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Author: Subject: KCLO3 by way of H2O + KCL
Xenoid
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[*] posted on 11-4-2008 at 20:52


Incidently - I'm not sure if I've mentioned this before, but a good way of mounting gouging rods in thin metal or plastic lids is to use rubber grommets. I used these on a lot of my early cells, before using the screw together cable glands. They last quite well, seal well (with a little silicone grease) and support the rod as well as electrically insulating it from a metal lid.

They come in a range of sizes (make sure they are a really tight, stretchy fit on the rod. The hole in the lid should be about 2mm larger than the diameter of the rod. Fit them in the hole first and then force the rod through with a little silicone grease.

They are available from electronic parts suppliers, automotive shops and engineering suppliers. They are normally used where electrical wires are passed through thin sheet metal, to protect the wires from cutting on the edge of the hole.

Grommets.jpg - 9kB
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Sciocrat
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[*] posted on 12-4-2008 at 14:03


Tnx for your fast replies. You were right, there was a short circuit. The lid is made of metal, and it wasn't properly insulated from the screws that connect to the cathode. I applied some electrical rubber tape on the part of the screw that was in contact with the lid, and now it works just fine. The cells have been working for 4 hours and so far, everything is fine. I hope it will remain that way untill the reaction is finished :)
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Pulverulescent
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[*] posted on 13-4-2008 at 12:24


Sciocrat, metal lids and spacers will corrode fairly quickly under operating conditions.
This corrosion will badly contaminate your electrolyte, making isolation of the product (NaCl03) very difficult.

If you replace them with plastic or rubber components electrolysis will proceed smoothly apart from some disintgration of graphite anodes.
NaCl is the preferred salt for chlorate production; potassium chlorate is obtained by metathesis.

If you use KCl, chlorate will precipitate after some hours of electrolysis once the solution cools; KCl03 is far less soluble than NaCl03 but the sodium salt works slightly better and causes less damage to carbon anodes.

The downside is---you'll have to wait longer for NaCl03 to precipitate, because of NaCl03's high solubility.

P
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dann2
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[*] posted on 13-4-2008 at 15:07


Hello,

A big down side to K salt when using Graphite anodes is that the Graphite sludge is difficult to remove from K salt. You usually end up filtering hot solutions to keep K Chlorate in solution. Use Na and you can filter cold. Using DSA, MnO2 this is not a problem as you can take solid K Chlorate and use directly as no cleaning up necessary.
Perhaps it is OK to use black K Chlorate (Graphite contamination) in Pyro stuff anyways?

Dann2
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12AX7
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[*] posted on 13-4-2008 at 19:30


Quote:
Originally posted by Pulverulescent
NaCl03


Subtle error: it's not spelled with a zero.

Tim




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Pulverulescent
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[*] posted on 14-4-2008 at 02:53


What difference does it make? It's still a cyclo-form!

P
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Aqua_Fortis_100%
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[*] posted on 15-4-2008 at 17:13


Hello guys,

Dried my chlorate today... The results were much worse I'd imagined.. Probably the water content of the crude product blinded me :(

After two recrystalisations and drying, the weight was around 360g which is a crap yield (about 25%.. Considering the chlorate dissolved in all liquors it would rise only to about 35-36%, at best), this liquor using Na2Cr2O7 :mad:

Why people claim that 50% efficience is easy to get? I dont remember seeing a person that reached that with gouging rod and no controled pH setup.
Even Tim website states crap yield for Na/K chlorate..

Well.. Anyway I'm happy, since is my first chlorate bath..

Hope better yields in next batches..

Pyrotechnics world, I'm here!!!!

[Edited on 15-4-2008 by Aqua_Fortis_100%]




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12AX7
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[*] posted on 15-4-2008 at 20:32


How large a cathode did you use?



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Aqua_Fortis_100%
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[*] posted on 16-4-2008 at 05:48


Very small infact...

I've used 7 small Ni rods, since was the only good material I'd at the time...
Now I see that was a great mistake (anodes around cathodes!) and IMHO certainly this was the most relevant thing to my anodes anodes premature death :( Uneven distribution of current on surface of graphite rods..

