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Author: Subject: Making NH4NO3 from Inexpensive Household Ingredients
AJKOER
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[*] posted on 20-7-2011 at 16:38
Making NH4NO3 from Inexpensive Household Ingredients


Ingredients: Solder (Pb and Sn), Bleach (NaClO), Hydrogen Peroxide (H2O2), Vinegar (Acetic acid CH3-COOH) and Ammonium Hydroxide (NH4OH).

1. Press the Solder into thin sheets and let dissolve in a solution of Vinegar and H2O2. This makes Lead (and Tin) acetate.

Reference: "An aqueous solution of lead(II) acetate is the byproduct of the 50/50 mixture of hydrogen peroxide and white vinegar used in the cleaning and maintenance of stainless steel firearm suppressors (silencers) and compensators. The solution is agitated by the bubbling action of the hydrogen peroxide, and the main reaction is the dissolution of lead deposits within the suppressor by the acetic acid, which forms lead acetate."

http://en.wikipedia.org/wiki/Lead(II)_acetate

CAUTION: Lead (II) acetate can induce lead poisoning and being soluble constitutes an environmental hazard if not properly treated (use H2SO4 or NaHSO4 to form the insoluble Lead sulfate salt).


2. To create the PbO2 which will oxidize the ammonia, next add NaClO to precipitate the Lead (IV) oxide. Reference:

"The hypochlorite ion
Adding a solution containing lead ions, such as lead nitrate, to a hypochlorite solution produces a brown precipitate of lead(IV) oxide.

2ClO- (aq) + Pb+ (aq) → PbO2 (s) + 2Cl- (aq) "

http://en.wikibooks.org/wiki/Inorganic_Chemistry/Qualitative...


3. Add/wash with H2O2 to breakdown any remaining NaClO:

NaClO + H2O2 --> NaCl + O2 + H2O


4. Filter out the PbO2. Now one can safely add NH4OH to the PbO2 to slowly create HNO3 and NH4NO3. A previously quoted reference on this forum:

"Lead dioxide... oxidizes ammonia to nitric acid, with the simultaneous formation of ammonium nitrate. It oxidizes manganese salt (free from chlorine) in the presence of nitric acid to permanganate." Encyclopaedia Britannica. Eleventh Edition. Volume XVI. edited by Hugh Chisholm. p318 (year 1911)"

I would guess the very slow reaction to proceed as follows based on the general oxidation of NH3 by metallic oxide (MxO):

NH3 + MxO --> H2O + N (or on occasion NO) + M (or on occasion MN)

or, in our case, my speculation on the multi-step reaction:

2 NH3 + 2 H2O + 3 PbO2 --> 5 H2O + 2 NO + 2 Pb + PbO

with the further oxidation of NO to NO2 and the eventual formation of HNO3 and NH4NO3. Filter to remove any metallic lead and/or tin and insoluble oxides. I would avoid excess ammonia that might create ammonia complexes.

Comments and suggestions welcomed as I have not as of yet attempted this recipe.




[Edited on 21-7-2011 by AJKOER]
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[*] posted on 20-7-2011 at 19:04


Why would you use this process for making AN? It's available readily as instant cold packs (watch out for the ones with urea). Solder, vinegar, bleach, ammonia, and peroxide aren't cheap for the amount of ammonium nitrate you get, even if you recycle the lead. Lead salts are very dangerous, and working with them is definitely not worth obtaining ammonium nitrate.
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[*] posted on 20-7-2011 at 20:09


why not, bleach, ammonia, vinegar and peroxide are household items and it justs a synthesis and in some places AN is not as available where i live most of the cold packs have been replaced by Urea, BTW nice procedure AJKOER



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[*] posted on 20-7-2011 at 23:06


@barley81. it is not about the ease of chemical procurement. it is about the science! and really, if you are afraid of mercury and lead, two very common elements (not to mention a host of other dangerous, explosive, toxic, or otherwise hazardous chemicals) then by all means, do not use them. as for me, that's what safety gear is for. that's why secure procedures are developed.

also if this procedure produces HNO3 then double score!




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[*] posted on 20-7-2011 at 23:22


very well written up, but wont the tin ions interfere with any of these reactions? Such as with ClO? I'm not sure, thats why I ask. Give this procedure a try and let us know how it goes.



