unconventional sodium

Hey Bromic,

Did you take a look at the patent I posted
further on up the thread regarding reduction of the nitrate with Sodium carbonate??

It is fairly comprehensive,explaining in detail,construction materials ect.

Some real good info for you there man.

Pretty please,give it a read.

Fuse them salts,lower the temps needed
collect you nitric acid.

Correcting my mistakes

Off Topic, but....

Neat!! I want to try the flaming popsicle stick thing now

The commercial draino is somewhat hydrated, that is the main impurity that I know of that causes it to melt at a lower temperature. As for the flaming popsicle stick I think there was a thread posted here about it. How the hydration of NaOH can start a fire. Put a popsicle stick that has water throughout it into molten NaOH and watch it make excessive energy from hydration and set it on fire

Wow, I guess I was mistaken about water of hydration being the main impurity.

My bad.

Regardless, I still stand by my belief that the inflamation of the wood in question is caused by the inheret moisture in the wood being acted upon by the hot molten hydroxide.

Quote:

Originally posted by chemoleo Bromic, your method doesn't seem all that different, except maybe the water addition. I dont understand why you'd get metalic Na globules - everyone who's tried it (inc. myself), one gets a dark grey mass, with the occasional yellow explosion from igniting H2/O2/Na. It's not like your temperature is low (judging by the mark on the wooden bench ), or that there is an oxygen deficiency in your local atmosphere (you wouldnt be writing this otherwise ) But seriously, I can't figure out why you'd get metalic sodium, as a nice little globule. How about upscaling this? Comments?

You guys with all your alkali burns are scaring me. And I want to get lithium from batteries soon (summer hoilday is coming in 2-3ish weeks!!)

Edit: typo

[Edited on 13-5-2004 by Saerynide]

Tacho: Ive tasted NaOH too. I was scraping sodium off the electrode with pliers and the electrode sprung up and flicked some sodium hydroxide onto my tongue. I still cant think of why my tongue was out at that moment though...

Quote:

Originally posted by rogue chemist Tacho: Ive tasted NaOH too. I was scraping sodium off the electrode with pliers and the electrode sprung up and flicked some sodium hydroxide onto my tongue. I still cant think of why my tongue was out at that moment though...

High boiling organics with densities greater than 1

You need an inert liquid with a density of 1 g/cm3 or above with a boiling point of greater then 100C. This is the technique used to purify lithium that I mentioned before, you melt the impure NaOH/Na mixture at the bottom and as it melts the pure-er Na will float to the top leaving the NaOH behind. You could use something like nitrobenzene possibly. I think most chlorinated hydrocarbons will react with Na at these temps and that is the massive drawback because most organic liquids that have a density of greater then 1 are halogenated hydrocarbons.

[Edited on 5/9/2004 by BromicAcid]

I thought I'd give a nitrated organic a try. I have toulene, so I prepared mono nitrotoluene (NT) according to Davis. It's a straightforward nitration with mixed acid. I placed a small ball of Na in the NT in a test tube. It appeared to darken a bit. I heated it carefully-- the Na began to react with the NT and soon all Na was consumed and the liquid, initially yellow, turned reddish brown. I suppose the Na is reducing the NT. Oh well, not much ventured..

[Edited on 16-5-2004 by Strepta]

[Edited on 16-5-2004 by Strepta]

Magnetic NaOH

I believe stainless reacts appreciably with NaOH(l) however I have no sources to back me up, some designs for castner cells call for cast iron which I come across even easier, it holds up fairly well. I use nickel whenever possible because for as far as I can tell it is nearly invulnerable to molten NaOH, I've used the same set of electrodes several times and no pitting and the molten NaOH does not turn colors from making nickel salts. Carbon will die in NaOH(l) there is no getting around it, I used graphite rods as electrodes and it quickly formed as semi-metalic solution that conducted electricity and thus accomplished no electrolysis.

As for where you can get soda lime glass, most everything made of glass that is not made for a lab is soda lime glass. But it needs to be thin, it should have a partial vacuum within it, and it does break after a period of use. NASICON ceramics are the way to go for a membrane that permits only Na though.

Edit: And Strepta, nice try, nice to see someone trying somthing an idea that I've put fourth, keep up the good work

[Edited on 5/18/2004 by BromicAcid]

I have tried electrolysis in Fe endcaps and Cu , and in food cans, and the food cans seem to withstand molten NaOH the best! In the other ones, it changes to brown quickly, and if I stick any iron or copper wires into the melt, it will turn brown too...

