Manganese Metal

[elementcollector1]

I'm reporting in to say that I just electrolyzed a solution of MnCl2 and successfully obtained a plating of pure manganese metal. The solution was very saturated, iron cathode and carbon anode about an inch and a half apart, and 2 amps of current was used if anyone wants to try this at home. Meanwhile, I'm going to go convert all my MnO2 to MnCl2... >;D

 

Pics will follow if I get a large enough yield.

[chilled_fluorine]

I'm reporting in to say that I just electrolyzed a solution of MnCl2 and successfully obtained a plating of pure manganese metal. The solution was very saturated, iron cathode and carbon anode about an inch and a half apart, and 2 amps of current was used if anyone wants to try this at home. Meanwhile, I'm going to go convert all my MnO2 to MnCl2... >;D

 

Pics will follow if I get a large enough yield.

 

Nice. That's pretty much the procedure I plan on following if I ever need a Mn electrode. Not that I think I will. XD

[elementcollector1]

Nice. That's pretty much the procedure I plan on following if I ever need a Mn electrode. Not that I think I will. XD

 

Wow, that was ages ago. Since then I have gotten a much shinier plate of Mn by using two half-cells, with the catholyte being concentrated MnCl2 and the anolyte dilute MnCl2, a copper PCB blank as cathode and 60/40 solder as anode (eliminates production of MnO2 at anode), and a 9V battery as power source.

I kind of wish I could build the plating up to a point where I could physically remove it from the electrode, but I'm still not entirely sure if that's possible with my setup. It would take forever, and I have to keep in mind that the cathode needs heavy cleaning with a towel every 15 minutes to an hour or so to keep that shiny coat of metal and not have it pockmarked with oxides and hydrogen bubbling sites.

[chilled_fluorine]

Wow, that was ages ago. Since then I have gotten a much shinier plate of Mn by using two half-cells, with the catholyte being concentrated MnCl2 and the anolyte dilute MnCl2, a copper PCB blank as cathode and 60/40 solder as anode (eliminates production of MnO2 at anode), and a 9V battery as power source.

I kind of wish I could build the plating up to a point where I could physically remove it from the electrode, but I'm still not entirely sure if that's possible with my setup. It would take forever, and I have to keep in mind that the cathode needs heavy cleaning with a towel every 15 minutes to an hour or so to keep that shiny coat of metal and not have it pockmarked with oxides and hydrogen bubbling sites.

 

You can give up on making any real amount of mn with that method, at least with a 9 volt battery as a power supply. Step it up a notch. Use a wall wart or a computer supply, of course you still won't get anything worthwhile. I just reduce mno2 with al powder, ball mill the slag, then refine. Works well enough for me. It could be purer, but it's good enough for anything I need it for.

[elementcollector1]

What exactly is your 'refining' step?

I tried upping the current/voltage to a car battery charger, but I got black, burnt Mn with noticeable hydrogen spots.

I've tried igniting manganese thermite for quite a while now with a blowtorch with no success. Ordered some good ignition chemicals, and I'm going to try to make better Al powder (from cans, not foil. Cans are pure enough to melt).

A tip from blogfast25, a poster on ScienceMadness who tipped me on manganese thermites: Mix in a 1.11 molar ratio of CaF2 to every mole of Al used. This acts as a heat sink and prevents some of the Mn from boiling away (yes, it does actually boil. No, I've never had this happen for above reasons).

[chilled_fluorine]

What exactly is your 'refining' step?

I tried upping the current/voltage to a car battery charger, but I got black, burnt Mn with noticeable hydrogen spots.

I've tried igniting manganese thermite for quite a while now with a blowtorch with no success. Ordered some good ignition chemicals, and I'm going to try to make better Al powder (from cans, not foil. Cans are pure enough to melt).

A tip from blogfast25, a poster on ScienceMadness who tipped me on manganese thermites: Mix in a 1.11 molar ratio of CaF2 to every mole of Al used. This acts as a heat sink and prevents some of the Mn from boiling away (yes, it does actually boil. No, I've never had this happen for above reasons).

