lead nitrate/acetate

[da man]

I now have access to sodium azide! And i obviousely want to make lead azide now, but im having trouble finding or making a soluable lead salt. I read somewhere that it can be made by dissolving metallic lead in heated nitric acid, i tried that with 70% nitric but had no luck, it wouldn't dissolve at all! I did a search on the forum, and the archives, but didn't find much. Does anyone know a relatively easy method of making lead nitrate/acetate from metallic lead? In one archive i did however read that lead acetate could be made by burning powdered lead with sulfur (forming lead sulphide i imagine), and then reacting that with acetic acid, would this work well, and would it work with nitric acid instead (i don't have glacial acetic acid)? Also i know that lead monoxide is amphoteric, so possibly if i could make that, i could simply dissolve that in nitric acid to make lead nitrate. But how would i make lead monoxide?
Any other methods for getting lead nitrate/acetate from mettalic lead are greatly appreciated!
Thanks!

[Pu239 Stuchtiger]

Amazingly, I have managed to prepare small amounts of lead acetate by placing lead sinkers in a solution of 5% acetic acid.

[da man]

really, thats strange that you have managed to dissolve it in a dilute solution of a weak acid, when i can't dissolve it in a concentrated solution of a strong acid!
How long did you leave it, and did most of it dissolve, how much did you get? Maybe it worked because your lead had formed a considerable amount of lead monoxide (from oxidation from air), because i noticed that when i put the (blackish) lead pieces in the nitric acid, it fissed for a second, and then stopped. I was thinking maybe it would be possible to oxidise lead completely to lead monoxide (without melting it for hours in air), possibly with ammonium persulfate or something, any suggestions?
Still any alternative methods for making lead acetate/nitrate are appreciated.

[kingspaz]

you could oxidise is via the KNO3. this is often used in explosive syth books because it also produces KNO2 for preparation of diazonium compounds.
Pb + KNO3 ---> PbO + KNO2
KNO2 is soluble so washes out leaving PbO. basically you heat a mix of lead powder and KNO3 to about 340*C and leave for a couple of hours at this temperature.
207g Pb for every 101g KNO3.

[Microtek]

Making lead nitrate is very easy, you just need to add lead chips to nittric acid and heat a bit. I use an inverted iron ( for ironing clothes - is there another word for this? ) as my hot-plate. It can be placed outside and has a thermostat to keep the temp within reasonable limits. Lots of NO2 is evolved in the reaction so don't do it without ventilation. Reaction is complete within an hour, and lead nitrate is relatively insoluble in dilute nitric acid. Pb(NO3)2 is a white, crystalline solid and once it is collected in a filter, wash it with alcohol to remove nitric acid traces.
Beware of soluble lead salts; they accumulate in your body.

[vulture]

The reason why weak acid concentrations attack metals easier is because they are more dissociated into H+ which is in most case the attacking ion. Highly concentrated strong acids also passivate alot of metals by forming a protective attacked layer on the surface.

You could electrolyse with Pb electrodes in a NaCl solution, this yields brown PbCl2. However, it's kinda hard to make nitrate from this I guess.

[da man]

Microtek, what concentration nitric acid do you use, and how hot do you keep the temperature? I used 70% nitric acid, and just made it warm, so that there was plenty of HNO3 fumes, but no NO2 fumes, and there was no visible reaction.

[VX]

If he uses an iron as a heat source, then I would say that it gets more than just warm. Also the 'strongest' solution of HNO3 is a 50/50 molar ratio of acid to water (when it is to act as a simple acid). i.e. just enough water to dissociate all of the acid molecules (HNO3 is a strong acid and so is more or less fully dissociated in water) but no excess water as this would begin to dilute the acid. I am not however sure what this is as a percentage concentration... sorry. :rolleyes:

The fact that your acid readily gives of HNO3 fumes suggests to me that there is quite a lot of 'free' acid in the mixture. This undisociated acid is unable to react, and must wait until it gains a molecule of water from the reaction, before it is able to partake in it, try adding a little more water to your acid.

