Sciencemadness Discussion Board

Soooodddddiiiiiuuuummmm!

m1tanker78 - 11-2-2011 at 23:36

Finally raked in some satisfaction today. I decided to fire-up my small scale sodium experiment and see how much I'd end up with. At ~5 grams: not too terribly well but not too shabby for a half hour. I cut it short because my collection tube is unfortunately mounted way too high so the Na solidifies half way up the stack. Couple more inches and it'd be able to slide down the chute and land in a soothing oil bath.

The contraption is crude but works some of the time. as an added bonus, I pulled out some calcium metal too - about 1 gram; unmistakable red flame. That's strange, I though CaCL2 didn't participate in the reaction, only bring the melting point down. Either way, I'm ditching CaCL2 from now on because all it seems to do is bring the melt morale downl

Bottom line, I have 5+ grams of metallic sodium sitting in my shop in a container filled with the cheapest, nastiest motor oil money can buy. Well, make that 4+ grams. My neighbor and I couldn't resist ;).

I'm going to put some ideas on paper and see how they would theoretically perform. Then on to the fab.

Tom

[Edited on 2-12-2011 by m1tanker78]

woelen - 12-2-2011 at 02:51

Which sodium experiment?

Fleaker - 12-2-2011 at 08:23

Pictures?

entropy51 - 12-2-2011 at 09:49

Quote: Originally posted by Fleaker  
Pictures?
Sworn affadavit?

5 ounces in 30 minutes? I think that would require 357 amps. I would indeed like to see pictures of this rig.

peach - 12-2-2011 at 10:31

I think he's talking about a retort of some description, with the mention of the stack, chute and collecting tube, yet no mention of power supplies or electrodes.

But yes... pictures!

UnintentionalChaos - 12-2-2011 at 10:35

To me, it sounds more like a downs cell, the sodium being forced up a collecting tube by it's much lower density than the fused salt mixture.

m1tanker78 - 12-2-2011 at 11:43

@Fleaker: I didn't take any pics because I didn't expect it to produce much Na. Most of the Na has gone to Heaven due to experimentation but I managed to snap a few pics of the leftovers with my cell phone. I'll post 'em when I figure out how to upload them from my phone.

@woelen: The main experiment was testing the setup to see if I could extract small quantities of Na (which surprisingly it did). It isn't easy to simply take a Downs Cell and just scale it down. Several problems arise such as:
1) SAFETY(!!!)
2) The container material.
3) Electrode material.
4) How to orient the electrodes.
5) Choice of salt(s).
6) How to isolate and collect the newly formed Na from the melt.
7) How to deal with the chlorine gas that is evolved - this is a biggie. (Lime has been good for me)
8) Power supply.
9) Material choice for partially isolating Cl and Na in the melt.

And a lot of others. It's not as easy as sticking 2 electrodes in a salt bath and having an ice cold beer while the crucible fills with Na. One can dream, though ;)

Anyway, my challenge was to collect a little Na in a steel tube with the electrodes introduced from the TOP of the cell. The collection tube was not part of the circuit. It would've been nice to collect the Na in a continuous manner - maybe next time.

Oh and using NaCl was the other main personal challenge (high MP, chlorine evolution). NaOH is much easier to work with but considerably expensive compared to NaCl. I ran some quick calculations and the lower MP of NaOH doesn't offset the extra energy required to fuse NaCl. The 'cheap' NaOH around here has a lot of foreign crap in it - including bits of aluminum catalyst.

I didn't know sodium peroxide could form in air. I thought it had to be formed in an O2-rich environment. If I quickly heat (burn) the Na, I get sodium oxide. If I indirectly warm the Na, I get sodium peroxide. I also see that it doesn't take much Na to drastically raise the pH of water.

Tom

m1tanker78 - 12-2-2011 at 12:55

Sorry for the confusion. I meant to say *grams* in my original post, not ounces. That's what happens when you post at 2a.m. and you're raised with imperial units. If I had 5 ounces of Na I would have taken a quick trip to the lake :D

Now that I know that this works to some degree, I promise to snap some pics on the next round (hopefully later today). I need to modify the rig so that more of the stack is submerged in the salt so the Na will remain molten further up and be able to decant. Or maybe modify the cathode to where it passes through the stack (easier said than done!). Plus, when the stack begins to fill with Na, it will effectively chathodize the stack meaning most Na would form on the outside. If there were some way to passivate the outside of the steel stack....... been there, tried that, failed.

