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Author: Subject: Make Potassium (from versuchschemie.de)
Pok
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[*] posted on 16-12-2010 at 12:16


Quote: Originally posted by blogfast25  
if one can replicate it then we'e essentially done here. If not, it's tar and feathers for our German friend...

Did I tell you that I am German? :) Some Austrians and Swiss would be deeply offended by ignoring their existence :D - most of them also speak German. ;)
And: I would take the tar and feathers if none of you will produce that kind of K balls that I produced! - therefore: please do your experiments with attentiveness - because I don't wanna look like a chicken. :D
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blogfast25
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[*] posted on 16-12-2010 at 12:43


No, but versuchschemie.de is German. I jumped to conclusions...
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Pok
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[*] posted on 16-12-2010 at 13:44


Quote: Originally posted by blogfast25  
No, but versuchschemie.de is German. I jumped to conclusions...

Your conclusions are correct ;). Although I'm not a "nazi" or so :D ...I hate these people even more than you (probably). I think everytime when I say that I am German I have to apologize for stupid Hitler and people who followed him. :( So maybe now you don't call me a German but just pok? :D
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[*] posted on 16-12-2010 at 13:53


No problems with being German though...
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[*] posted on 16-12-2010 at 13:55


Hi Pok

before this all ends in an endless flamewar, i would suggest that you use the improvements in technology and set up an live video stream (maybe a chat client like IRC with video support) and let some of the skeptical users here look live at your reaction and comment it. (Some user shall sugest an good live chat client with video support as I don´t know much about it)

If you faked it, this probably also could be faked, but it will be much harder (if someone says you should move your hand in front of the camera and nothing happens, it´s an inevitable prove of faking)

Greez
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Pok
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[*] posted on 16-12-2010 at 14:12


Quote: Originally posted by hinz  
Hi Pok

before this all ends in an endless flamewar, i would suggest that you use the improvements in technology and set up an live video stream (maybe a chat client like IRC with video support) and let some of the skeptical users here look live at your reaction and comment it. (Some user shall sugest an good live chat client with video support as I don´t know much about it)

If you faked it, this probably also could be faked, but it will be much harder (if someone says you should move your hand in front of the camera and nothing happens, it´s an inevitable prove of faking)

Greez


This is a very good idea. But I (1) don't have a webcam - just a normal digicam. (2) I'd have to buy a new stopper :D - my last one is "dead". I want to repeat the experiment as soon as I have a new stopper :cool: ...I still have some nice short videos of the boiling reaction mix at different times (from beginning to the end where you can already see the large rolling and jumping K balls) - maybe this could help you?

[Edited on 16-12-2010 by Pok]

[Edited on 16-12-2010 by Pok]
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Pok
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[*] posted on 16-12-2010 at 14:29
videos


the pictures you already know. now some videos of the same (1st ever) procedure.

(1) one of my produced tiny K balls in water (doesn't prove anything but that I have K).

(2) my first procedure ever: 50ml at beginning - unfortunately very dark.

(3) same procedure: at the end - K balls jumping. (dark, too)

I hope you have Windows Media Player.

Now you can be sure: its either Na, K, Cs or Rb (or an alloy of mainly alkali metal +x) that you see in the last video. No "woods metal" (or other mainly heavy metal alloy), no mercury, no gallium - because no transparent liquid is existing with such a high densitity that these heavy metals could form such balls.


Attachment: Film.wmv (1.5MB)
This file has been downloaded 964 times

Attachment: 50ml - beginning.wmv (1.4MB)
This file has been downloaded 957 times

Attachment: 50ml - end.wmv (1.5MB)
This file has been downloaded 971 times

News from versuchschemie.de / versuchsgenie.de:

german: http://www.versuchsgenie.de/forum/viewtopic.php?f=16&t=1...

google translation:
http://translate.google.de/translate?js=n&prev=_t&hl...

[Edited on 17-12-2010 by Pok]
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[*] posted on 16-12-2010 at 14:34


Quote: Originally posted by Pok  
I think everytime when I say that I am German I have to apologize for stupid Hitler and people who followed him.