BromicAcid, does that mean I could use the glass in a lightbulb? It is pretty thin and will withstand a vacuum. If only the wires inside of the lightbulb touched the edge Then you could just plunk a lightbulb into the NaNO3 melt and connect it to your power source, as it already has a vacuum inside, run the cell, get the sodium, and crack the bulb open!

Inside a light bulb isnt a vacuum. Theres a noble gas in there, I cant remember which one though.

But I was also thinking about using lightbulbs to melt or heat stuff in, since I dont have pyrex, and if light bulbs can withstand constant heating, I hope they can withstand a gas stove

Edit: I was going to open a light bulb by removing the connector and taking out all the crap in it, to get a flask like container. But now come to think of it, Im kinda worried that H2 might build up in the bulb (since it has a narrow opening) and with the Na forming, it might turn the lightbulb into a glass pipebomb

[Edited on 20-5-2004 by Saerynide]

Sounds very interesting.
I bet polyethylene would work. I should test that.
I just need to go get some Mg (tomorrow)
at $0.25 a lb from a scrap dealer. I think its a powder too. Amazing. I love the Market.

Then I can get around to all those reactions I've been saying I would do.

All of my previous experiments with sodium have failed.

I did 2 early experiments with NaOH a while back, but I forget what, I just remember that they were hopeless.

Electrolysis 3 - 9v battery, molten NaOH in food can, copper wires. nothing happened- I think the battery was nearly dead by then .

#4- larger 12 v 0.5 a (iirc) power supply,
molten NaOH in food can, Fe wires. Some bubbles, pops, fizzes. The current helped heat the melt, not enough to keep it molten though. Melt turned green at one wire, brown at the other.

More coming in this sector.

I cleaned out the soda-lime glass lightbulb, and filled the bottom with copper wires. Then I found another smaller lightbulb which had a Cu wire actually TOUCHING the glass for some reason. Yes!!! Now I don't have to supply vaccuum, heat, and electricity, just heat and electricity!

More coming here.

Sodium thermites

I heated about 1 g NaOH, 1 g Na2CO3, 1 g NaCl, 2.3 g Al in a copper test tube - (got that one for .90$ on one of my recent excursions from Persia to Home Depot) The Al was not a fine powder, more like finely crumpled shreds of Al - it was from a blender, I have almost no fine Al left.

the apparatus looked like this

_____________________
/ ______________####_- more pipe
/ / __ 90 degree fitting, teflon tape seal
| |
| |- copper test tube
| |
|* | * = thermite
| *|
|* |
|* | # = steel wool
* /
/

After heating for about 0.5 minutes with my torch, there was a loud thump, I lit the H2 gas escaping with the torch, after about 1.5 minutes, the bottom half of the test tube started glowing very brightly for about 0.5 min, more than the torch could get it alone.

I let it cool, and then looked at the steel wool - should be gobs of Na, right? NOTHING!!! The inside of the copper pipe seemed to have a light white haze on it. The leftover reactants could not be chipped out, so I added water. Then the fun started. The tube got hot, the mixture fizzed, and lots of H2 came off- enough to light in medium sized fireballs. I did the reaction again, and the tube gets too hot to hold when water is added.

Then I tried doing the experiment just like Tacho did- lower bowl, upper bowl with water and ice- I heated the lower bowl red hot in places, H2 came off- enough to make the upper bowl filled with water jump a cm or to into the air , but no violent reaction happened. The lower bowl did not glow bright red except where the torch was. No residues on the upper bowl at all. Argg!

The only thing I can think of is the Al could be bad- it came from Al foil and the blender. What do you think of the copper condenser apparatus- it's cheaper and easier to work with than steel pipes.

Sorry for the longevity of the post.

Ok, I was exaggerating about my expectations for nice shiny globs of sodium- dirty stuff is fine for now. And yes, the Na will be a vapor when it is produced- but some should deposit on the steel wool if it is cold enough, clean or not.

Edit, why won't the sodium be pure- if its done in an inert gas, assume, and the only products are MgO, H2, H2O and Na, what is the impurity? NaOH? MgO? NaH? NaOH can be removed, but I don't know about the others-could the sodium be distilled to purify, even if it won't melt?

