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m1tanker78
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Sodium Garbage Time And Unusual Results
First, let me explain what 'garbage time' or 'trash time' is. I normally reuse the electrolysis blocks 2 to 4 times before I chuck 'em and start over
with fresh, clean ingredients. I normally limit the run times to 30 - 60 minutes. When I decide that the block will be discarded, I usually take
around 30 minutes extra at the tail end to introduce different stuff to the melt or generally try something new which usually contaminates the block.
This aptly earns the term 'garbage time'.
I did a 1 hour run this weekend + 1 hour GT. When garbage time came around, I replaced the anode with a 18/0 'stainless' fork but didn't leave it for
very long. I began to see a yellow-green substance condense around the melt. I don't use a fume hood, only forced ventilation and was concerned about
chrome toxicity.
After I replaced the anode, I introduced some small chunks of cinder block to the melt and let it brew for a little while. Of course, there isn't any
set composition for cinder block; it's just a mixture of aggregate and (supposedly) ash.
I had some unusual difficulty coalescing the sodium that resulted (I included a video below). When the nugget cooled, it appeared to have a
bluish-purple-gray color and moreover, it seemed to form a skin on the nugget. I've seen this skin effect with calcium contamination before but not
that color! I haven't conducted any flame test or anything yet. I'm open to suggestions for determining impurities. With such a high MP, I don't see
how chromium could be the culprit but can't rule it out just yet. Potassium and calcium seem like good candidates...
A shot of the nugget and the contrast it creates. The mass is 3.6g
This video demonstrates the slight difficulty I had coalescing the beads. They normally 'pop' together in a matter of 5 - 10 seconds with
little or no need to guide them together. If you look closely toward the end, you can see impurities 'swimming' on the surface of the molten nugget.
The black masses are normal; easy to remove. PLEASE RESERVE STUPID COMMENTS ABOUT CLEANLINESS AND "METH LAB" BULLSHIT. THANKS!
<iframe sandbox title="YouTube video player" width="640" height="510" src="http://www.youtube.com/embed/RAwca9B1BN4" frameborder="0"
allowfullscreen></iframe>
Please share your thoughts (cinder block content, nugget color, chrome, etc.).
Tom
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blogfast25
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What do you mean by 'electrolysis blocks'?
Any dirt on the surface of the nuggets will somewhat hinder their coalescence (I see that a lot with K too...) but this sodium seems to coalesce
really just fine to me.
What's your electrolysis apparatus?
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m1tanker78
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Blog, 'block' is a generic term I use for the solidified melt. I use an iron vessel for the crucible, steel cathode and carbon anode.
Tom
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cyanureeves
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m1tanker78 arent you the one who said your method of making sodium was ridiculously simple?how simple?how do you do it with cathode and anode?with a
welding machine? do you zap a heap of sodium hydroxide?do you have a video of such process?have you seen the prices for sodium on that site nurd rage
posted?you can make money even.
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m1tanker78
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Quote: Originally posted by cyanureeves  | | m1tanker78 arent you the one who said your method of making sodium was ridiculously simple?how simple?how do you do it with cathode and anode?with a
welding machine? do you zap a heap of sodium hydroxide?do you have a video of such process?have you seen the prices for sodium on that site nurd rage
posted?you can make money even. |
I don't know what site you're talking about but I don't aim to sell it.
Tom
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cyanureeves
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wow! symboom posted a youtube video of sodium being made with what looks like a battery charger,two electrodes and molten sodium hydroxide. also
posted a video of a humphrey davey using the servants quarters to do experimental lab work with potassium.very interesting and smart dude.
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m1tanker78
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@cyanureeves: I'm fascinated with Davy's work. I know other scientists of that time did work with alkali metals but as far as I'm concerned, Davy is
the patron saint of alkali metals.  What I'd give to live in those times
(temporarily) LOL.
I might publish some of my work here in the near future. It takes quite some time to condense notes, edit videos, etc just to have the discussion
derail into personal attacks and such. For now, could someone kindly give me a simple procedure that I can use to test the nugget for
chromium?
For example, can I cut a little piece off, put it in cold distilled water (to react Na/K/Ca). After reaction, acidify with HCl and possibly add a
little H2O2 and look for a _______ tint?
Does this sound like a reasonable test? If so, what color would Cr(III)(?) produce in acidic solution? Some sources say amber, others say green. I
know several members here have experience with Cr compounds so let's hear it!
Tom
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plante1999
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ad it to melted naoh and than ad it to water you will get orange sol if Cr is present. if no.... i think you know...
I never asked for this.