Pok, you don't have to apologize for the actions of your ancestors any more than the rest of us. My wife's ancestors (Vikings) terrorized the living hell out of my UK/Irish ancestors. I don't look for apologies from her. I'm in the driver's seat now (I think). :D




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[*] posted on 16-12-2010 at 17:15


You can hardly call one of the few sets of posts with any relevant scientific content in this thread trolling. So either you are angry or you are just have no idea of how science works.

You wont me to repeat this stuff, fine Ill do it now not because of what Pok posted, I dont want to encourage trolls, but as a last good-will gesture, for you, in a university chemical laboratory, using all the chemicals as listed, temperature controlled oven, reflux condenser. This stuff is normally used to do far more complicated reactions. This is about level 0 on degree of difficulty. So if its true, it should work. If it doesnt goodbye to you and your mate.
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[*] posted on 16-12-2010 at 18:34


I want to make the add-on that i'm using magnesium that's been stored in a glovebox since the day it was purchased and I've used it to make grignards before without the need for additional surface activation.

To do my potassium experiments, I take the portion i need out of the glovebox and its on air for about 20 minutes before it's tossed into the reaction mixture.

I'm not sure if the magnesium is the "special sauce" for this, but i just thought i'd inform everyone where it came from.
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[*] posted on 16-12-2010 at 19:19


I must ask due to videos I have seen on the internet that show ignition of Mg+KOH producing elemental K. Isn't this reaction exothermic? When they ignite the mixture it turns into a roaring flame, How come the reaction here does not pick up pace like that of normal KOH+Mg reaction? What would moderate this reaction to make it benign where as solventless reactions go heywire?




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[*] posted on 16-12-2010 at 23:48


Quote: Originally posted by Sedit  
I must ask due to videos I have seen on the internet that show ignition of Mg+KOH producing elemental K. Isn't this reaction exothermic? When they ignite the mixture it turns into a roaring flame, How come the reaction here does not pick up pace like that of normal KOH+Mg reaction? What would moderate this reaction to make it benign where as solventless reactions go heywire?


I could image that the slowness of the reaction here is due to the low solubility of t-BuO K in Shellsol as already considered possible here. And: the low temperature!

[Edited on 17-12-2010 by Pok]
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[*] posted on 17-12-2010 at 00:10


Quote: Originally posted by len1  
[...] You wont me to repeat this stuff, fine Ill do it now not because of what Pok posted, I dont want to encourage trolls, but as a last good-will gesture, for you, in a university chemical laboratory, using all the chemicals as listed, temperature controlled oven, reflux condenser. [...]
That would be very nice and I really do appreciate that effort!

I am (and most likely many others as well) looking forward to read what your results will be. Most of us have to do with less than ideal approximations of a real lab, so when you can do this under precisely controlled conditions and you have positive results, then that would mean a giant step forward in finding out the conditions, necessary for success.




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[*] posted on 17-12-2010 at 06:27


Well I performed the experiment and the results are in.

First I would like to thank Wilco for getting me to do it. However I cant blame myself for thinking the whole thing was trash given it was clear to me some parts of it were, and I did initially think some parts of it were real - but here is what happened.

100ml shellsol D70 were placed into a 250ml conical flask with 19/26 joint, connected to a Liebig condenser, which was attached to a 3-way adaptor at the top. Argon was flushed through one of the attachments (only at the beginning), the second attachment was vented through an oil bubbler, and the third, vertically above the condenser was plugged with a septum.

100ml Shellsol D70 were placed in the 250ml flask, 12.4gms KOH flakes added through a powder funneled, followed by 6.2gms of completely oxide free magnesium shavings (see photo I dont have the mesh).

The setup was placed in an air oven and heated over the course of 60mins to 200C. At about 130C water evolved - not violently as the patent says, whereupon the KOH flakes rose through the magnesium and assumed a twisted shape (as they gave up water). At 210C reflux commneced, at which point 1.2gms t-BuOH mixed with 1.2gms D70 were added in portions of about 0.5gms every 5 minutes with swirling. Vigorous reflux of the t-BuOH (bp about 80C from memory) ensued in the lower part of the Liebig. After the addition, nothing much happened for about 15mins, and I assumed the reaction will follow its previous path. At about this point however the D70 become very cloudy, and it became obvious a reaction was occuring - this was the first difference from last time. After 30mins shiny balls of molten metal - less than 1mm in diameter started appearing. With shaking and over the course of several hours these grew up to 1cm diameter in size. The whole flask and solution was coated in fine MgO sand. (Picture)

I have not the yield yet - I will establish it accurately tomorrow, but judging by the amount of MgO present, and lack of visibility of any magnesium, it appears in the range 50-100%, making this at least a liquid-phase surface layer reaction. The yield precludes solid phase, and I do not believe it to be liquid phase due to my results before.