 

A brief soak in certain acids, to remove al and al2o3. A battery charger is probably going to be too much current. I don't use caf2, I just use courser aluminium to prevent boiling. You can melt foil, it is just so high surface area it tends to become useless slag. Foil powder will work fine, as long as it is fine enough. Blowtorches suck at igniting thermite. What I do is use mg ribbon, or kno3 and al. They say the latter doesn't ignite, but it does work. Drop a glowing bit of charcoal on the mix, and it will sizzle and burn blindingly. That's the only way I've been able to ignite it, without in turn lighting IT with mg. If you're close enough to get it with a blowtorch, you're to close to want it to go off. Play safe.

[elementcollector1]

Well, it's a bit late for me to use 'coarse' aluminum...

The ignition mix I ordered is the classic mix of potassium permanganate and glycerin with some Mg ribbon mixed in.

 

Have any pics or weights of your Mn yield?

[chilled_fluorine]

Well, it's a bit late for me to use 'coarse' aluminum...

The ignition mix I ordered is the classic mix of potassium permanganate and glycerin with some Mg ribbon mixed in.

 

Have any pics or weights of your Mn yield?

 

Wow, it's been so long since I last made mn, I don't have much use for it... Anyways, I think I got around a 50 gram yield, that was one bright thermite. No pics, sorry. Took a while to make that al from foil, didn't want to waste my good stuff. I still say kmno4 sucks, it's only good for larger amounts, it does a lot of contaminating, and it's just not very reliable. If your reducing agent and it mix, then you essentially have a pile of flash powder, itching to blow up in your face. It's also just about the messiest shit I've ever seen... BTW, mix vinegar 5% and 3% h2o2 in a 1:1 to clean permanganate stains. This works on skin (finally something non-toxic), and pretty much anything else you can think of, saved me from my parents as a kid more than once.

[elementcollector1]

Good to know about that permanganate stain cleaner!

I can make potassium nitrate, but I'd be using precious ammonium nitrate... although I don't have much of a use for nitric acid anyway.

[chilled_fluorine]

Good to know about that permanganate stain cleaner!

I can make potassium nitrate, but I'd be using precious ammonium nitrate... although I don't have much of a use for nitric acid anyway.

 

Or you could buy it as spectracide stump remover for 3.99 a pound. 97%+ purity, nice and finely powdered. More than good enough for black powder and stuff like that.

[John Cuthber]

Lemon juice removes permanganate stains and, in my personal opinion, smells better than vinegar.

[elementcollector1]

Nope, no Spectracide here. Instant cold packs, though.

[chilled_fluorine]

Lemon juice removes permanganate stains and, in my personal opinion, smells better than vinegar.

 

I tried lemon juice once, but I have to say my method works much better. Lemon juice never worked on skin for me...

 

Nope, no Spectracide here. Instant cold packs, though.

 

If you live in the uk, do you know if you can still get sodium chlorate as weed killer? Don't try that with the aluminium of course.

[elementcollector1]

I tried lemon juice once, but I have to say my method works much better. Lemon juice never worked on skin for me...

 

 

 

If you live in the uk, do you know if you can still get sodium chlorate as weed killer? Don't try that with the aluminium of course.

 

Live in the U.S., and again, unfortunately no. Don't I wish...

The available OTC chems in my neck of the woods are:

-Sulfuric acid, 78%-93.2%

-Hydrochloric acid, 31%

-Sodium hydroxide

-Calcium chloride

-Hydrogen peroxide, 30% (haven't bought this, seen it once)

-Oxalic acid

-Chromium (III) oxide, Vanadium (V) Oxide, etc. at a pottery shop some distance away

[chilled_fluorine]

Live in the U.S., and again, unfortunately no. Don't I wish...

The available OTC chems in my neck of the woods are:

-Sulfuric acid, 78%-93.2% Drain cleaner? The only good purity stuff (low concentration though) we have here is battery acid. ~35% I believe. I just boil it. The neighbors hate me...