Next time I will use better things as cathode..

thanks




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Sciocrat
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[*] posted on 10-5-2008 at 04:43


One question - On a few sites I noticed that scientists/engineers(?) named Foerster and Mueller described the conversion of chloride to chlorate by eletrolysis, but I can't find any more useful information about them. I would be thankful if someone mentioned something related to them, or recommended sites where the info could be found. I'm writing a paper about potassium chlorate synthesis, and have been told to provide more info about these individuals...

Tnx in advance...
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phlogiston
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[*] posted on 10-5-2008 at 06:38
Foerster and Mueller


They published their observations in the first decades of the last century, say 1900-1930.

Use google. For instance, using 'Foerster Mueller chlorate' as the search string, this yields some relevant literature, for instance this link:

http://www.rsc.org/publishing/journals/article.asp?doi=ca900...

Click on 'pdf' to get the free full-text article, which contains a bit of literature, from the year 1900, by Foerster and Muller themselves about chlorate formation.

The very first hit using Google is:

Landolt D et al, Anodic chlorate formation on platinized titanium, J. Applied Electrochem (1971) 2:201-210

which is more recent and elaborates quite a bit about certain details/hypothesis of Foerster and Muller.

Other relevant references:

Z. Elektrochemie (1903) 9:195
Z. Elektrochemie (1902) 8:515

However, you will need access to a pretty good university library to access them due to their age, and (as a lot of chemistry literature from that era), they are written in German.




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dann2
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[*] posted on 19-6-2008 at 10:59


Hello,

Has anyone here ever purchased one of these (or one like it) for making (Per)Chlorate.

http://www.pyrosecrets.com/chloratecellplans.html

Do they make the Perchlorate my heating the Chlorate?
What's the story with the DSA Anode instructions?

Perhaps I could try the references section...........:P

Dann2
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Armistice19
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[*] posted on 7-5-2009 at 12:27


Don't waste your time with that stuff, there is plenty of information in this forum, all over the internet, and at your local library about preparation of chlorate and perchlorate. Just do some hearty reading and make sure to double check all your sources.



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Xenoid
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[*] posted on 7-5-2009 at 12:48


Quote: Originally posted by Armistice19  
Don't waste your time with that stuff, there is plenty of information in this forum, all over the internet, and at your local library about preparation of chlorate and perchlorate. Just do some hearty reading and make sure to double check all your sources.


LOL... Good one, Armistice19. Are you aware that Dann2 is responsible for most of the infomation on amateur chlorate and perchlorate production both on this forum and also the internet..... :)
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Formatik
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[*] posted on 7-5-2009 at 12:58


Speaking of which, Geocities is killing all of their webpages later this year: http://help.yahoo.com/l/us/yahoo/geocities/geocities-05.html So enjoy dann2's website while you can.
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[*] posted on 10-5-2009 at 18:03


Quote: Originally posted by Formatik  
Speaking of which, Geocities is killing all of their webpages later this year: http://help.yahoo.com/l/us/yahoo/geocities/geocities-05.html So enjoy dann2's website while you can.


Yes indeed the peep show is coming to a close.
Ladies and Gentlemen, time please, time please, order you last drinks and get you final peeps and finish up............

I would not mind getting a peep at those 'instructions' for Chlorate and Perchlorate making.
@Armistice19 Did you actually get your eyeballs onto the instructions or are you assuming they are just a repeat of alot of the stuff that is already known?
Cheers,
Dann2
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uchiacon
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[*] posted on 3-7-2009 at 21:32


Hey guys, I'm just here because roguesci is no longer operational(removed by the US dept of defense :mad: ), and there was this great thread on chlorate production which had loads of details. Now its lost to the net I must relocate to a alternative thread.

Ok, so I think I'm going to be making mainly chlorate(I dont see myself making proper fireworks anytime soon using perchlorate, but it'd be nice to have)
and I have two options.
Platium plated niobium mesh(Pt coating of 2.54microns thick and $5USD per square inch). Suitable for perchlorate, but if misused will lose Pt coating, and Pt has a high resistance to current.
OR
MMO coated Titanium anodes. Cheaper than Pt but unable to be used for perchlorate and has less resistance to current than Pt. Heres all the details www.anometproducts.com//App_Themes/anometproducts/PtCladNb_M...

So what do you guys think? Which one would be better for a person slightly less experienced in chlorate production?
Cheers
Oh, and if anyone has the pyrosecrets instruction manual on the chlorate production I'd love to download it!

