Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
 Pages:  1  2  
Author: Subject: Ammonium permanganate preparation
Axt
International Hazard
*****




Posts: 778
Registered: 28-1-2003
Member Is Offline

Mood: No Mood

[*] posted on 25-10-2004 at 17:31


It says 7.9 @ 15°C in CRC. One of them has it wrong.

0.8's a typo I reckon! If that were the case you wouldnt need an excess of AN, as it would precip immediately.

[Edited on 26-10-2004 by Axt]
View user's profile Visit user's homepage View All Posts By User
The_Davster
A pnictogen
*******




Posts: 2861
Registered: 18-11-2003
Member Is Offline

Mood: .

[*] posted on 25-10-2004 at 18:27


I had a go at ammonium permanganate yesterday. I used Axt's procedure except 10x less.
Everything was the same as in Axt's procedure untill the cooling step. I was on this site, lost track of time and when I went to the freezer to check on the cooling of the beaker it was a slurry as some of the water had begun to freeze. I poured/scraped this slurry into the filter paper and let it sit there melting. Soon I received a nice ammount of purple crystals. I ended up leaving the filtration for a day accidently because I was busy with other things. I come back to it today, everything has dried out, and the bottom of the filter paper is incredibly brittle and darkened. This ended up contaminating the product sugnificantly.

The low VoD Axt mentioned is obvious, even the combustion of the product seems quite...unenergetic




View user's profile View All Posts By User
Axt
International Hazard
*****




Posts: 778
Registered: 28-1-2003
Member Is Offline

Mood: No Mood

[*] posted on 28-10-2004 at 13:54


What did the crystals look like, If you went as far to freeze it I think it less then pure. While it isn't terribly interesting it should at least pop into a cloud of MnO2.

You really want to get it as it first starts to precipitate, which isnt easy since you cant see into the dark purple solution.
View user's profile Visit user's homepage View All Posts By User
The_Davster
A pnictogen
*******




Posts: 2861
Registered: 18-11-2003
Member Is Offline

Mood: .

[*] posted on 28-10-2004 at 16:32


The crystals are a very dark purple, however not as dark as potassium permanganate. The ammonium permanganate is in the form of a very fine powder with no discernable crystal shape and some longer crystals. About a 2:1 ratio of powder:crystals.
I get the cloud of MnO2 upon ignition and after ignition there is no unflamable residue other than the manganese dioxide. However the combustion does spread some unburned ammonium permanganate over a smal area, I know that this is ammonium permanganate and not some potassium permanganate impurities because they still are flamable.

I forgot to mention earlier, but after filtering but before letting the crystals sit in the damp filter for days, I did wash the crystalls with a small ammount of water just above freezing. This would have removed any ammonium nitrate impurities and hopefully some potassium permanganate impurities( I know I would have lost some ammonium permanganate this way).




View user's profile View All Posts By User
mark
Harmless
*




Posts: 25
Registered: 23-10-2004
Member Is Offline

Mood: No Mood

[*] posted on 29-10-2004 at 17:59


I have just prepared what I think is NH4MnO4, I used Axt Procedure accept 10x less and Ammonium sulphate instead Ammonium nitrate. I boiled some water and added to the beaker with KmnO4 in it at 90 degrees I added the ammonium sulphate. At 50 degrees I realised I didn’t do the pouring step. Which I then did, I chilled down the mixture and filtered it this is now drying. I also filtered the undissolved stuff and it’s all drying now. I’ll tell you later if it works or not.

Edit

Also is NH4MnO4 soulable in acetone?

[Edited on 30-10-2004 by mark]
View user's profile View All Posts By User
mark
Harmless
*




Posts: 25
Registered: 23-10-2004
Member Is Offline

Mood: No Mood

[*] posted on 30-10-2004 at 18:29


I made another batch yesterday as well using the proper method with pouring. I poured it into the beaker when it was at 70 degrees. After drying it the burn tests using a propane torch failed miserably. It only decomposed and now explosion or flame or anything was seen. It seems NH4NO3 is the best way to go.
View user's profile View All Posts By User
Blackout
Harmless
*




Posts: 25
Registered: 26-11-2004
Location: Canada
Member Is Offline

Mood: No Mood

[*] posted on 6-1-2005 at 16:08
KMnO4


Sorry to bring back an old post but...

2 MnSO4 + 5 PbO2 + 3 H2SO4 => 2 HMnO4 + 5 PbSO4 + 2 H2O

Then:
HMnO4 + KCl => KMnO4 + HCl

Could it be possible?