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[*] posted on 21-7-2011 at 02:26


This is not totally related but I thought it was interesting, and maybe some of you will too. ELECTROCHEMICAL PROCESS FOR THE PREPARATION OF NITROGEN FERTILIZERS: http://www.freepatentsonline.com/y2011/0120880.html
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[*] posted on 21-7-2011 at 04:12


On the economics, I agree except perhaps for a home chemists who has the time and most of ingredients already on hand. Also, scaling (both large and small) are positives for the suggested process for the home chemist.

I would like someone to comment on the possible electrochemical path to speed up the reaction. For example, note the similarity to the classic Lead-acid battery half cell reactions :

Anode: Pb(s) + SO4 2–(aq) --> PbSO4(s) + 2 e

Cathode: PbO2(s) + 4H+(aq) + SO4 2–(aq) + 2 e --> PbSO4(s) + 2H2O(l)

Overall reversible reaction:
Pb(s) + PbO2(s) + 4H+(aq) + 2SO4 2–(aq) <---> 2PbSO4(s) + 2H2O(l)

In our case (need help), we could have an alkaline cell (think of replacing H+ with NH4+, and also SO4 2- with OH- ) where the NH4OH electrolyte is consumed (decomposed into H2O and NO).
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[*] posted on 21-7-2011 at 05:02


This would be so much more interesting had actual experiments been reported here.

But few will be tempted to synth. something that's so readily available or can be synth. easily from other stuff.

[Edited on 21-7-2011 by blogfast25]
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AJKOER
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[*] posted on 21-7-2011 at 05:40


Thanks for the patent reference which is very relevant to my thoughts on a possible electrochemical modification to speed up the reaction.

Completely surprising to me is how quickly a possible electro-chemical oxidation modification of the century old recipe that is the starting point of this tread, leads to a potentially significant commercial application.

However, I am still short on precise equations and construction details.
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[*] posted on 21-7-2011 at 07:47


I'll give it a try because I have the stuff and want some experience. Here is what I did so far. Sorry for my earlier comment, discouragement, and nonproductivity.

~200mL of white vinegar were measured out and put into a 500mL Erlenmeyer flask, along with ~140mL of 3% H<sub>2</sub>O<sub>2</sub>. 10g of cut up 60/40 tin-lead solder with 2% rosin flux (a bit of 0.032", mostly 0.10" diameter) were added. The solder fizzed gently and the mixture became cloudy and foamed slightly. Half an hour or so later, there is a white powder on the bottom of the flask and the solder is discoloured and has a rough texture, still fizzing from peroxide decomposition. I think the powder may be hydrous tin (IV) oxide. If that's the case, then more peroxide may need to be added later.

Yes, I said I was afraid of using lead, but might as well go for it and be very safe.

[Edited on 21-7-2011 by barley81]
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[*] posted on 21-7-2011 at 08:00


Quote: Originally posted by hkparker  
very well written up, but wont the tin ions interfere with any of these reactions? Such as with ClO? I'm not sure, thats why I ask. Give this procedure a try and let us know how it goes.


Lead shot is often sold for the purpose of fishing weights. I do not know of the impurity levels though.

One can buy non-jacketed bullets ( for ammunition manufacture) in, I believe, stores like Cabelas and possibly Dicks sporting goods. These are usually somewhat lubricated though and would require cleaning.
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[*] posted on 21-7-2011 at 08:24


Quote: Originally posted by barley81  
I'll give it a try because I have the stuff and want some experience. Here is what I did so far. Sorry for my earlier comment, discouragement, and nonproductivity.

~200mL of white vinegar were measured out and put into a 500mL Erlenmeyer flask, along with ~140mL of 3% H<sub>2</sub>O<sub>2</sub>. 10g of cut up 60/40 tin-lead solder with 2% rosin flux (a bit of 0.032", mostly 0.10" diameter) were added. The solder fizzed gently and the mixture became cloudy and foamed slightly. Half an hour or so later, there is a white powder on the bottom of the flask and the solder is discoloured and has a rough texture, still fizzing from peroxide decomposition. I think the powder may be hydrous tin (IV) oxide. If that's the case, then more peroxide may need to be added later.

Yes, I said I was afraid of using lead, but might as well go for it and be very safe.

[Edited on 21-7-2011 by barley81]


I tried the same with lead shot used as fishing weights, and I have the same observations as you. I will let it go a little longer. I have another source of lead I will try later
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[*] posted on 21-7-2011 at 08:28


Now, on the Tin (Sn) alloy in the solder, upon treatment with fresh dilute NaClO, any SnO2 created (which is a colorless, diamagnetic solid) is known to be insoluble in aqueous acids and bases, so hopefully not an issue.

