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strontiumred
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[*] posted on 2-7-2011 at 08:30


Here is some blue sodium hypomanganate, Na3MnO4.
Thanks to Mixell for the method.

12NaOH + 4MnO2 + O2 ---> 4Na3MnO4 + 6H2O.

<a href="http://www.flickr.com/photos/strontiumred/5894390500/" title="Hypomanganate.jpg by strontiumred, on Flickr"><img src="http://farm6.static.flickr.com/5151/5894390500_c959d89115.jpg" width="450" height="434" alt="Hypomanganate.jpg"></a>

[Edited on 2-7-2011 by strontiumred]

[Edited on 2-7-2011 by strontiumred]

[Edited on 2-7-2011 by strontiumred]
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spotlightman1234
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[*] posted on 2-7-2011 at 11:54


Quote: Originally posted by strontiumred  
Here is some blue sodium hypomanganate, Na3MnO4.
Thanks to Mixell for the method.

12NaOH + 4MnO2 + O2 ---> 4Na3MnO4 + 6H2O.

<a href="http://www.flickr.com/photos/strontiumred/5894390500/" title="Hypomanganate.jpg by strontiumred, on Flickr"><img src="http://farm6.static.flickr.com/5151/5894390500_c959d89115.jpg" width="450" height="434" alt="Hypomanganate.jpg"></a>

[Edited on 2-7-2011 by strontiumred]

[Edited on 2-7-2011 by strontiumred]

[Edited on 2-7-2011 by strontiumred]
Wow, what a beautiful compound! could you please send a link to the thread with the synthesis, or tell me how to make it?
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Xenomorph
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[*] posted on 2-7-2011 at 12:50


Here is some nitroguanidine I made. First one is impure stuff, second one is recrystalized from boilig water. I will use it to make aminoguanidine, but I am quite busy right now. Is it safe to store this in dry form? I have read this is pretty insensitive and also I have read this is stored with 20% water not in dry form.

P1010671 (Small).JPG - 46kBP1010675 (Small).JPG - 36kBP1010698 (Small).JPG - 50kBP1010708 (Small).JPG - 58kB
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ItalianChemist
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[*] posted on 3-7-2011 at 03:19


this is my sodium hypomanganate(V), obtained from sodium hydroxide and MnO2

DSC01969 1 copia.JPG - 93kB
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strontiumred
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[*] posted on 3-7-2011 at 08:29


Hi,

Mixell suggested this method:
Quote:

Mix (very well) molar amounts ( 3:1 ratio) of NaOH (prills or powder) with a finely divided manganese dioxide powder, I used 10-15 grams of NaOH. Put it all in a beaker and mix well. Put it on a hotplate and heat the hotplate to about 300 degrees, so if you put a prill of NaOH directly on the hotplate- it will melt (but do not heat above that). Steer and divide possibly accumulating masses of matter every few minutes. Check every 10 min a small sample of the mix, when all of it will be blue (allow for a tiny bit of unreacted MO2 to remain, if they refuse to react, you can't win them all) switch off the hotplate and allow it to cool while stirring every 2-3 minutes, thats basically it. Be prepared for the fact that the bottom of the beaker will be slightly damaged. If all goes well- post some pictures, May be I will do the same in a few days.


I don't own a hotplate (yet) so I simply ground 350mg manganese dioxide and 550mg of sodium hydroxide together and heated over an alcohol lamp for about 15 seconds, removed for 5 seconds and continued like this for about 20 minutes or so. Obviously any glass will be attacked by the hydroxide so if you have a steel crucible that would produce better results.

One thing is you have to keep the solid totally dry. Any water formed must not be allowed to consense back into the mix as it will cause the following reaction. 2Na3MnO4 + 2H2O ---> Na2MnO4 +MnO2 + 4NaOH.

DerAlte has posted some great info in the permanganates thread including this:
MnOxy.doc
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dann2
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[*] posted on 7-8-2011 at 18:25



Some Oxide spots on Nb by placing drops of KCl solution on a Nb sheet and connecting the sheet to + and putting a resistor end into the blob of KCl solution. (sheet an Anode, resistor end the Cathode).
The different colours are different thicknesses of Oxide. Better pictures on web if you look.
Dann2

nb.jpg - 67kB

[Edited on 8-8-2011 by dann2]
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blogfast25
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[*] posted on 22-8-2011 at 10:05




Amethyst coloured Ferric alum ‘geode’ (about 600 g of ammonium ferric sulphate dodecahydrate)




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[*] posted on 22-8-2011 at 10:56


Wow, a pretty photo thread.

Here's my contribution:


WP I photographed few days ago.


ZnS phosphorescent dust.


Fresh iron sulfate heptahydrate.

some rupert drops against a polarizer
my first handmade liebig cooler - never actually tried how it works...
my hand grounding a germicidal tube - It was turned off, but connected to the mains ;)




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[*] posted on 23-8-2011 at 04:32


Love that zinc sulphide!




About 500 g (about 100 mm wide) of ferrous sulphate heptahydrate, recrystallised from garden grade (unknown mixture of hydrates with an anti-caking agent - bweurk!)


[Edited on 23-8-2011 by blogfast25]




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MrHomeScientist
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[*] posted on 23-8-2011 at 06:16


@Endimion17:
That FeSO4 looks identical to the masses of crystals I'm getting from my current project of dissolving Nd magnets in sulfuric acid, neat! Your WP is beautiful too.
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[*] posted on 23-8-2011 at 06:33


Large quartz crystals, lab made :) One was traded to Theo Gray.


