Ephoton
Hazard to Others
Posts: 463
Registered: 21-7-2005
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Mood: trying to figure out why I need a dark room retreat when I live in a forest of wattle.
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retrofitting ;)
hey guys ive got a bit of a problem that I think some of you here have
overcome and would love some advice.
I wish to do a mixed klobe condensation with lead acetate.
now from what ive seen and heard I get left with a nasty
rock at the bottom of my flask that is very hard to remove.
I wish to do this then in a 1 liter solvent tin to prevent this from
being a problem.
this leaves me with the question how do I connect my glassware
to a solvent tin and still keep it air tight at temps up too 300C.
any advice would be great.
of course how to clean out the rock would be even better.
would I be right in beliving that the rock left would be lead
oxide and metallic lead mixed.
[Edited on 24-9-2008 by Ephoton]
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not_important
International Hazard
Posts: 3873
Registered: 21-7-2006
Member Is Offline
Mood: No Mood
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It's mostly lead oxides, which react with glass and ceramics fairly readily. Nitric acid wil dissolved it, in metal you can use hot concentrated
NaOH/KOH solution. But the fused oxides are fairly slow to dissolve, banging on the cold metal container to knock as much loose first is likely the
best starting point; followed by not worrying too much about having a little left in there.
'
You can buy stainless steel flasks with joints to fit the Standard Taper joints of glassware, that's the best way. The next is to make an all metal
assemble for all the hot area, if needed connect to glassware using corks or rubber stoppers at points were it's cool enough.
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Ephoton
Hazard to Others
Posts: 463
Registered: 21-7-2005
Member Is Offline
Mood: trying to figure out why I need a dark room retreat when I live in a forest of wattle.
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thanx MR important 
sounds like my line of thought was right.
if I treat the rock as I would the metal I make the lead salt with
I should get most of my lead salt back as well as cleaning my flask.
I will try using acetic acid first then if that does not work try with peroxide
as well. I have to make a large purchase of nitrate before I can start working
with nitric unfortuantly as the only source I can get is farm nitrate.
this reaction with glass that your talking about is that like crystal glass being formed
via lead being dissolved in the glass.
not good if so as it will weaken the glass over time.
well you have given me a great starting point not_important to look into this.
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