-Hydrochloric acid, 31% I get 38% from the pool store. So many fools I have met think you can have 100% at standard conditions... LOL

-Sodium hydroxide Drain cleaner?

-Calcium chloride Here in the far U.S. south, we can't buy it, so I make it with limestone (very abundant) and hcl.

-Hydrogen peroxide, 30% (haven't bought this, seen it once) I haven't seen this in stores, just 15% at the barber's. Would you care to say what it was sold for, a brand name, and hopefully the store you bought it in? I really need some more...

-Oxalic acid Barkeepers friend, right?

-Chromium (III) oxide, Vanadium (V) Oxide, etc. at a pottery shop some distance away Vanadium pentoxide is the orange crap, right? And chromium oxide the green, knew that.

 

I still find it hard to believe you can't find spectracide stump. Have you checked Lowes, Home Depot? They have it in so many places, but I get mine from home depot. I used to make it in few gram batches with bat crap and KCl... Then I found spectracide. And nitric acid.

[elementcollector1]

I still find it hard to believe you can't find spectracide stump. Have you checked Lowes, Home Depot? They have it in so many places, but I get mine from home depot. I used to make it in few gram batches with bat crap and KCl... Then I found spectracide. And nitric acid.

 

Yup. Checked everywhere, no luck. No OTC nitrates here but ammonium, from the local Rite Aid.

Haha, 100% HCl. Now that would be fun to work with.

Yep. Drain opener, but the point is the same. No aluminum shavings, either.

I'll have to go back and check about that H2O2, no idea about the other 70%.

No, actually it's pure oxalic acid as wood bleach. Very expensive, but I hardly ever need to use it.

Vanadium pentoxide is the orangey-yellow, toxic crap, yes. Chromium oxide is the green stuff that's never pure and annoying to synthesize (raise your hands if you want to work with hex-chrome!)

Here's a funny story: I was stocking up on HCl, NaOH, CaCl2 and H2SO4 the other day, and I go up to the McLendon's counter. The woman says, pointing to the NaOH, "You need to be 18 or older to buy that." So my dad, who's there for some rust remover (my fault for working with acids inside the garage), buys it for me. The woman completely ignores the HCl and 93.2% H2SO4. XD

 

Anyway, back on topic, I'm remaking my aluminum powder (but I do need to melt some more aluminum!) This stuff is shiny, not the dull, pencil-streak gray of the previous batches. As for the MnO2, I have 4 ounces of the stuff filling a plastic container to the brim, and I'm assured of its purity (as I made it myself from pure MnCl2), so I'm all set on that end. The CaF2 should be arriving with the ignition stuff any day now, and I prepared some NaNO3 as a backup option.

[chilled_fluorine]

Yup. Checked everywhere, no luck. No OTC nitrates here but ammonium, from the local Rite Aid.

Haha, 100% HCl. Now that would be fun to work with.

Yep. Drain opener, but the point is the same. No aluminum shavings, either.

I'll have to go back and check about that H2O2, no idea about the other 70%.

No, actually it's pure oxalic acid as wood bleach. Very expensive, but I hardly ever need to use it.

Vanadium pentoxide is the orangey-yellow, toxic crap, yes. Chromium oxide is the green stuff that's never pure and annoying to synthesize (raise your hands if you want to work with hex-chrome!)

Here's a funny story: I was stocking up on HCl, NaOH, CaCl2 and H2SO4 the other day, and I go up to the McLendon's counter. The woman says, pointing to the NaOH, "You need to be 18 or older to buy that." So my dad, who's there for some rust remover (my fault for working with acids inside the garage), buys it for me. The woman completely ignores the HCl and 93.2% H2SO4. XD

 

Anyway, back on topic, I'm remaking my aluminum powder (but I do need to melt some more aluminum!) This stuff is shiny, not the dull, pencil-streak gray of the previous batches. As for the MnO2, I have 4 ounces of the stuff filling a plastic container to the brim, and I'm assured of its purity (as I made it myself from pure MnCl2), so I'm all set on that end. The CaF2 should be arriving with the ignition stuff any day now, and I prepared some NaNO3 as a backup option.

