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blogfast25
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In an undisturbed liquid of the same density as liquid potassium they'd HAVE to be.
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blogfast25
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And did you see this:
Peter, 28/11/2010; 1:36 at:
http://www.versuchschemie.de/hartmut.php?t=14677&postday...
He wrote near the end of his report: “Überraschung: Plötzlich stiegen einige, max. 0,5 mm größe K-Kügelchen auf.”
Transl.: “Surprise: suddenly a few K-globules rose up, max. 0.5 mm.”
Wishful thinking? Susceptibility? Or truth?
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len1
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Thats an interesting point. However I am not 'theorising' I have them sitting around, and potassium nuggets that large are buttons, no more than 1cm
high.
That also follows from theory. When they have exactly the same density as the solvent (as K does at about 80C in paraffin) they ARE perfectly round,
but then they do not sit on the bottom but float all around the liquid. The reasomn the nuggets are flattened in D70 is that at its solidification
point the density of K rises to about 0.89, that of D70 is about 0.75 - a differential of 0.14 gm/ml. An approximate formula for the height of
globules is
h = sqrt(2 * surface tension/(g * density differential))
giving about 0.5 cm, in rough agreement with my results. As you can see 3cm 'nearly round' globules are impossible in D70. So a merry troll Xmas to
Pok, and you can see the reason for his desire to quickly disappear from here.
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woelen
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@len1: Please do not say Pok is a troll. Let's keep this constructive  My
experiment at least shows that K-metal can be made. Now we need to find a method to make it more effective and to have the K-metal clump together into
balls. Remember, we are talking about making K-metal, something which is not supposed to be easy at all. So, I am determined to put more effort in
this to find out how this can be optimized.
Your remark about a solid-solid reaction is correct, but I agree with Pok that this does not need to be a solid-solid reaction. In my experiment I saw
the KOH liquefying when the temperature went through 200 C or so. The Mg touches the somewhat liquiefied KOH (I actually think it is a liquid layer
around the solid material, the liquid maybe some K-butoxide and KOH mixed). So, occasional stirring helps, bringing fresh Mg to the KOH, but constant
stirring does not help, because then the Mg particles float around in the paraffin oil and do not get in contact with the KOH/K-butoxide.
Another reason why occasional stirring might help is that it brings back t-butanol in solution. In my experiments I noticed formation of droplets,
sticking to the glass (you can see that in one of the pictures I made) and when you shake, then these droplets again are brought into the solution
again.
I am eagerly waiting for my ShellSol D70 to arrive. I still did not receive it, while the order already was confirmed by Kremer-Pigmente last Friday
 When it arrives, I will exactly copy Pok's experimental setup, using my 65...100
um magnesium powder and then I'll let it reflux for 4 hours or so. If this setup still does not work, then maybe we should consider purchasing some of
Pok's Mg-metal, but for the time being I am inclined to believe that any source of decent quality Mg, any source of decent quality KOH and any source
of t-butanol should do the job. I indeed think that the size of the magnesium particles is critical and that this is the hard part of this, simply
because Pok made the particles himself from larger pieces of Mg-metal.
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Sedit
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This is what I expect the reaction to look like at the end even if it where successful yet poks reaction displayed no precipitate,
It is the results of Peters first experiment you can see what I would expect and that is a flask full of Magnesium hydroxides(oxides?) precipitate.
You suggested it was a weak argument but im not so sure im as easy to convince and even less so now that I see an experiment repeating poks that looks
the way I would expect it to.
I wish he had taken pictures of the so called formed K that came up with the addition of IpOH at the end so I could come to something more conclusive.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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blogfast25
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@Sedit:
Hmmm… looks to me that Peter’s precipitate is simply more floccular than pok’s but what does that mean or prove to you? To me not much, IMHO.
The bottom gunge does look quite different from what magnesium powder/sand is supposed to look like but photos are notoriously deceptive in these
circumstances.
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blogfast25
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@woelen:
I wouldn’t have chosen the term ‘troll’ but I really think we cannot a priori exclude the possibility of a hoax by pok. I’m not
fussed about possible ‘motives’: unless he confesses these are essentially ‘unknowable’ and thus of no concern to us.
