Sodium metal

[Seoul_lasers]

Testing Cs synth with very small quantities should be relatively safe. I remember seeing a video of 250mg of Cs being dropped into water via breaking an ampoule and letting it fall in a tub of water. It was VERY mild, just a poof, really. Trying it with such a small yield will let you know how volatile the process is.

True enough...

btw, I think I should mention about the Castner NaOH Process, The current you'll need will be in the neighbourhood of 6-8Vdc @ ~35A. Remember that the current will further raise your electrolytes temperature. Going above 330c and you'll end up dissolving any produced elemental sodium back into the NaOH.

I suggest either using a high accuracy non-contact IR thermometer (fluke) or a Platinum resistance thermometer for precise measurements for those of us that are "evil" enough to expand the production size. Muahahhah!

I'm going to try doing this process again once things settle down here. (Spring project?)

 

[Sigurthr]

While the yield and efficiency of the Castner process is undisputed, it relies upon a durable and well constructed castner cell, which is not easy to procure or make!

see: Sciencemadness Discussion Board - Sodium metal - Illustrated Practical Guide - Powered by XMB 1.9.11

I started to write out a description of the apparatus I had envisioned but quit half way through and decided to draw it in paint. Enjoy.

 

[Seoul_lasers]

While the yield and efficiency of the Castner process is undisputed, it relies upon a durable and well constructed castner cell, which is not easy to procure or make!

see: Sciencemadness Discussion Board - Sodium metal - Illustrated Practical Guide - Powered by XMB 1.9.11

I started to write out a description of the apparatus I had envisioned but quit half way through and decided to draw it in paint. Enjoy.

Excellent Castner cell idea Sig! :beer::beer:. Sciencemadess has some excellent resources on all matters of things chemistry!

 

[Sigurthr]

Thanks! I forgot to mention there is a book about similar Na Castner cells on google books Small-Scale Synthesis of Laboratory Reagents with Reaction Modeling - Leonid Lerner - Google Books

I'm eager to begin work on my Potassium-Mg Redox project. I am currently waiting on the Mg powder, Erlenmeyer Flask, scale, lab scoop, IR thermometer (I do have a resistance high temp probe but accuracy is questioned so a second thermometer was necessary) and mineral oil to arrive in the mail. I am a little concerned with the purity of the Mg powder and the mineral oil. I couldn't source any mineral oil locally that did not have mixed tocopherols blended in, and I don't know if the vitamin E would react with the potassium. I had to search far and wide to grab an 8oz bottle of "100% mineral oil" for cosmetic purposes. Who knows if it is actually 100% but let's hope. Research shows that impurities in the Mg shouldn't be too much of an issue if metallic, and nonmetallic impurities should precipitate out and likewise not interfere with the main reaction.

My yield goal is quite conservative however, and that is something I have going for me. I only require 5 grams for this to be a success. I'm hoping that will be an easily surpassed milestone.

 

[DashApple]

In liquid sodium hydroxide the sodium will float up , that's the reason in a Castner the cathode enters in the bottom though a neck with solid sodium hydroxide around it .

Also using the case as a anode isn't the best idea as it will erode a way , the best way to do it is with a nickel ring that sits in a ring near the bottom , nickel is very resistant to molten sodium hydroxide

Excellent Castner cell idea Sig! :beer::beer:. Sciencemadess has some excellent resources on all matters of things chemistry!

I read a page over there on someone who made a Castner , with a 50A drive current he got 200 grams of Na per 30 Hours at a yield of 23% and a cost of 7.9 USD per Kg of Na

 

[Sigurthr]

Aye the cell I pictured isn't ideal but a bottom fed cell is hard to construct. So what I drew is a compromise.


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[Seoul_lasers]

In liquid sodium hydroxide the sodium will float up , that's the reason in a Castner the cathode enters in the bottom though a neck with solid sodium hydroxide around it .

Also using the case as a anode isn't the best idea as it will erode a way , the best way to do it is with a nickel ring that sits in a ring near the bottom , nickel is very resistant to molten sodium hydroxide



I read a page over there on someone who made a Castner , with a 50A drive current he got 200 grams of Na per 30 Hours at a yield of 23% and a cost of 7.9 USD per Kg of Na

yes, I was just reading up on his process. I believe the transformer he used was a rewound Sanyo MOT for 6-8Vdc operation. I have seen others using 12Vdc at lower currents, but I guess the essential key is current to continuing the molten state of the NaOH.
:can: hmmm, making me want to experiment ASAP.