 

I remember the days when I made chromium oxide with ammonium dichromate, I had a lot of the stuff for some reason. It's definitely not annoying to synthesize. Light up some dichromate, soak in water, and there you have it. :raises hand: Btw, your aluminium is probably too course if it is still shiny. The good stuff is always gray. Why is fun so directly proportional to danger? The great question... I'm looking forward to your response about the h2o2.

[elementcollector1]

I remember the days when I made chromium oxide with ammonium dichromate, I had a lot of the stuff for some reason. It's definitely not annoying to synthesize. Light up some dichromate, soak in water, and there you have it. :raises hand: Btw, your aluminium is probably too course if it is still shiny. The good stuff is always gray. Why is fun so directly proportional to danger? The great question... I'm looking forward to your response about the h2o2.

 

It might be a while before I go back to the hardware store, but when I do, I'll search for that product.

The thermal decomposition of ammonium dichromate was discussed on another forum, but we eventually abandoned the approach as a route to chromium oxide because of the abundance of impurities. Washing the ash with boiling distilled water helped improve the color, but not by much. The way I have to do it is make sodium chromate, concentrate it, acidify and add an alcohol to reduce to Cr(3+), and precipitate the oxide with sodium carbonate (washing soda). This produces a green-gray precipitate, Cr(OH)3, which calcines to the desired Cr2O3.

I took a closer look at my aluminum, and under the microscope it's not powder, but very fine turnings. *Sigh* time to bring out the old ball mill again...

[chilled_fluorine]

It might be a while before I go back to the hardware store, but when I do, I'll search for that product.

The thermal decomposition of ammonium dichromate was discussed on another forum, but we eventually abandoned the approach as a route to chromium oxide because of the abundance of impurities. Washing the ash with boiling distilled water helped improve the color, but not by much. The way I have to do it is make sodium chromate, concentrate it, acidify and add an alcohol to reduce to Cr(3+), and precipitate the oxide with sodium carbonate (washing soda). This produces a green-gray precipitate, Cr(OH)3, which calcines to the desired Cr2O3.

I took a closer look at my aluminum, and under the microscope it's not powder, but very fine turnings. *Sigh* time to bring out the old ball mill again...

 

Turnings, how I remember. The neighbourhood kids got a lot of mg turnings, ball milled into dust, filled a glass bottle with it, and you can guess what happened next. Naturally I was there to see it... Damn bright it was. The cold pack manufacturers are starting to get smart and cutting the good stuff with ammonium chloride and urea nitrate... Stupid DEA... Watch out for purity, I hear they're making a new type with no AN at all.

[elementcollector1]

Turnings, how I remember. The neighbourhood kids got a lot of mg turnings, ball milled into dust, filled a glass bottle with it, and you can guess what happened next. Naturally I was there to see it... Damn bright it was. The cold pack manufacturers are starting to get smart and cutting the good stuff with ammonium chloride and urea nitrate... Stupid DEA... Watch out for purity, I hear they're making a new type with no AN at all.

 

Mm. Should I stock up on AN then?

Ah, the magic of explosives. Fireworks are nice, but unless you're setting them off or 10 feet away, they're not nearly as fun.

I hate cutting through magnesium and aluminum to get nice turnings, but I'll try using a drill. That might work better (I've seen someone get quite a lot of good, fine turnings with a wide drillbit). I just hope the metals don't break the drillbit, otherwise I have to pay for a new one.

 

I've seen lab reagent aluminum that was a bright silver powder, and the stuff from Etch-A-Sketches actually stained my hand bright silver for a time. (It was pretty cool, better than paint. Combustible, too!) Of course, the reagent-grade stuff was likely made by injecting molten aluminum through a very fine droplet outlet into argon gas, so it's probably still ultra-reactive and stuff.

