making potassium (per) chlorate

[Mumbles]

I can in no way promote the use of HF for anything, much less it's preparation. HF is sold commercially as tarn-x or something like that. It comes in a gold bottle. Should be pretty easy to look up if you want. Reaction of this with NaOH is probably the best bet. I'd be too worried about getting too much HF in the air and poisoning someone(me) if were to prepare it.

[tentacles]

Then it's fortunate I picked up a kilo of NaF today.. also a k of CaF. Grabbed some 200 mesh silica also, and 2kg soda ash (sodium carbonate).

[TheSidewinder]

Just FYI, Tarn-X contains (according to its label that I just read)...

 

thiourea and sulforric acid.

 

And, oddly, although it warns you about not getting it on your skin or in your eyes, it says NOTHING about using it in a ventilated area.

 

Hmmm... I know it smells like shit when you use it. Smells like hydrogen sulfide to me, but I'm not sure.

 

I have no idea what the chemical structure of either of those are.

 

Mumbles??

 

M

[Mumbles]

Thiourea is S=C-(NH2)2

http://www.inchem.org/documents/cicads/cicads/v49ci02.gif

 

I know this is bad for skin contact for sure. I can't remember what it does, but it's not good.

 

I assume you mean sulfamic acid, not sulforric. It's a pretty common cleaning product.

 

It's a condensation product between NH3 and SO3

http://content.answers.com/main/content/wp/en-commons/thumb/5/59/150px-Sulfamic-acid-zwitterion.png

 

 

 

 

 

Anyway, I had the product wrong, but the bottle right. It's Whink rust remover which is HF

http://www.whink.com/images/rr_label.jpg

Around 4% IIRC

[tentacles]

mumbles: that's good to know, a combination of HF and nitric is used to desmut cast aluminum prior to anodizing, next time I feel like prettying up my hotplate I will try it.

[TheSidewinder]

(I'm looking at the bottle at the moment.)

 

No, it says sulforric acid.

 

At least, that's how they spelled it on the English side of the label.

 

But I bet that's a bad misprint, because the Spanish side of the label says that it's:

 

acido sulfamico (with a forward-pointing accent mark over both A's)

 

Sounds like Sulfamic to me. Wonder why the English side is saying Sulforric?

 

M

[Mumbles]

Yeah, it seems to be a misprint on the spanish version of the product. It's the only reference to sulforric acid I can find besides a bad scan job where "Sulfonic" was read as sulforric by the program. Probably the same for the product you have, the a and m coming over as o and rr.

 

Sulfonic acids exist, but not in this context.

[jacob]

I've made some KCLO3 i want to convert to KCLO4 by bakeing it, but first i want to know if mixing it with sugar, droping some sulfuric acid on it and seeing if it ignites is a thorough test for residual chlorate? if not what is? and one more question, to convert hypochlorite back to chloride i just dissolve the chlorate into boiling water and boil it for a few minutes right? i'm so excited to be makeing this stuff myself .

[Mumbles]

The test with sugar isn't sensitive enough. It will probably only be sensitive down to around 5% chlorate. If your produce doesn't light with acid, it doesn't mean it's acceptably chlorate free. Chemical methods are the only real ways to check appropriately via colors and precipitates. By using heat decomposition you will never get appropriately pure perchlorate for anything containing ammonium perchlorate, or sulfur or things like that.

 

As far as the hypochlorite, that is correct. However, it produces 2:1 chloride:chlorate so isn't appropriate for removal of hypochlorite from perchlorates.

[jacob]

By using heat decomposition you will never get appropriately pure perchlorate for anything containing ammonium perchlorate, or sulfur or things like that.

Couldn't i disolve the perchlorate in boiling water and and then persipitate (spelling?) it back out, chlorate free?

 

However, it produces 2:1 chloride:chlorate so isn't appropriate for removal of hypochlorite from perchlorates.

Do you mean one hypochlorite converts to two chloride, i'm confused.

[WarezWally]

no, the chlorate will also precipitate out. You would have to dissolve everything then destroy the chlorate properly

[hashashan]

the sugar test wont show you chlorate for up to 20%.

I used the phosphoric acid + MnSO4 reagent.

its quite easy to use

That and more tests are here :

 

http://www.geocities.com/CapeCanaveral/Cam...rate/tests.html

 

@tentacles :

I would never use any fluroride anywhere ... I also wanted to use it but then i heard some information about fluoride poisoning and decided to never come across with mister F.

 

Congrats on the Ti, going my way ah?

 

@wally, you can plate over the Ti, there will be an oxide, but because the currents are low and were not stressing the anode then it will grow.

[Mumbles]

Hypochlorite decomposes like the following:

 

3 ClO- ---> 2Cl- + ClO3-

 

Thus, hypochlorite will produce a 2:1 ratio of chloride to chlorate. I was originally thinking you were trying to convert the hypochlorite in perchlorate. In chlorates, the chlorate would obviously pose no problem.

