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Author: Subject: Problems with wet chemical sodium synthesis
EliasExperiments
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[*] posted on 17-5-2020 at 01:36
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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[*] posted on 17-5-2020 at 04:10


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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[*] posted on 17-5-2020 at 05:23


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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[*] posted on 17-5-2020 at 07:41


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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[*] posted on 17-5-2020 at 21:09


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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[*] posted on 18-5-2020 at 04:33


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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[*] posted on 18-5-2020 at 07:38


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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[*] posted on 18-5-2020 at 10:15


Can the dirty Magnesium shavings/turnings not be washed to make them more pure?
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monolithic
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[*] posted on 18-5-2020 at 16:44


Quote: Originally posted by G-Coupled  
Can the dirty Magnesium shavings/turnings not be washed to make them more pure?


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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[*] posted on 18-5-2020 at 20:46


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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[*] posted on 19-5-2020 at 03:54


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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[*] posted on 20-5-2020 at 02:11


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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[*] posted on 24-5-2020 at 13:42


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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[*] posted on 24-5-2020 at 15:59


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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[*] posted on 30-5-2020 at 21:57


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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[*] posted on 31-5-2020 at 05:09


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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[*] posted on 1-6-2020 at 22:29


Okay I'll try to do that next time. Thank you for the feedback. :-)
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monolithic
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[*] posted on 4-6-2020 at 15:44


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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