The power supply is a DC inverter welder (200 or 225 amp). I manually modulate the amperage from between 20 to 80-ish amps though to try and strike a balance between melt temp/production/anode deterioration.

I'm using steel for the cathode and carbon for the anode.

Tom

peach - 12-2-2011 at 13:07

Grams and ounces aside, still sounds interesting!

Please do get some photos!

blogfast25 - 12-2-2011 at 14:30

Oookaaayyy. So this is classic electrolysis of NaCl/CaCl2 (now even minus the CaCl2!) Forget about scaling that up in a garden shed lab. Len1’s NaOH cell is hard enough…

Want electrolytic sodium? Try a simple NaOH ‘cell’, an argon blanket to protect the nascent sodium, a gauze spoon to scoop blobs of molten Na into an oil filled recipient. It’s not really terribly hard to do but as entropy51 pointed out, it takes lot of electron juice to make appreciable quantities.

You pulled out some calcium pellets too? Wrong voltage, I’m guessing…

m1tanker78 - 12-2-2011 at 16:29

Quote: Originally posted by blogfast25  
Oookaaayyy. So this is classic electrolysis of NaCl/CaCl2 (now even minus the CaCl2!)


Yes.

Quote: Originally posted by blogfast25  
Forget about scaling that up in a garden shed lab.


C'mon, now! :o

Quote: Originally posted by blogfast25  
Len1’s NaOH cell is hard enough…


If we're thinking about the same thread, I read through the ENTIRE thing, twice. Very long but interesting thread indeed. Hard? Yes. Impossible? Heck no!

Quote: Originally posted by blogfast25  
Want electrolytic sodium? Try a simple NaOH ‘cell’, an argon blanket to protect the nascent sodium, a gauze spoon to scoop blobs of molten Na into an oil filled recipient. It’s not really terribly hard to do but as entropy51 pointed out, it takes lot of electron juice to make appreciable quantities.


I'm definitely not discounting the use of a NaOH cell nor anyone else's cell design. I may very well end up using NaOH if/when I would like to extract some Na. I like the idea of using NaCl, though. Not necessarily from a practical standpoint; more experimental than anything. My NaCl 'cell' did just that and there are MANY improvements that can be made to it to increase efficiency as well as some autonomy. Heck, I extracted a few grams of relatively clean Na with a welder and some junk I had laying around the shop.

Quote: Originally posted by blogfast25  
You pulled out some calcium pellets too? Wrong voltage, I’m guessing…


Hell yes! Wrong voltage is an understatement...

@Peach: I'm uploading a few pics as well as a short video. My phone gets a case of the ass when I want to upload media. :mad:

Tom

entropy51 - 12-2-2011 at 16:58

Quote: Originally posted by m1tanker78  
Sorry for the confusion. I meant to say *grams* in my original post, not ounces. That's what happens when you post at 2a.m. and you're raised with imperial units. If I had 5 ounces of Na I would have taken a quick trip to the lake :D
Really? You wrote ounces three separate times in your original post. Hardly a slip.

You're also the guy who wanted to make NaOH by dissolving Na metal in H2O.

I think you were, and are still, feeding us fairy dust.

m1tanker78 - 12-2-2011 at 17:27

Quote: Originally posted by entropy51  
Really? You wrote ounces three separate times in your original post. Hardly a slip.

You're also the guy who wanted to make NaOH by dissolving Na metal in H2O.

I think you were, and are still, feeding us fairy dust.


Yeah, that must be it. But seriously, why would I feed anyone B.S.? You're not obligated to believe it.....

I'm no chemist but:

Quote:
Sodium reacts with water to form sodium hydroxide and hydrogen gas according to the
equation:
2 Na (s) + 2 H20 (l) ---> 2 NaOH (aq) + H2 (g)


Practical or not, it is possible.

Tom

Sodium pics and vid.

m1tanker78 - 12-2-2011 at 18:15

Here's a couple of pics of what's left of my Na and a short vid where I drop a couple of specks in some alkaline water. The pill bottle contains small chunks/specks while the larger container has larger chunks in it. Take it for what it's worth - Na or "fairy dust" and forgive the poor quality....