So why the change from last time? I can not say definitively at this stage, but my best guess is as I stated earlier in the thread - the KOH and Mg must be left alone to come into close contact - as would be the case for a boundary layer reaction, with t-BuOH probably acting in the fashion described earlier in the thread. If this was purely a liquid phase reaction I would have succeeded in forming at least some K last time since there was plenty of fresh Mg surface. However the patent clearly states stir constantly.

However a lot of what I was saying before is still true. There are large differences between the post of Pok and reality. I said I was expecting the MgO particles to stick to the K like glue - and they clearly do. Sedit wrote he would expect much MgO sand in the reaction product. I agree its everywhere in my reaction, yet in the germans pictures there is no MgO to be seen. Possibly a little trick.

SO is he a troll? Strictly no, although by playing a few games with us he made me believe so. How did he get those large clean balls? Possibly by purifying and inserting back into the mix so that he would have the best looking results. Clearly he will now claim otherwise. Maybe hes one of the patents authors, I dont know.

I will repeat the experiment a few times varying the reflux temperature, amount of t-BuOH and shaking regime, to see if any improvement is possible.

The potassium balls can be coalesced (I think I have about 10-20 will have to check tomorrow) and this is a viable K generation method for the home chemist. It is not for the professional and I do not see it replacing the electrolytic method I have been using at this stage because the reaction fairly slow judging from the rate of H2 evolution (< 1 bubble per sec) and the potassium needs a lot of work to purify.

K1.JPG - 24kBK2.JPG - 14kB
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[*] posted on 17-12-2010 at 06:50


Len1, many thanks for doing this experiment and sharing the results. And congrats for having (at least to a great extent) success. VERY good!
There may still be issues with Pok's experiment and writeup but this definitely proves that he is not fucking up a lot of people.

This makes me more and more eager to do thus myself. Hopefully tomorrow!




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[*] posted on 17-12-2010 at 07:13


Quote: Originally posted by len1  
I have not the yield yet - I will establish it accurately tomorrow, but judging by the amount of MgO present, and lack of visibility of any magnesium, it appears in the range 50-100%, making this at least a liquid-phase surface layer reaction.
Example 1 in the patent computed yield by a workup that includes solvent removal (vacuum distillation or filtration), a density separation of product K from solids with 1,4-dioxane, upon which molten K will float, and suction filtration of molten K.

Personally, I'd like to know the mass balance of the t-BuO moiety in the products and residues, to see where it ends up and if there are side reactions in practice that lead to its destruction.
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[*] posted on 17-12-2010 at 07:33


Yes, here are some more pictures. I did not have time to let the potassium cool to rt and opened the flask to the atmosphere at about 70C. Immediately the fairly clear D70 above the potassium (as most of the MgO had settled on 1hr standing) went cloudy. This had a positive side to it proving theres solved t-BuOK - and there is nowhere else for the t-butanol to go, in the D70. This must be the key to the reaction and its yield, t-BuOK solved in paraffin reacting with Mg to give K and (t-BuO)2Mg + 2K, the former reacting with the water to regenerate t-BuOH. I dont think this is known is scientific circles.

On examining the product I have only about 5-6 balls of potassium, so the work involved in purification is not extensive, and this might be a viable method in the lab as well. Ill know for sure tomorrow when I get to coalescing/purifying and determining the yield.

K3.JPG - 80kB

[Edited on 17-12-2010 by len1]

K5.JPG - 17kB
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[*] posted on 17-12-2010 at 07:35


Wonderful work, Len. Such an easy method to synthesize alkali metals, alkali metal production in the home lab is now child's play!

And Pok, you are my hero. This synthesis deserves a pdf in the prepublication and the sciencemadness library!

Ever since this thread started, i've been looking for t-butanol, unfortunately, I still don't have any. I'm dying to try this...

And Pok , please stick around sciencemadness, your posts are much appreciated.