 

[Sigurthr]

Temperature control to prevent dissolving the Na yield into the NaOH melt appears to be the most critical aspect. In my reading I found some mention to cell poisoning at which point the reaction stops but the cell continues to pass current, but the research papers and books didn't go into what causes it or how it worked. I remember that one source said it was related to dissolved H2O in the NaOH melt and that by adding a precise amount of H2O they got the reaction going again, but only if the poisoning was not complete or too far gone. It also said that if it was too far gone only a new melt would suffice. I originally thought it might have been an electrode poisoning but the replacement of the melt alone is contradictory to that.

Alas, as I am going the Potassium-Redox route and not the Na-Electrolysis I won't know the answer unless one of you fine gentlemen get going with the experiments! Wink wink, nudge nudge.

 

[Seoul_lasers]

Temperature control to prevent dissolving the Na yield into the NaOH melt appears to be the most critical aspect. In my reading I found some mention to cell poisoning at which point the reaction stops but the cell continues to pass current, but the research papers and books didn't go into what causes it or how it worked. I remember that one source said it was related to dissolved H2O in the NaOH melt and that by adding a precise amount of H2O they got the reaction going again, but only if the poisoning was not complete or too far gone. It also said that if it was too far gone only a new melt would suffice. I originally thought it might have been an electrode poisoning but the replacement of the melt alone is contradictory to that.

Alas, as I am going the Potassium-Redox route and not the Na-Electrolysis I won't know the answer unless one of you fine gentlemen get going with the experiments! Wink wink, nudge nudge.

Yup... :beer: to that ! !
I am still asking around for the T-amyl alcohol here in Seoul.
There are a (few) related alcohols that could potentially be used in substitution.

Happy Potassium extracting!! :san::san:

 

[Sigurthr]

Ah, much appreciated! Yup I can expensively source t-butyl ($60/500ml) but there's no direct references that state it will work equally as well as t-amyl, so the 15ml of 97% t-amyl I have will definitely be the limiting factor for now.

When you fellas get it going please take good video of the apparatus and reaction. There's only poor cinematography and photography online for the process.


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[DashApple]

T-amyl ( 2-Methyl-2-butanol ) in the UK from a lab supplier is £25 for 250mL ,

 

[Seoul_lasers]

T-amyl ( 2-Methyl-2-butanol ) in the UK from a lab supplier is £25 for 250mL ,

And how much is the additional hazmat to ship it ?
Very unlikely they'll ship to a non-laboratory address without some kind of verification esp. coming from the UK.
This material is classed as a Narcotic substance.

 

[Sigurthr]

Yes, apparently it was used as an anesthetic at one point and is subject to substance abuse due to its higher potency than ethanol and not being metabolized into toxic metabolites.

I really hate how the lowest common denominator sets the bar for legality of an item or substance; a sentiment very pertinent on a laser forum.

 

[Seoul_lasers]

Yes, apparently it was used as an anesthetic at one point and is subject to substance abuse due to its higher potency than ethanol and not being metabolized into toxic metabolites.

I really hate how the lowest common denominator sets the bar for legality of an item or substance; a sentiment very pertinent on a laser forum.

Not meaning to burst your bubble... Also not trying to set the bar on any legality of any substance. We should have the right as experimenters to
have access to this stuff free from government interventions.
However, I have looked at the UK as a source as well. The paperwork and hazmat for T-Amyl was cost prohibitive (far more than the item). It also requires a registered (laboratory) address. UK is a very prohibitive country on a range of things.... :thinking:

I am trying here locally where laws are a little flexible cost also not being quite as prohibitive.

 

[Sigurthr]

Completely agreed, S_L. There does not appear to be any hazmat charges for tertiary alcohols here in the states, but it is up to the supplier to determine if they will sell any to an address not registered as a business or laboratory. $2/ml is the cheapest I've found for small quantities of <30ml. Tert butyl is a bit cheaper and far more available per amazon and ebay listings.

 

[DashApple]

And how much is the additional hazmat to ship it ?
Very unlikely they'll ship to a non-laboratory address without some kind of verification esp. coming from the UK.
This material is classed as a Narcotic substance.

Never bothered to look , as you said practically all main chemical companies in the UK wont ship to non lab based addresses , I've looked many times before