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Boffis
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[*] posted on 10-2-2013 at 15:18


@DJF96

I’m not sure that they are polymorphs, for various reasons I think their formation is pH or perhaps temperature dependent. The former is based on the differing reactions between acetates and chlorides of the same metal; violuric acid is a weak acid (pK 4.70) but slightly stronger than acetic acid (pK 4.76) but much weaker than hydrochloric acid. I intend to investigate this with various organic buffers (to avoid adding ammonia or alkali metals since they react too) and ion exchange resins.

When I did the initial work many years ago I started in an unheat lab in winter at about 8 C, subsequent work was all done at normal room temperature. A third facture may be purity of reagent, which I am currently investigating, because I made the early batches in small quantities and each time used a different method. A possible side product is 5-nitrobarbituric acid which forms sparingly soluble salts but I have no data on their colours.

Violuric acid forms both salts and chelates; alkalis and alkaline earths + some organic bases form salts of the nitroso tautomer while Fe and Co form extremely soluble chelates (Fe intense deep blue and Co deep orange) (eg Leermakers & Hoffman JACS 1958 p5663). Most of the post 1800 work deals with the chelates and almost nothing appears in relation to the salts. Mn2+, Zn2+, Cd2+ and UO22+ all resemble alkaline earth metals in the way they react. Cu2+ appears to form a sparingly soluble olive green chelate.

So there are lots of possibilities and I could write a book on this fascinating compound and is numerous close relatives! When I get more time in the lab I’ll investigate further and report.
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kristofvagyok
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[*] posted on 10-2-2013 at 23:58


Working with trinitrobenzene-Li salt what has a strong fluorescence under UV:



And my gloves after I have made Nurd Rage's blue smash glow crystals in a flask that accidentally cracked in my hands:




I have a blog where I post my pictures from my work: http://labphoto.tumblr.com/
-Pictures from chemistry, check it out(:

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Zan Divine
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[*] posted on 11-2-2013 at 13:32


I've posted some K & Na ampoules before. The ones I'm making for my present client are bigger. The below is sodium (ca. 1/2 lb.), for comparison is 15 lb. Marvin.



Attachment: phpIruPfF (62kB)
This file has been downloaded 747 times Attachment: phplTxDXQ (90kB)
This file has been downloaded 750 times



[Edited on 2/11/2013 by Zan Divine]




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Pyro
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[*] posted on 12-2-2013 at 14:28


holy crap! that's amazing!!



all above information is intellectual property of Pyro. :D
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elementcollector1
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[*] posted on 12-2-2013 at 14:38


How do you DO that?!



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bfesser
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[*] posted on 13-2-2013 at 09:21


Quote: Originally posted by Mailinmypocket  
A molybdenum compound in formation
[Edited on 26-1-2013 by Mailinmypocket]


I have a special place in my heart for molybdenum … right after copper. Could you please post some details on this in another thread? Or if I just plain missed it, could you please PM me with the TID?




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Zan Divine
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[*] posted on 13-2-2013 at 10:33


Quote: Originally posted by elementcollector1  
How do you DO that?!


Conceptually, it's actually easier than the method I described for the 3/4 " tubes last summer. The glass is 1.5" in diameter and is really more than a single flame torch (what I have) can handle easily.

Consequently, my constricted areas are very short and tricky to seal.

The method is simple, devil is in the details. Long glass tube, seal one end, make a constriction where you want the ampoule to end. Add coarse SS wool ball above constriction and balls of OIL FREE metal above that. Attach vacuum pump. Tilt tube at 45 degrees, wrap with heating tape. Melt metal. It flows into the ampoule which is then torch sealed.

Any oil you miss makes the tube cloudy. Molten metal continuously flowing over constriction tries to wet it making sealing doubly tricky.

