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Vlassis
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Oxalic Acid from Ethylene Glycol/Nitric Acid
![100_0140.JPG - 178kB](http://www.sciencemadness.org/talk/files.php?pid=239007&aid=17762)
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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:
![](https://lh3.googleusercontent.com/-1sS8ihCY64I/Tz1XduZrbgI/AAAAAAAAAgY/Gp6oKmsdwa4/s400/20120213_135757.jpg)
Tank
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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. ![;)](./images/smilies/wink.gif)
Phthalic acid
![peuf_20120301_5.jpg - 364kB peuf_20120301_5.jpg - 364kB](http://www.sciencemadness.org/talk/files.php?pid=239079&aid=17777)
Phthalic anhydride boiling/condensing/freezing
![peuf_20120301_4.jpg - 420kB peuf_20120301_4.jpg - 420kB](http://www.sciencemadness.org/talk/files.php?pid=239079&aid=17778)
[Edited on 3-2-2012 by AirCowPeaCock]
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blogfast25
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Quote: Originally posted by AirCowPeaCock ![](images/xpblue/lastpost.gif) | 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. ![;)](./images/smilies/wink.gif)
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 ![](images/xpblue/lastpost.gif) | 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 ![](images/xpblue/lastpost.gif) | 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 ![](images/xpblue/lastpost.gif) | Quote: Originally posted by AirCowPeaCock ![](images/xpblue/lastpost.gif) | 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 ![](images/xpblue/lastpost.gif) |
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...
![PiperineClose.jpg - 194kB](http://www.sciencemadness.org/talk/files.php?pid=239283&aid=17793)
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 ![](images/xpblue/lastpost.gif) | 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
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blogfast25
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Quote: Originally posted by Bot0nist ![](images/xpblue/lastpost.gif) | 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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