2011-02-12173546.jpg - 85kB 2011-02-12173602.jpg - 73kB 2011-02-12173815.jpg - 122kB

And here's the youtube vid:

http://www.youtube.com/watch?v=kdgKQPPIP-A

Tom

bfesser - 12-2-2011 at 18:18

You might want to keep your work area just a bit cleaner--looks a bit too much like a meth lab to the authorities, if you don't.

m1tanker78 - 12-2-2011 at 18:19

Good Lord! I hit the wrong button. I meant to post this as a reply to this thread:

http://www.sciencemadness.org/talk/viewthread.php?tid=15498

Mods, can this be moved?

Tom

entropy51 - 12-2-2011 at 18:31

Well, that's convincing evidence of, errr, ummm...inconclusiveness.:D

Sedit - 12-2-2011 at 18:59

Stop fucking trolling, you asked for proof and he gave it to everyone. Enough said, sheeesh does this place have to turn into a troll fest for everything?

entropy51 - 13-2-2011 at 08:12

Quote: Originally posted by Sedit  
Stop fucking trolling, you asked for proof and he gave it to everyone. Enough said, sheeesh does this place have to turn into a troll fest for everything?
That would be funny if it weren't so lame. You were one of the main Troll Testers in the thread about Pok's potassium method.

The video tells us nothing about how the sodium (?) was made. I've seen CaO give more reaction when added to water. He said he used an arc welder. I've made more Na than he shows using a benchtop power supply.

[Edited on 13-2-2011 by entropy51]

blogfast25 - 13-2-2011 at 08:17

@Sedit: look up the definition of trolling. Expressing doubt or being skeptical doesn't do it.

@m1tanker78: making NaOH by reacting Na with water is the naffest idea since Mozes. They practically pay you for buying it!

Even more so because NaOH is in fact produced by electrolysis of NaCl brine. If you’re interested (and serious) I’ll provide more info.

Re. your current sodium, I doubt if there’s 5 g there. I know what 5 g of potassium globules looks like and it’s a helluvalot more than that.

Next run: capture your Na in kerosene, paraffin (light) oil, paraffinic baby oil (but not silicone oil) instead of cheap motor oil…


[Edited on 13-2-2011 by blogfast25]

Fleaker - 13-2-2011 at 09:14

I was interested in seeing his idea of a Downs cell. I experimented with that about the time I joined this forum as Fleaker. My setup was in a coffee can that I had coated with kaolin. The whole setup was heated in a small furnace I had made out of a stainless steel stock pot and perlite+1600 C castable refractory. It was propane fired. The salt had to be melted and consistently kept hot, I used the same CaCl2/NaCl eutectic that this fellow did. Temperature control was almost impossible. I remember getting chlorine, but I can't remember if I ever got any sodium. I used black iron piping with a reducing adapter (bell-shaped) to collect the sodium.

Seeing as that was 7 years and several computers ago, I don't remember much more about it except that I concluded it was impractical to do on the small scale because success was limited. I suppose a small unit could be built if one has electric heating and does it in a kiln. For the small size of what I was doing, resistive heating of the bath was not sufficient to keep it liquid. I should have pictures or maybe a drawing in MS Paint of the system. Now that sodium is (for me) cheap and readily available, this is of academic interest.

blogfast25 - 13-2-2011 at 10:09

Talk about a homemade Downs Cell: cop a load of this, the link below is about the design of a Downs Cell, planned to operate at about 8 V and 400 A (!):

http://4hv.org/e107_plugins/forum/forum_viewtopic.php?1987

Notice the size of the anode! And note also that the thread goes dead in mid 2008... Sadly because the design is exquisite!

Sedit - 13-2-2011 at 10:33

Blogfast I was expressing doubt and skeptism in Poks Sodium thread. Thats how its done, Not once did I come right out and tell pok hes a liar only that I had suspicions he may be.

Expressing concerns then Asking for pictures only to still complain even after the person supplies them is trolling. His intent was to get a reaction from M1 and had nothing to do with furthering the thread or expressing any concerns. To many threads are getting derailed lately and it should stop.

blogfast25 - 13-2-2011 at 10:56

Sorry, but I saw no derailment here. Nor was anyone called a liar. M1’s initial reporting was shoddy: to claim 5 ounces and then backpeddle to 5 g is (was) indeed suspicious, as is the claim ‘I pulled out some calcium metal too’. How pray, tell? Sodium contaminated with calcium, possibly. Calcium and sodium are (apparently) only partly miscible so it’s not impossible…

The video is worthless: it doesn't even show the apparatus.

