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Vlassis
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Oxalic Acid from Ethylene Glycol/Nitric Acid
 
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Diablo
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copper acetate
A mix of copper acetate and copper metal in Hdpe dish.
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AirCowPeaCock
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Pretty, though you should get a picture that shows the full dish centered. It would be more appealing, and more balanced.
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m1tanker78
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I love the needle crystal pics lately. I'll try to keep the theme going with one of my own.
Testosterone barbs/needles forming and settling out:
Tank
Chemical CURIOSITY KILLED THE CATalyst.
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White Yeti
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How much testosterone is that? Looks like quite a bit you got there!
"Ja, Kalzium, das ist alles!" -Otto Loewi
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Diablo
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There we go centered.
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AirCowPeaCock
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It's surprisingly beautiful, and now we can see the copper metal. If only I had the brains to take pictures of these things when they happen. 
Phthalic acid
Phthalic anhydride boiling/condensing/freezing
[Edited on 3-2-2012 by AirCowPeaCock]
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blogfast25
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Quote: Originally posted by AirCowPeaCock  | It's surprisingly beautiful, and now we can see the copper metal. If only I had the brains to take pictures of these things when they happen.
Phthalic acid
Phthalic anhydride boiling/condensing/freezing
[Edited on 3-2-2012 by AirCowPeaCock] |
Nice phtalic acid! Did you synth it yourself and if so, how? 
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AirCowPeaCock
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That phthalic acid was synthesized using the same process nurd rage uses--which I dislike. Its not as much as it looks, its mostly air--based on my
phthalic anhydride yield (4.3 g) I'm going to guess it was about 4.3 g, which would be an optimistic ~ 89.15% yield on the conversion (alot of gloves
for so little, atleast I have 200g of PVC powder now). I'm going to try a xylene oxidation in a few days. Since its cheap and plentiful I could
probably produce 50+ g with little trouble, and I will have two xylene isomers left. I'm going to make some luminol and potassium hydrogen phthalate
with it, and Ill keep some of the anhydride in a little bottle in case I find later use for it.
[Edited on 3-2-2012 by AirCowPeaCock]
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mr.crow
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Preposterous amounts of testosterone! Preposterone!
Double, double toil and trouble; Fire burn, and caldron bubble
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Pulverulescent
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Sure puts the 'tossed' in testosterone ─ a 'testament' to all things testicular . . .( )
"I know not with what weapons World War III will be fought, but World War IV will be fought with sticks and stones"
A Einstein
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blogfast25
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| Quote: Originally posted by AirCowPeaCock | That phthalic acid was synthesized using the same process nurd rage uses--which I dislike. Its not as much as it looks, its mostly air--based on my
phthalic anhydride yield (4.3 g) [...]
[Edited on 3-2-2012 by AirCowPeaCock] |
Ah: solvent extraction of DOP from pPVC (gloves), followed by hydrolysis of he DOP, right? Been there, done that: expensive in gloves!
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AirCowPeaCock
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yeah, its not too expensive--atleast not if you just want a few gram. I don't know how he got 13g of Phthalic anhydride from 50g of gloves. I could
only get half that will 200g of gloves! -- my gloves must suck!
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blogfast25
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| Quote: Originally posted by AirCowPeaCock | | yeah, its not too expensive--atleast not if you just want a few gram. I don't know how he got 13g of Phthalic anhydride from 50g of gloves. I could
only get half that will 200g of gloves! -- my gloves must suck! |
Even 13 g of PAA from 100 g of gloves would sound improbably high to me. DOP content of gloves: max 30 %, something like that?
Also: try an old shower curtain, cheaper than virgin gloves!
[Edited on 3-3-2012 by blogfast25]
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AirCowPeaCock
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I think the way to go is xylene oxidation, I've found a few references to oxidation in the liquid phase. Even with 5% efficiency (I imagine) it
would be much cheaper than any PVC source.
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dann2
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Hope I am not repramanded for (bad speelling too pehaps) putting ugly pictures in the pretty pictures thread.
Here we have a bar of pure Copper that has had the top portion melted into a ball. Copper has a high melting temperature and I have been able to
achieve this melting feat using a lit match! The flame of a lit match can easily melt Copper as the picture shows.
