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menchaca
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[*] posted on 13-3-2003 at 05:12
lead nitrate synthesis


well im not sure if it works because i have never try it but maibe it works... i need your help to know if this can work or if doesen´t.
All you will need is:

a piece of lead
sulphur
hidrochloric acid
sodium or potasium nitrate
sodium hidroxide
NaHSO4(i dont know how does it write in english)

well reaction is quite simple i thing:

Pb+S --> PbS

PbS + 2HCl --> PbCl2 +H2S(gas.)

PbCl2 + 2NaOH --> NaCl + Pb(OH)2 with precipitates

Pb(OH)2 + 2NaOH --> Na2PbO2 + 2H2O


Edit by chemoleo: changed terrible spelling.

[Edited on 28-3-2005 by chemoleo]
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[*] posted on 14-3-2003 at 12:26


Pb+S --> PbS

Melted lead + slow addition of sulfur under absence of air? - i never tried that...
PbS is identical with the natural mineral "lead glance" also called "galena"

PbS + 2HCl --> PbCl2 +H2S(gas.)

This works!-H2S is highly toxic!!!-Beware.

PbCl2 + 2NaOH --> NaCl + Pb(OH)2

Lead chloride is insoluble in cold water, but soluble in hot water.
I think the pricipitation of Pb(OH)2 is also possible with Na2CO3(Pb(OH)2 has a lower solubility than PbCO3, which would have the advantage not to redissolve lead by taking too much NaOH...).

Pb(OH)2 + 2NaOH --> Na2PbO2 + 2H2O

This also works, you can redissolve precipitated Pb(OH)2 with excess NaOH.....but what do you intend with that??

[Edited on 15-3-2003 by BASF]




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[*] posted on 14-3-2003 at 13:00


What about that(i have tried that already:) ):

Lead metal + NaHSO4 + KNO3 + gentle heating and evolution of NOx.

Use a wide glass container.
The result is a mix of KNaSO4, Pb(NO3)2 and eventually rests of the reactants.

It is difficult to seperate the lead nitrate form the alkali sulfates, but maybe multiple recrystallization can do it.

Another idea i had would be to precipitate the sulfate with CaCl2 with better chances to seperate the salt-mix then, because NaCl forms and this has a constant solubility at all temperatures, as opposed to Na2SO4, for example.


P.S.:
Keep in mind that Pb(NO3)2 is a mutagenic substance, don´t touch with fingers as it can be absorbed through the skin!




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[*] posted on 27-3-2005 at 18:17


This is a rather old topic, but since it pertains to the subject at hand (sort of)...

Can't one produce lead nitrate like this?

CuSO4 + 2NaOH -> Na2SO4 + Cu(OH)2 [One product is soluble, the other is not. Fairly pure Cu(OH)2 can be had]

Cu(OH)2 + 2NH4NO3 -> Cu(NO3)2 + NH3 [One product is a gas. Fairly pure Cu(NO3)2 is formed]

Cu(NO3)2 + Pb -> Pb(NO3)2 + Cu [It works with copper acetate, so should for the nitrate as well, no?]

With lead, ammonium nitrate, copper sulfate, and sodium hydroxide being availible OTC in root killer, fishing sinkers, drain opener,and cold packs (Obviously not in that order), that seems to be the easiest route to lead nitrate, even if it's not the fastest.

[Edited on 28-3-2005 by LUEshi is my god]




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[*] posted on 28-3-2005 at 01:22


hmm..another method posted before is this:
mix lead(II) carbonate with ammonium nitrate and heat. lead(II) nitrate should be formed as well as ammonia(escapes) and carbon dioxide(escapes).




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[*] posted on 28-3-2005 at 04:03


Cut lead in small chunks, or grind it to coarse powder, and add 30% HNO3... heat and stir for a few hours, untill most of the lead is dissolved. Decant the liquid (is very easy due to the high desity of lead), and evaporate until dryness. Redissolve in dH2O, and evaporate again, to remove the rest of the acid.



