:15

http://www.sciencemadness.org/talk/viewthread.php?tid=154741...

This is the post to the previous method to
produce ammonium nitrate from CAN and
ammonium sulphate. No longer needed for
me because I found it relatively cheap here
in the U.S. in agricultural prill form for
$2 USD/pound.

Fyndium - 23-10-2020 at 12:35

That looks like a good post. I thought it the other way, adding calcium nitrate to crash any ammonium sulfate out. Anyway, it appears obvious that any mixture containing calcium and sulfate in soluble form, will form an insoluble form, no matter how you put it. Both are easy to test.

The post is excellent if one wants pure ammonium nitrate. In my instance, I was only looking to extract all nitrate as nitric acid, and any H2SO4-inert spectators shall remain, because they will be drained anyway. I initially thought as far as recovering the ammonium sulfate and finally sodium sulfate. I don't actually have found any use for AN, because it is thermally unstable and generally any nitrate substitutes as a source of nitrate ion. If I ever happen to need pure AN, I'll give it a look.

For my mushy mess, I recall that I filtered off a huge amount of glue-like mass, and I wouldn't be too off to say it would balance to 75% of total volume. I remember buying two bags of 20kg of the stuff when it was on clearance sale for 70% off or something, and I ended up a bucket full of mushy concentrate, and couple of buckets of glue-gunk. Hence the mush might already be process-ready ammonium nitrate with some minor solutes. The fertilizer it was bought was purposes as a general garden fertilizer, not meant to be sprayed or pumped, hence it forming solids upon mixing doesn't matter.

N-P-K

MadHatter - 24-10-2020 at 10:18

Here are some N-P-K values when considering
nitrogen fertilizer.

Ammonium Nitrate: 35-0-0
Ammonium Sulphate: 21.2-0-0
Calcium Nitrate(anhydrous): 17.1-0-0
CAN: 15.5-0-0
Potassium Nitrate: 13.8-0-46.5
Sodium Nitrate: 16.5-0-0
Urea: 46.6-0-0

[Edited on 2020/10/24 by MadHatter]

Fyndium - 24-10-2020 at 14:09

It must also be noted that packages usually state "nitrogen from urea" and "nitrogen from nitrate". So a high nitrogen content fertilizer may be far from useful.

I also find it stupid that there are many fertilizers that contain little to almost no nitrates at all, instead they are filled with all kinds of other things, even when sold as "general purpose fertilizer".

I actually managed to find a fertilizer sold in 10, 20 and 40kg bags for general use that consists 60% of CAN and 10% of AN, balance being probably calcium carbonate and stuff. It is even for sale as winter is coming, so I might pick one up just for fun.

Mixes

MadHatter - 25-10-2020 at 08:09

I agree. Match up the ingredients list
to the N-P-K rating. Unless it corresponds
to something in those ratings you could
end up with a bag of "natural" fertilizer
which could be nothing more than dried
up horse shit.

Fyndium, in your case it sounds like you
have the genuine article. Not a bad
starting point. Is it coated with
paraffin ?

[Edited on 2020/10/25 by MadHatter]

Fyndium - 25-10-2020 at 13:37

I need to buy it first to find out what it contains. I found out that CAN is sold in two ways, either with calcium nitrate or with calcium carbonate. If the latter, the product will be easily processed into highly pure AN. I believe although it is the second one.

2-Chemical-composition-of-common-inorganic-fertilizers-or-constituents-of-fertilizer.png - 62kB

The NPK ratings tell only so much. Many compounds have nitrogen, even lots of it, but only limited few have it as nitrate. It is the MSDS that is of a much better reference, or if the ingredients are actually listed on the product by some means.

Btw, for being bored, I purchased a 2.5kg pack of garden fertilizer for 9€. The stuff looked just as horrible as any fertilizer - like it's dug from the corners of a piglet. MSDS stated it consisted of about 50-60% of KNO3, balance being some form of sulfate, and apparently urea phosphate - and red dye. Fancy that it had zero solid residue - the solution was clear, although very, very dark, burgundy-colored due to the dye. It looks like the same dye that is used for fuel oil.

I pre-washed quickly the batch with 0C cooled water with mixed ice, decanted most off and heated it to boil and added enough to dissolve all, and left for crystallize at 0C for overnight. I decanted the water, suction filtered the crystals dry, washed with just enough of 0C water, and then with little ethanol. Most of the color was gone, but I sort of like it how they look. I don't bother to recrystallize them second time, because I will feed them to sulfuric acid anyways. The yield? 980 grams, or about 78% based on MSDS. From 2.5kg, it's not good to be honest. I hate it how they just fill everything with either air, water, chaulk or something else unusable.

I found that the same stuff is sold under couple of other brands, and they state the KNO3 content between 35 to 65 percent, so I guess we're in the ballpark.

Well, this has nothing to do with ammonium nitrate, but boy, is the KNO3 pleasure to work with, compared to the mushy sludge of the AN. I was afraid when I saw the progress, but now I'm fascinated by the beauty of the crystals and the ease they formed - just dissolve it and wait, and you've got pretty much pure KNO3 at hand. I think 8-year olds get excited when they do their first recrystallizations, but I still find it one of the best things in chemistry.

[Edited on 25-10-2020 by Fyndium]

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