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Author: Subject: The lead salts preparation thread!
jock88
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[*] posted on 3-5-2014 at 12:38




http://www.sciencemadness.org/talk/viewthread.php?tid=30287

Lead Nitrate from Car battery + Nitric Acid
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blogfast25
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[*] posted on 3-5-2014 at 13:20


Please don't use abbreviations without explaining them first. We're supposed to scientists, not mind readers.

I mean, do you know what ROFPM means?

[Edited on 3-5-2014 by blogfast25]




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annaandherdad
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[*] posted on 3-5-2014 at 14:02


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.



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[*] posted on 3-5-2014 at 14:10


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?
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Boffis
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[*] posted on 3-5-2014 at 15:44


Simply recrystallize it from water, lead nitrate is freely soluble in hot water, the slight excess of nitric acid will prevent hydrolysis, and cool. If you are patient and use more dilute hot nitric acid you can almost neutralise the acid since lead dissolves slowly even in very dilute nitric acid.

I use lead oxide or white lead pigment but the latter is is getting hard to come by these days. Lead monoxide is usually available on ebay.
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annaandherdad
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[*] posted on 3-5-2014 at 18:29


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?


No, you don't add the NaOH to the lead nitrate-nitric acid mixture, you just use it in a separate container to absorb the vapors that are evaporated from it. HNO3 will evaporate along with the water, and NaOH will absorb both.

Or do what Boffis says, or the lead carbonate method. You can make lead carbonate by taking a sample of your lead nitrate-nitric acid mixture, and add sodium carbonate (slowly, or else it will fizz over). This will neutralize the nitric acid and precipitate lead carbonate, which you can filter and wash. Then add that to the rest of your lead-nitrate nitric acid mixture, to neutralize the excess acid.




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[*] posted on 5-6-2014 at 23:16


I use lead metal as the limiting reagent along with 30-35% HNO3 to reduce
NO2 formation. Filter while hot to remove impurities.
After that I put the flask in the fridge to ppt as much lead nitrate out as possible.
Then I decant the mother liquor off and save it.
Then I wash the crystals in the flask with anhydrous methanol.
Pour of the methanol in a separate beaker ..... The crystals are scraped off to dry.
Within a few hours of air drying .... I have storable lead nitrate crystals.

[Edited on 6-6-2014 by Motherload]




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[*] posted on 6-6-2014 at 02:42


The easiest way of purifying the acidic Pb(NO3)2 is by dissolving it in as little as possible of hot water (90 C or so) and then letting it cool down. You can allow some of the water to evaporate to regain more of your Pb(NO3)2. The crystals which separate will have lost nearly all of their acid.

Do not allow all water to evaporate. Some of the water should remain. That water will contain nearly all acid, and it also will contain other impurities. If you allow everything to evaporate to dryness, then you'll get acid trapped in your crystals again, and you also keep other impurities.

What you can do is evaporate the water in a separate container. Then you get two batches, a large pure batch and a small impure batch.




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[*] posted on 6-6-2014 at 05:10


Leas salts thread:

http://www.sciencemadness.org/talk/viewthread.php?tid=5490
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[*] posted on 11-6-2014 at 09:04


Previously I dried all my crystals in a glass dish .... But it's happy days are done.
So I switched to a decent quality heavy gauge Teflon coated baking tray I bought for about $10.

Anyways .... My last batch of methanol washed Lead Nitrate crystals are turning brown and the tray dark grey patches. The Teflon has not peeled off or anything.
I am going to assume that the brown in my Lead Nitrate crystals is Iron contamination and the dark grey patches on the tray are Lead metal.

If that is true .... Then are the ions diffusing through Teflon and the crystals were just damp ?? It continued after they completely dried.

I took them off now .... I have to recrystalize the batch again.




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[*] posted on 8-3-2015 at 07:56


I discussed producing lead monoxide and lead nitrate from the lead dioxide from an old lead acid battery here:

http://www.sciencemadness.org/talk/viewthread.php?tid=26572&...

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...

Removing Lead Dioxide from Battery.jpg - 515kB Disassembling Battery.jpg - 283kB Lead Dioxide from Battery.jpg - 526kB Calcining Lead Dioxide (1).jpg - 218kB Calcining Lead Dioxide (2).jpg - 251kB Lead Monoxide.jpg - 195kB Lead Monoxide with Lead Tetroxide Contamination.jpg - 237kB


Attachment: Homemade Yellow Lead Oxide & Lead Acetate.pdf (358kB)
This file has been downloaded 328 times


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




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[*] posted on 3-11-2017 at 14:15


How is possible to remove white stain on glassware from lead nitrate? Nitric acid and aqua regia doesn't work. Maybe oxalic will help but I want to ask before buying or synthesising it.
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[*] posted on 4-11-2017 at 02:05


@Metallic, it depends what the white stains are but a good general stain remover for white lead compounds like lead carbonates halides and sulphate is sodium thiosulphate solution, a 2-3% solution is adiquate. It sounds like your stain is lead sulphate because most other lead salts are soluble in either acid or water. Lead halides are fairly soluble in warm water and ammonium acetate acccentuates this solubility. For lead sulphide staines treat with 6% hydrogen peroxide for a few days until it turns white (the sulphate) and then use the thiosulphate solution.
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[*] posted on 4-11-2017 at 23:03


Thank you, but I can't believe that stain is from lead sulfate because it needs to be formed from something like sulfuric acid. Actually, in another beaker I got very similar white stain from lead acetate, but is more transparent. I will try with sodium thiosulfate but first I need to synthesis it because I can't buy/find it in my country.
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[*] posted on 23-11-2017 at 02:25


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.



Ammonium Chloroplumbate.jpg - 145kB

[Edited on 23-11-2017 by nezza]




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[*] posted on 23-11-2017 at 10:44


Are lead fishing sinkers pure lead or is the lead sometimes contaminated with antimony and/or other metals that help harden the lead metal?

EDIT: I happen to have a ~250 g lead sinker that I got at a sporting goods store for about $3.

(Beautiful sample of ammonium chloroplumbate by the way nezza)

[Edited on 11-23-2017 by ninhydric1]




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[*] posted on 26-11-2017 at 08:37


Hard lead is almost always lead alloy, most often lead-antimony. The most pure lead is the softest.



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