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[*] posted on 6-4-2005 at 04:24


Can I make lead nitrate from 60%HNO3 + Lead metal by elecrtolysis (lead is anode).
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[*] posted on 6-4-2005 at 07:50


You don't need electrolysis, simply place the metal in the acid. Dilute the acid a bit, at least add 1/4 it's volume of distilled water. Add an excess of Pb filings and decant when effervescence stops. The soln contains lead (II) nitrate. Evaporate off the water till crystallization occurs, viola.

Edit: For Christ's sake, look at the post above yours next time!!! This doesn't even need the use of a search engine man!

[Edited on 6-4-2005 by Esplosivo]




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[*] posted on 6-4-2005 at 17:13


Assuming an excess of nitric acid was used, would the remaining liquid still evaporate? I once tried to make copper sulfate by dissolving a copper penny in dilute H2SO4 + H2O2. The liquid would never evaporate to give me the copper sulfate. I ended up having to neutralize it with a base, wash the copper hydroxide, and then carefully add just enough H2SO4 to again dissolve the copper hydroxide again. Does this problem not occur when using nitric acid to make nitrates? What about when making chlorides with HCl?
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[*] posted on 6-4-2005 at 17:43


It sounds to me that you had extra sulfuric acid present. It being a nonvolatile acid, it wouldn't have evaporated easily. Nitric and hydrochloric acids, however, are volatile, so you shouldn't get this problem.
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thumbup.gif posted on 7-4-2005 at 09:40


Dropping pieces of lead into molten ammonium nitrate should work, first lead is oxidized by the nitrate ion to PbO, then the nitrite reacts to nitrogen and water with the ammonium, then the ammonium reacts with PbO to produce lead nitrate, ammonia gas and water vapour. Or, if you're paranoid about AN sensitizing due ta lead nitrate, add AN bit by bit into molten lead nitrate.



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[*] posted on 16-4-2005 at 14:25


I just finished making some lead nitrate from lead metal and HNO3. I used 2.1g of Pb metal and 70% HNO3 diluted about 1:1 with water. After letting the liquid evaporate (took several times longer than water would to evaporate), I ended up with a bunch of small square crystals that look almost exactly like table salt. The yield was 3.2g (theoretical is 3.35).

A couple of notes. It took a long time for the lead metal to dissolve in the HNO3. I found it helped quite a bit to immerse the test tube I used for the reaction in hot water. Quite a bit of gas (NO and NO2) is evolved - the lead bubbles vigorously for a long time. I put a wet paper towel over the test tube and this did a very good job of getting rid of the fumes. In fact, I didn't smell anything until I took away the paper towel. The paper towel did become saturated with HNO3 though, and turned my fingers yellow where I picked it up.

It took a couple of hours for the Pb metal to dissolve completely (even with the hot water) and a couple weeks for the remaining HNO3 to evaporate.

I tested my Pb(NO3)2 by making a couple drops of solution of it in water on a paper towel and verified that the wet part of the paper towel turned black when I exposed it to H2S.
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[*] posted on 17-4-2005 at 07:52
Hey there


Most of the proceedures discussed here seem workable but I have a much safer and easier method in mind. Espeically if you have lead that has antimony alloyed with it it may not want to dissolve in HNO3 too well. Mixed glacial acetic acid with 30% H202 and you will have lead acetate in solution. Take this and precipitate lead carbonate then add dilute HNO3 until gas evolution stops. No hot concetrated acids or deadl NOx fumes here. Not to mention the insidious H2S formed from handling sulfides with acid.

[Edited on 4/17/2005 by chloric1]




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[*] posted on 18-4-2005 at 22:16


Well, that's good if one can obtain glacial acetic acid...

Is boiling off the liquid instead of slowly evaporating a problem in the HNO3 method?

[Edited on 19-4-2005 by Quince]




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[*] posted on 2-5-2005 at 13:23


hey, look here:
Pb3O4 + 4 HNO3 ---> 2 Pb(NO3)2 + PbO2 + 2 H2O

Pb3O4 is a brown-red powder that can be found in paint store as an anti-rust for iron enclose
HNO3, well...




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[*] posted on 2-5-2005 at 17:21


The way I see it, if you got nitric just use plain lead metal and let the hydrogen rip... why pay someone for oxides.