This experiment is worth a hell of a lot more skepsis that pok's did. Pok's description was clear as a bell, as crispy as his photos. At least so far... Here we have lots of jubilation but little explanation.

[Edited on 13-2-2011 by blogfast25]

m1tanker78 - 13-2-2011 at 11:34

@Blogfast: I agree about NaOH from Na + H2O is silly. I had to try it for myself, though. Now that I've done it, I can put it behind me. Although I did get some very CLEAN NaOH...

As for the oil situation - you should have seen the look on my face when I switched off the power supply and pulled that stem out after the bath cooled some. My choices were motor oil, WD40, dirty kerosine (lamp oil), or chain oil. The exposed Na was burning so I grabbed the motor oil and dunked the entire stem in it. Oddly enough (or not) the oil now smells strongly of NaOH and the Na has tarnished quite a bit so I'm going to look for one of the other oils you mentioned before the next run.

@Fleaker: I'd be interested to share notes with you about your previous attempt if you could dig them up.

@All: Some of this shit -IS- borderline trolling. It defeats the purpose of sharing ideas and thoughts. Having doubts isn't trolling but if you're going to doubt everything then why even follow the thread? Discount the thing and move on if you don't believe it or if it's child's play to you...

One other thing. What's the deal? Do people come on here and make fake claims about stuff? I've been lurking the forum for a while and none come to mind.

I was trying to show that an amateur (like me) can extract a considerable amount of Na from plain old NaCl without going over 100 amps (less, actually). If you don't want to believe it then move on! You're not obligated to believe and I'm not obligated to bend over backwards to prove it. Right?

Simmer down people!!!

Tom

entropy51 - 13-2-2011 at 11:45

Quote: Originally posted by m1tanker78  
@All: Some of this shit -IS- borderline trolling.
Trolling is coming to a chemistry forum and asking, apparently seriously, if you can make saturated NaOH solution by adding Na metal to H2O. Now that is trolling.

It's like asking if you can make a gallon of water by burning hydrogen. Well of course you can, but what is the point of the question that justifies starting a new thread?

Don't forget that you originally made claims of making significant amounts of sodium, then retracted those claims. The little bit of something that you show is less than can be made using a small power supply. It is not the "considerable amount" that you are still claiming. One or two members of the forum have actually done that. You have not.

cyanureeves - 13-2-2011 at 12:08

Quote: Originally posted by m1tanker78  
@Blogfast: I agree about NaOH from Na + H2O is silly. I had to try it for myself, though. Now that I've done it, I can put it behind me. Although I did get some very CLEAN NaOH...

As for the oil situation - you should have seen the look on my face when I switched off the power supply and pulled that stem out after the bath cooled some. My choices were motor oil, WD40, dirty kerosine (lamp oil), or chain oil. The exposed Na was burning so I grabbed the motor oil and dunked the entire stem in it. Oddly enough (or not) the oil now smells strongly of NaOH and the Na has tarnished quite a bit so I'm going to look for one of the other oils you mentioned before the next run.

@Fleaker: I'd be interested to share notes with you about your previous attempt if you could dig them up.

@All: Some of this shit -IS- borderline trolling. It defeats the purpose of sharing ideas and thoughts. Having doubts isn't trolling but if you're going to doubt everything then why even follow the thread? Discount the thing and move on if you don't believe it or if it's child's play to you...

One other thing. What's the deal? Do people come on here and make fake claims about stuff? I've been lurking the forum for a while and none come to mind.

I was trying to show that an amateur (like me) can extract a considerable amount of Na from plain old NaCl without going over 100 amps (less, actually). If you don't want to believe it then move on! You're not obligated to believe and I'm not obligated to bend over backwards to prove it. Right?

Simmer down people!!!

Tom

sorry for messin up. but please show us how you made it.

cyanureeves - 13-2-2011 at 12:14

Quote: Originally posted by cyanureeves  
Quote: Originally posted by m1tanker78  
@Blogfast: I agree about NaOH from Na + H2O is silly. I had to try it for myself, though. Now that I've done it, I can put it behind me. Although I did get some very CLEAN NaOH...