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cyanureeves
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if its chromium it will turn bright canary yellow. i just did the method plante1999 did to extract chromate from nichrome wire using lead acetate and
got a bright orange precipitate just as bright as sodiumdichromate. since your chromium is already mixed with sodium it probably will turn yellow as
soon as you use hcl.but you forgot about iron because when i carbonated the acidic chromium/iron solution and back to acidic with vinegar i got a
purple solution. youtubers bad mouth alot about drug manufacture and appearaces,but probably not here.
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bob800
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| Quote: Originally posted by cyanureeves | | wow! symboom posted a youtube video of sodium being made with what looks like a battery charger,two electrodes and molten sodium hydroxide. also
posted a video of a humphrey davey using the servants quarters to do experimental lab work with potassium.very interesting and smart dude.
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Where are these videos??
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cyanureeves
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@ bob800 right here, right now. second page under sodium by electrolysis.
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m1tanker78
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bob800, http://www.youtube.com/results?search_query=molten+sodium+el...
Tom
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blogfast25
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I don’t see any videos signed ‘synboom’.
Tanker78, your search for chromium may just be a wild goose chase.
Here’s a tentative explanation for the brown film: thin layer diffraction. It’s very common on the surfaces on many transition
metals where an oxide layer of only a few molecules thickness can cause all sorts of colourful effects to appear, much like a thin film of petrol on a
puddle of water does. Nb, W, Mn, V and Ti have all shown this property to me.
Now, Na isn’t a hard transition metal of course but an unusually obtained film of Na oxide/superoxide might still generate unusual colours.
Just an idea…
Alternatively, just peel that ‘potato’, dissolve the 'peel' in water (add HCl for water insolubles) and test for chromium: it’s easy to do
[Edited on 26-4-2011 by blogfast25]
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m1tanker78
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I cut a small piece of sodium in question and dropped it in dilute HCl. Most of it shot out (as expected). I reset and dropped another small piece in
cold distilled water. After it got done skimming around, I acidified with HCl. There may have been a hint of yellow (but it could have been the HCl,
itself. After an hour or so, I added a little bit of H2O2 to the solution. No strange color changes.
**************
The inside of the nugget is most definitely contaminated with something. A cross section where I sliced it revealed a dark(er) substance in the
center. This I've never seen with pure Na or even low potassium NaK alloy...
Any suggestions??
**************
Blog and others, the videos that are being talked about don't belong to symboom. He posted links to them in another thread. The videos depict the
author(s) electrolyzing molten NaOH.
Tom
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blogfast25
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Tanker78:
Trying to dissolve Na in even dilute HCl isn’t clever: the metal needs to be tamed, not irritated, don’t play with the dragon’s tail!! Alcohol
or methanol is actually a better solvent for analytical work on Na metal. Then add water or HCl to dissolve the insoluble bits. Or evaporate the
alcohol and dissolve the obtained Na ethoxide (or methoxide) in water, which will almost completely hydrolyse it to NaOH + alcohol. The colour of the
alkoxide residue alone should be telling (Na alkoxides are white)…
Seems to me your colour was simply surface oxide: people have reported all kinds of colours for oxidising sodium.
Suggestions? Not to worry so much! That spec could be a vacuole or a minor solid contaminant caught in the sodium close to melting point. Your metal
seems of very good quality on the whole, so when are you going to show the set up?
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m1tanker78
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Blog, the spec could be a gnat that fell in the oil for all I know.
I was talking about the dark patch around the speck. This was visible just as soon as I sliced the nugget. That isn't normally seen in pure samples of
alkali metals or alloys. I'm not too hung up on it, just a little curious about it. The crystallization pattern is also way off the mark.
These photos show a comparison of what pure sodium (different nugget than above) looks like after being cut and after the
crystallization patterns become visible...
==================
Any ideas concerning the cinder block content?
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m1tanker78
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| Quote: | | Alcohol or methanol is actually a better solvent for analytical work on Na metal. |
Would 91% IPA be good enough for this?
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m1tanker78
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I put a small piece from the sodium nugget in question into 91% IPA. After the reaction was complete, there were 3 layers. The bottom layer turned
yellow and has some small black specks in it...
I included the video of the reaction here in case anyone would like to watch it...
<iframe sandbox title="YouTube video player" width="640" height="510" src="http://www.youtube.com/embed/As2TKGtRQRc?rel=0" frameborder="0"
allowfullscreen></iframe>
I'm not too concerned with the black specks - probably carbon. What is the middle layer and what should I make of the yellow stuff?
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cyanureeves
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ha!one of the neatest thing ever. it looks like naplam falling from the sky. the solid would be sodium something?is that a so called ethoxide
solution?it looks like something separated from water.was the mist cold?how about the solution?your yellow stuff looks pretty concentrated too and not
so much like a tincture.