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[*] posted on 17-12-2010 at 11:47


I can also confirm i was able to make potassium using candle wax solvent. It requires a much more extensive and dangerous workup to get clean balls of potassium but it can be done.

I also tested with tert-amyl alcohol and had similar success.

I'll be making a video on my candle wax process in the near future. First i'm going to try ways to make it safer.

In my opinion, the D70 method is safest for the amatuer.

Anyway, I'm formally saying potassium can be made from magnesium and KOH along with a tert-alcohol and an aliphatic solvent.
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[*] posted on 17-12-2010 at 12:09


Quote: Originally posted by len1  
There are large differences between the post of Pok and reality.
This is true in 1 point for your experiments observations: MgO dust instead of MgO crusts. Nothing else.

The other observations by you sound like mine:
- After 30mins shiny balls of molten metal
- less than 1mm in diameter started appearing.
- yield appears in the range 50-100%
Quote: Originally posted by len1  
SO is he a troll? Strictly no, although by playing a few games with us he made me believe so.
If you consider "answering questions" as "playing games" - yes. then I played games.
Quote: Originally posted by len1  
How did he get those large clean balls?
My MgO formed crusts instead of dust. Thats the explanation for no MgO dust on K surface.
Quote: Originally posted by len1  
Possibly by purifying and inserting back into the mix so that he would have the best looking results. Clearly he will now claim otherwise.
Exactly. I claim otherwise! This would mean that I lied. I didn't lie 1 word in this forum. WHY should I do this? If my K was covered with MgO - I would show it - because this kind of K is 100% better than no kind of K. You only seem to believe your own eyes. If you didn't get it: nobody is able to get it??? No.
Quote: Originally posted by len1  
Maybe hes one of the patents authors, I dont know.
I would be proud to be one of the authors. Unfortunately, THEY are the real heros here. Not me.
Quote: Originally posted by condennnsa  

And Pok, you are my hero.
:) And the patents authors are MY heros :D.
Quote: Originally posted by condennnsa  
And Pok , please stick around sciencemadness, your posts are much appreciated.
Unfortunately, I don't really know so much details about chemistry like you all. This really was my one and only "luck luck luck experiment". I made potassium nitrite in another experiment in high yield and purity. But nothing else. I need the information on sciencemadness and versuchschemie.de much more than you will need me :D.
Quote: Originally posted by NurdRage  
I can also confirm i was able to make potassium using candle wax solvent.
This is a very usefull information for many people! cheaper and easier available. Little or small K is better than no K for home chemists (although a more dangerous K isolation as you say)! And if this method will be shown to be improvable: perfect!

[Edited on 17-12-2010 by Pok]
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[*] posted on 17-12-2010 at 12:56


len1: fantastic, congrats and thanks for taking woelen’s (and others’) advice and finally replicate it. If anyone here could do it, it was always going to be you…

pok: congrats to you as well. Vindicated and all shadows of suspicion lifted. Please go and inform versuchschemie.de, if you haven’t already.

And I’ve got everything ready to go tomorrow or Sunday. Exciting times!
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[*] posted on 17-12-2010 at 13:07


Good job, its Christmas come early! My t-BuOH is coming in January, grr



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[*] posted on 17-12-2010 at 15:11


Len,

Thank you for doing the experiment! I was more excited reading your post than watching the game-winning goal of a football game! It is easy to be sceptical and sit on one's ass and speculate on the merits of a reaction but you sir, have never been one to sit in the armchair!

I eagerly await the purification and the yield!

Pok,

I think we're all glad you didn't deceive us and that this patent actually turned out to not to be bullshit.




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[*] posted on 17-12-2010 at 16:22


len1: excellent experimental work as always. But I feel you disgrace yourself by trying to (still!) accuse Pok of chicanery, after essentially proving him correct. One would think that after reproducing his success so closely, you would chalk up any remaining discrepancies to other minor differences in experimental conditions rather than trying desperately to salvage this 'pok must be a troll' idea. Why not just man up and apologize?

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[*] posted on 17-12-2010 at 17:13


holy s*** nurdrage is here!!

and holy s*** it actually worked!!!

this is like christmas comes early I know someone said it but I want to say it again!!

thanks len!! gj to all of you!! tia
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