29 replies to this topic

[fruitfulsteve]

You could work it out, however the easy way would be to just keep adding the carbonate until no more reacts then filter out the excess.

Yep I used those carbon electrodes from the zinc carbon batteries when I was a kid for electroplating. IIRC they were pretty soft and deteriorate pretty quickly.

Thats what i'm doing and every time the bubbles settle i check the PH. I'm boiling some pencils to get the graphite which seems to be working (i have 3 full lengths) i kept breaking them just stripping them with a stanley knife . wikipedia says to use kcl with the electrolite but that would surley give me sr contaminated with k what do you reckon?

[digger]

Thats what i'm doing and every time the bubbles settle i check the PH. I'm boiling some pencils to get the graphite which seems to be working (i have 3 full lengths) i kept breaking them just stripping them with a stanley knife . wikipedia says to use kcl with the electrolite but that would surley give me sr contaminated with k what do you reckon?

I would not bother with the KCL, maybe it is there to improve electron density. Someone with more knowledge of the process may chip in with an answer to that one.

Edited by digger, 08 June 2009 - 07:01 PM.

[Arthur Brown]

Do you really think Wiki is going to suggest an acid!

[digger]

Do you really think Wiki is going to suggest an acid!

?

[fruitfulsteve]

Got it down to PH6 it don't seem to want to absorb any more srco3 (despite heating) so i have it filtering now i'll retest the PH when it's done!!

[a_bab]

Some thoughts from an element collector who's planning to get these metals too:
-electrolysis would work properly for Sr only; Ba is a "difficult" metal to get in pure form (electrolysis will get you something like 85% Ba). The KCl is used to lower the melting point; the Sr won't be *very* contaminated anyway. After all, in industry they make many steps for purification. Good luck getting constant 900 degrees C or so necessary for the electrolysis of the melted salt(s), while not even able to secure a graphite anode and getting mad at those pesky pencils (iron wold work better; the graphite in pencils contains clay, oil and other things and this will dissintegrate them instantly such high temps if not "cooked").

There are many old copyright - free books that are describing what you're after; I recommend you "A dictionary of applied chemistry /by Sir Edward Thorpe". In it, you'll get detailed instructions of how to get these metals.

-the best, clean, easiest method is aluminothermic reduction. As a pyro you should already have different Al meshes, or better yet some Mg powder. The reaction should be carried in a closed system, prefferably in an iron pipe, closed at both ends. Put the theoretical amounts + a bit of extra salt in the system (think a "pipe bmb") and drop it in a fire. BTW, the metal should be in a corse form. The pressures could reach as much as 100 atm; this is a VERY dangerous thing to do, but you'll certainly get your metals in fairly pure form (99% or so).

What I'd say: grow up a bit; understand some more chemistry and the risks involved, and don't go for too big things, for now. There are lots of things you need to learn; wiki is just not enough. Before atempting something as dangerous as electrolysis of a molten salt, learn what a splash of molten salt can do to your eyes (it happends all the time during the electrolyses of molten salts). No offence, but you can't do a simple neutralisation reaction without being spoon-fed on the board and you want to get the most reactive alkaly-earth metals in such a pure form that they are not 'contaminated with Na" without knowing what that actually means practically speaking.

Ebay is a good source for what you are looking for. Maybe not lately, as I had noticed with reactive metals. There are others elements collectors too (some hundreds in the whole world I'd guess), and usually they are more then willing to trade.

[digger]

-the best, clean, easiest method is aluminothermic reduction. As a pyro you should already have different Al meshes, or better yet some Mg powder. The reaction should be carried in a closed system, prefferably in an iron pipe, closed at both ends. Put the theoretical amounts + a bit of extra salt in the system (think a "pipe bmb") and drop it in a fire. BTW, the metal should be in a corse form. The pressures could reach as much as 100 atm; this is a VERY dangerous thing to do, but you'll certainly get your metals in fairly pure form (99% or so).

Interesting reply

I assume you mean by using the oxides of the elements in question.

Yep that is certainly one dangerous experiment that would require quite some knowledge of design of pressure vessels at high temperatures allowing for the reduction in material strength. High temperature low creep alloys such as inconel would be required or a vessel with an extremely thick wall. Obviously a small bore would work in your favor to reduce the hoop stress.

I would also imagine during the reaction localised temperatures could spike upto 2000K.

If I were designing it I would clearly use a PRV to limit the internal pressure to a couple of bar, with a vacuum breaker to purge with an inert gas upon cooling.

However not really an amateur experiment I would say (I know that is what you were saying).