[Edited on 2/13/2013 by Zan Divine]




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Mailinmypocket
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[*] posted on 13-2-2013 at 11:03


Quote: Originally posted by bfesser  
Quote: Originally posted by Mailinmypocket  
A molybdenum compound in formation
[Edited on 26-1-2013 by Mailinmypocket]


I have a special place in my heart for molybdenum … right after copper. Could you please post some details on this in another thread? Or if I just plain missed it, could you please PM me with the TID?


Sure! Ill just post it here. I meant to show the final product but I forgot, so I dug it out just now and mixed a bit into water to display the color. The compound is molybdenum blue, a hydroxide of molybdenum, Mo4O10(OH)2. It's a dark royal blue powder. The preparation was followed almost as per Brauer, except I mixed the MoO3 powder into the dilute HCl very well, and then added the Zn granules:

"MOLYBDENUM BLUE, Mo4O10(OH)2
Obtained by reaction of nascent hydrogen with MoO3.
Fifty ml. of distilled water and 10 ml. of cone. HCl, followed
by 3 g. of analytically pure zinc granules, are added to 10 g. of
MoO3. The mixture is left standing overnight; the blue precipitate is then filtered off, washed until no chloride reaction is evident, and dried over P3O5.

Alternate methods: a) Reduction with SnCl3 • 2 H3O in HC1
solution.
b) Synthesis from MoO3 and Mo powder (O. Glemser and G.
Lutz, see below).

PROPERTIES:
Formula weight 477.82. Blue crystalline powder. In air,
oxidizes very slowly to MoO3. Stable to NH3 and alkalies. Good
electrical conductivity.

REFERENCE:
O. Glemser and G. Lutz. Z. anorg. allg. Chem. 264, 17 (1951)."


blue.JPG - 103kB

[Edited on 13-2-2013 by Mailinmypocket]
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mayko
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[*] posted on 18-2-2013 at 17:38


Quote: Originally posted by Xenon1898  


Good use of a microscope in the lab. I am wondering, do many people find microscopes useful in the home lab? This seems like a great example of a good use (two pure crystals forming as the same time). Seems like it would be a reasonable investment as an analytic qualitative tool to identify crystal structure(?)


That one wasn't actually taken under the scope, but I do have a USB microscope. I don't currently know enough about crystals to do much identification, but I am sure that in the right hands it would be a powerful tool. Thusfar, I've mostly been getting up close and personal with dead bugs, my warts/moles/hangnails, etc. Here's some of the crystal shots I took thought.



Copper acetate feathers






Closer view of copper acetate






Surface of a copper sulfate crystal






Thermite leftovers





Epsom salt

I'm really glad I got it - next I'm gonna get some polarizing filters and do some video of vitamin C :D

edit: bugs etc can be found here

[Edited on 19-2-2013 by mayko]
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MrHomeScientist
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[*] posted on 20-2-2013 at 15:00


A tiny amount of Elephant Toothpaste that I had leftover after a large scale demo. Rather than washing it down the drain, I mixed the few drops of each solution that was left over and it foamed up mightily :) There's a bit of starch added in to color the foam blue.


20130215_132650.jpg - 255kB
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kristofvagyok
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[*] posted on 21-2-2013 at 14:46




Long ago someone mentioned that how bad could be when something is overreacting... Someone in our lab had a large scale nitration (3 mol aromatic aldehyde and a lot nitric and sulfuric acid) what was accidentally left over.... Do not try to reproduce it.




I have a blog where I post my pictures from my work: http://labphoto.tumblr.com/
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AndersHoveland
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[*] posted on 23-2-2013 at 02:50


Crystals of copper(II) acetate:

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Pyro
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[*] posted on 23-2-2013 at 04:54


how do you make them grow like that? that's really cool!



all above information is intellectual property of Pyro. :D
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[*] posted on 23-2-2013 at 09:20


That photo is taken from Wikipedia.
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kristofvagyok
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[*] posted on 23-2-2013 at 14:22




Finally a successful nitration. This time bit more than 400g of 4MeO-acetophenone was nitrated:D




I have a blog where I post my pictures from my work: http://labphoto.tumblr.com/
-Pictures from chemistry, check it out(:

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Organikum
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[*] posted on 24-2-2013 at 09:28
Microwave Powered Steam Distillation


Out of the endwise vertical microwave comes a 29/32 to some addition thingie, to a splashhead and away through a 40cm high performance condensor to the far far away collecting flask.
800 nominal Watt of MW power, when heated up it steams 4-500ml in 20 minutes on 80%, cleaner and faster then a steamgenerator.