As for the oil situation - you should have seen the look on my face when I switched off the power supply and pulled that stem out after the bath cooled some. My choices were motor oil, WD40, dirty kerosine (lamp oil), or chain oil. The exposed Na was burning so I grabbed the motor oil and dunked the entire stem in it. Oddly enough (or not) the oil now smells strongly of NaOH and the Na has tarnished quite a bit so I'm going to look for one of the other oils you mentioned before the next run.

@Fleaker: I'd be interested to share notes with you about your previous attempt if you could dig them up.

@All: Some of this shit -IS- borderline trolling. It defeats the purpose of sharing ideas and thoughts. Having doubts isn't trolling but if you're going to doubt everything then why even follow the thread? Discount the thing and move on if you don't believe it or if it's child's play to you...

One other thing. What's the deal? Do people come on here and make fake claims about stuff? I've been lurking the forum for a while and none come to mind.

I was trying to show that an amateur (like me) can extract a considerable amount of Na from plain old NaCl without going over 100 amps (less, actually). If you don't want to believe it then move on! You're not obligated to believe and I'm not obligated to bend over backwards to prove it. Right?

Simmer down people!!!

Tom

blogfast25 - 13-2-2011 at 13:06

Quote: Originally posted by m1tanker78  
One other thing. What's the deal? Do people come on here and make fake claims about stuff? I've been lurking the forum for a while and none come to mind.

I was trying to show that an amateur (like me) can extract a considerable amount of Na from plain old NaCl without going over 100 amps (less, actually). If you don't want to believe it then move on! You're not obligated to believe and I'm not obligated to bend over backwards to prove it. Right?

Simmer down people!!!

Tom


M1tanker78:

Unfortunately we do have people here, mostly non-scientists, that make the most risible claims (I can substantiate that). Recently someone claimed to have made sodium metal from sodium chloride and lithium metal. Well, it took all my powers of reason and persuasion to make the experimenter see that the ‘obtained metal’ was in fact… lithium (no reaction had taken place)! In the mean time some equally non-scientific members had started to believe NaCl + Li --- > Na + LiCl is possible, despite this not being the case.

So scrutiny, even harsh scrutiny, is highly necessary on a forum like this and is the life-blood of Good Science.

BTW, we still haven’t had a decent description or image of your experiment. That lack too is part of Bad Science. Come on: keep us in suspense no longer!

m1tanker78 - 13-2-2011 at 13:39

Blog and Reeves: If it's the 'aparatus' you want to see, it's laughable (speaking of non-scientific). I'm making a slight modification to it right now. I'm hoping that this will increase the yield before I have to shut it down and collect the Na.

The best way I can describe it in a few words is a modified (dumbed-down) Downs cell. It's little more than an open crucible with the electrodes and collection tube introduced from the top. I use stacked trays from an old food dehydrator to reduce or eliminate the chlorine fumes with lime in the trays.

Hey, in all fairness, science can be FUN sometimes when you break from conventions and just use a little common sense (mainly for safety's sake). I'm not knocking scientists or the scientific process. I'm trying to demistify (not necessarily disprove) the whole 'fused salt in the shed' realm and those who say "it can't be done."

I'm going to finish up the mod to the collection tube and hopefully fire up the bath tonight. I WILL snap some pics and/or take a little video - whether it fails or succeeds. If my last run is any indication, it should be fairly successful but I won't know 'till I fire it up.

Tom

cyanureeves - 13-2-2011 at 17:58

m1tanker78 that sounds cool as heck.with table salt! temptation and a better burning bush got the best of me when i made it with magnesium and sodium hydroxide.i kept dropping it in water until it was all gone.

m1tanker78 - 13-2-2011 at 19:42

Reeves, I've always wanted to try that reaction but from what I've seen, the Na is pretty contaminated. Either way, setting that bad boy off sounds like a blast (pun intended).

Unfortunately, the mod I made on the collection tube didn't work well. What I did was took the existing collection tube, drilled a hole about an inch and a half from the bottom, took another tube and drilled a hole about 2.5 inches from the bottom and welded them together. So basically the 2 tubes were welded together with the holes aligned. The idea was that the Na would begin to fill the primary collection tube and spill over into the other one.

That additional tube gave me all kinds of problems. Not in itself but because I had to bump the amperage up to fluidize the salt more so I could plunge the collector in the bath. Well, I had to bump the amperage so much that my cathode melted! The F'd up part is that I didn't realize that it melted until I had the collector in place. I noticed that the 'fireflies' were popping up in the wrong place and after a little while, I decided to pull the cathode out of the bath. Needless to say, the "business end" was missing! I decided to call it quits for tonight because it's impossible to keep the 'fume hood' over the damned thing when I'm constantly having to manipulate it.