[fruitfulsteve]

Wow i wish you had posted all that info at about 6pm at about 7pm my pencil graphite 'electrodes' exploded in my very hot but not molten srcl . I think the kcl would have also worked in some way as a ph buffer (low sodium salt is no good, presumably because of the anti caking agent reacting with the hcl) i've given up on that now, so i'm just going to buy a little ampuole. pm me if you want the details of the supplier i beleive he ship,s abroard!! I have most of the alkaline metals I just thought it would give me a bit more satisfaction to actually 'make' a few, at least i tried !!

[a_bab]

The reduction would work with the chlorides too. I was thinking more about the chlorides then oxides.

Just think: the gypsum "flash" (plaster of paris + Al powder, set hard and ignited) would actually render Ca metal; because it's done in the air, the Ca just burns as it is formed.

[Arthur Brown]

Learning about molten active metal by trial and error is not to be recommended! DIY pressure reaction vessels are even more hazardous - one miscalculation and it's just a pipeb0mb and horrendously dangerous and incriminating, and brings the forum into disrepute.

[digger]

The reduction would work with the chlorides too. I was thinking more about the chlorides then oxides.

Just think: the gypsum "flash" (plaster of paris + Al powder, set hard and ignited) would actually render Ca metal; because it's done in the air, the Ca just burns as it is formed.

I am sure it would. I was just thinking of the aluminium chloride formed not the nicest of stuff. Quite a strong lewis acid if I remember my A-level chemistry properly.

DIY pressure reaction vessels are even more hazardous - one miscalculation and it's just a pipeb0mb and horrendously dangerous and incriminating, and brings the forum into disrepute.

Pretty much what I said

Edited by digger, 10 June 2009 - 06:48 AM.

[a_bab]

Well, the actual topic was totally off the track of this forum's subject. An admin should have closed it in the first place; these kids tend to blow themselves up. There are other forums willing to discuss such, why not, interesting subjects.

An accident can happen at any time; even a most ridiculous one like a barium poisoning while making that nice Bleser's strobe. But trying to get a reactive metal in molten state while not even being able to spell properly (not to be misunderstood, but it clearly shows ignorance and lack of knowledge) is kind of suicidal.

[fruitfulsteve]

Well, the actual topic was totally off the track of this forum's subject. An admin should have closed it in the first place; these kids tend to blow themselves up. There are other forums willing to discuss such, why not, interesting subjects.

An accident can happen at any time; even a most ridiculous one like a barium poisoning while making that nice Bleser's strobe. But trying to get a reactive metal in molten state while not even being able to spell properly (not to be misunderstood, but it clearly shows ignorance and lack of knowledge) is kind of suicidal.

Firstly thanks for your first post on this subject it was very helpful and i have noted it's content, you clearly know what your talking about. However if you go on to patronise people and make assumptions about people who just want to learn that's not so helpful !!The spell check did point out my mistake, i just thought it would be more ammusing to leave it. I did mention at the biginning that it did not have anything to do with pyro yet it still had nearly 30 posts and only one person winged about it being of topic!! I may not be a professer of chemistry but i'm not an idiot and i did take precautions (blast shield,fullface visor and welding gloves) Ok it didn't work but at least i tried.
Also if you consider 42 a kid you must be well old!!!

[a_bab]

You are a kid in chemistry pyro etc. But we all grow up.

The age is not relevant at all, and I personally really find odd that an "old" person like you is keen to such things, but that's OK too (I'm close to your declared age).

So if you feel offended by my patroniZing attitude, it's because I have seen too many missing limbs, and I'm an old grouchy fart.

PS The spelling mistake was amusing indeed, and I knew it was on purpose. But I'm a grammar nazzi too

[fruitfulsteve]

You are a kid in chemistry pyro etc. But we all grow up.

The age is not relevant at all, and I personally really find odd that an "old" person like you is keen to such things, but that's OK too (I'm close to your declared age).

So if you feel offended by my patroniZing attitude, it's because I have seen too many missing limbs, and I'm an old grouchy fart.

PS The spelling mistake was amusing indeed, and I knew it was on purpose. But I'm a grammar nazzi too

I don't want to grow up too quickly.
Even funnier i'm going to be taking a entry level course soon and then hopefully starting a 2year OU then 2 years full time course for a degree in chemistry, so i do need to learn a lot of stuff pretty quick!!
Your patroniZing didn't offend me, I was more shocked that someone with your level of intelligence would make assumptions and or patronise!!
Prehaps if you put a bit more thought into how you put your obvious knowledge across more people would take note and you'd not have so many limbless associates
I see their about to name element 112 (anything to do with you?) if so i think you should call it FRUITFULIUM