Also, I tried magnesium turnings and sodium hydroxide under molten candle wax today, I heated the candle wax till boiling, there was vigorous bubbling of hydrogen, the Mg turned black, the wax caught fire- when the torch was placed straight at it, the flames billowed about 1m high.. When placed under water, nothing happened. (the reactants were covered in solidified wax) If a decent way of extracting the Na from the wax and the MgO/ Mg(OH)2 is found , this might be a simple and promising method.

Halfway throught the reaction, I discovered that a prill of NaOH had located themselves on my arm, and were busy making Cyrus-soap... I was most annoyed because I had to stop watching the reaction and wash myself.


[Edited on 18-6-2004 by Cyrus]

[Edited on 18-6-2004 by Cyrus]

A hair raising experience

Today, I tried to make sodium. Once again.

I used the copper test tube setup previously described, but I used lots of teflon tape to keep the joints secure, and the outlet of the setup went diagonaly into a food-can with about 2 cm of mineral spirits in the bottom.

I used 1g of NaOH and 0.6 g of Mg, this mixture was placed into the bottom of the test tube. I was doing this quick and dirty, so I didn't even bother using a clamp to hold the setup in place, I just held the food can with my left hand, and held the torch in my right. Bad move.

Upon heating, some bubbles peacefully drifted out of the copper setup for a minute or two. I began thinking, either this reaction is very slow, or it takes a while to get started. Then

Whumphh!

I remember
-1- a very bright flash and a loud noise
-2-a large wave of heat
-3-a hot and sticky sensation
-4-the apparatus decomposing into several flaming objects,
-5-my goggles dislocating themselves from my head somehow

At this point I decided it would be best to leave the area, and then I noticed that the wave of heat was COMING FROM MY HEAD!

I ran into my garage looking for a bucket filled with ice-cold water (there are no buckets of water in my garage, ever) while beating down the flames on my head with my hands.

Finally, I put the flames out.

Aftermath
-the still flaming apparati were burning holes in the grass
-the propane burner was still on, only heating concrete, though
-mineral spirits were all over me, the concrete, and my goggles
-the goggles were on fire
-All hope of sodium was lost (the most important)
-Oh yes, and the last 0.5 cm of almost every hair on my head had turned white and crinkled, including my eyebrows and lashes, which were behind the safety goggles! One of my ears was burnt.
My hair sticking up in fused masses at every angle, I truly looked the mad scientist.

I smelled like burnt hair and mineral spirits. Pleasant.

Things I have learned
-BromicAcid has good reason to use those beefy iron pipes-which I will use from now on.

-Do NOT stand within 3m of such reaction.

-Teflon tape will not hold very well when using magnesium- it works with Al.

-Water is very good to have at hand.

All in all, a very exiting day. I think I'll take a little siesta from reactions for a day or two though.

Nevertheless, SODIUM SHALL BE MINE!

So where you expecting this? Magnesium oxide can be added to help moderate the reaction.

Best of luck with future experiments, and those 'big beefy pipes' really do make you feel safer

[Edited on 6/23/2004 by BromicAcid]

No, I was not being cautious enough.

But I was using large Mg turnings, not fine powder, (as Tacho advised IIRC) and about 2 g total materials, so I just expected the reaction to go "nice and quickly",
not explode like a small bomb. I was not expecting anything like what happened, of course.

Now that I have done it, it is not a reaction I would say proceeded "nice and quickly"


Don't worry about my health, the ear is doing ok, and all of the crisped hair seems to have fallen off, thankfully.

Bromic acid, with your large steel pipes, to prevent suckback, instead of using a one way valve, why not make the level of water such that whenever it gets sucked back, the water level lowers enough to let air through. This has probably been said somewhere before, but oh well.

Be warned, I have just caught the phosphorus bug.


[Edited on 23-6-2004 by Cyrus]

[Edited on 23-6-2004 by Cyrus]

Thanks for the good advice - the act is now together, for all such future reactions I'll use some clamps, thick iron pipes, a "blast shield" made out of spare sheetrock, and more common sense. And I'll be farther away.

I'm glad this happened because it was a good warning.

Tacho, the apparatus was not a closed tube, it had an opening, but my description may have been confusing.

Chemoleo, what did you do to yourself, and also, if I want to make/distill sodium, I think flammable liquids must be used to bubble the vapors through, any suggestions?