Failure to oxidize all Tin (II) oxide (which has two stable forms, blue-black and a metastable red form), however, may leave some amphoteric SnO that will dissolve in aqueous acids and bases. Also, the use of old bleach (meaning no longer highly alkaline which can promote the presence of free chlorine, which appears to be a function of pH) may result in the formation of Tin chloride as a product impurity as well.



[Edited on 21-7-2011 by AJKOER]
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[*] posted on 21-7-2011 at 11:04


For those performing the reaction and on the creation of PbO2 Step, here is an interesting reference that may be useful:

http://books.google.com/books?id=PjmQnVX4OmUC&dq=NH4OH+%...

The author notes that the precipitation of PbO2 proceeds seemingly as a standard chemical deposition (or CD defined by the author as a deposition of a film on a solid substrate from an in-solution reaction), but is more of an electroless deposition mechanism (which is akin to electrodeposition witness usually by metals except that the charge is generated internally by the redox reaction itself).

The author also notes for this different path for the creation of PbO2 the use of a small amount of AgNO3 as a catalyst and the influence of temperature and pH.
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[*] posted on 21-7-2011 at 11:30


Quote: Originally posted by AJKOER  
Failure to oxidize all Tin (II) oxide (which has two stable forms, blue-black and a metastable red form), however, may leave some amphoteric SnO that will dissolve in aqueous acids and bases.
[Edited on 21-7-2011 by AJKOER]


Both stannous (II) and stannic (IV) hydroxides are amphoteric.

barley81 is seeing probably Sn (IV) hydrated oxide precipitating, because the acetic acid (well, vinegar!) is too weak to keep the Sn (IV) in solution...
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[*] posted on 21-7-2011 at 11:31


Yes you'll easily get lead fishing weights for sea fishing, last time i went fishing they were 50 pence for a 5 oz one!
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[*] posted on 21-7-2011 at 11:58


Quote: Originally posted by sternman318  
One can buy non-jacketed bullets ( for ammunition manufacture) in, I believe, stores like Cabelas and possibly Dicks sporting goods. These are usually somewhat lubricated though and would require cleaning.
Lead for cast bullets is frequently alloyed with antimony to make it harder. Ditto for wheel weights. Lead for just its density, as with fishing weights, is less likely to have more-expensive-than-lead alloying agents added to it.
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[*] posted on 21-7-2011 at 13:11


Although NH4NO3 is generally easily available, I think it is important to have different routes available, as in the future some of the current sources may become unavailable in some locations.

NH4NO3 can also be prepared from KNO3 through fractional crystallization, as potassium sulfate is less soluble, the difference in solubility being more pronounced in hot water:

KNO3 + (NH4)2SO4 --> K2SO4 + (2)NH4SO4

Or alternatively, NaNO3 can be prepared from heating a solution of baking soda and NH4NO3 if the latter is more readily available:

NH4NO3 + NaCO3H --> NaNO3 + H2O + NH3(g) + CO2(g)


"Lead dioxide... oxidizes ammonia to nitric acid, with the simultaneous formation of ammonium nitrate. It oxidizes manganese salt (free from chlorine) in the presence of nitric acid to permanganate." Encyclopaedia Britannica. Eleventh Edition. Volume XVI. edited by Hugh Chisholm. p318 (year 1911)" [this quote actually first appeared in this forum in one of my posts]

Quote: Originally posted by AndersHoveland  

I do not know if lead dioxide which has been dissolved alkaline (forming the hydroxyplumbate ion, Pb(OH)6[-2] ) can oxidize ammonia, or ammonium hydroxide reacts with solid PbO2. The article is not clear about whether lead dioxide needs to be acidified to attack ammonia. While lead dioxide is an oxidizer even while alkaline, oxidizing Cr[+3] to CrO4[-2], the salt ammonium chromate does exist, so this does not imply that it would necessarily oxidize ammonia.


As I previously had stated, the source does not give much detail about the reaction. I do not know if the PbO2 needs to be either acidified or made alkaline to oxidize ammonia. One would expect that PbO2 would be a stronger oxidizer in acidic solution, but ammonia is more resistant to oxidation in acidic solutions, as the NH4[+] ion forms. Some experimentation is needed for this interesting reaction.