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unionised
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I'm not sure about the 3 layers but sodium hydroxide solution does not mix with IPA and wet IPA may not mix with some hydrocarbon oils.
Had the Na been kept in oil?
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blogfast25
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In all likelihood the formed sodium isopropoxide (sodium 2-methylpropoxide) is ‘salting out’ the 91 % IPA, that is: it’s driving out the water,
explaining the layers. At the same time the isopropoxide is hydrolysing to NaOH due to the water. It’s also possible that the sodium is reacting
preferentially with the water, thus forming NaOH (which then salts out the IPA). Pure IPA isn't soluble in water with high salts contents...
To answer your previous question about the suitability of 91% IPA, in short; ‘NO!’
But you can repeat the experiment in a meaningful way as follows: look up ‘salting out IPA’ (or similar terms): there are plenty web pages that
detail how to convert 91% IPA to almost 100% IPA by adding lots and lots of NaCl to it. The salt ‘pulls’ out the water leaving you, after
filtering usually, with quite pure isopropyl alcohol.
Next, instead of dunking a whole nugget into the alcohol, cut a neat piece, totally free of skin and protective oil and see how it reacts and whether
you’re getting a clean, clear solution of sodium isopropoxide in IPA. Any oil would probably emulsify into the alcohol, creating deceptive
results…
Alternatively, use any dry alcohol: methyl, ethyl, propyl…
Salting out IPA:
http://www.instructables.com/id/How-to-Salt-Out/
[Edited on 27-4-2011 by blogfast25]
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m1tanker78
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Thanks Blog, I'll repeat the experiment with some [almost] dry IPA.
FYI, this particular nugget was mostly free of the superficial crust. The reason it's rounded is because I remelted it in some heavy oil. I made every
effort to manually remove the oil from it but a little undoubtedly transferred to the IPA.
cyanureeves, I'm blind and lost when it comes to organics so maybe another member can answer your question. My belief is that the white flakes were
(mostly) NaOH which settled at the bottom then pulled water from the IPA. It didn't take them long to dissolve and form an aqueous layer.
+++++++++++++++++++++
EDIT: I'm a little confused. The questionable nugget is now silvery-white (was purplish). It still shows a darker band in the cross section. The
bottom most layer of the IPA sol'n is fading from yellow to crystal clear and a white satin-like substance is dropping out in what was the middle
layer. *SIGH*.....
Here's what the nugget looks like now. It's the one that's been cut:
Tank
[Edited on 4-28-2011 by m1tanker78]
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blogfast25
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It points to my hypothesis that this is a purely superficial phenomenon, involving a surface oxide layer that's changing in thickness and composition.
I really wouldn't worry about it too much: I've seen far, far worse looking sodium.
The alcohol-to-alkoxide (alt. alcoholate) test is more significant IMHO because it tells you something about the bulk of the metal, if properly
executed.
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cyanureeves
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yipee! i made sodium today. i charged my piece of crap 12v black and decker weed wacker battery pack and hooked it to two pieces of welging rods held
by clothes pins,pour some sodium hydroxide,warmed it and the current kept it molten.little bb's kept forming but i couldn't scoop them out because i
was too excited so they just blended back into the unmelted portion. i did scoop up some bb's and dropped them in oil but a good many just went back
into the puddle also.what becomes of the poor lost little bb's?do they turn back into sodium hydroxide?i hope so because i'm using the same melt over
again.some bb's were cover in the hydroxide and when i dropped them in water they would only fizz but when i squished them,then they would do the
sodium dance on the surface. time to invest in a battery charger! hey, would that green draino work? it has salt,sodium nitrate,sodium hydroxide and
aluminum.
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m1tanker78
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First of all, if you intend to go down the sodium hydroxide road then len1's work is required reading. Those threads should answer all your questions.
Let me add that if you're going to spend the bucks on a 12V battery charger, you might want to consider buying a cheap DC inverter welder with
adjustable current setting instead. The main thing to look for in any case is the DUTY CYCLE. A cheap welder will probably provide more juice at 100%
duty cycle; something to consider.
NaOH has it's advantages but I quit NaOH because it's expensive (relatively), it's very hygroscopic (think about it - hard to reuse!), it's very harsh
for certain electrodes, it produces caustic fumes, it spits and splatters a lot, IIRC it requires a cell separator for decent efficiency.
There's also a very finite temperature window - 10*C IIRC. Under that, little or no sodium. Over, Na diffuses back into the melt.
If you get it going then post up some alkali metal porn.
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