\"Si vis pacem, para bellum.\"
\"If you wish for peace, prepare for war.\"
View user's profile View All Posts By User
mark
Harmless
*




Posts: 25
Registered: 23-10-2004
Member Is Offline

Mood: No Mood

[*] posted on 6-1-2005 at 17:37


KMnO4 reacts with HCl to give chlorine.
View user's profile View All Posts By User
K9
Harmless
*




Posts: 21
Registered: 28-10-2003
Member Is Offline

Mood: No Mood

[*] posted on 15-2-2005 at 08:31


Sorry to dig up an old thread for the second time, but I just made some and after drying for one day the powder/crystals are quite dark. The drying product also caused the filter paper to start disintegrating. My question is just how long should it be before it's completely dry. I did a little burn test last night and it crackled as it burned and I assume this is from retaining moisture.

EDIT: Ok scratch that, it's dried out. Goes up quickly with a little puff.

[Edited on 15-2-2005 by K9]
View user's profile View All Posts By User This user has MSN Messenger
chemoleo
Biochemicus Energeticus
*****




Posts: 3005
Registered: 23-7-2003
Location: England Germany
Member Is Offline

Mood: crystalline

[*] posted on 15-2-2005 at 18:58


It might be a good idea to rinse the crystalline material on the filter paper with cold ethanol or acetone (more the latter as it is oxidised), which can be dried faster than with water. However, test it with a small amount first, you may know about the experiment of KMnO4 and glycerin which spontaneously ignites, ethanol is an alcohol too.
Although - my personal guess would be that there won't be a problem as long as it is cold.
But try it first, under supervision.

To make things more interesting- I wonder how permanganates of i.e. formaloxime (H2C=NOH)/methylamine/ethylenediamine will fare. If we assume a final product of Mn2O3, it would mean that per MnO4 moiety, 2.5 oxygens are available for oxidation. With ammonium permanganate, there'd be a slight excess of oxygen. Maybe it could be used to produce a more energetic amine salt.




Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
View user's profile View All Posts By User
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
*****




Posts: 1986
Registered: 2-3-2011
Member Is Offline

Mood: No Mood

[*] posted on 20-12-2011 at 20:42
Ammonium Permanganate


http://www.youtube.com/watch?v=Bh-maHh0nvU

(NH4)2MnO4 explodes with a copious cloud of dark brownish-purple smoke. The substance is sensitive to friction, and very easily is set off by flame.

It is not entirely chemically stable, and slowly degrades. It can be stored for about 4 months.

The permanganate ion is much more reactive oxidizer than perchlorate, which is why this salt is so sensitive and chemically unstable.

Like ammonium perchlorate, ammonium permanganate is another ammonium salt that is not very soluble (most ammonium salts are very soluble). Unfortunately, potassium permanganate is not very soluble either, so this is not advantageous for making it.


Preparation 1 (the below has not been tested)

Sodium permanganate can be made by dissolving a manganese compound, such as MnCl2 or MnO2 (but do not use potassium permanganate for this procedure), in bleach. The reaction turns purple. Add extra manganese compound to be sure that all the bleach has reacted. After thorough mixing for 30 minutes, a test is to add a little piece of manganese dioxide, which then should not dissolve, indicating all the hypochlorite in the bleach has been reacted.

Separately, mix a small quantity of ammonium sulfate (or ammonium nitrate or ammonium chloride), but only add a small quantity, with some ammonia. Too much ammonium sulfate will make the reaction acidic, which is bad since that will make the permanganate oxidize the ammonia. If you have a pH strip, the ammonia mixture with the ammonium sulfate should be preferably neutral, or slightly basic. Be sure all the ammonium sulfate is dissolved in the ammonia, some extra water might be added to help dissolve it.

Add the second mixture to the first, then lower the temperature to 10degC until purple crystals appear. Use a spoon to scoop out the crystals, then flter out the crystals using coffee filter paper, washing with with a little water. The crystals are ammonium permanganate. Note that no potassium compound can be used in the above preparation, since the potassium permanganate would then solidify out.

If there is trouble crystallizing out the ammonium permanganate, some ammonia (the concentrated type) can be added to the solution, which should help because of the "common ion effect". The solution should not be cooled too long, otherwise sodium sulfate (salt) will begin to solidify out with the ammonium permanganate. Actually, ammonium chloride or ammonium nitrate are better than ammonium sulfate to use in this procedure, because the sodium sulfate is less soluble than sodium chloride.