There is some oxide on the ball. I should have perhaps cleaned up the Copper with an acid dip or somesuch.
The bar of Copper (I should mention) is 48swg Copper wire.
Dann2
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Endimion17
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It's been a really cold winter here, and my benzene has frozen solid, so I uploaded the photo to Wikipedia.
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UnintentionalChaos
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| Quote: Originally posted by blogfast25 | | Quote: Originally posted by AirCowPeaCock | | yeah, its not too expensive--atleast not if you just want a few gram. I don't know how he got 13g of Phthalic anhydride from 50g of gloves. I could
only get half that will 200g of gloves! -- my gloves must suck! |
Even 13 g of PAA from 100 g of gloves would sound improbably high to me. DOP content of gloves: max 30 %, something like that?
Also: try an old shower curtain, cheaper than virgin gloves!
[Edited on 3-3-2012 by blogfast25] |
I found shower curtain to have much lower DOP content than the gloves. The shower curtain I tried to extract contained 10% DOP based on mass lost
after several hours of soxhlet extraction.
The gloves I used were a solid 36% DOP and I scraped 73.6g of fairly clean phthalic acid from 570g of gloves following a recrystallization (85% yield)
Department of Redundancy Department - Now with paperwork!
'In organic synthesis, we call decomposition products "crap", however this is not a IUPAC approved nomenclature.' -Nicodem
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blogfast25
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| Quote: Originally posted by UnintentionalChaos |
I found shower curtain to have much lower DOP content than the gloves. The shower curtain I tried to extract contained 10% DOP based on mass lost
after several hours of soxhlet extraction.
The gloves I used were a solid 36% DOP and I scraped 73.6g of fairly clean phthalic acid from 570g of gloves following a recrystallization (85% yield)
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Yes, I remember that now, UC. Still, USED pPVC is a lot cheaper than virgin gloves. Shower curtains are made of a slightly harder pPVC compound, so
less plasticiser. I also used pPVC flooring once: also less yield but FOC raw material...
Today you'd have to avoid the 'Phthalate FREE!' products for that sort of thing.
I may revisit DOP extraction/hydrolysis to makse some pure K hydrogen phthalate, a primary standard for acid/base titrations.
[Edited on 3-3-2012 by blogfast25]
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Bot0nist
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Recrystallization of Piperine
Got to love the needles. Here is piperine (&chavicine?) that was extracted from black pepper with IPA being recrystallized from 10ml of etOH/IPA
mix. Slowly cooled overnight. One of my favorite things is watching a recrystallization come to fruit. Ever so satisfying...
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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White Yeti
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| Quote: Originally posted by AirCowPeaCock | | I think the way to go is xylene oxidation, I've found a few references to oxidation in the liquid phase. Even with 5% efficiency (I imagine) it
would be much cheaper than any PVC source. |
Here's a video UC did on the synthesis of phthalic acid. I think this is many orders of magnitude cheaper than PVC, but I've never tried it myself.
@Bot0nist Nice crystals! Those rival the beauty of those on the wikipedia page.
May I ask, how much pepper did you use to make that sample?
"Ja, Kalzium, das ist alles!" -Otto Loewi
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Bot0nist
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25grams fresh ground aromatic pepper. Followed the same workup I used <a
href="http://www.sciencemadness.org/talk/viewthread.php?tid=10676&page=2#pid222835">here</a> .
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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blogfast25
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Excellent, WY. That's been bookmarked.
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mr.crow
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Excellent photos guys!
The piperine looks really spicy. Solid benzene looks like ice in a soda
I once melted a copper wire in a similar way using a neon sign transformer. The arc melts it into a little glowing ball
I just bought some phthalic anhydride instead of the popular messing around with gloves method hehe
Double, double toil and trouble; Fire burn, and caldron bubble
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blogfast25
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| Quote: Originally posted by Bot0nist | 25grams fresh ground aromatic pepper. Followed the same workup I used <a
href="http://www.sciencemadness.org/talk/viewthread.php?tid=10676&page=2#pid222835">here</a> .
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Were you posting with a different handle? There seems to be no Bot0nist on that thread...
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