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Author: Subject: Pretty Pictures (1)
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[*] posted on 1-3-2012 at 10:56


Oxalic Acid from Ethylene Glycol/Nitric Acid

100_0140.JPG - 178kB100_0137.JPG - 292kB
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[*] posted on 1-3-2012 at 12:44
copper acetate


A mix of copper acetate and copper metal in Hdpe dish.


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[*] posted on 1-3-2012 at 13:13


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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[*] posted on 1-3-2012 at 15:23


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:


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[*] posted on 1-3-2012 at 15:28


How much testosterone is that? Looks like quite a bit you got there!



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[*] posted on 1-3-2012 at 19:00




There we go centered.
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[*] posted on 1-3-2012 at 19:19


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
peuf_20120301_5.jpg - 364kB




Phthalic anhydride boiling/condensing/freezing
peuf_20120301_4.jpg - 420kB

[Edited on 3-2-2012 by AirCowPeaCock]




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[*] posted on 2-3-2012 at 06:47


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? :cool:




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[*] posted on 2-3-2012 at 10:10


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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[*] posted on 2-3-2012 at 10:32


Quote: Originally posted by m1tanker78  
I love the needle crystal pics lately. I'll try to keep the theme going with one of my own.


Preposterous amounts of testosterone! Preposterone!




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[*] posted on 2-3-2012 at 10:50


Sure puts the 'tossed' in testosterone ─ a 'testament' to all things testicular . . .(:P)



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[*] posted on 2-3-2012 at 12:15


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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[*] posted on 2-3-2012 at 12:20


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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[*] posted on 2-3-2012 at 16:08


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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[*] posted on 2-3-2012 at 17:01


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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[*] posted on 2-3-2012 at 17:29



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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[*] posted on 2-3-2012 at 17:45


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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[*] posted on 2-3-2012 at 19:35


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)




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[*] posted on 3-3-2012 at 06:43


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)


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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[*] posted on 3-3-2012 at 11:25
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

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[*] posted on 3-3-2012 at 11:44


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?




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[*] posted on 3-3-2012 at 11:54


25grams fresh ground aromatic pepper. Followed the same workup I used here .






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[*] posted on 3-3-2012 at 12:45


Quote: Originally posted by White Yeti  

@Bot0nist Nice crystals! Those rival the beauty of those on the wikipedia page.



Excellent, WY. That's been bookmarked.




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[*] posted on 3-3-2012 at 13:23


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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[*] posted on 3-3-2012 at 16:11


Quote: Originally posted by Bot0nist  
25grams fresh ground aromatic pepper. Followed the same workup I used here .




Were you posting with a different handle? There seems to be no Bot0nist on that thread...




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