And it looks beautiful as I recognized when sorting the pics today :D

/ORG




[Edited on 24-2-2013 by Organikum]

P2230303.geaendert2.JPG - 255kB
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Organikum
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[*] posted on 26-2-2013 at 21:49


Thats now only indirectly chemistry related but I think it is cute so I hope I will be forgiven.

And its a riddle: What is it?



P2240313.geaendert.JPG - 158kBP2240315.geaendert.JPG - 173kB
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[*] posted on 26-2-2013 at 23:27


It's a geared motor with a low rpm output shaft. Peristaltic pump?



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mayko
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[*] posted on 27-2-2013 at 11:12


Copper ammonium oxalate. The crystals were so tiny that they had to be microphotographed, but I was quite pleased with them.

CuOx-2.jpg - 51kB
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[*] posted on 2-3-2013 at 05:53


Guys, there's more and more great photos here, well done. :)

Anders, how big are those awesome crystals? 5 mm?

Here's a really overexposed photo of you know what. ;)
(It was taken during the time I was purifying the accumulated batches. I don't work with it anymore. Thanks to my friend for letting me use his camera.)

<img src="http://i135.photobucket.com/albums/q136/endimion17/pokusi/cuttingpurewhitephosphorusindark.png" width="800" />

I think it was a half minute exposure, perhaps more. I was really afraid I was "tickling the dragon's tail" as it looked as it was few seconds short of bursting into flames, but had to be very still with the knife and the tweezers.

<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: reduced image width]

[Edited on 7/7/13 by bfesser]




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Pok
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[*] posted on 3-3-2013 at 09:04


Quote: Originally posted by Endimion17  
Here's a really overexposed photo of you know what. ;)
That's really amazing! It seems to glow like a light bulb. :o

Here are some of my copper compounds: acetate and sulfate.

test.jpg - 104kB
It now weights about 500 grams and that's enough. :D

test1.jpg - 146kB
Some copper acetate crystals

test2.jpg - 46kB
The largest one...

test3.jpg - 83kB
...and a smaller one.

All of them were grown from only metallic copper, acid and air. The formation of these two salts from these 3 reagents took 1-2 years and the growth of the crystals took 3-5 years.
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kavu
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[*] posted on 3-3-2013 at 09:11


Quote: Originally posted by Organikum  

And its a riddle: What is it?


That would be the turntable synchronous motor for microwave ovens.
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Mailinmypocket
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[*] posted on 3-3-2013 at 09:47


Pok! Amazing copper crystals!!

On the subject of crystal growing, has anyone tried growing crystals in gel? Came across this page last week...

http://chemmovies.unl.edu/chemistry/smallscale/SS072.html


[Edited on 3-3-2013 by Mailinmypocket]
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[*] posted on 3-3-2013 at 11:55


Quote: Originally posted by Mailinmypocket  
kavu! Amazing copper crystals!!

On the subject of crystal growing, has anyone tried growing crystals in gel? Came across this page last week...

http://chemmovies.unl.edu/chemistry/smallscale/SS072.html


Hmmm, interesting... I haven't tried it myself, but I have crystallized CuSO4 with a low temperature procedure.
I wonder how many incredible Ru crystals would form if you melted ruthenium and kept the temperature just below its melting point, decreasing it each day very little, letting it crystallize very slowly, forming enormous metallic crystals!




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[*] posted on 3-3-2013 at 12:57


Pok, those are spectacular. I think you could make some serious money if you sell them.



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