Tim
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[*] posted on 2-5-2005 at 18:12


the precipited PbO2 can be filtred out and reacted with conc. H2SO4 and MnSO4 to form HMnO4 then precipitate out KMnO4 by the addition of a conc. solution of KCl to the diluted acid...



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[*] posted on 2-5-2005 at 18:46


Quote:
Originally posted by 12AX7
The way I see it, if you got nitric just use plain lead metal and let the hydrogen rip... why pay someone for oxides.


Nitric acid + lead gives you water, lead nitrate, and NOx, not lead nitrate and hydrogen. You’d be loosing a good deal of your acid as nitrogen oxides here.
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[*] posted on 2-5-2005 at 21:01


Right, it hates people and gives NO2 with less reactive metals...

Tim
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[*] posted on 30-5-2005 at 11:57


Another cheap way of making it would be by making an separated cell (saltbridge) and electrolyse with KNO<sub>3</sub>/NaNO<sub>3</sub>. Use Pb as anode, cathode can be made of any resistant material. The same works for making AgNO3. Think I read this in another thread.

But now I have a question. With nitric acid I believe the redox works like this:

The nitrate ion is reduced:

NO<sub>3</sub><sup>-</sup> + 2H<sup>+</sup> + e<sup>-</sup> ---> NO<sub>2</sub> + H<sub>2</sub>O

Or with lower pH:

NO<sub>3</sub><sup>-</sup> + 4H<sup>+</sup> + 3e<sup>-</sup> ---> NO + 2H<sub>2</sub>O

And lead being oxidized:

Pb ---> Pb<sup>2+</sup> + 2e<sup>-</sup>

I believe it goes like that, but what I can't figure out is how it looks in the cell. What do the anode reaction look like? Will NO<sub>x</sub>-gases form then aswell?
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[*] posted on 30-5-2005 at 14:05


Nitric in both half-cells?

[Edited on 30-5-2005 by Quince]




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[*] posted on 31-5-2005 at 11:29


How about simply mixing aquaeus solutions of CuSO<sub>4</sub> and Ca(NO<sub>3</sub>;)<sub>2</sub> which would precipate CaSO<sub>4</sub> (gypsum) and leave Cu(NO<sub>3</sub>;)<sub>2</sub> in solution, the latter easily converted to lead nitrate by metallic lead added to soln (PbO might work too).

Ca(NO<sub>3</sub>;)<sub>2</sub> is found naturally occuring in 10kg bags in garden shops, "chalk salpetre".




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[*] posted on 31-5-2005 at 12:07


Yes, it can be done that way. The CaSO4 has a low solubility in water, so I guess it can be filtered out quite easily.

Lol I liked this:
Quote:

Ca(NO3)2 is found naturally occuring in 10kg bags in garden shops, "chalk salpetre".




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[*] posted on 31-5-2005 at 13:07


No, I can assure you that will not work. The CaSO<sub>4</sub> precipitate is extremely difficult to filter out, if not impossible. More than one person on this board has tried something like this and utterly failed. It’s like trying to filter the water out of mud, IIRC.
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[*] posted on 31-5-2005 at 13:14


Errr.... neutrino, I wrote a big post(s) about this once, and I can personally vouch for it that it works VERY nicely.
Unless you think making more than 1 kg of lead acetate from calcium acetate, CuSO4 and lead metal is a failure :o

Anyway, using calcium nitrate instead of the acetate works of course too. Just be patient when filtering, and best is to mix the nitrate with the copper sulphate, and pour this onto a coffee filter. Compress the CaSO4 now and then, using a spoon. Once everything is filtered, you can wash it with H2O to extract more of the Cu nitrate. You won't get the CaSO4 completely white however, as I believe some mixed crystals are formed. Regardless this procedure works very well, the only true patience that is required is to react the Cu(NO3)2 with the Pb.

Once the reaction is done, the solution is completely clear. It might take a couple of weeks or longer depending on the surface area of the lead/stirring/temp etc.

Then you could evaporate the solution to isolate the leadnitrate by crystallisation, add Ethanol, or whatever suits you.

[Edited on 31-5-2005 by chemoleo]




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