 

That NaNO3 is taking forever to dry. Not as long as the MnO2 did, but sodium hydroxide dessication isn't making the thing any less damp.

[chilled_fluorine]

Mm. Should I stock up on AN then? Of course... Once the zombies attack no more will be made...Seriously though, the DEA is just itching to abuse the social contract. They could make it as hard to get as hydriodic acid any day. :remembers a day when it was easy to obtain:

Ah, the magic of explosives. Fireworks are nice, but unless you're setting them off or 10 feet away, they're not nearly as fun. Unless you're in Pakistan... No offense to any peaceful Pakistanis out there, just the violent ones. Thermobaric weapons are admittedly quite fun. Until you start to kill people with them.

I hate cutting through magnesium and aluminum to get nice turnings, but I'll try using a drill. That might work better (I've seen someone get quite a lot of good, fine turnings with a wide drillbit). I just hope the metals don't break the drillbit, otherwise I have to pay for a new one. You seriously think you can break a carbide or hardened steel bit with al or mg? Good luck. You need yourself a good bench grinder. For parts and stuff (except maybe anodes for boats) al and mg are pretty much useless without alloying agents like copper or nickel. Either one could effectively screw the reactivity of your powder, so watch out for impurities.

I've seen lab reagent aluminum that was a bright silver powder, and the stuff from Etch-A-Sketches actually stained my hand bright silver for a time. (It was pretty cool, better than paint. Combustible, too!) Of course, the reagent-grade stuff was likely made by injecting molten aluminum through a very fine droplet outlet into argon gas, so it's probably still ultra-reactive and stuff. Get enough powdered al on you, and it will be so cool you will die of al poisoning... Try a quick soak in vinegar to get it off, maybe add a little peroxide to the mix. That stuff just cleans everything, now that I think about it. Atomized powder is spherical, and by nature can be shiny at lower particle sizes. Atomized powder also sucks. A sphere has the lowest possible surface area of any 3d figure I can think of (please don't say: but x 4 dimensional thing has less) per given mass, and considering the purpose of powder is to be high surface area, atomized is worthless.

 

That NaNO3 is taking forever to dry. Not as long as the MnO2 did, but sodium hydroxide dessication isn't making the thing any less damp. That is the one reason I don't use nano3. The stuff is ridiculously hygroscopic. Leave a bit of it outside here, where the humidity regularly exceeds 70% at 25c, and it will be a puddle within an hour. It should come as no surprise that air drying the stuff here is not physically possible 19 days out of 20. I used to use calcium oxide as a desiccant, but then I burned myself, and started to just heat it. Likewise for AN. Look into making kno3 from bat crap, I used to do that with a little success. Don't expect much though. It would be cheaper just to buy it.

This is completely random, but try putting steel wool in 3% h2o2, and then 30% h2o2. Even in 3%, the reaction is surprisingly vigorous.

[elementcollector1]

This is completely random, but try putting steel wool in 3% h2o2, and then 30% h2o2. Even in 3%, the reaction is surprisingly vigorous.

 

H2O2? What does it do, get catalyzed back into water and oxygen? Or does the wool oxidize?

Just tried the magnesium + drill today, and HOLY SNAP, that's a lot of shavings. I got a container very loosely half-full of these things, and they get bigger the longer you drill. I only drilled in a few spots, too, and the holes produced were very shallow. I might have to try this with aluminum... >

 

Al poisoning? I heard it was a neurotoxin, but not to what extent. Also, the exposure rate of aluminum in our everyday life is massive, from aluminum antiperspirant to aluminum cookware and much more. Admittedly, powder has some risks of its own, but the Wiki throw for 'health concerns' mostly speaks about how nontoxic it appears to be.

 

Should I physically dry the NaNO3? I have it with sodium hydroxide dessicant as we speak, with little action on the dessicant's part except for clumping together.

[chilled_fluorine]

H2O2? What does it do, get catalyzed back into water and oxygen? Or does the wool oxidize? With 3% it bubbles vigorously, making heat and rust. With 30% it bubbles VERY vigorously and catches on fire (if any is still dry).