[jacob]

Ok, thanks guys, i think i understand it now. would i be able to first thermally decompose my Potassium Chlorate to Perchlorate, and then destroy any residual Chlorate with HCl, or would there be too much Chlorate left in the Perchlorate to do that? it seems like the easiest way to go.

[Mumbles]

I had thought about using an acidified sugar soln to "wash" the perc perhaps. Not sure how it'd work. It's hard to give definitive answers with no experience. If you have any perc and chlorate laying around a contaminated product of known concentration could be prepared and tested. Some sort of qualitative test would have to be used though. The manganese one above is probably the easiest.

 

Side note, but I've been considering getting some of the expensive dyes and reagents used to test for chlorates, and selling them at the PGI and such. I'd have to buy Eric H a beer though for stirring up the controversy.

[WarezWally]

They are not that expensive if you look around, there is a seller on ebay who sells most of them cheaply.

 

methylene blue can be purchased at pet stores for fish

[Mumbles]

shhhhhhhhh, the price is the secret to my plan

 

I was actually looking into chlorate tests, not perchlorate tests. Methylene blue tests for perchlorate, not chlorate. Indigo Caramine and the manganese-phosphoric acid were the ones I was going to look into. Maybe sell Ag/Pb nitrates for chloride testing. There are some good ones for nitrates.

 

And thus my empire of pyro chemical purity testing products has begun :evil laugh: In all seriousness there are a lot of people concerned about purity, who don't have the knowledge to test them. Perhaps testing in house from samples would be better. Anyone have an extra UV-Vis spectrophotometer they want to send my way?

[WarezWally]

With chlorates and perchlorates your home made product will most likely be much better than they stuff you buy. There is a interesting PDF on pyrobin.

 

Chinese and domestic is fucking horrible, lots of added crap and metal filings. They recovered a large amount of unknown anticake and the domestic turned brown when water was added. The best was the Taiwanese which had no anti cake.

 

Ive got a small amount and its horrible to work with as it turns to hard lumps but its much more 'pure' than the Chinese and domestic shit.

 

As long as you kill of the nasty stuff (hyperchlorite and anything else you add) your set. A small amount of NaCl or KCl wont hurt, and hey it will still perform much better than the stuff you buy.

[hashashan]

jacob : thermal decomposition of chlorate in order to produce perchlorate is a risky operation.

 

you know molten explosive is not a good idea, besides you do understand what will happen if some organics will get into the molten salt?

 

usually it is done in small quantities.

 

besides suppose that you dont kill yourself doing that, the operation itself isnt simple. There is much foaming and the perhlorte may decompose into chloride and oxygen if the temperatures are too high. You will need to babysit the molten salt in order to make perchlorate.

 

If you can buy pure chlorate I would recomend buying a Pt wire to convert it into perch.

[WarezWally]

Ditto, melt a small amount of chlorate in a test tube and drop a sugar cube into it. The amount of energy released is quite disturbing for such a small amount.

 

 

You are royally fucked if something goes tits up.

 

My MMO anode should be here soon, anyone here used one before? This anode is has been designed to make chlorates and its the same one used in industry (according to the pdf this place send me some people make many many tons of chlorate a year)

 

Only thing I don't know is the currant density and I doubt I will get a email back till next year.

 

EDIT: Just looking around it seems I can run it at 600 A/m2 in sea water (saturated NaCl is pretty close). The anode has a surface area of 48cm2 so according to my calculations I can run this bad boy at close to 30A and according to the site it should be able to do this for 20 years.

 

 

sweet

[tentacles]

wally: How much was the anode, and is it suitable to run to low chloride levels? Whatever happened to the LDA group buy? No go?

 

I'm looking into a piece of tantalum to plate with LD; the preparation for plating is very simple compared to Ti. I tried hashashan's method of plating LD next to Ti, and the result was unsatisfactory; part of my problem was probably plating at too high of a current, like 12ma/cm2 from the start.

[Mumbles]

I'm well acquainted with Eric's PDF. I still don't fully buy it however. I have a few tests of my own to do.

 

It should be noted that metal filings, and metal oxides would make the product burn more vigourously. There is some speculation that the Sweedish stuff had a measurable amount of chlorate in it, which made it so reactive. Purer is not always better for all applications.

[WarezWally]

Apparently lead dioxide is a restriced export from India, go figure

I got my anode from this guy, http://stores.ebay.com/JJFLASH-PYRO-LAB-COMPUTER-SUPPLY

Sells half decent platinum plated stuff as well

 

Mumbles: You don't see a problem with having chlorate in perchlorate?

[Mumbles]

Oh no, I do for most applications I use perchlorate in. Just stating that contamination isn't always detrimental to effect.

 

This is beside the fact that I think chlorate has an unfair stigma to it. It is made out to be much worse than it truely is.

[jacob]

hashashan, i suppose you have a point, i can just see a leaf or something geting into the molten chlorate and ruining everything, i guess it's not as easy as just throwing some chlorate in a toaster oven and bakeing away, oh well, i'll use the chlorate for something, i'd like to find out just how sensitive mixtures made with it are.