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Author: Subject: KCLO3 by way of H2O + KCL
12AX7
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[*] posted on 7-11-2007 at 23:09


It's probably too resistive.

I don't know that there's any advantage to titanium, it just sounds cooler. :)

On the other hand, something like that could be very awesome for, like, filtering molten aluminum metal.

Tim




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[*] posted on 10-11-2007 at 05:55
Chlorate using divided cell?


I was cruising the information superhighway looking for information on Li perchlorate (as one does) when I came across this procedure in Google Books for making Na chlorate. The procedure seems to contradict just about everything I've learnt about chlorate making over the years. The book is entitled:

The Preparatory Manual of Black Powder and Pyrotechnics By Jared Ledgard

and it can be found here:

http://www.google.co.nz/books?id=370UwG8CuNwC&pg=PA113&a...

The procedure can be found on pages 105-106 (note you need to read all of column 1 over the two pages, then column 2 otherwise it makes even less sense.

The method is based on a divided cell concept and the author seems happy to use just about anything for an anode. The porous membrane (a plant pot) is first "charged" - made conductive using magnesium sulphate electrolyte. It is then used in a divided cell to make chlorate. I can see that the anode compartment would be kept at a low pH and chlorate would be formed by diffusion through the plant pot. But what's the point of this method, what about anode erosion, the author does not even discuss it.

Regards, Xenoid

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[*] posted on 10-11-2007 at 12:47


Hello,

Reading the opening lines it says, Sodium Chlorate is widely used in pyrotechnics also used to make Ammonium Chlorate and Perchlorate which are used in powerful solid rocket propellents.... Does not sound too good.


The battery charger only works when plugged in...

The entry on Lead Dioxide has been snipped :(

Have not seen anything like it before.

Dann2
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[*] posted on 10-11-2007 at 13:00


I had one of his other books and throughout his methods are questionable. Two items from memory, a solvay type synthesis with potassium salts, making silver perchlorate from boiling bleach with silver nitrate. I purchased one book on ebay and emailed him asking him if he had success with any of the synthesises and he stated tey ALL worked but never elaborated. He list a Bachelors degree as one credential but I hardly believe it.



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[*] posted on 10-11-2007 at 13:01


It would appear, the author never attempted this method. Else, he made it intentionally useless for some reason. Obviously it would not work: the anolyte will become increasingly acidic, producing only chlorine gas. Meanwhile, the sodium ions migrate into the catholyte, making it more basic.

Why titanium, chromium and lead are suggested is beyond me. Graphite will certainly withstand chlorine gas. Titanium will not conduct at all. Chromium will dissolve quantitatively, forming chromium chloride solution. Lead will oxidize to a flaky layer of PbO2 and PbCl2, giving poor efficiency and even poorer conductivity.

Note also that most of the molecular structures are wrong. Wow, a three-membered ring for sodium azide! A four-membered "red phosphorous " ring, with two double bonds! Covalent bonds on ionic substances! An iron (2+) center with four potassium (+) ions and six randomly-arranged neutral cyanide groups bound to it!

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[*] posted on 10-11-2007 at 14:55


Another circular filable crap book from a conartist / pyro expert pretender
and chemist wannabee .

Put the authors collected works on CD and call it a coaster :P

[Edited on 10-11-2007 by Rosco Bodine]
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[*] posted on 10-11-2007 at 15:29


Aside from the questionable methods I also suspected his research as he even states that most of the literature comes from various patents but never references to specific ones! Very unprofessional. Also, in his chemical guide, he introduces reaction equations and states only the desired product be wrote as the result! Further more he states that balancing equations and listing all products is not done in the professional world:o That seems hard to believe considering that even non active by products can affect how the desired product is separated, identified, and made ready for purification.


Oh yea, using aluminum anodes in salt water and creating aluminum hydroxide.:D:P This would work for about 45 seconds




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[*] posted on 10-11-2007 at 16:02


Quote:
Originally posted by dann2
Reading the opening lines it says, Sodium Chlorate is widely used in pyrotechnics also used to make Ammonium Chlorate and Perchlorate which are used in powerful solid rocket propellents.... Does not sound too good.

The battery charger only works when plugged in...
Dann2


Check out the Ammonium Chlorate on page 463.....

... well, my battery charger only works when plugged in also!

Yes, now that I have perused some of the other "content" I can see there are quite a few "howlers"! Some good information, mixed with a lot of bad. Who knows whats what!

Perhaps it's fortunate that the lead dioxide section is missing:D

Regards, Xenoid
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[*] posted on 15-11-2007 at 20:56


http://webpages.charter.net/dawill/tmoranwms/Chem_Chlorate3....