Preparation 2 (has been tested)

20 grams of potassium permanganate is dissolved into 200ml of boiling water, to this mix is added 250g of ammonium nitrate and allowed to dissolve. The solution is poured off into another beaker to leave any undissolved or decomposed products in the bottom. Chill the solution to 10°C to precipitate the NH4MnO4, the solution can be poured off to retrieve the reddish-purple crystals. Place the product onto absorbent paper and leave to dry at room temperature. Excess ammonium nitrate must be used, otherwise it is difficult to preferentially precipitate out only the ammonium permanganate, since it is not much less soluble than potassium permanganate.


For preparing solutions of permanganic acid:

2 MnSO4 + 5 PbO2 + 3 H2SO4 => 2 HMnO4 + 5 PbSO4 + 2 H2O

The reaction is slow. The lead sulfate solidifies out, then is removed. To the remaining solution, add baking soda to make more alkaline (otherwise HMnO4 is a reactive oxidizer), then add the ammonia. The sodium ions are not as problematic as potassium ions, since the sodium permanganate is much more soluble.

Aqueous solutions of permanganic acid partially decompose when heated to 40degC, and completely decompose if boiled. The solutions slowly degrade at room temperature, especially above 20degC. The decomposition products are hydrated MnO2 and oxygen gas. If the water is allowed to evaporate out, the oxygen that forms from decomposition contains traces of ozone, giving it a distinct odor. The solutions slowly oxidize elemental sulfur after a few days to dilute sulfuric acid.


Alternatively, ammonium sulfate to the barium permanganate would work, the barium sulfate would solidify out and could be separated out, but use plenty of water, since the ammonium permanganate is not very soluble either. the solution will then contain ammonium permanganate, and the water could be evaporated out in a warm dark place. After some evaporation, lowing temperature will help crystallize out product.

Unfortunately, potassium ferrate K2FeO4, oxidizes ammonia, so ammonium ferrate is not possible.
View user's profile Visit user's homepage View All Posts By User
Berrilium
Harmless
*




Posts: 46
Registered: 31-3-2012
Member Is Offline

Mood: No Mood

[*] posted on 31-3-2012 at 10:18
Toxicity of Ammonium Permanganate


I couldn't find any info as to the toxicity of ammonium permanganate, i would think that it isn't toxic at all.

Also, what about TATP?
View user's profile View All Posts By User
neptunium
International Hazard
*****




Posts: 974
Registered: 12-12-2011
Location: between Uranium and Plutonium
Member Is Offline


[*] posted on 31-3-2012 at 10:26


its probably because it is way too unstable to even be consider for a toxicity study...



View user's profile Visit user's homepage View All Posts By User
woelen
Super Administrator
*********




Posts: 7723
Registered: 20-8-2005
Location: Netherlands
Member Is Offline

Mood: interested

[*] posted on 31-3-2012 at 10:27


Ammonium permanganate is not especially toxic, not more than the well-known potassium permanganate. But ammonium permanganate is very unstable. How would you want to make this compound? It certainly is not available commercially. The only route I can imagine is through the insanely dangerous Mn2O7.

TATP also is not especially toxic, but it is equally dangerous and even can explode by looking angry at it.

I would say to you: Stay away from these typical K3WL chemicals if you value your limbs.




The art of wondering makes life worth living...
Want to wonder? Look at https://woelen.homescience.net
View user's profile Visit user's homepage View All Posts By User
Vikascoder
National Hazard
****




Posts: 309
Registered: 28-1-2012
Member Is Offline

Mood: No Mood

[*] posted on 31-3-2012 at 10:35


en.m.wikipedia.org/wiki/Ammonium_permanganate ammonium permanganate is not toxic according to wikipedia are you thinking to detonate with TATP
View user's profile View All Posts By User
barley81
National Hazard
****




Posts: 481
Registered: 9-5-2011
Member Is Offline

Mood: No Mood

[*] posted on 31-3-2012 at 11:18


Toxicity of potassium permanganate:
http://members.tripod.com/~Prof_Anil_Aggrawal/poiso024.html

It is the permanganate ion that is toxic, not potassium. Ammonium is not toxic either (salmiakki is licorice containing ammonium chloride in amounts up to 8%) If ammonium permanganate indeed is stable, it will be roughly as toxic as potassium permanganate.
View user's profile View All Posts By User
Berrilium
Harmless
*