To be honest, I don't think you have much chance of condensing Na vapours in those oils. I played around a little with potassium in inert oils, and the metal tends to separate into thousands of tiny globules rather than condensing into a coherent one. With K/Na - vapours.... I'd rather think you will get an emulsion... if that. Sodium gas... sounds good in theory... but again, I doubt very much it occurs for real, with the thermite reaction. Remember I tried it, several ways. Distillation in an inert atmosphere is the only way I can see this to work (with massive heat, well above the boiling point of Na), if that. Even then, I do think most of the thermite products are aluminates/aluminium hydrides, despite stoichiometric equations. As I said above once, I tried heating the thermite product in petroleum, for several hours, to release the Na (which should melt) but it didn't work at all.
If I was you I wouldnt pursue it because I'd doubt it would work, and I'd be too worried about saftey (open flame and mineral spirits).

I think it's very interesting what Tacho mentioned about reaction with alcohols (i.e. ethanol) - he described evolution of gas (H2?), where the product still reacted violently with water.
May I ask whether it was absolute alcohol??

If yes, it sounds like a very decent method for preparing alcoholates, I wish I had tried it.

Does anyone have some experience in purifying/playing with alcoholates?

For instance, Tacho, once you react your thermite product with alcohol, what did you do with it? Did you try to react it with something, to confirm you had truly some NaOC2H5??? Please elaborate!

PS On the note of my past incidents... I will elaborate on taht one day... in the 'most serious injury' thread. Never found the guts to do so so far but dont worry I am not disfigured or anything... you cant see it.... although it's left me with a healthy permanent scar of being cautious. And you, Cyrus, sound just like me when I was 16... and I paid a dear price for that. Be warned, seriously!! I didnt get such a warning (I didnt know of the internet then), while you DO! Be careful, man! no more thermites with Bunsens igniting it by hand! I mean it! A tiny bit of neglect can cause you more harm than you can imagine.

[Edited on 24-6-2004 by chemoleo]

I started reading them, my computer is more than slightly slow though, (Win 95!)
I didn't get very far, but I will try again!

Tacho, melting the Na/impurities under an inert atmosphere might help. (if this is in a centrifuge it might help too) Then putting it in one of the perforated ladles described elsewhere will remove the NaOH, perhaps other impurities too. Maybe you could mount the ladle onto the centifuge.

Molten sodium filtering! That ought to work, but Na has a lot of surface tension, so it would have to be under pressure to drive the Na through the filter. Or under a vacuum to pull it through.

Sorry if I am rambling.

SODIUM!

Doesn't teflon react with molten alkali hydroxides also?

Edit: Just made some sodium, using an upper ice-cold bowl and the lower bowl to do the reaction in. I didn't measure anything out, just added NaOH and Mg till it looked right. I mixed these together a little in the lower bowl, and set this in my reaction chamber.

I was being ridiculously safe on this
one.

Then after heating for a minute or two, there were bright orange flames, which lasted about 10 seconds. I heated for another minute, just to make sure the reaction was done, and let it sit for 3 minutes. On the bottom of the lower bowl, there was a very thin white covering/paste, which when I scraped it into xylene, caught on fire in the air, some of it falling to the ground in burning spheres, some catching the xylene on fire. DON'T WORRY, I was prepared. I covered the can, the fire went out. Now xylene ought not to eat sodium, but the mixture started fizzing and frothing-this is from residual moisture I assume, could it be water from the fire itself? So that was all wasted. Will vegitable oil work?

Upon opening the lower bowl, there were about 6 different globs that glowed bright yellow. A couple minutes later, the globs had turned a dull pale green. The whole mass of reactants had hardened into a cylinder at the bottom of the lower bowl by now. This was lifted out, several sections looked metallic. Anyways, there were several extremely small balls of sodium that fell out from somewhere,
they fizzled in water. Ahh.

Sorry Tacho, I did not try the reaction with NaCl, Na2CO3 and NaOH. That will have to wait until tomorrow.

[Edited on 26-6-2004 by Cyrus]

[Edited on 26-6-2004 by Cyrus]

Great Work! Congratulations!

Yes, I got some sodium, but I was wondering what the other stuff was. Sorry for the dumb question I forgot all about hydrides.

I am planning to make a charcoal furnace, so then NaCO3 + 2C -> 3CO + Na. The Na vapors will bubble into molten paraffin.