Update time! Pictures, and a tally of what I've produced this year. Conclusion: efficiency is lower than a snake's belly. Read all about it.

Tim




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[*] posted on 8-12-2007 at 06:13
How to use PC PSU in a chlorate cell


Recently I'm starting the eletro-chlorate synthesis and still trying a very small batch with a 1A AC/DC adaptor. Seems very bad to massive production of chlorate..

But yesterday I acquired a old used ATX PC PSU and above it comes a small chart with the (resumed,quick & dirty) following info:

http://i242.photobucket.com/albums/ff176/tnitrato/ps-psu.jpg

Just to see the 'power' developed by this new power source, I plugged it in the wall (110V ac) and adapted the 12v yellow wire with the anode wire of my mini cell and the black with the cathode wire ..when turned on ,instanstaneosly, a fast and violent development of gas on both electrodes was reported and the thin wire on cathode released smoke..then I quickly turned off the PC PSU..all this happened in less than 5 seconds !!!

So, I'm full of doubts :D

how I may know the real current of the out-put using the above chart?
And how thick should be the wire used in the connections of the electrodes?

(sorry, I'm still a begginer in electrolysis , and also my knowledge on eletronic/related stuffs is very limited..also the search engine this time wasn't very helpful for me in this specific, although I know there are some threads on ATX PSU ..)

Chlorates are very pleasant to have lying around, not only because of their usefulness in amateur pyrotechnics (although very dangerous when compared to ClO4- salts) and also in other chemicals..
Thank you guys very much!




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[*] posted on 8-12-2007 at 07:27


Quote:
Originally posted by Aqua_Fortis_100%
Just to see the 'power' developed by this new power source, I plugged it in the wall (110V ac) and adapted the 12v yellow wire with the anode wire of my mini cell and the black with the cathode wire ..when turned on ,instanstaneosly, a fast and violent development of gas on both electrodes was reported and the thin wire on cathode released smoke..then I quickly turned off the PC PSU..all this happened in less than 5 seconds !!!

So, I'm full of doubts :D

how I may know the real current of the out-put using the above chart?
And how thick should be the wire used in the connections of the electrodes?



Oh Dear! Where do I start! I'm sure this has been talked about elsewhere many times, I know I have mentioned it once or twice!

A small chlorate cell only requires about 3 - 3.5 volts to operate at a suitable current, which may be 1 to 4 amps or so in your case.

The table you refer to is not really relevent and refers only to the maximum and average ratings that the power supply is capable of running at. Firstly, you should be using the +5V supply (probably the red and black) any red as they all go to the same place! The +5V is the most desireable as it is closest to the 3 - 3.5V you require. It is also capable of supplying the most current (Amps).

You really need a couple of cheap multimeters, or at least one to measure the current through your cell. And a large (physically) resistor to limit the current to acceptable levels, (a few amps). The resistance will have to be determined using Ohms Law, (Voltage = Current x Resistance). If you want 1 Amp to flow through your cell, you rearrange the equation like so Resistance (Ohms) = (5 volts - cell voltage) / current (Amps).

thus R=(5-3.5) / 1

R = 1.5/ 1 or R = 1.5 ohms

Every cell is different and in practise you will have to experiment with different values of resistance ( say .5 to 2 ohms) until you get what is right for your cell. Nichrome wire is a suitable starting point, remember it will get hot because it is getting rid of all that excess power which would otherwise be heating up your cell.

Power (watts) = volts x current, in this case the resistor power will need to be;

watts = 1.5 x 1 = 1.5W

If you are wanting higher currents your resistor will need to be lower and its wattage will need to be higher, try substituting 2, 3, and 4 amps into the equations above!

Please look on the internet for tutorials on the use and application of ohm's law!

To operate a chlorate cell you need to understand ohm's law and you really need to be able to measure the current (amps) flowing through it!

[Edited on 8-12-2007 by Xenoid]
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[*] posted on 8-12-2007 at 13:03


Xenoid, thank you. You actually was very helpful.

About Ohms Law,and earlier posts talking about the same, please, sorry. As I did said before, I have very poor knowledges in eletronic stuff, but you solved many of my own doubts.

I've got more interested in ATX PSU after looking the 3rd page of this thread and looking the Tim's pic:

http://i242.photobucket.com/albums/ff176/tnitrato/ClO3_by_Ti...

Looking happy in the first, I thinked that he plugged directly the red and the black wires from the ATX PSU to the cell.. After some posts he said:
Quote:
Originally posted by Tim:
Ah, that's just an AT power supply with load resistors on the +5 and +12V rails. Should be running around 30A and done in a week's run time or so.