Having said that, I’m proceeding as if I’m sure it’s not. Next run with t-butanol, Shellsol D70 and conditions replicating pok’s as much as
possible.
An interesting thought is that if pok’s right and honest about the 70 – 80 % yield then the reacting away of Mg should in itself make coagulation
of the K much easier than if you only produce tiny amounts…
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Sedit
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Quote: Originally posted by blogfast25  | @Sedit:
Hmmm… looks to me that Peter’s precipitate is simply more floccular than pok’s but what does that mean or prove to you? |
I can't say that it proves anything other then Peter honestly performed the experiment. It does imply to me however that Poks results are not adding
up with experimental data.
| Quote: Originally posted by blogfast25 |
The bottom gunge does look quite different from what magnesium powder/sand is supposed to look like but photos are notoriously deceptive in these
circumstances.
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Its not so much that Poks precipitate looks off what strikes me as odd is the complete lack there of. The more I look at it the less sense it makes to
me. It just looks like metallic sand of some kind(perhaps even the woods metal len was speaking of) just melting down and forming bigger balls around
some KOH flakes. I don't see a change in the KOH only a change in the "Mg" thats around it and that bugged me from the start.
I have some faith in the reaction considering Mg+KOH ignited produces Potassium but im having a hard time getting my head around this working the way
its claimed. I see little to gain in faking it other then false praise so its warping my mind a bit.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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len1
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Destructive is when you try to bring another persons argument down with no good reason. And there is plenty of this around here. However when a person
is lying to you, its constructuve to put an end to it. Im used to getting crap from students, although unlike here most of them do it honestly -
beating about the bush in that instance is only superficialy constructuve. It actually harms people in the long term. Same here.
Further posting a lot of stuff about this before you have been able to reproduce his wonderful balls of K only serves to encourage future trolls - hes
having a great time watching you all.
Regarding the liquid-solid reaction, its interesting that a person who knows not the difference between water of crystalization locked inside a dry
powder and water picked up from the atmosphere by a deliquesent substance, would suddenly categorically state that this is a solid-liquid reaction,
without having shown any inclination towards theory before that statement. He did this of course to get out of a tight situation in what he thought
would be the best way he could.
[Edited on 15-12-2010 by len1]
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watson.fawkes
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| Quote: Originally posted by len1 | | Destructive is when you try to bring another persons argument down with no good reason. And there is plenty of this around here. However when a person
is lying to you, its constructuve to put an end to it. |
If you have definitive evidence that he's lying,
please present it. Nothing I've seen here rises to that status. There are suggestive things that support a hypothesis of lying, but neither are these
unambiguous nor do they support only a single hypothesis. I have not yet seen anything like clear and convincing evidence of a lie here.
What we do have here, and most certainly so, is an absence of evidence that he's not lying, given the absence of reproduction of his synthesis report.
I shall assume that we here all know the difference between absence of evidence and evidence of absence, so I shan't belabor the point.
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condennnsa
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| Quote: Originally posted by Pok | I'll be back next year or so - or if I see the first pictures of large K balls here  . I think my presence isn't needed anymore. Read the patent, read versuchschemie.de, read here: you will do it - if I forgot about this thread: keep me in mind as the hero who gave you somehow the
"gold of the hobby chemists".
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I agree with Len1. Pok, if you are truly genuine, you have the responsibility to stick with us all the way. After all, I don't think we take up much
of your time with our questions, so why leave us? While some here may be convinced this is fake, there are others who are not, and woelen's results
are encouraging. And yes, If this really turns out to work, you will be a hero here, one further reason to stick around...
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DJF90
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Whats the point in him sticking around. He's probably fed up of those making accusations, and he's told us everything we need to know to make it work
like he did. Until someone replicates the experiment several times under exactly the same conditions he used and still have no result, I'm going to
regard this as genuine.
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Magpie
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Next year = 2 weeks of Christmas vacation. Perhaps pok is going sailing in the Caribbean. 