Lead(II) hydroxide does not dissolve in ammonia. Indeed, soluble Pb(NO3)2 s actually reacts with ammonia to precipitate out basic lead nitrate, Pb2O(NO3)2. (unlike lead, AgOH and zinc hydroxide do dissolve in aqueous ammonia) Thus I have doubts about the reaction taking place in alkaline solution. Perhaps the PbO2 could first be dissolved in NaOH to form the soluble Na2Pb(OH)6, then reacted with the ammonia.

Trying to balance a possible reaction for the oxidation under mildly acidic conditions:

(4)PbO2 + (8)NH4Cl --> (4)PbCl2 + NH4NO3 + (6)NH3 + H2O

Note that lead(II) chloride would be insoluble unless the solution contained excess ammonium chloride:
PbCl2 + (2)NH4Cl --> (2) (NH4)2PbCl4

I do not really know if lead(II) hydroxide would even dissolve in a solution of NH4Cl. The complexity of the reaction makes it difficult to write a reaction formula and predict what would happen, but I thought I would give it a try.

Also, H2O2 can oxidize ammonia to NH4NO3, but a catalyst such as an iron salt or acetamide is needed. Supposedly, if there is a great excess of ammonia, ammonium nitrite NH4NO2 can even be obtained.

[Edited on 21-7-2011 by AndersHoveland]




I'm not saying let's go kill all the stupid people...I'm just saying lets remove all the warning labels and let the problem sort itself out.
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AJKOER
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[*] posted on 21-7-2011 at 21:45


I believe I have an alternate explanation of the cloudy precipitate (which I am also currently observing) by my previously cited reference (link below). My Lead source is solder containing 62% Sn, 36% Pb and 2% Ag (I thought that the Silver impurity might prove beneficial given the author's comment on the catalyst effect of AgNO3). A possible explanation is the formation of a compound salt, specifically 6PbCO3.3Pb(OH)2.PbO, which the author has identified by XRD, formed by a reaction with CO2. The author cites air as the source of the Carbon dioxide, but I would include in our case any dissolved CO2 in the vinegar and H2O2 as well as it appears to immediately form.

http://books.google.com/books?id=PjmQnVX4OmUC&dq=NH4OH+%...


[Edited on 22-7-2011 by AJKOER]
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[*] posted on 22-7-2011 at 05:48


Quote: Originally posted by AJKOER  
I believe [snip] A possible explanation is the formation of a compound salt, specifically 6PbCO3.3Pb(OH)2.PbO, which the author has identified by XRD, formed by a reaction with CO2. The author cites air as the source of the Carbon dioxide, but I would include in our case any dissolved CO2 in the vinegar and H2O2 as well as it appears to immediately form.

http://books.google.com/books?id=PjmQnVX4OmUC&dq=NH4OH+%...


Where's the reference to that lead salt?

Its [the cloudiness] immediate appearance is proof of nothing: if the cloudiness is indeed caused by SnO2.nH2O (or whichever way one wants to write hydrated stannic oxide) then it too would form immediately, the equilibria being what they are.

For tin there really are only few decent solvents: conc. HCl in which it dissolves fairly slowly to SnCl2 and mixtures of HCl and HNO3 to which it dissolve very quickly to SnCl4. H2SO4 doesn’t attack it much, HNO3 on its own causes SnO2 to form.

The most likely explanation when using vinegar + H2O2 is that hydrated SnO2 is formed, which in weak acids is insoluble. Allow it to sediment off (it tends to peptise, so filtering isn’t a good option), that should give (a little!) lead acetate…

No matter how you look at it, this synth. is a slow boat to China, especially considering soluble lead salts (and thus also freshly prepared PbO2) are readily available. Messing with solder, vinegar and weak peroxide is tiresome and ineffective.


[Edited on 22-7-2011 by blogfast25]
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AJKOER
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[*] posted on 22-7-2011 at 09:56


blogfast25:

For the compound salt reference see page 260 of "Chemical solution deposition of semiconductor films" by Gary Hodes. Try this link:

http://books.google.com/books?id=PjmQnVX4OmUC&dq=NH4OH+%...

Now while it could be SnO2.xH2O (to be honest I am not sure), its white color in an aqueous solution may be an issue to some. I have two sources (one is the "Concise Encyclopedia Chemistry" by DeGruyter under Stannic acids, p. 1019 and the other link below is an observation in an experiment) describing Tin dioxide hydrate as a voluminous (or gelatinous) colorless precipitate. This is in contrast to the dry SnO2 salt which is either an amorphous (white) powder or a trigonal, hexagonal or rhombic crystal (clear?) per deGruyter also except for my () comments.

