EliasExperiments
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Problems with wet chemical sodium synthesis
So I tried Nurd Rages wet chemical sodium synthesis and everything first of all seemed to work fine. It looked like I produced a lot of sodium and the
reaction mixture was reacting vigorously with water or ethanol. So I am quite sure that the sodium production was sucessfull. But for some reason I
could't get the sodium to coalesce into some nice beed that would actually be useful. I documented my entire process in this video:
https://youtu.be/shrFZVei5Ok
Does anybody have any idea what I could be doing wrong?
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XeonTheMGPony
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Miss heard never mind
you need dry dioxane to separate effectively, it seems to flux the coalescing effect.
but to make that happen your first couple runs will basically sacrificial to dry your solvents
[Edited on 17-5-2020 by XeonTheMGPony]
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monolithic
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I haven't performed this reaction yet (but I want to!) so take this with a grain of salt, but I think your stirring is too slow. If you watch the
NurdRage videos he has rapid stirring. This is why he uses a flat bottom flask, because you get much better mixing as the stir bar won't have a
tendency to sit on top of the reaction mass. I believe rapid stirring would lead to better yield and better coalescence of the sodium.
Also, your magnesium looks a little dirty. Are you sure it's pure magnesium? I've heard it's common for technical grade magnesium turnings (from a
machine shop, etc.) to include a lot of crap, basically whatever the machinists were turning that day. This could include steel, iron, etc.
[Edited on 5-17-2020 by monolithic]
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XeonTheMGPony
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After watching again your scale is a bit too small, the losses from dehydrating is not leaving too much effective to coalesce effectively.
Start by using the thermite method, do that a few times till you start getting good amount recovered via dioxane (this will get you starter sodium and
dry your dioxane for minimal effort.
Then do a larger scale reaction via the current method.
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EliasExperiments
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Thank you for all the advice!
Okay I think by now that it is my magnesium which is at fault.
Great that I still have 4 kg of that stuff...
Oh well I guess I can still use it for pyrotechnics.
I will try it again with better quality magnesium later.
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monolithic
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In the USA you can buy small quantities of relatively pure magnesium turning/powders on eBay. Maybe the same in your country?
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Herr Haber
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You could try getting Mg from the usual Polish suppliers but their good are mostly for pyros and you have plenty of that.
I'm pretty sure Onyxmet can get you better quality for a price.
Of course, there is eBay but it's a bit of a gamble.
Last Mg I ordered from eBay was from China, came in 100g vacuum bags, that was perfect.
I just realized so far I watched all of your videos. I'll try to send one of my family members to Wölsenberg to pick up some rocks and soil samples
The spirit of adventure was upon me. Having nitric acid and copper, I had only to learn what the words 'act upon' meant. - Ira Remsen
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G-Coupled
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Can the dirty Magnesium shavings/turnings not be washed to make them more pure?
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monolithic
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If there's other metals there could be competing reactions, in which case washing the magnesium wouldn't do much.
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EliasExperiments
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Yes I can buy better magnesium turnings on Ebay. I will do that and get the reaction to work eventually. Maybe I will have that done by Friday the
29th if everything goes well.
I also doubt that I can clean the magnesium cause if it is alloyed with aluminium or lithim or anything like that I would have no idea how I could
separate that out without investing a lot of time and effort.
I mean I could try washing it with acetone if there is any grease on the surface, but that would be just as expensive as buying more magnesium I
suppose.
I'll check out Onyxmet, thanks for the advice!
@Herr Haber: Make sure to keep me updated with your Wölsenberg explorations! :-)
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XeonTheMGPony
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Hot water electrodes for aluminium tanks is fairly pure Magnesium, down side is it is just a large solid bar.
but if you have a friend with a lath, or a hell of a lot of time to spare a file!
or make a furnace to melt it under a nitrogen atmosphere and a drop tube to make spheres!
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EliasExperiments
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For magnesium you need an argon atmosspehere cause it can form magnesium nitride at 300 °C (Wikipedia).
Other then that the drop tube is an interesting idea. Also I could use propane or butane as protective gases.
Hm actually I will think about ist, because solid magnesium is cheaper then turnings...
Great idea!
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monolithic
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For anyone else trying this reaction, I would not recommend magnesium powder/dust unless you have very good mechanical stirring which can scrape the
bottom of the flask for maximum agitation. The reaction essentially stalled after an hour because the majority of the magnesium had formed a paste
which settled at the bottom of my conical flask, in spite of rapid magnetic stirring. I have some magnesium shavings on the way, should work much
better. This is what I was working with: https://i.imgur.com/rkgaMN9.jpg
[Edited on 5-24-2020 by monolithic]
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XeonTheMGPony
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Quote: Originally posted by EliasExperiments  | For magnesium you need an argon atmosspehere cause it can form magnesium nitride at 300 °C (Wikipedia).
Other then that the drop tube is an interesting idea. Also I could use propane or butane as protective gases.
Hm actually I will think about ist, because solid magnesium is cheaper then turnings...
Great idea! |
Good catch, and ya propane will work, the crucible is the hard part! any good long steel pipe aut to work, One could use the propane protective gas to
fuel the melting crucible to use it effectively.
Playing with flows and orifice size on the crucible may be able to get all sort of sphere size.
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EliasExperiments
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So I got it to work with higher quality magnesium as shown in this video:
https://youtu.be/lWjYcvIZ35A
I still have a lot to improve, but I guess that is good for a start.
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XeonTheMGPony
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you need to break down the magnesium turnings to allow then to flow. a few quick bursts in 2 blender should do it
The sodium jump start is only to scavenge any moisture, so you do not need nearly that amount, for that scale I'd bet 3 grams sodium be plenty to dry
it
To your broken measuring cylinder flame treat those edges to round them!
Take your glass wear apart while hot! they still obey the laws of thermal expansion!
Relax, go slow, double check each action in your mind and think ahead several steps
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EliasExperiments
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Okay I'll try to do that next time. Thank you for the feedback. :-)
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monolithic
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I bought new magnesium and it was very fine, curly shavings like your second video. I didn't even bother trying to run the reaction because 10 g of
the shavings took up a volume of about 200 ml, far too much dead space for efficient stirring. I think ribbon cut into small chunks or coarse turnings
would be ideal. Blender might work but you would have to be careful, wouldn't want to risk sparking or something catching 10 grams of magnesium on
fire.
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