The single most important condition for a successful synthesis is good mixing - Nicodem
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Pok
potassium Prometheus
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@ len1
| Quote: Originally posted by len1 | | The reasomn the nuggets are flattened in D70 is that at its solidification point the density of K rises to about 0.89 |
Where do you got this info from? english wikipedia? Solid K is 0.856 - 0.862 (different sources). As far as I know, potassium doesn't have a density
anomaly like water. In the liquid state it therefore should have an even lower density: density of liquid K < 0.86.
http://kremer-pigmente.de/shopint/PublishedFiles/70470shd.pd... - page 5 "dichte" (=density) - 0.792 at 20°C - lower at 15°C (0.787) - at 100°C
maybe even higher ? (I don't know): density of shellsol at 100°C > 0.792.
the real differential therefore should be around 0.07gm/ml or so.
As you can see: they are possible!
| Quote: Originally posted by len1 |
So a merry troll Xmas to Pok, and you can see the reason for his desire to quickly disappear from here. |
Quickly? I've answered ANY question here. Even strange ones. Merry troll Xmas to you as well, len  .
@ woelen
If you want it: please give me a U2U message as I won't find any request here in the thread after some days. But as I said: you won't need my Mg.
@ Sedit
| Quote: Originally posted by Sedit |
Its not so much that Poks precipitate looks off what strikes me as odd is the complete lack there of. [...] The more I look at it [...] It just looks
like [...] I don't see [...] |
Your scepticism seems only to be based on my photos. And I already explained the reason for lacking of a dust-like percipitate. Do you really think I
would fake the hole synthesis so perfectly and forget about such a simple thing??? If you want to believe in a fake, you will see
"woods metal" and "unchanged KOH". If you are a scientist: repeat and value afterwards!
At the beginning it is very white and voluminous at the end the so called "KOH" is gray MgO (due to impurities I think)! If I look at it, I can follow
your argument. But it is not true. Another point (I'll answer it befor the question may arise): look at versuchschemie: The first pictures show the
erlenmeyer deep in the sand (50ml mark) - at the last pictures the erlenmeyer stands on the sand. The hight of the ingredients
doesn't seem to have changed - but if you now know this background maybe this point is explained now.
@ len1
No. I'd rather see my experiment reproduced. You shouldn't be so aggressive only because I did the experiment successfully where you made mistakes.
Everyone makes mistakes. Even me (remember my not willing to coalesce tiny K
globules).
| Quote: Originally posted by len1 |
a person who knows not the difference between water of crystalization locked inside a dry powder and water picked up from the atmosphere by a
deliquesent substance |
You really must be joking now  . I told you at the first time: I
know that techn. KOH contains water. I also said: thats why hydrogen is evolved before t-butanol is added. I said
"But maybe during grinding you raised the water content from 10% to 20%."
| Quote: Originally posted by len1 |
categorically state that this is a solid-liquid reaction, without having shown any inclination towards theory |
Look at versuchschemie.de. I already referred to this site here. I said (translate with google if you want)
"Erklärung:
Magnesium reduziert Kaliumhydroxid zu Kalium. Tert.Butanol dient als eine Art Katalysator, wobei mit KOH Kalium-Alkoholat gebildet wird, welches mit
Mg reagieren kann und den Alkohol wieder freigibt (schätze ich).
2 Mg + 2 KOH -> 2 K + 2 MgO + H2
Die anfängliche Wasserstoffbildung vor tert.Butanol-Zusatz ist durch Restwasser aus dem KOH zu erklären:
H2O + Mg -> MgO + H2"
K-alcoholate (solved in Shellsol) - behaves like a liquid and reacts with Mg (solid).
| Quote: Originally posted by len1 |
He did this of course to get out of a tight situation in what he thought would be the best way he could. |
"Of course". You can read my mind! (OMG!)
@condennnsa
Sorry. But I don't have the responsibility. I have a real life as well. and: (1) Nobody is asking me anything anymore (2) Nobody has come close to my
procedure. - I'm not interested in the exact mechanism behind the reaction. So I don't want to read everything in this thread (which
also deals with the mechanism). If you wanna ask me, please put an "@Pok" infront of your question (if there are still questions left
which only I can answer - this shouldn't be the case if you adhere to the patent where absolutely everything is described in the
neccessary extent). Otherwise I will not answer, because I don't wanna search the word "pok" in the hole text. I will answer them tomorrow. This will
be the last time as I don't wanna go into the internet and everyday reading tons of suspicions without anyone having done it my way and adhering to my
advices (see in this thread).