Castner

Sodium (and others) from Halide salt reduction with CaC2

From "Comprehensive Inorganic Chemistry".

BTW, sodium carbide is only stable up to 400C, therefore removal before reaction is not a problem, same with hydrogen, sodium hydride is only stable upto a lower temperature, it can safely be held under a hydrogen atmosphere in a Castner cell without reaction, it maintains a mirror sheen to it in such a case.

Ohhhh... I'm posting this without spell checking it, bad boy, bad!

Edit: Spelling....

Oh, and... Cyrus

Run the vapors into a copper spiral condenser immersed in heated mineral oil to the melting point of sodium, the sodium will condense and the liquid sodium can run into your paraffin

[Edited on 9/3/2004 by BromicAcid]

Yesterday, I decided to try making sodium using the pressure bomb method. I wanted to see the difference between Na and K when reacted with Mg in an inert atmosphere. Some have suggested that Na + Mg makes a near flash powder. But just as my potassium experiments showed the previous day, that only seems to happen out in the open and not in a negative oxygen environment.

2.43gm Mg + 4gm NaOH were ground to a fine powder in a mortar and pestle while under argon. A small amount ~.1 gm was transferred to a small flask that had been flushed with Ar, placed in a hood and lit with a hot wire loop. It was not much more impressive than my similar KOH+Mg experiment.
http://img208.echo.cx/img208/9361/naohmgar2kw.jpg

On to the confined reaction… I placed ~2gm of the above NaOH+Mg mix in the parr bomb and sealed while under Ar.
http://img208.echo.cx/img208/7578/fillparrna5vh.jpg

This then was wired up and set out to fire. I still use the blocks even though from the outside, nothing much seems to be happening. Picture taken 30 seconds after ignition.
http://img208.echo.cx/img208/962/nabmbsetup8zl.jpg

After allowing the bomb to cool for 10 min or so, I cracked the seal while waiting for a hiss of escaping hydrogen but none was heard as before in my K experiments. Very interesting I thought, where had it gone? The contents after opening under mineral spirits and washing with 1, 4 dioxane, were very different then the potassium experiment. You can see light and dark silver/grey and blue coloration.
http://img208.echo.cx/img208/51/indioxane6md.jpg

Sodium hydride.
Merck says: prepared by passing hydrogen into molten sodium dispersed in oil or mixed with a catalyst such as anthracene above 250º. Reacts explosively with water, violently with lower alcohols, ignites spontaneously upon standing in moist air.
So this method isn't going to work if one is after solid sodium metal but I think it has promise for potassium since it does not form hydrides in this reaction. I am still working on improving the Kbomb and will post the further results as I have them.

The upper layers in the parr cup were lighter in color and certainly contained a greater percentage of MgO and were a brittle crunchy mass. The lower layers were more metallic yet not like sodium is supposed to look. The picture is of the solid upper mass that came out of the cup.
http://img208.echo.cx/img208/3686/wetchunk0gb.jpg

Upon tossing the chunk into water this is what happened.
http://img208.echo.cx/img208/479/uplayerinh2o5no.jpg
Not nearly as fun as what happened when small portions of the lower layer were tossed in.
http://img208.echo.cx/img208/6785/lowlayerinh21gb.jpg

For those who don't happen to have an oxygen combustion bomb lying around, one could make a heavy metal, threaded capped tube and drill and tap one end for a small spark plug. One could then attach a fine nichrome wire between the center electrode and the ground tang. Voila instant reaction chamber.

Marvin, of course I would trade magnesium for K or Na since I have plenty of Mg lying around and none of the latter. I read the patent you referenced and thought I might try a small version in test a tube and see if it might work. I placed a stoichiometric mix of NaOH + Mg in heavy mineral oil and began heating. The contents did become very frothy and I continued this heating for roughly 20 minutes. After that time I added a few ml of 2-propanol as a catalyst as suggested in the patent. I continued heating for another 30 minutes. After heating the contents settled and no visible difference in the magnesium was noted. I washed the contents on filter paper with 1,4 dioxane and tossed it into some water looking for any reaction. There was none. It's possible that the mineral oil interfered or the reaction times were too short.