I can post more crystals of salts and stuff, I completely forgot I had a box of sealed samples. Also stuff from my friend Ivan at www.periodictable.ru :)
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[*] posted on 23-8-2011 at 11:33


Not aesthetically pleasing but pretty, in the sense that I was able to observe and photo the fleeting existence of this complex.


Triiron Dodecacarbonyl - Fe3(CO)12

Tank
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[*] posted on 23-8-2011 at 16:47


Quote: Originally posted by Endimion17  

my first handmade liebig cooler - never actually tried how it works...


That's a really neat homemade condenser! Did you use an ordinary bunsen burner or blowtorch to melt the glass? I've been trying to make a crude Allihn condenser, but I can never get the bulbs to form... maybe my propane bunsen isn't hot enough.
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blogfast25
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[*] posted on 24-8-2011 at 04:51


Quote: Originally posted by m1tanker78  
Triiron Dodecacarbonyl - Fe3(CO)12

Tank


Curious as to how you made that complex!




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Lambda-Eyde
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[*] posted on 24-8-2011 at 05:59


Benzoic acid crystals made from sodium benzoate and NaCl. Maybe some of you have seen it in the Wikipedia article..? ;)







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Endimion17
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[*] posted on 24-8-2011 at 05:59


Quote: Originally posted by bob800  
That's a really neat homemade condenser! Did you use an ordinary bunsen burner or blowtorch to melt the glass? I've been trying to make a crude Allihn condenser, but I can never get the bulbs to form... maybe my propane bunsen isn't hot enough.

Thanks. Propane-butane blowtorch, no additional oxygen. Bunsen can't do it because flamerorking requires sharp flames. It's ok for sooty annealing, though.
It's very difficult to make because of several glass connections and lots of stresses, but now I understand the price of a professional cooler.
Your bunsen burner probably is hot enough. The problem is in heat delivery i.e. gas consumption. Some burners consume less gas, so their energy output is lower, though the temperature is sufficient.

@Wizzard: lab made? w00t!

[Edited on 24-8-2011 by Endimion17]




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[*] posted on 24-8-2011 at 06:17


Quote: Originally posted by Wizzard  
Large quartz crystals, lab made
How do you make them?
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[*] posted on 24-8-2011 at 07:44


Quote: Originally posted by watson.fawkes  
Quote: Originally posted by Wizzard  
Large quartz crystals, lab made
How do you make them?


Isn't quartz supposed to be somewhat soluble in super saturated steam or something like that?

Otherwise, crystalisation from a melt?

Good luck with both in a home lab!




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[*] posted on 24-8-2011 at 08:27


Oh, I didn't make them :) Somebody with a large autoclave did, and these were produced as the process was being learned, judging by the shapes.
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[*] posted on 24-8-2011 at 11:50


Quote: Originally posted by Wizzard  
Large quartz crystals, lab made :) One was traded to Theo Gray.




That must be a really small $20 bill:P
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[*] posted on 26-8-2011 at 14:19


Quote: Originally posted by blogfast25  
Quote: Originally posted by m1tanker78  
Triiron Dodecacarbonyl - Fe3(CO)12

Tank


Curious as to how you made that complex!


Ditto!
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[*] posted on 27-8-2011 at 05:19


Quote: Originally posted by sternman318  
Quote: Originally posted by blogfast25  
Quote: Originally posted by m1tanker78  
Triiron Dodecacarbonyl - Fe3(CO)12

Tank


Curious as to how you made that complex!


Ditto!

In my case, it's the direct union of hot CO with hot, finely divided iron. Some of the pentacarbonyl converts to the [solid] dodecarbonyl which collects on and around the vent cracks.

Tank
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[*] posted on 2-9-2011 at 14:27


You might find this pretty, or not.
This is an aluminium (air) cell, an exotic cell that not many people are familiar with. The anode is made of aluminium foil and the cathode is made of graphite rods from pencils. The extra twist is that I'm using Fenton's reagent as an oxidiser instead of air, which allows a much higher power output, as shown.
The white LED is hooked up to a joule thief because it needs 3V to operate while the cell only supplies half of that.
In my opinion, this surely beats a lemon battery :)
It doesn't show up very well on the camera, but the white LED is bright enough to give retina burns if you stare into it for a few seconds.

EK2.jpg - 243kB
If you would like a sense of scale, the glass jar is about 10cm tall (4 inches).

[Edited on 9-2-2011 by White Yeti]
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[*] posted on 2-9-2011 at 14:39


Nice! You could put 2 cells in series to get enough voltage. What's a joule thief?



The single most important condition for a successful synthesis is good mixing - Nicodem
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[*] posted on 2-9-2011 at 15:49


I could have put two cells together to get enough voltage, but I was running out of chemicals at the time (I didn't even have any iron acetate catalyst!), I barely had enough to build one cell.

I'm restocking in peroxide tomorrow, I have some fresh iron salts I prepared this morning to play with, and I have some new pencils and aluminium foil.

A joule thief is a small electronic circuit used to boost voltage from a low voltage source. If you try to light a white LED with a fully charged AA battery, you will find out that it won't light up because it needs at least 3V in order to function. Lithium button cells have voltages exceeding 3V so they can light up white LEDs on their own, but all the other cells, including this one, cannot.
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