Tomorrow I'll retry the experiment in the same way I did a couple of days ago. KISS, I guess. I'll have to make another collection tube since I used the original one with the mod. No biggie, It'll take 3 minutes. The problem with the original collection tube is that the Na only creeps up about 2.5 inches up the tube before it begins to solidify. A few grams of Na is better than none; that's for damned sure! The following mod will probably be trying a slightly larger diameter stack.

By the way, the collection tube's ID is 3/4" x 3/4". So I pulled out approx 1.4 cubic inches of very pure Na the other day. A quick conversion put that at just under 23 cc's. Widipedia isn't always right but says Na's density at RT is just under 1 gram per cc. So I actually had closer to 20+ grams, right? There was quite a bit more that solidified in the crucible. It wasn't immediately apparent but after a while, the surface began to turn white then yellow. From what I've read, that was sodium oxide taking on extra oxygen to become sodium peroxide. The stuff in the crucible was pretty contaminated anyway.

I guess I shouldn't rely on large paper clips for gram weights... Next time I'll try gently warming the tube with the torch; having the tip submerged in oil to see if it'll come out as one bulk. Last time, I scraped bits of it out with a screwdriver - was afraid to have it out of the oil for very long.

Tom

metalresearcher - 14-2-2011 at 02:04

I think making Na chemically by heating Na2CO3 + 2 C => 2Na + 3CO is easier. Put the reactants in a bent stainless steel tube welded together on the 'hot' side and ducked into an oil bath the cold side.
Heat it to 1200oC in a propane furnace (you get this after 15 minutes) sit and wait..... (with face mask on ).

a_bab - 14-2-2011 at 02:10

...for 2 days, with a truck filled with propane tanks at hand (that's described in Muspratt, albeit using coal ;) ).

Sodium will start to come off after several hours, in small amounts much like WP. In order to see when does this happen, you are supposed to let the exaust into open air and ignitr the CO that will be released. When the flame turns very yellow it's the show time.

m1tanker78 - 19-2-2011 at 19:35

Quote: Originally posted by metalresearcher  
I think making Na chemically by heating Na2CO3 + 2 C => 2Na + 3CO is easier. Put the reactants in a bent stainless steel tube welded together on the 'hot' side and ducked into an oil bath the cold side.
Heat it to 1200oC in a propane furnace (you get this after 15 minutes) sit and wait..... (with face mask on ).


I considered trying this before going the NaCl route but found this website while poking around the net (might be the same one you're referencing):

http://www.metallab.net/Na.php

He used a SS retort and dead-ended it into some mineral oil like you mentioned. It looked promising at first but the only Na he extracted was a little that condensed in the tube. I wish he would have attempted the NaOH/thermite reaction in that thing as others on the net have done in a cooking pot. It's been a while since I've looked at those but I seem to remember that there were 3 disadvantages to this reaction.

1. The starting materials.
2. Unpredictable and/or small yields.
3. Highly contaminated yield and no easy way of separating from the Na.

It's been a LONG week for me so I wasn't able to take any more shots at this except for one and it was a quickie. I tried to reproduce the successful run I did the other day so I limited the collection time to 30 minutes and tried setting everything up the same way. Approx 90%/10% NaCl/CaCl. The CaCl wasn't fully dehydrated.... (ughhh!).

I ran out of 3/4" square tubing so I used the closest thing I had on hand which was 5/8" I.D. square tubing. I let everything cool down for 2 or 3 hours and found I had ...... I'm not even going to speculate here; I'll just say that the 'cake' was a little over 1/2" thick in a 5/8" x 5/8" tube minus the big hole I made (I'll explain below). Much less than the first good run but still do-able. I'm still working on purchasing some basic essentials like a sensitive scale, some glassware, etc so I have no way to accurately weigh things at the moment. The Na was virtually pure except for a little contamination that can be seen on the upper left portion. I believe that was copper chloride. I was in a hurry and didn't etch all the copper off the carbon rod before I started but who knows...

I snapped a pic of the tube after it cooled a while and sat in the oil a bit.

