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entropy51
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[*] posted on 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Don't forget that you originally made claims of making significant amounts of sodium, then retracted those claims.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.
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[*] posted on 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
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[*] posted on 13-2-2011 at 12:14
sorry for messin up. but please show us how you made it.


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
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blogfast25
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[*] posted on 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!
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m1tanker78
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[*] posted on 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
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[*] posted on 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.
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[*] posted on 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
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[*] posted on 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 ).
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[*] posted on 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.
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[*] posted on 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
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[*] posted on 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.




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[*] posted on 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.
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[*] posted on 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... :)
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[*] posted on 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
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[*] posted on 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!
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