[Microtek]

My acid is 62% HNO3. You should heat it until you see a reaction beginning to take place and then keep it at around that point. Exact temp is not so critical; if it is too high you'll waste a little HNO3, but that is all.

[rjche]

didn't find this thread before posting "Homemade Lead Nitrate" in the chemicals forum. A method to make lead nitrate is there now.

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Actually, it's HERE now. :D NBK
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HOMEMADE LEAD NITRATE

REQUIRED MATERIALS:"
OLD AUTO BATTERY
NITRIC ACID
HYDROCHLORIC ACID

Charge old battery to restore as much active material as possible and drive out as much sulfate from plates as possible. This means overcharge it (but don't make it hot to the hand) for several hours after cells are bubbling gas a lot.

Then pour out the acid (this will be sulfuric at about 25% concentration with some dissolved lead sulfate in it. It can be poured into the ground but away from where people live.

A junk yard in Florida (and lots like it) for 20 years bought about ten car batterys a day, and turned them upside down on the sand in a ditch in front of their yard, to get liquid out of em so he could transport them to the bigger yard sans liquid. They would not take those withe liquid in them.

He put several tons of lead sulfate laden sulfuric acid in a drainage ditch that was normally dry except in rains. It cause NO visible effects. Grass growed in the ditch, trees grew 4 ft away, etc. S0, lead sulfate is NOT a major hazard to the environment. The government does not see it that way, so take care.

When drained, fill all cells with water, and charge some more, then pour that out.

Repeat that about 3 times, or so, then after the last pour out, fill again with water, and let sit a day so most acid in plates diffuses out.

Again dump all liquid from the battery, and let it stand upside down a day, draining all that will come out.

Then take apart the battery by cutting the top off just above the plates with a saw. Cut the connector posts also when doing this so you end up with just the plates and post stubs on them, and no top.

Pull out the cells by pliers grabbing their cross straps. Seperate them into negative (gray) and positive(brown).

Dispose of the case, tops and cell insulator plates by burial or burning. DO NOT leave them around. They shout at all persons (This guy took my lead and did something terrible with it).

Keep the plates wet to prevent dust problems. Wear waterproof gloves to protect skin when handling them.

Put all brown plates in a plastic bucket, and pound them with a flat stick to knock out most of the brown powder from the plate grids.

Pound the brown stuff in to a coarse powder, but keep it damp so there is NO dust. Do not try to make fine dust, no need, and its hazardous.

To 240 grams of brown dust, add 200 cc Nitric acid, of 50 t0 60 % (or whatever strength you got, just adjust the 200 cc about enough to compensate for your acid conc. Too much is better than not enough for the brown lead you got. not enough will show brown stuff in your white stuff, and be hard to seperate, so more acid will have to be added and it done again. OVERDO THE ACID!

Put the lead dioxide (brown powder) in a quart of jar volume for every 240 grams brown powder. Pour the Nitric acid on it. Nothing happens. Might see some white fumes from the acid but no reaction usually.

Pour in 10 cc of pool hydrochloric acid (about 30% stuff), all at once so conc HCL goes down on the powder through the nitric acid.

Where it hits the powder a reaction ought form, (no heat needed).

Bubbles of oxygen will come off. Let it sit. No need to stir, and speed up the reaction. It won't become a runaway, No red fumes or stuff, but it can bubble up and foam. If it's going pokey, stir ONCE and see what that does. Then stir to suit your desires so long as you don't cause it to get out of your container.

NOTICE, THIS LIQUID IS VERY POISONOUS AND WILL CONTAMINATE HELL OUT OF THE GROUND WITH SOLUBLE LEAD NITRATE. DO KEEP ANOTHER CONTAINER, LIKE A PLASTIC BUCKET UNDER YOUR REACTION VESSLE JUST IN CASE YOU HAVE AN ACCCIDENT.

When all done there will be a white precipitate where the brown powder used to be, and a pale yellow liquid above it.

Pour off the liquid, (easy to do because the lead nitrate is very heavy and does not like to follow the liquid that is flowing out). Work over a containment in case you spill.