[Edited on 04-07-09 by uchiacon]

[Edited on 04-07-09 by uchiacon]
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hissingnoise
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[*] posted on 4-7-2009 at 06:51


Quote: Originally posted by uchiacon  
Hey guys, I'm just here because roguesci is no longer operational(removed by the US dept of defense :mad: ),

The DoD?---Yeah, right!
Mega's probably sorting out RS's problem right now and the site'll be back anytime now. . .
Everything anyone needs to know about chlorates and perchlorates is contained in threads like this one---all you have to do is read a few posts!
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[*] posted on 4-7-2009 at 08:49


Quote: Originally posted by uchiacon  
Hey guys, I'm just here because roguesci is no longer operational(removed by the US dept of defense), and there was this great thread on chlorate production which had loads of details. Now its lost to the net I must relocate to a alternative thread.
Have you actually heard from Megalomania personally? What is his email address now? Did he tell you that the U$ DOD removed roguesci.org, and WHY did they do it? Does he have an up-to-date backup of it, and does he plan to move it to a hosting server outside the U$A?
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uchiacon
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[*] posted on 4-7-2009 at 15:12


Well guys, the fact remains the roguesci is down, and Idefense(a US internet censorship agency working for US DoD) has closed them down before. If you google "what happened to roguesci" you should come across the email sent to users in 2004 when it last went down.

Anyway, can I get some opinions here about what I should buy?
Pt plated niobium mesh or MMO mesh? Details are in my post further up.

And no, the information I need is regarding Pt mesh and MMO mesh for use as anodes, how indestructable they are, what is the max current and voltage they can take and what levels does chloride have to get down to before they start to erode.

[Edited on 04-07-09 by uchiacon]
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hissingnoise
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[*] posted on 5-7-2009 at 04:08


I'd go for lead dioxide anodes if I wanted perchlorates and graphite gouging rods for chlorates, but I found long ago that not all gouging rods are equal. . .
Producing perfect LDAs is by all accounts an art but they're now used commercially for perchlorates.
They can go from chloide to perchlorate in one go and this makes them convenient.
As for RS, a suspension implies reinstatement at some point, so I expect to see the site back sometime. . .not that I had a great interest in it at any time.
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uchiacon
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[*] posted on 6-7-2009 at 00:13


Choices are for Pt anode
www.anometproducts.com//App_Themes/anometproducts/PtCladNb_M... @ $5USD a square inch.
Or
MMO pool chlorinator - www.directpoolsupplies.com.au/prod733.htm

So I might be making a small amount of perchlorate in the futute, it'd be nice to have that option open. But is Pt still as good as MMO in a chlorate cell?
I'm still unsure on this, can somebody just point me in the right direction?(scroll up for original post.)

Cheers
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[*] posted on 7-7-2009 at 19:00


Oh, yeah and I was just wondering if I have the process running correctly... should the electrolyte be black with graphite? I switched from art pencils(pretty shit at conducting the current, and they blister quickly) to hard graphite electrodes from a 6v battery. So the electrolyte had a faint yellowish tinge to it from the day or so that the art pencil was in. Want a better anode guys, give me some opinions!

And the second picture is after about 2-3 days on 5v, 30a current. Very, very racially sensitive.
Considering all that though, at the amount of graphite in the water would you suspect that perchlorate is starting to be made? There is so much of it, and I have no way to test if chloride levels are low lol, and I haven't bought my KCl yet. Which I will have soon.

[Edited on 04-07-09 by uchiacon]

[Edited on 04-07-09 by uchiacon]
For some reason cant post pictures...just imagine a very very well tanned picture of a very dark electrolyte. Graphite dark.

[Edited on 04-07-09 by uchiacon]
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[*] posted on 8-7-2009 at 04:06


Graphite never makes perchlorate. Graphite should come off, but not as much as you are evidently seeing. Try 5A on that anode.

Tim




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hissingnoise
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[*] posted on 8-7-2009 at 06:11


Tim, using chloride-free NaClO3, graphite *will* make perchlorate, but anodic erosion will be runaway and the rate of perchlorate production will be tiny. . .
And using compressed carbon sticks from batteries seems a waste of time, since they're usually made from compressed amorphous carbon.
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