387 replies to this topic

[sasman]

lord_dranack Did you manage to make some Perchlorate?,Im tempted to try the thermal decomposition route i have a kiln and can control the temperture ,its just the thought of the low yield as you get lots of KCl as a by product ..I have Got 2 platinum Electodes waiting to be used .

They are Platinium Coated Titanium Mesh the largest is 6.5cm wide By 11.5 cm long they are about 2 mm thick the mesh holes are Diamond in shape about 5 mm By 9mm So its hard to Calculate the surface Area .. But im estimating 80 Cm2

,I''m waiting for some bearings from the USA to make a better ball mill so can't experiment with any pyro until i build my new mill, so i think ill start trying to Make some Perc.. while i have nothing to do..Hope you can give me some Tips..

Cheers

Edited by sasman, 15 March 2005 - 05:41 PM.

[lord_dranack]

I never got round to attempting it! I moved on to simpler projects, but it's still there at the back of my mind on my to do list, if I get any time.

Let us know how you get on...

[sasman]

Er this may sound a stupid question.. But what Do i connect my Pt Anode too??? is it the Positive + Terminal?..

I have just turned on my cell and there is lots of bubbling at my Stainless Steel Cathode which is connected to the Negative - Terminal. Now i thought the anode was the Positive, But i just read that it can also be the Negative in certain types of Cell ....Hope some one can help??

I have read all the pages on http://www.wfvisser....nl/indexEN.html and http://www.geocities...e/chlorate.html and cant find any answer as to what is positive or negative?

Thanks

Edited by sasman, 15 March 2005 - 05:43 PM.

[Stuart]

The positive terminal. The Anode needs to be charged positively

[The_Djinn]

Purely out of curiosity,
Are you trying to make perc because you haven?t found a supplier or are you doing it for the challenge ?

Mark

[sasman]

Purely Because i havent Found a supplier at a realistic price! Some things are nice to make but making perc is being done because i cant get it any otherway..

,Im only doing a small experimental cell to see if it works before i make the bigger cell.its bubbling along nicely lots of bubbles from the stainless steel cathode but not many bubbles from the Pt anode thats why i was concerned about the polarity..cant smell much chlorine either?

Edited by sasman, 24 March 2005 - 06:55 PM.

[Stuart]

Well if you can smell some, then it is probably working. Are you adding a small amount of Sodium Hydroxide or similar alkaline to regulate the pH as the Chlorine may be disproportionating in the water.

[sasman]

Just letting you know I ran the Cell for about 2 days i was passing 15 amps through the cell.

.The cell was only 1 litre 500 grams Chlorate Stainless steel Cathode Pt/Ti Mesh Anode Power Was from 300 watt Pc power Supply..I kept the cell temp about 50 C Ph was about 8.5 Altho i was using my old electronic Ph meter which i havent used since i was 20!! thats was 20 years Ago! So i asume it was an acurate reading..

...I Filtered the Hot electrolyte to remove any solids then added Super Saturated solution of Potassium Nitrate To precipitate the Perchlorate out of the solution..I filtered the White precipitate whashed it a few times Then dissolved - recrystalized it a few times..And thats about it I have No Chemicals to do the test to confirm Perc has formed no way of destroying the residual ClO3 ..Sods law has stepped in and My Local Lab supplier Has gone Bust .


.So I have to find another supplier for the other chemicals i need ,I have found 1 lab supplier but they do 100 pound Min order ...EEEKKK. Wouter mentions That you can identify ClO3 from CLO4 from crystal shapes so i started looking for My microscope... Sods law Again!! ..

I Just moved into a new House On thursday so every thing is Boxed Up ...So i will have to wait a day or so until the boxes get unpacked...But i cant stop thinking about My Luverly Perc so i thought stuff it and went out and bought another Microscope!..
Ok started looking at all those crystals and what do i see ? lots of little crystals,but no they dont look Monoclinic(Chlorate) and there not rhombic(Perchlorate) so god knows what i got AAARRRGGHHHH.....I'll just have to wait until i get some Chems to do proper tests....


To be continued....

[Stuart]

http://www.geocities...rate/tests.html

http://www.geocities...te/destroy.html

You can test for Perchlorate's using Potassium Chloride (unless is was Potassium Perchlorate you were making,top link)

You can destroy Chlorate's using Ferrous Sulphate which is used as a fertiliser (easy to get, bottom link)

If it is Potassium Perchlorate you have made, then check for Chlorate's and destroy them. Then make a mix of sugar and make sure that it burns. If it does, then you probably have Potassium Perchlorate. You could also find out how much Potassium Perchlorate will dissolve in a certain amount of water at a certain temperature and see if you can dissolve it all.

Edited by Stuart, 26 June 2004 - 01:47 PM.

[The_Djinn]

Okay guy?s

Something to eliminate the headache of synthesising KCIO4 and a whole lot easier...

For further info, see the BPS members area under the KCIO4 link.

Mark

Edited by The_Djinn, 30 June 2004 - 06:27 PM.

[burningbush]

The positive terminal. The Anode needs to be charged positively

anode = /line in + pos

cathode = /neutral /can also be ground - neg

allways in any language.

Peace
Pc.

Edited by burningbush, 26 November 2004 - 05:49 PM.

[broadsword]

So where does everyone else get thier Potassium Perchlorate from?

[mnementh]

Hi guys,
had a quick google search and found this;

http://www.logicsout...stuff/kclo4.txt

Don't know if it's been posted before, or tried out. Any comments on the procedure, welcome,

Sandy

[burningbush]

Hi guys,
had a quick google search and found this;

http://www.logicsout...stuff/kclo4.txt

Don't know if it's been posted before, or tried out. Any comments on the procedure, welcome,

Sandy

I ran across this too and was tempted to try it,
I read in a nother post by big g that you want to use a leaddioxide and platnium for the cell rod and cathode . from my limited chemistry knowledge , I think it would work , and even be productive if you could controll your variables "ie. temp /ph/amps and volts through cell, also filtering carbon out from rod decay and chlorates elimination are issues too.
I read some where that carbon rods can be saturated in linseed oil to slow erosion in perchlorate/chlorate cells but I need to try that to see if true or false.
Whats really stopped me at this point isnt lack of equiptment and know how, It's not having a properly vented work space, This IS VITAL! If you want to experiment w/making chlorate cells.
Ohh also use a flamable location exhaust fan so you dont shoot any hell fire out the vent in your workshop from hydrogen gas off cell's.

If you can ,Buy your perchlorate/chlorates .
Its alot more fun spending time making things that go bump"or flash "in the night ,then checking your java script:emoticon('')poision/flamable gas producing cells every hour for 3-5 days. or thats just me.java script:emoticon('')

[burningbush]

So where does everyone else get thier Potassium Perchlorate from?

Discount pyro usa "Best price Best service"
Firefox second choice usa "lots of items "
I have ordered from both and others many times
The others"not listed" had problems that could not be from any thing else then stupidity and lack of respect .
If you dont respect your"QUALITY" customers then your already going out of business! java script:emoticon('')
Sorry, dont know any UK or canada suppliers.

Pc.