You can salvage the liquid by pouring it into an excess of brown powder . When it finishes, heat the liquid and brown powder to dissolve all the nitrate you can, then pour it off. The liquid will contain lead nitrate, dry it to get the powder.

240 grams brown powder will yield 330 grams lead nitrate.

A car battery has several kilos of brown lead in it.

The grey plates are made mostly of lead powder. It's hard to react, so it can be melted and bullets made of it. What don't melt will be a lead compound which ought react with the weak aqua regia mix above. (NA + tad of HCL)

Take care of the lead nitrate. Being very soluble in water, it can cause peak pollution levels in streams etc which cause monitoring instruments to go crazy, and launch local nothing-to-do search parties to go find where it entered.

Experimenting mad scientists don't need that kind of stuff. Don't scare hell out of everyone that knows zilch about things, and they will leave you alone.

Remember all "monitor" personnel crave attention, worse than a sub crewman back from a year without seeing light of day, craves sex.

So expect them to say wild things about the pollution, and make it sound like they saved the world from asteroid impact. YO Ass will be their podium while they doin all that. Someone might even start yelling tarrrrouussst,...damned tarrorist... and you know where it will go from there. Just use your common sense, and don't invite trouble.

Be a responsible experimenter, even if it hurts.

To dispose of lead nitrate, with minimum hazard, mix it with sulfur and burn it into lead sulfate + some lead sulfide (galena) both very insoluble in water, and not capable of a pollution that would sound alarms. Avoid the fumes (stand so wind carries fumes away from you and toward a wilderness. Not good to send stink into neighbor's window. If he finds out what it came from he could cause a stink of his own.)

330 grams lead nitrate plus 64 gms sulfur ought burn like a road flare, and stink a lot since sulfur dioxide takes out the excess oxygen. It would be wise to burn it in a tin can and under ground in a wilderness area, so stink stayed there and the nitrate changed to sulfate there, and no harm done. It is a crummy grade of black powder level stuff.

WASH YOUR HANDS AND FACE BEFORE EATING AFTER FOOLING WITH LEAD CHEMICALS. Don't want you to die before the government gets to kill you in some economic war to steal more oil.

<small>[ August 03, 2002, 05:53 PM: Message edited by: nbk2000 ]</small>

[Polverone]

If you don't happen to have old batteries and nitric acid on hand, try heating lead metal (shot, powder, wire, plates, whatever) in ammonium nitrate solution. Ammonia will be given off and you'll be left with a white, heavy powder (you may need to periodically scrape the surface of the metal if you're using larger chunks). I'm not sure whether this is an oxide, hydroxide, whatever of lead, but it dissolves in acetic acid to form lead acetate. I've only used glacial acetic acid but I imagine that even vinegar would work if you gave it enough time and maybe a push with heat.

[Pu239 Stuchtiger]

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">You could electrolyse with Pb electrodes in a NaCl solution, this yields brown PbCl2. However, it's kinda hard to make nitrate from this I guess.</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">Electrolysis of sodium chloride in aqueous solution with lead electrodes yields sodium hydroxide and lead chloride... and those react with each other.

PbCl2 + 2NaOH ----&gt; Pb(OH)2 + 2NaCl

[Jumala]

Only an idea-
what happens if you use dilute HNO3 instead of NaCl solution for electrolysis.

[Pu239 Stuchtiger]

You'll get lead nitrate. If there isn't enough nitric acid present, you'll also get lead hydroxide.

[rapdogg21]

Is this thread still alive?

I have prepared lead nitrate by putting 100 grams lead chips in 100ml water at a temp of 50C, then added 90ml of 65% nitric acid and 90ml water. Then I filtered the solution, sealed and kept in a refrigerator for 24 hours. Significant appearance of lead nitrate crystals appear.

I get the crystals and have the rest of the solution evaporated to dryness. I got approximately 110 grams of lead nitrate crystals with this method.

[nightandday]

Lead is readily dissolved by a mixture of concentrated acetic acid and hydrogen peroxide 30% - without evolution of hydrogen. On evaporation and subsequent cooling, lead acetate is precipitated, which may be filtered off and dried. Purity is according the lead used.