@Magpie
No. I'm just bugged by questions I already answered  . Or by statements which
don't deserve an answer (e.g. "woods metal"). Caribbean would be nice - but Xmas without snow? .
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len2
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Here's my advice:
Learn to read english sentences
check the density of potassium
en.wikipedia.org/potassium
learn about the behaviour of density for most liquids with temperature
stop trolling, and leave these people alone.
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Pok
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@len2
do you talk to me?
I'll try it. And you please learn german ...and hindu .
The only sentence I can imagine what youre aiming at is len1's statement that I don't know the difference between "water of cristallization locked
inside a dry powder" and a "wet" compound. I know that KOH can contain water of crystallization. But it doesn't matter in which form the water is in
the KOH. KOH * H2O also absorbs water from the air and forms KOH * 2H2O or even KOH * 4H2O. The amount of H2O molecules will increase in bought KOH
(containing a little KOH*H2O) if you don't handle it as fast as you can (not grinding) while keeping it in air (e.g. for weighting). It can take up to
4 molecules of water (wikipedia says) and will still look dry. THAT (more or less) may have happened during grinding in len1's case.
If I remember correctly, len1 said that both the unchanged and the ground KOH contained 10-12% water. I really have doubts about that. You can't grind
KOH in air without raising its water content because air contains water and KOH is highly hygroscopic. A question to len1 would be: (how) did you
measure the water content? and how long did you let the KOH remain in air (how long did you grind)?
It says:
"Liquid density at m.p.: 0.828 g·cm−3" - my 0.07 difference compared to shellsol D70 therefore should be
lowered to 0.03 or so - I therefore should thank you for your advice
Yes. "most liquids" - I also gave you the pdf of Shellsol D70 with 2 temperatures and increasing density from 15°C to 20°C. From this point, I asked
"maybe?" and "I don't know"
that density may rise with rising temperature (although even I wouldn't understand it).
stop being aggressive without arguments. this is poor.
[Edited on 15-12-2010 by Pok]
[Edited on 15-12-2010 by Pok]
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Pok
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@ len1: I forgot about this:
| Quote: Originally posted by len1 | An approximate formula for the height of globules is
h = sqrt(2 * surface tension/(g * density differential))
giving about 0.5 cm, in rough agreement with my results. |
I must admit that I don't know this equation (as I'm not a chemist I don't have to know it ...but its interesting...you always learn) and therefore I don't know
whether it is correct. It looks plausible to me. But: where do you got the value (which you didn't show us) of surface tension of K? And: isn't it also dependent on the sourrounding medium? (I only remember water tension which
shows differences if its pure or when soap is added) - where do you got this value from?
I rearranged the equation to get your value. If your "g" is 9.81, it should be: 0,0171675 N/m. ->
where do you got this from?
After (hopefully correct) recalculating it (0.036 (more exactly than 0.04) instead of 0.14 density difference), it would still only be 0.99 cm height.
possible reasons (because my balls in ca. 3 cm dimensions were nearly round):
- surface tension value isn't correct
- equation isn't correct (or another factor is needed to include the medium properties (shellsol) on surface tension)
- K and Shellsol have even much lower difference in density*
- something I don't know
*the difference in density of K and Shellsol would have to be 0.005 instead of 0.036 to let the potassium height rise up to 2.6cm (if surface tension
and equation are correct) - a value quite imaginable in my case. I'm quite sure about the K and Shellsol densities. But the difference of 0.005 and
0.036 only is 0.031 - maybe the densities change in a different way at high temperatures (esp. that of the Shellsol - maybe
decreasing in a much lesser extent (or even increasing?) than that of K)- and/or the surface tension or equation may
not be correct.
-> I suspect both: (1) different density change at rising temperature and (2) surface tension value is not correct (my calculation based on a
rounded figure (0.5cm) based on a probable estimation (?) of surface tension by you).
BTW: you talked about "0.5 cm, in rough agreement with my results" - and I also think you said that you've observed liquid K in
Shellsol D70 - I showed you my "balls" - would you like to show me your "balls" now?