Just tried the magnesium + drill today, and HOLY SNAP, that's a lot of shavings. I got a container very loosely half-full of these things, and they get bigger the longer you drill. I only drilled in a few spots, too, and the holes produced were very shallow. I might have to try this with aluminum... >Mg is easier to shave, in my experience. Don't expect it to be as easy with al.

 

Al poisoning? I heard it was a neurotoxin, but not to what extent. Also, the exposure rate of aluminum in our everyday life is massive, from aluminum antiperspirant to aluminum cookware and much more. Admittedly, powder has some risks of its own, but the Wiki throw for 'health concerns' mostly speaks about how nontoxic it appears to be. The original actor for the "tin man" in the wizard of oz film almost died after using al powder to color his skin like "tin". He failed his entire career because of it.

 

Should I physically dry the NaNO3? I have it with sodium hydroxide dessicant as we speak, with little action on the dessicant's part except for clumping together. If I recall correctly, there really isn't enough difference in hygroscopicity to make naoh an effective desiccant for nano3. Try a stronger desiccant, like sodium oxide or calcium oxide (both very dangerous). I still have to reccomend heating the stuff. After all, anhydrous sodium nitrate is much cheaper than sodium or calcium oxide. You could make the latter at home, however. This completely random, but have you ever tried to cut a piece of caesium metal? It's ridiculously soft. About as soft as butter, I would say. Any info about the h2o2?

[Phi for All]

The original actor for the "tin man" in the wizard of oz film almost died after using al powder to color his skin like "tin". He failed his entire career because of it.

Really? I heard he became a millionaire and moved to Beverly Hills.

[elementcollector1]

Posted Today, 06:21 PM

 

elementcollector1, on 22 September 2012 - 11:32 AM, said:

 

H2O2? What does it do, get catalyzed back into water and oxygen? Or does the wool oxidize? With 3% it bubbles vigorously, making heat and rust. With 30% it bubbles VERY vigorously and catches on fire (if any is still dry).Oh, I've got to try that. Free chromium oxide if I boil the rust in NaOH, too.

Just tried the magnesium + drill today, and HOLY SNAP, that's a lot of shavings. I got a container very loosely half-full of these things, and they get bigger the longer you drill. I only drilled in a few spots, too, and the holes produced were very shallow. I might have to try this with aluminum... > Mg is easier to shave, in my experience. Don't expect it to be as easy with al.

Darn. Still, the thing was a huge success. Even if the aluminum is harder, it should still work pretty well if it's pure.

 

Al poisoning? I heard it was a neurotoxin, but not to what extent. Also, the exposure rate of aluminum in our everyday life is massive, from aluminum antiperspirant to aluminum cookware and much more. Admittedly, powder has some risks of its own, but the Wiki throw for 'health concerns' mostly speaks about how nontoxic it appears to be. The original actor for the "tin man" in the wizard of oz film almost died after using al powder to color his skin like "tin". He failed his entire career because of it.Well that's certainly... interesting... says nothing about that on the Wiki page.

 

Should I physically dry the NaNO3? I have it with sodium hydroxide dessicant as we speak, with little action on the dessicant's part except for clumping together. If I recall correctly, there really isn't enough difference in hygroscopicity to make naoh an effective desiccant for nano3. Try a stronger desiccant, like sodium oxide or calcium oxide (both very dangerous). I still have to reccomend heating the stuff. After all, anhydrous sodium nitrate is much cheaper than sodium or calcium oxide. You could make the latter at home, however. This completely random, but have you ever tried to cut a piece of caesium metal? It's ridiculously soft. About as soft as butter, I would say. Any info about the h2o2?Or what about heating in a beaker on a stove? Force-drying. Microwave, even. I'm just afraid it might catch on fire...As for the H2O2, not really. I haven't found the time, sorry. Also, the McLendon's site doesn't have a product list or search engine, so the only way to find out if that concentrate even exists is to actually visit the store.

Might I suggest this video, if you have a hotplate: