The lead salts preparation thread!

Quote: Originally posted by annaandherdad

TurboZ, if you make lead nitrate with lead and HNO3, you can get rid of the excess acid by evaporating it in a plastic desiccator with NaOH as the desiccating agent. Using the carbonate works well, too.

Quote: Originally posted by TurboZfreak

Quote: Originally posted by annaandherdad   TurboZ, if you make lead nitrate with lead and HNO3, you can get rid of the excess acid by evaporating it in a plastic desiccator with NaOH as the desiccating agent. Using the carbonate works well, too. But as stated before, wouldn't that leave impurities in the lead nitrate?

Quote: Originally posted by Hennig Brand

A while back I too took lead dioxide from an old car battery, but I didn't try and react the lead dioxide with acetic acid and I am not sure that it would even work. I made sure the lead dioxide was well rinsed of sulfuric acid then I put it in an old steel soup can with a loose fitting steel cover. I then put the steel can on/in a bed of hardwood coals in my wood stove and opened the draft to let more air/oxygen in and make the coals hotter. The soup can was held at bright red/orange (ca. 650-800C) for 10-15 minutes or so at which point the can was removed and cooled. The lead dioxide was nearly all converted to yellow lead monoxide. Yellow lead monoxide can be easily converted to lead acetate or nitrate with the corresponding acid. I know you said that you don't have nitric acid, but you must be able to get or make at least low concentrated nitric acid. Even 10% nitric acid can be used, it just means removing more water to concentrate the lead nitrate solution later on. Add an excess of yellow lead monoxide to fairly warm or hot nitric acid and then filter out what does not dissolve before concentrating the lead nitrate solution. There are a few more details, but that should get you started.

I had a few pictures saved from last year that I never posted that I thought I should post here. There are pictures from a couple of different batches. The attached instructional pdf was taken from here:

http://www.musketeer.ch/blackpowder/homemade%20lead%20acetat...




Attachment: Homemade Yellow Lead Oxide & Lead Acetate.pdf (358kB)
This file has been downloaded 1160 times


[Edited on 8-3-2015 by Hennig Brand]

Here's a sample of Ammonium chloroplumbate I recently had a go at making. The procedure :-
1. Dissolve lead in acetic acid/hydrogen peroxide (Nitric acid is impossible to get now).
2. Boil down and crystallise. Dissolve the crystals in water for the Lead dioxide preparation.
3. Add excess sodium hydroxide and sodium hypochlorite to hot lead acetate solution. Mix well.
4. Filter off the precipitated Lead dioxide.
5. Add to ice cold concentrated hydrochloric acid. A yellow solution is produced (Plumbichloric acid).
6. Add saturated Ammonium chloride to precipitate out the chloroplumbate.
7. Wash with a little COLD water and dry.
Obviously wear gloves and dispose of any waste appropriately as lead is a cumulative poison.





[Edited on 23-11-2017 by nezza]

I prepared several lead salts using a lead-acid battery as a source of lead. May be these notes could be useful for somebody who tries to get different pure lead salts.

The old battery I have is probably a gel battery (when I turned it upside-down no liquid was flowed out). I used a hacksaw to open the battery. I found the best way is to cut it from a side of a negative pole. (First I tried to cut the upper cover but it led to a short circuit - you should no try to saw the battery along the long side).



The negative plate can be easily removed. It consist of some frame and a kind of lead powder inside.



I put the plate in 480 ml of 7% HNO3. The dissolving process was accompanied by evolution of hydrogen and was slightly exotermic (it became warm but not boiling). I covered the beaker and put it inside a bigger inverted beaker to protect the environment from toxic droplets. After few hours the liquid became clear and the evolution of hydrogen was slowed down. pH of the liquid at this stage was around 3. I poured the liquid to a flask (through a filtering paper), put a boiling chips and used a distillation to concentrate it to approx. 75 ml. The distilled water could be reused for the next batch. The reason why the distillation setup should be used is a volatility of Pb(NO3)2 as well as of nitrates of some other heavy metals which can present. I found that there is no visible salt evaporation at 50 C but in range 80-100 C volatile water-soluble salts covered the cooler walls.



After cooling I added 30 ml of 53% HNO3. Pb(NO3)2 solubility drops very fast with increasing of HNO3 concentration, so this addition of the acid leads to a big amount of precipitate. It was filtered through a vacuum filter and washed with a nitric acid of the same concentration as a mother liqueur. After that the salt was dried. The yield of Pb(NO3)2 was 43 g. The mother liqueur as well as a washing solution as well as distilled water was used for the next batch preparation of Pb(NO3)2.

The Pb(NO3)2 at this stage is very impure and actually can contain nitrates of all metals used for making the negative battery plate - Cd, Bi, As etc. So, it requires a purification. I tried 2 possible method - through PbCl2 and PbSO4. For both purposes I used the same Pb(NO3)2 solution - 10-11 g of impure Pb(NO3)2 in 60 ml H2O. At 50C it dissolves very fast and solution was clear several days without any signs of hydrolyses (I think this is because the salt absorbed some HNO3 which preserved that).

The first method is very simple - I've added a stoichiometric quantities of NH4Cl and got PbCl2 precipitate. I think any chloride could be used - NaCl, KCl etc. This PbCl2 could be also used as a precursor for PbO2 (didn't try that yet but NaOCl should work). There is one drawback - to recover HNO3 the rest should be distilled with H2SO4 (otherwise you will end with very impure KNO3/NaNO3/NH4NO3). The PbCl2 is one of few insoluble chlorides (together with Hg and Ag), so theoretically it could be quite pure but it is well known fact that when the salt deposits as very fine crystals (in this case - like curd) it absorbs other water soluble salts from a mother liquer which is impossible to wash out. So, for better purity you can try the second method.

The second method is a bit more complex, uses 2 unique lead reactions for better purity and allows to prepare few other salts. Add 2 ml of concentrated H2SO4 (95-98%) per 15 ml of Pb(NO3)2 solution (of course H2SO4 with lower concentration could be also used - just use more it). The addition of the acid deposits insoluble PbSO4. The filtrate contained HNO3 which could be used for the next preparation of crude Pb(NO3)2 directly.

The PbSO4 could be solved in concentrated NH4CH3COO and this reaction has a very good selectivity on Pb. To prepare such solution I took 115 ml of 99,5% acetic acid and added 96 g of powdered ammonium carbonate to it. The reactions proceeds by endothermic way with self-cooling to 4C so, to make it happen I used a microwave. Several minutes (with periodic checks) on power level 100-300 W will create a clear syrupy solution without CO2 bubbles (don't use high power - otherwise you will get a very violent reaction as well as acid evaporation). After I've got it I diluted it to the volume of 150 ml (to add some fluidity). The density was around 1.11 g/ml.
The solution such prepared could be used for dissolving fresh precipitate of PbSO4 even at cold. Actually I used the fresh PbSO4 from 15 ml of Pb(NO3)2 solution and 2 ml and to that I added 90 ml of NH4CH3COO solution and 30 ml of H2O and warmed it a bit on a water bath. It dissolved PbSO4 almost completely. Some turbidity was filtered out. I found that addition of a small amount of water to the filtrate could make it even more clear (if a filter paper was unable to do their job perfectly).
This solution of PbSO4 in NH4CH3COO I used to prepare more Pb salts:
- yellow PbCrO4 (by addition of K2Cr2O7). It was fail when I tried to prepare this salt from Pb(NO3)2 or PbCl2, but PbSO4 gave it perfectly.
- PbCl2 by addition of equal volumes of water and concentrated HCl, but the yield is very poor because PbCl2 forms a complex [PbCl3]- . But it could be used for pure PbS preparation - I decanted the clear solution from PbCl2 crystals and added orange-red Na2Sx (polysulphide) solution which was prepared by dissolving sulphur in a hot NaOH solution, it gave me pure black PbS (it was a fail to prepare this salt from crude Pb(NO3)2 (gave a mix of sulphides with different colour - probably due to other metals contamination), PbCl2 (gave a brown lead chlorosulphide), PbSO4 in NH4CH3COO solution (violent reaction with evolution of gases and S deposit).

It was a fail with all my tries to oxidise PbSO4 in NH4CH3COO to PbO2. The reaction with H2O2 is quite remarkable. In acidic media it doesn't react. In alkaline media it reacts by very unusual way. When I dropped Pb solution into KOH + H2O2 it was a brown coloration (possible PbO2) which in few seconds oxidised H2O2 and disappeared. So possible H2O2 worked as an oxidiser on the first phase and produced PbO2 but then was reduced by PbO2 formed.
Ammonium persulfate also didn't work.
It is possible to get some PbO2 from such solution by addition of H2O2 and small amount of H2SO4 till formation of a small PbSO4 precipitate and then changing pH to alkaline with KOH. In this case PbSO4 precipitate turns to brown (PbO2?) and the reaction of H2O2 reduction and Pb oxidation goes with the same speed, so after 24 hours there is still some PbO2 not reduced flying up and down on oxygen bubbles.

Hope this information could be useful for the topic of lead salts preparation.

Quote: Originally posted by AJKOER

Successfully created PbO2 with standard household chemicals! After dissolving my Lead source in weak H2O2/Vinegar (forming Lead Acetate), it was necessary to create an alkaline Pb salt. I added OxyClean, which contains Sodium Percarbonate (2Na2CO3.3H2O2) and Sodium carbonate as not every household has pure NaOH or Ca(OH)2 lying around. I believed I saw some jelly like substance and added distilled water to the mixture to this very milky/foamy solution. After a few hours, I added an excess of NaClO. At first no obvious signs of a reaction (but a lot more foam), but within 6 hours deposits of a brownish-red salt (PbO2) appeared and foam was nearly gone. I was hoping for a larger yield but again my Solder is low in Lead (need better cheaper source). I am investigating other paths to PbO2 as well as using only readily available ingredients keeping in mind the goal of oxidizing ammonia in a mildly acidic environment (which occurs, for example, using ferrate salts at room temperature). [Edited on 24-7-2011 by AJKOER]

Quote: Originally posted by kazaa81

Here is a link of a zip containing tables extracted from Handbook of Chemistry and Physics, with lead salts properties: Lead Salts properties.by.kazaa81

Who has the file? The link no longer works

[Edited on 200514 by fusso]

All right, I found some metallic lead around.

My plan is following:

I melt the lead and cast it through mesh into water to form it into shots for max surface area.

Then I get copper sulfate and react calcium acetate with it to form copper acetate, and filter.

Then I dump the shots into copper acetate solution, and a single displacement reaction should take place, forming copper metal and lead acetate.

Should this work?

I was wondering if I should re-treat the copper with sulfuric acid, dry it and send it back because the store allows returns and it's expensive...

[Edited on 14-5-2020 by Refinery]

Lead chloride crystals

I made some nice looking lead chloride crystals today. I already described the method of lead purification by pouring 3 layers of liquid - Pb(NO3)2 solution, water and HCl acid on the top. This method allows separate lead from other impurities and get average size of crystals for easy washing. The problem is that it is very hard to make separate layers (without accidental mixing) especially when the surface area is big like in a beaker. Without separate layers I get a powder and I don't like powder because it is harder to wash a powder. Reaction of Pb(NO3)2 with gaseous HCl also gives a powder. So, the idea was to try 3 layers with different densities.

ZnCl2 (bottom) - ~ 3 g/ml (6 g ZnCl3 per 3 ml H2O)
Zn(NO3)2 (middle) - ~ 2g/ml (saturated)
Pb(NO3)2 (top) - ~ 1.5 g/ml (saturated)

By this method I've got 2 different forms of crystals - prisms and "feathers". Prisms were a result of diffusion from top to bottom and feathers - from bottom to top.

I think it is just a nice experiment to how how this interesting salt (a quite rare insoluble chloride) is growing in slow diffusion conditions. It's interesting to check whether PbCl2 absorbs any Zn ions, but taking very high solubility of ZnCl2 I doubt it is the case.





(Should I try an experiment with ZnI2 ?)

[Edited on 30-8-2020 by teodor]

I prepared and recrystallized the double displacement reaction produce.

The initial concentrate from the metathesis was just plain chunky black syrup. It was first suctioned dry from any residual water, and then dissolved in hot water and was left for crystallize and finally put into ice.



First recrystallization did bring out the yellow-brownish crystals. I did not actually take a picture from the mother liquor.

P.S. Piranha solution cleaned the clogged brown-gunk-impinged frit filter to a perfect condition.



After second recrystallization it was already much more pure.

The third recrystallization was enough to finalize the process, and shiny, white crystals were a result. No pics from third rec as well, because I accidentally deleted the pics.



I also made a second batch just for fun from reagent grade GAA and PbO. The reaction kinetics were PITA, but it resulted in a crystal clear solution, which is left for crystallize.



The solution apparently did not want to crystallize on it's own, so a seed crystal was dropped and then it turned into ice within a minute and heated up quite a lot.

I uploaded a little clip of the seeding.

https://vimeo.com/466935179