Posts: 46
Registered: 31-3-2012
Member Is Offline

Mood: No Mood

[*] posted on 31-3-2012 at 13:51


To answer questions, no I don't intend to use TATP to detonate anything at the moment as it is just not something I would even think of. But I was just wondering as I have made both NH4MnO4 and TATP and was wondering about the dangers that aren't of thought of

As for synthesis of the ammonium permanganate I make it by preparing a saturated solution of ammonium nitrate and water (this is all together 100ml) as I am using fertilizer grade I filter it a few times and then heat it until boiling point and add 6 grams pottasium permanganate. Stir and cool. Works for me. :)

View user's profile View All Posts By User
Vikascoder
National Hazard
****




Posts: 309
Registered: 28-1-2012
Member Is Offline

Mood: No Mood

[*] posted on 31-3-2012 at 19:39


Is ammonium permanganate is sensitive to TATP . Can TATP alone detonate ammonium permanganate
View user's profile View All Posts By User
AndersHoveland
Hazard to Other Members, due to repeated speculation and posting of untested highly dangerous procedures!
*****




Posts: 1986
Registered: 2-3-2011
Member Is Offline

Mood: No Mood

[*] posted on 31-3-2012 at 20:31


Ammonium permanganate is considered a fairly sensitive explosive. It can detonate from open flame.
View user's profile Visit user's homepage View All Posts By User
Vikascoder
National Hazard
****




Posts: 309
Registered: 28-1-2012
Member Is Offline

Mood: No Mood

[*] posted on 1-4-2012 at 00:17


Then it is going to be a nice time now i will try to use it as a booster charge 0.5 gm of mercury fulminate or 0.5 gm of hmtd i will use to detonate ammonium permanganate then if possible try to detonate any other thing.
View user's profile View All Posts By User
Berrilium
Harmless
*




Posts: 46
Registered: 31-3-2012
Member Is Offline

Mood: No Mood

[*] posted on 1-4-2012 at 02:45
Ammonium Permanganate


I have found that ammonium permanganate is way more stable than people say, I'm not sure if this is due to dampness/impurities but i stried to make a small charge using ammonium permanganate as my primary, it was suppose to be ignited by a christmas light and then detonate.

It did not work, i then proceeded to shoot it with an air rifle to dry dispose of it, it didnt detonate. I poured out the contents and hit it with a hammer. Only then did it detonate... When i burn it it barely burns... all in all it is pretty useless explosive/oxidizer
View user's profile View All Posts By User
Vikascoder
National Hazard
****




Posts: 309
Registered: 28-1-2012
Member Is Offline

Mood: No Mood

[*] posted on 1-4-2012 at 05:04


in your previous post you have mentioned that you have TATP . try detonating ammonium permanganate withTATP and post your results. it is so easy to make so its potential of using it as booster can be developed if it works.
View user's profile View All Posts By User
Adas
International Hazard
*****




Posts: 711
Registered: 21-9-2011
Location: Slovakia
Member Is Offline

Mood: Sensitive to shock and friction

[*] posted on 1-4-2012 at 11:34


It is very unstable and decomposes. I have made it once and before it dried, most of it decomposed to some crap.



Rest In Pieces!
View user's profile Visit user's homepage View All Posts By User
Vikascoder
National Hazard
****




Posts: 309
Registered: 28-1-2012
Member Is Offline

Mood: No Mood

[*] posted on 4-4-2012 at 00:31


I am thinking to make ammonium permanganate by dissolving diammonium phosphate in water then adding potassium permanganate . Since the solubelity of dipotassium phosphate is very high and of ammonium permanganate is very low it can be easily filtered of. Will this process work
View user's profile View All Posts By User
Vikascoder
National Hazard
****




Posts: 309
Registered: 28-1-2012
Member Is Offline

Mood: No Mood

[*] posted on 4-4-2012 at 19:17
A new method for ammonium permanganate


Hello friends in my country diammonium phosphate is easily available so i thought to prepare ammonium permanganate from it and potassium permanganate . The method is to make saturated solution of diammonium phosphate then add KMnO4 until no more precipitate form . Since the solubelity of di potassium phosphate is very i high as i read on wiki pedia so it will stay in solution and ammonium permanganate can be filtered off easily.
View user's profile View All Posts By User
 Pages:  1  2  

  Go To Top