[Edited on 15-12-2010 by Pok]
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len2
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I see from the general gist of what you are saying and your mistakes that you have no idea what potassium does near its melting point. You have never
worked with it have you? Thank you and goodbye
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Pok
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@len2
the general things? I can't give you a contra argument if you remain unclear. Give me an example! I think you don't have any. That's why you have to
remain unclear. Mistakes? I think I was very lucky NOT to make mistakes in my procedure.
It either solidifies or liquefies. What do YOU think it should do? Emitting light? Do you know what potassium is? Its a metal. Have you ever seen it?
I did. Have you ever made it? I did.
What a nice question. Everyone shall think that YOU of course did work with it. Am sure you never did. I really think that YOU have never SEEN it.
You don't have to thank me. I didn't do it for you .
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blogfast25
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| Quote: Originally posted by len2 | Here's my advice:
Learn to read english sentences
check the density of potassium
en.wikipedia.org/potassium
learn about the behaviour of density for most liquids with temperature
stop trolling, and leave these people alone. |
Assuming len2 = len1 then len1 is now showing serious mean spiritedness for which at times he’s been known in the past. Anger is not always a good
adviser… He seems now to have descended into conspiracy theory… His argument abiout densities, surface tension and height of K balls seems thrown
together from a far distance and doesn't convince me...
Pok, you are more than entitled to leave and have no responsibility to stay, whether or not your results are genuine. You’ve gone out of your way to
accommodate us, even if that still doesn’t prove it’s genuine: only full replication can prove that.
It’s up to us to try and replicate your results, something which, all said and done, almost no one here has really seriously tried with all four
cylinders firing. We have woelen’s experiment as with promising but incomplete results and that’s about it. I wil try full replication soon...
And if we really believe you’re hoaxing us then that really is up to us to prove it…
Those who want to stay do so of their own volition. But gentlemen, this is supposed to be science, not a chat room for hormonally charged
teenagers!
And pok's English is fine, a damn sight better I bet than most here people's German.
[Edited on 15-12-2010 by blogfast25]
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woelen
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@len2: Please stop flaming! I now have seen enough of it and I am getting tired of it. Whether Pok's results are real or fake is not up to you as long
as you don't have any real evidence. All the equations and numbers you are bringing with you do not do justice to Pok's work.
From now on I want to see decent scientific discussion and no more flaming. Further flaming will be removed. Only scientific arguments against or in
favor of Pok's experiments are accepted from now on. I really do not want this interesting thread to see derailing into an ordinary flame war.
The fact that no one could reproduce Pok's results for the time being is not an indication of trolling or faking. As Pok has written, no one did the
experiment as he did. I am in the process of doing so (waiting for my ShellSol D70) and I think in the next week or so more people will try that when
their chemicals arrive. Let's see what all those attempts bring us and then we have new results to base our judgements on.
Let experiments say the final words and not one's adrenalin or hormones
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plastics
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| Quote: Originally posted by len1 | Destructive is when you try to bring another persons argument down with no good reason. And there is plenty of this around here. However when a person
is lying to you, its constructuve to put an end to it. Im used to getting crap from students, although unlike here most of them do it honestly -
beating about the bush in that instance is only superficialy constructuve. It actually harms people in the long term. Same here.
Further posting a lot of stuff about this before you have been able to reproduce his wonderful balls of K only serves to encourage future trolls - hes
having a great time watching you all.
Regarding the liquid-solid reaction, its interesting that a person who knows not the difference between water of crystalization locked inside a dry
powder and water picked up from the atmosphere by a deliquesent substance, would suddenly categorically state that this is a solid-liquid reaction,
without having shown any inclination towards theory before that statement. He did this of course to get out of a tight situation in what he thought
would be the best way he could.
[Edited on 15-12-2010 by len1] |
Yes in my limited time on the board len1, len2, lenx whatever is prone to increasingly vitriolic outbursts when his tail feathers are up. Witness his
attack when his elegant electrolytic preparation of sodium was replicated by me using a coffee tin and piece of wood:
https://www.sciencemadness.org/whisper/viewthread.php?tid=97...