Following US patent 4725311

Finally got around to getting the pictures off my computer (which is somewhat broke now) attached is the reaction sequence, the first picture showing all the reactants in the flask before the heat was applied. The second picture shows nearly 4 hours later, the metal still visible is magnesium, most of it had reacted though. However I had to leave and could not work up my solution and as a result I had to leave it and come back the next day, it was left for a few hours exposed to the atmosphere more then I would have liked because I didn't want to cap boiling kerosene. The final picture is from the next day before re-heating to melt any potassium, note that the color is now brown, potassium peroxides/superoxides, oxidations products of those compounds with the kerosene... etc, definatley something considering the striking color change, and as I noted the magnesium turnings recovered gave an almost violent reaction with isopropyl alcohol dissolved in kerosene.

[Again, although this is somewhat off topic this can be thoretically be applied to sodium as well.]

Glyme?

Today I attempted the preparation of potassium following the information from the patent posted by BromicAcid. The following was the pathway taken.

30g of finely ground KOH was mixed with 16g of Magnesium powder. To the mixture, 200mL of toluene GPR was added. A reflux setup (with an oil bath) was used to bring the mixture to the boiling point of toluene (i.e. approx. 111 deg C). The increase in temperature was done slowly. At an oil bath temperature of approx. 50 deg C 12mL of absolute ethanol were added to the mixture. On increasing the temp. effervescence was noted, especially above 70 deg C (oil bath temperature). At an oil bath temperature of approx. 90-100 deg C vigorous gaseous evolution occured. Collection of the sample of the gas, using an inverted tube over the mouth of the condensor, and combustion of the gas immediately gave the expected 'pop' indicating Hydrogen.

Reflux of the mixture was continued for a further 3 hours. The mixture was left to cool to 90 deg C (oil bath temp) to check for gaseous evolution. At the 3rd hour gaseous evolution slowed down and I decided to stop there. On examining the contents of the RBF, little KOH was left, some magnesum hydroxide was present at the surface, whereas tiny granules with a metallic lusture were present (which I assume were potassium).

The yield was extremely low, most probably because of the low boiling point of the hydrocarbon used. Next time I will try distilling some diesel so to purify it and run the experiment again. All chemicals were GPR grade. Pic attached shows the product.

PS. I have some other pictures of the gas evolution but I do not know how to use scipics. If anybody is interested and ready to help please U2U me.

[Edited on 4-2-2006 by Esplosivo]

Edit to change picture size-davster



[Edited on 24-12-09 by The_Davster]





[Edited on 2-16-2010 by Polverone]

so boron is the way to go? is boron easy to make? what i have read so far is melt down boric acid for the oxide then reduce with magnesium - so we are basically using the magnesium twice.. first to make the boron then the sodium metal

too bad boron is so friggin expensive

[Edited on 29-3-2006 by jimmyboy]

Ordenblitz this is some really fine work - producing elemental sodium and NaBH4 all before supper. This is a quantum leap for MadScience!

I'm intriqued by your Parr bomb calorimeter. I have never seen one before. Do you use it in support of your "real" work? What size is it? Can you show us a picture of its parts in more detail and describe their features? I looked on the Parr website but they don't give much for construction details.

So thats why a bomb calorimeter is used and not an open reaction vessel....


I added 0.4g NaOH prills, 0.8g Mg filings and 0.5 g boric acid to a 100mL beaker and mixed well with a stirring rod. I then added two scoops of this mix to a testtube which was then heated over an alcohol burner. White fumes were given off then a orange fireball shot out of the tube, bounced once, then came to a stop leaving a glowing pile of something. The glowing pile(after it cooled) was added to cold water, the aqeuous part decanted and acidified. No bubbles formed. The remainder of the residue in the tube was heated for a few more seconds on the burner, then removed and allowed to semi cool. Cold water was added to the tube and some hissing was observed, it might have been some sodium in there reacting with water or it might have just been really hot still. The aqueous layer of the tube was decanted and acidified. Strong bubbling occured.

Seems simple enough, but now I gotta air out my basement....

But in any case, this is a cool method for making borohydride or sodium, I just gotta get some pipe parts I guess. What are the chances of by doing this reaction in a sealed container that it could rupture and kill me? Or is the pressure produced minimal?


[Edited on 30-3-2006 by rogue chemist]

Sounds like you have had some experiance with the flame as well eh.

I am thinking the white fumes were just MgO being lofted by hot air in the tube or even potentially water vapour from NaOH absorbing water from the air.

