387 replies to this topic

[tentacles]

As the Pb ion plates out of the tank, the nitrate ion will be left and forms HNO3 - you really don't want a very low PH in your plating solution. The "high nitric" plating baths are primarily to prevent Pb from plating out at the cathode - which you can prevent by using a copper cathode, or using copper nitrate (plates Cu at the cathode, essentially makes your cathode copper). The idea was to redissolve any Pb as it plated out. What you're going to want is some PbO, PbCO3 or PbOH to add new Pb ion to your plating tank. PbO is suggested, since you can just dump a bunch in and let it dissolve as the plating progresses. Litharge (PbO) is sold for mining/assaying purposes and also at a few ceramics shops - many stores like to be "lead free" which is bad for us, maybe good for potters. There are several ways to produce it, and none of them really appeal to me at the moment.

[marble]

So all i really need is:

Lead nitrate
Lead oxide
Copper cathode (copper sheet)

And the material I wish to plate?

/this photographic supplier has some interesting items, uranium nitrate and mercury chloride to name a few

Edited by marble, 19 November 2007 - 03:16 AM.

[Anders Greenman]

Nice Then I will not have to make Copper Nitrate again! I have no PbO, and I'm not in the mood to buy so I'l make it myself, either from the nitrate or heating raw lead.

[hashashan]

good luck with heating lead.
I dont believe its too practical.

[marble]

I just tried

It sucks.

The lead melts, after a while the top turns yellow, you disturb the lead to allow fresh Pb to be oxidized, rinse and repeat.............

For 45 mins work I yielded some yellow crap that I cannot separate from the lead anyway.

bah

Edited by marble, 20 November 2007 - 10:44 AM.

[marble]

I just noticed there is a agent for titanindia in the UK, he sells pt plated Ti and MMO anodes. Ill see if he can get TSLD anodes.

Worth a shot if they are reasonably priced

[tentacles]

marble: I found a method somewhere that involved melting KNO3 and slowly adding your lead to the melted salt. This formed PbO, somewhat more practially than merely heating lead.

[hashashan]

tentacles good luck with that too you too.
The nitrate sinks down and doesnt react with the Pb. You need some sort of a mechanical (maybe a magnetic stirrer will do there(I dont know what will happen wo the teflon magnet in those temps) stirring in order to do this reaction.
Ive tried it, very low yeilds and lots of toxic PbO and NaNO2

oops just noted that you wrote to melt the KNO3 and not the lead.
anyway the procedure calls to melt the lead.
I believe that if youll melt the KNO3 the lead will ignite.
anyway molten nitrates is just an invitation for bad news.

once again the simplest way to PbO is
Pb(NO3)2+2NaOH = Pb(OH)2 + 2NaNO3
Pb(OH)2 + heat = Pbo + H2O

any soluble lead salt will do, you dont have to use the nitrate

Edited by hashashan, 22 November 2007 - 02:36 PM.

[marble]

I may have found a commercial source for lead dioxide anodes, a ebay seller who sells MMO and pt plated anodes thinks he may be able to get lead dioxide anodes from his supplier. Hes looking into it for me, if they are cheap enough I think i may have solved my perchlorate problem once and for all.

Sells MMO anodes for $40, hopefully lead dioxide will be around the same

[marble]

Ok, ive got a MMO anode in the mail and It seems I'm all alone with this. I cant find anyone who has used one before.

[Resix]

Ok I just purchased 2 Pt coated Ti Anodes. Can i use one as a cathode and one as an anode? Some guide i read a few weeks ago or so said that it would work, but he was the only one claiming this. I havn't goten that far yet in my College Chem course. (Start solution chemistry when school goes back on the 14th.) So, Will that work? Or did i just buy an extra Pt Anode?

Edited by Resix, 04 January 2008 - 06:48 AM.

[JamesH]

Does anyone know a supplier of Pt coated Ti, Ti or MMO anodes at a decent price? Preferably a UK supplier.
Thanks.

[pkhow]

I am surprised here at the lack of discussion or attempts at Chlorate and Perchlorate using DSA(MMO) anodes. Don't dismiss
DSA anodes for Perchlorate because some with some of the newer material it is possible.
I have been DSA anodes for Chlorate Production for Years and have experimented a lot with Perc Production using the newer
Low salinity DSA electrode. This can be operated at up to an increadable 90degC with saline as low as 2000ppm.
In the past it was the low salt concentrations that caused the coating loss.
Running it as a Perch cell is hard on the coating but if designed corrrectly is still viable.

[MDH]

Where did you guys manage to obtain your potassium chloride?

I can only find it at health food stores where 300 grams is going for $5. Obviously not a viable resource.

[Mumbles]

It is fairly common as both a water softener salt, and a fertilizer. As a fertilizer it is sold as "muriate of potash". I've purchased it as normal potash as well inadvertantly. I obviously wanted the potassium carbonate variety, not KCl, which I have plenty of. The water softener salt type of variety is about 3x as expensive as the sodium chloride variety. This puts it at a whopping $6 or $7 per bag. In the US it is in a white 40lb bag by Morton's.