Reference:
http://books.google.com/books?id=7SMAAAAAMAAJ&pg=PA523&a...

Other than the color of this unidentified salt in the aqueous solution, it appears that Tin is fairly resistance to oxidation, so if H2O2 does oxidize Sn, why is it not the soluble SnO in vinegar variety? In other words, should not the chief product be Tin Acetate in accord with the Pb reaction?

I would also like to add another observation for confirmation. To the mixture of Solder + H2O2 + Vinegar that has formed some white powder at the bottom of a cloudy solution, add more Vinegar and shake. Does the white powder deposit and any white powder in suspension temporarily vanish, but the solution remains cloudy and there is an accompanying foaming noise, but no obvious gas generation?

[Edited on 22-7-2011 by AJKOER]

[Edited on 22-7-2011 by AJKOER]
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[*] posted on 22-7-2011 at 10:23


How voluminous a given hydrated oxide (or hydroxide) is, depends strongly on conditions of precipitation. I've precipitated 'SnO2' several times from Sn(IV) solutions and never found it to be very gelatinous at all. It also ages quickly and tends to peptise annoyingly. If you can make your stuff run through a filter after washing repeatedly with clean water it's almost certainly SnO2 in some form or other.

I also don't believe the conditions are conducive for the formation of a PbCO3 based salt: the concentrations of CO2 in an acid solution are far too low, IMHO. People manipulating PbAc<sub>2</sub> don't report problems with CO2 getting to it, AFAIK.

Make your life easier and start from fairly pure lead or a fairly pure lead (II) salt. Using solder just adds variables to an already not so simple proposition...
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[*] posted on 22-7-2011 at 17:28


I have found a quite good 2004 thread on this very forum discussing the preparation of PbO2.

http://www.sciencemadness.org/talk/viewthread.php?action=pri...

Some of my observations: The hypochlorite method for the creation of PbO2 is recommended. However, there is an added step, the Lead Acetate is treated with "your favorite hydroxide" to form Pb(OH)2 to which NaClO or Ca(OCl)2 is added to create the PbO2.

SAFETY WARNING: PbO2 and H2O2 are, per the cited MSDS, INCOMPATIBLE. I will guess a very violent decomposition reaction. So please DO NOT perform this part of the recipe to remove excess NaClO (since we were going to add NH4OH which is incompatible with NaClO) until further notice to avoid injury.
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[*] posted on 23-7-2011 at 08:33


That's the 'standard' method for preparing PbO2, nothing special (oxidise a Pb (II) compound in alkaline conditions). Simples.

Re the chemical incompatibilities, PbO2 is a strong oxidiser, thus ‘incompatible’ with many oxidisable substances. But as chemists we exploit those incompatibilities. Perhaps with very strong or pure H2O2 you’d get a violent reaction, but not with commercially dilute hydrogen peroxide.
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[*] posted on 23-7-2011 at 18:44


I agree with your assessment, but express caution as I have seen the YouTube video made by reacting 30% H2O2 + FeCl3 (it was a surprisingly strong explosion). Someone possessing 30% H2O2 may use it here in place of the dilute commercial variety with possibly injurious consequences.

As an example of what could happen in a closed reaction vessel see:

http://www.youtube.com/watch?v=L5M9saSuSIA&feature=relat...

And for H2O2 + MnO2 in an open test tube see:

http://www.youtube.com/watch?v=Xkv1v7pee7E&feature=relat...

I would assume similar results with 30% H2O2 + PbO2, hence the warning.

On another note, more on Pb(OH)2 interesting properties, to quote:

"Lead(II) hydroxide, Pb(OH)2, is a hydroxide of lead, with lead in oxidation state +2. Although it appears a fundamentally simple compound, it is doubtful if lead hydroxide is stable as a solid phase.[2] Lead basic carbonate (PbCO3·2Pb(OH)2) or lead(II) oxide (PbO) is encountered in practice where lead hydroxide is expected. This has been a subject of considerable confusion in the past."

Also, "When an alkali hydroxide is added to a solution of a lead(II) salt, then a hydrated lead oxide PbO·xH2O (with x < 1) is obtained. Careful hydrolysis of lead(II) acetate solution yields a crystalline product with a formula 6PbO·2H2O = Pb6O4(OH)4."

Source:
http://en.wikipedia.org/wiki/Lead_hydroxide




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