When I have more time(ie not a few weeks before exam time like I am now) I would like to try this again with a tin can with a diameter a couple inches at least and a lid on top held down with a brick. The reactants could be arranged in an inverted conical pile such that in the centre of the bottom there is little reactants and along the outsides the piles grow steeper. Heating would be started in the centre of the bottom of the can. Hopefully such a design could prevent the ignition from lofting everything everywhere.

Also this is an outdoor or garage experiment next time

By the way, the sodium borohydride MSDSs list its decomposition as 400, what exactly does it decompose into at this temp?

Igniting a mix from the bottom seems like a bad idea...

Don't forget that sodium is gaseous at the reaction temperature. The bomb keeps it pressurized in liquid form. That would explain the homely blob of sodium found in the first test.

So lemme see here,
NaOH + Mg = Na + MgO + 1/2 H2 = NaH + MgO. Lye reacts with magnesium to produce thermodynamically favored magnesium oxide (or likewise with aluminum), yielding sodium vapor and hydrogen gas. However, the reaction products can react further, producing hydride, useless for the goal of sodium metal.

So, you try something like,
NaOH + Mg + B = Na + MgO + BH3 (assuming boron is the stronger 'hydriphile' so to speak). Which works pretty well, but requires boron, so you might use more common materials:
NaOH + Mg + B(OH)3 = Na + MgO + BH3 [unbalanced], but there's too much oxygen and hydrogen to go from boric acid directly: NaOH + 4Mg + B(OH)3 = 4MgO + NaBH4. Same results as with plain lye, except boron has been reduced too. Of course if you want sodium hydride or borohydride, you can use either method, (somehow) extract them from the magnesium oxide, and smile.
One good way to reduce the hydrogen is to dehydrate things:
NaOH + 4Mg + B2O3 = 4MgO + 2B + Na + H, my this has some strong potential, let me rewrite that,
6NaOH + 9Mg + B2O3 = 9MgO + 6Na + 2BH3
Wonderful, it doesn't even need much boric oxide it would seem!

You could also start with sodium (or potassium? ) borate, probably a fused product (as with the boric anhydride) to ensure it is anhydrous.

Lemme see, borax is sodium "tetra"borate, which really means Na2B4O7 IIRC, so you'd have to add a good bit of lye even to that already.

Heyyy, when you melt things, gaseous anions tend to go away.. (at least, when glasses are analyzed, you only see oxides listed). You might be able to melt borax (or boric acid) with sodium carbonate, get it good and hot until it stops bubbling, then pour the molten glass into a bucket of mineral oil (obviously, something other than water) to quench it while remaining anhydrous, then wash with solvent, grind and you should have very little hydrogen whatsoever! Why, then you'd get a bunch of plain boron because there would be no hydrogen... oh, so you could reduce the boron present... ah, but the assumption is that sodium carbonate or hydroxide won't turn to sodium oxide on its own, so some must remain...?

Tim

[Edited on 3-30-2006 by 12AX7]

2g NaOH, 4.8g of Mg filings and 3 g boric acid were mixed in a soup can. The can was tilted adn then returned to normal such that the reactants were slanted inside the can. The lit was placed on the can and secured with a single strip of ducttape. I could not find a brick so I used a slice of railway track on top of the can. A big plastic flower pot was placed over everything and the can heated with a propane torch on the side with the least reactants. After a few seconds of heating there was a hissing sound and the entire apparatus glowed orange...smoke excaped the can and floated up to the garage ceiling. I extinguished the flaming ducttape with some water and opened the garage door....that smoke can't be healthy.... I left and came back 5 min later when the garage was mostly vented and the can had cooled down. The big flower pot was white inside from the white smoke. 400mL of ice/wate was added to the can slowly...there was a small orange explosion so some sodium must have been formed. A sample of the water extract was acidified and strongly bubbled. It is being filtered currently of all the other crud in there. Is there any way that an aqueous solution of borohydride coul d be used to make isoproplamine via reductive amination of acetone, the places I saw were unclear on this?

EDIT: Weird...the aqueous filtrate does not bubble when acid is added, but the residue in the filter does...I thought borohydride was soluble in water? And it worked for you ordenblitz...weird...

EDIT2: Is it possible that boron could form? I got a good deal of black insoluble flakes...

[Edited on 2-4-2006 by rogue chemist]

I was wondering something