Anyhow I think it is time to put away the flames and get the test tubes out. There appear to be less than a handful of practical attempts to replicate
Pok's work and page after page of non-productive waffle
Rant over
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Fleaker
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@Len, chill out! If this is utter bunk, it'll be ferreted out. I doubt that it's entirely hogwash. You are a superb experimental scientist, and one
here that actually does experiments when he says he will and quite well. While I find this patent dubious if you had no success, I cannot now rule it
out without having tried it myself (after seeing some reports). Sadly, due to silly socio-political reasons and prevailing zeitgeist, I no longer
experiment at home. So trust me when I say would be testing this out as well; I miss this very much! I could have very easily tested this remarkable
low T route to a remarkable element.
So far, Woelen has shown some validity to it. I presume he's worked with potassium before and knows the difference between potassium generated fire,
and hydrogen produced from water/magnesium/KOH (which may produce KOH-tainted H2) that may light from the heat of the reaction. That was my chief
issue with Woelen's experiment--I feel that a mixture of KOH and magnesium in an organic solvent will always generate H2 upon addition of water and
that the characteristic spectral colour of K might be seen as bubbles of K+ rich water are present in the mist produced as the metal dissolves. If,
however, it [H2] spontaneously flames, that is a strong indication that potassium is present. I think potassium is produced--the thermodynamic data
supports this.
The only questions I have are "how efficient, and how easily separated and purified?"
Neither flask nor beaker.
"Kid, you don't even know just what you don't know. "
--The Dark Lord Sauron
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blogfast25
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What woelen said… Totally seconded. Even if all this peters out we’ll still have had some fun, IMHO…
I conducted a simple side experiment to try and show reactivity of 2-methyl-2-butanol (2M2B) (as a substitute for t-butanol, in the post) with KOH,
NaOH, Mg ‘powder’ and Al.
About 4 ml of 2M2B was subjected to 1 g KOH (tube 1), 2.6 g NaOH (tube 2), 0.2 g Mg (tube 3) and 0.3 g Al (tube 4):
All were subjected with regular 'shaking' to 30 mins of steambath, average temperature about 97C, just below 2M2B’s BP of 102C:
Here are the tubes after wiping dry and cooling:
First off, tube 5 (previously not shown) which is KOH with methylated spirits (EtOH with small amount of MeOH) after boiling. KOH
dissolves effortlessly and completely in this solvent to a slightly yellow solution of presumably KOEt, KOMe, EtOH + MeOH and some water. As stated
higher up by Nicodem.
Tube 1: KOH and 2M2B started discolouring right way and this continued right throughout the test. But I can’t say whether or not significant amounts
of KOH reacted with the 2M2B. 'Something happened'...
Tube 2: similar to tube 1 but less intense discolouration.
Tubes 3 and 4: no reaction or visible change with either the Mg or Al.
It would be tempting to see if 1 and 2 contain some resp. K or Na 2-methyl-propa-2-oxyde but that's not so easy to do. But if any reaction took place
it is certainly not comparable in scale to the dissolution of KOH in ethanol/methanol.
[Edited on 15-12-2010 by blogfast25]
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len1
National Hazard
Posts: 595
Registered: 1-3-2007
Member Is Offline
Mood: NZ 1 (goal) - Italy 1 (dive)
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Wilco I must say Im surprised at you. Im not sure where you see flaming in my short posts. Just because its not obvious to you the guy is trolling
does not mean it is not clear to someone who has done this reaction and has made potassium, and would be harder to hoodwink. In such a situation I
would be asking why it is that its fake, rather than acting as if I know it all. I have also used quite a bit of scientific argument which did not get
an adequate reply, but it appears no one here, who cared to express an opinion, understood it. Some have even been expressing admiration 'whether
he's genuine or not' suggesting they actually want to be conned. So the thought enters my head why have I been wasting my time?
Fleaker, I chose not to do the experiment even though it would only take me a few hours because it became obvious to me the guy is faking - he has no
idea of the properties of potassium which somone who made a substantial amount of it would know. The so called-successes can be explained - heating
KOH with Mg solid can give some K (I have got it that way in a vacuum) but in these conditions you might be lucky to get a few milligrams.
Unlike the previous posts this last post contains no science because Im just wasting my time. It appears the future of this forum is more Pok's rather
than people like myself.
Of course I was angry, for the waste of my time reading this, replying to him and getting ready to do the experiment. But this is a personal thing, if
others get joy out of it, thats their right.
[Edited on 16-12-2010 by len1]
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