2011-02-12 11.08.45(3).jpg - 80kB

I accidentally punched a big hole in the cake while it was still hot. I use a dipstick, for lack of a better word, to feel inside the collection tube. It's just a solid SS rod. I wear thick chemical gloves and thick leather welding gloves on top of them so it's very hard to manipulate small objects. Just before I cut the power, I decided to check the Na once more. The F'n rod slipped out of my hand and down the collection tube and punched a hole. I initially thought I'd lost almost all the yield because there was a bit of a firestorm in the crucible (burning Na).

Anyway, I'm not even going to take a guess at the yield; use your imagination here. Also, I used mineral oil this time around (thanks BlogFast) but noticed that the Na reacted with it significantly quicker than it did with the cheap motor oil. It was right out of the bottle too so it was unexpected. Maybe tiny air bubbles from when I poured it or traces of moisture in the container. When I get some time I'll pull a vac on some of the MO and see if it outgasses and/or releases moisture.

Tom

peach - 20-2-2011 at 01:20

That's his site, the guy you're replying to.

There was a thread here on the forum where it was discussed. <--- link

There was a fairly major problem with the tube melting, even though he was running it at what was thought to be below it's MP, perhaps due to the tube being somewhat thin and under load. From what I remember, the yield was never isolated or checked - there was only some crackling when the tube was later put in water.

"The F'n rod"? Are you sure you're from Texas? The only place I usually hear people saying that is Scotland. :D

Even if you can't take a really tidy picture of it working, can you put the bits together in roughly the same they were used for a quick and dirty photo?

Theoretically, the idea of making sodium is simple. In practice, it's proving to be very tricky to get clean, sizeable amounts in a lot of these tests. Len is the only person who has managed to get a very clean, reproducible result; likely as a result of the amount of thought and care he put into designing the thing.

watson.fawkes - 20-2-2011 at 08:24

Quote: Originally posted by peach  
"The F'n rod"? Are you sure you're from Texas? The only place I usually hear people saying that is Scotland. :D
Peach, sometimes a rod is just a rod.

blogfast25 - 20-2-2011 at 09:24

Quote: Originally posted by watson.fawkes  
Quote: Originally posted by peach  
"The F'n rod"? Are you sure you're from Texas? The only place I usually hear people saying that is Scotland. :D
Peach, sometimes a rod is just a rod.


Personally I think he's making a rod for his own back... :)

m1tanker78 - 20-2-2011 at 15:16

@Metalresearcher: Sorry, I didn't know that was your web page. Ever consider doing the thermite(?) reaction in your retort to see what would happen? I have a feeling that if the Na does vaporize over, it'll disperse in the oil but it'd be a fun experiment anyway.

@Peach: Yep, I stepped right into that one with my choice of words. Let's see, "F'n rod"; "Collection tube" :D . But no, the Lone Star State is my home and I wouldn't have it any other way. Only 5,000-ish miles away from Scotland. :D

@Blogfast: What process were you referring to for NaOH production? Is it the chlor-alkali cell? Just so you know, I'm not planning on using the Na I produce to make NaOH (intentionally). I wanted to know if I can dunk the crucible in a container with some water to capture the NaOH that is left after the Na reacts with air and moisture. Well, I know I can do it because I've already done it. Still have some NaCl mixed in though. I don't care about the salt one bit. It costs ~0.15$ to fill the crucible and maybe a couple of pennies to keep it going if I reuse the same salt with subsequent melts. Any thoughts on this?

I drew a quick and dirty diagram of my cell. Nothing to it really. The most important aspects are the cathode (Ohm's Law) and the spacing between the electrodes and crucible (again, Ohm's Law) if it's made of steel or any conductive material. If using a non conductive crucible, this doesn't matter too much but cathode must still be "J" shaped with hard bends and aligned with the anode. Everything is drawn on the left but in reality, it should be somewhat centered.

Sodium Cell Drawing.jpg - 54kB

Tom

blogfast25 - 21-2-2011 at 08:45

M1tanker78:

Commercially NaOH is produced by electrolysing a concentrated solution of NaCl in water (brine). This produces OH- ions and a mixture of NaCl and NaOH in solution is thus obtained (the maximum conc. of NaOH that can be obtained this way is described in the lit.) The solution is then evaporated (presumably in the absence of CO2 to avoid carbonate formation) to about 50 % NaOH, at which point the NaCl drops out (and is recycled). Filtering and further evaporation of the solution then yields the solid NaOH. Great if you want to mess around with hot concentrated NaOH solutions!