So these 'load resistors' seems to be the same thing you are talking to use in ohms law.. And I will use after I get sure in what I'm doing...But for now, I still doing the procedure using the 1 amp power source @ 4.5V ..

The only improvement made today was to cut the plastic sides from this AC/DC adaptor and putting a cooler (which I get along with the ATX PSU in a eletronic store as 'souvenir') in one side and plugging this to another AC/DC adaptor (9.3V @ 850mA)..this all to cool the first adaptor (since using it in electrolysis make it getting very hot in some hours..) .. This is appearing to work fine to solve the heat problem..

It could be great if I could associate these two sources and running the resulting current in the cell (and after putting more graphite anodes ), but ... I dont know ! (Looking the battery example were associating in parallel could give more current and same voltage I didn't know what will happen if I will try the same with my power sources, because of the different voltages (one at 4.5 @ 1 A and the other at 9.3 V @ 850mA, as said before) :(

[Edited on 8-12-2007 by Aqua_Fortis_100%]




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[*] posted on 8-12-2007 at 13:33


I would not recommend connecting the supplies in parallel!

Have you got a multimeter, something to measure the current, voltage and resistances!

How big is this chlorate cell, what is it constructed of?
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[*] posted on 8-12-2007 at 14:50


The load resistors I used were to protect the power supply from overvoltage. Switching supplies usually need a certain minimum load to work correctly.

A better example would be the series ballast resistor on my current cell (well it would be current if I had anodes, right Fleaker?), which is a piece of steel wire coming to about 30 miliohms resistance (60A * 0.03 ohm = 1.8V. My power supply is good for about 5V at 60A, which is far too much for a chlorate cell. The 1.8V drop gives 3.2V for the cell, much better.

Of that particular experiment, two things are of note:
1. The power supplies (note the plural!) failed quickly. This was partly due to corrosive salt fume, which negligiently, I was not containing at the time. The other part was, when the cell was in good shape, it drew too much current at 5V, which it ought to. Cells should run in the range of 3V.
2. Electrode wear wasn't great. The graphite anode strips became grooved and much more porous. Probably, the main factor limiting current was how I attached the anodes to the buss bar, which was rather loose and prone to corrosion.

Tim




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[*] posted on 9-12-2007 at 06:10


@Xenoid, is a very small cell.. a 250mL PETE bottle (not pop bottle) with aprox. 200-225mL brine... 4 pieces of gouging rods and a espiraled iron wire as cathode. all in the place through the lid with hot melt glue on it. there are also a aquarium tubing (I don't know what kind of plastic is that made out) attached to the lid and going to another bottle to a improvised inverted funnel on a Na2CO3 solution and another aquarium tubing going from it to the outdoor through the window.

So, according to you, to get best results I will really need of a multimeter for every cell I make? And also to see the real current going to the cell (and also to make the running times eh?).
So I will browse the hardware store aisles to see any..

@12AX7 , thank you, really.. I dont want to ruin my ATX PSU. So need I to lower the voltage from +5V to +3-3.5V with the load resistors and also with the use of these is to avoid the overvoltage, right?
But where come from your PSU "5V at 60A"(I never had see a atx(?) psu with this current)?

How long I may let a ATX PSU turned on? There is a risk of it overheating and .. burning or ruining?




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[*] posted on 9-12-2007 at 08:50


Quote:
Originally posted by Aqua_Fortis_100%
@Xenoid, is a very small cell.. a 250mL PETE bottle (not pop bottle) with aprox. 200-225mL brine... 4 pieces of gouging rods and a espiraled iron wire as cathode. all in the place through the lid with hot melt glue on it. there are also a aquarium tubing (I don't know what kind of plastic is that made out) attached to the lid and going to another bottle to a improvised inverted funnel on a Na2CO3 solution and another aquarium tubing going from it to the outdoor through the window.

So, according to you, to get best results I will really need of a multimeter for every cell I make? And also to see the real current going to the cell (and also to make the running times eh?).
So I will browse the hardware store aisles to see any..

@12AX7 , thank you, really.. I dont want to ruin my ATX PSU. So need I to lower the voltage from +5V to +3-3.5V with the load resistors and also with the use of these is to avoid the overvoltage, right?
But where come from your PSU "5V at 60A"(I never had see a atx(?) psu with this current)?

How long I may let a ATX PSU turned on? There is a risk of it overheating and .. burning or ruining?


I wouldn't put anymore than about 4 Amps through that cell. Instead of spiral wire use a sheet of steel or preferably stainless steel for your cathode.

Not necessarily a multimeter, an ammeter say from a car or old instrument. If you have several small cells, just insert the multimeter in each one, say once or twice a day to check the current! If you find the current has dropped you will know something is wrong....:( check the anode connections for corrosion....:o Make a note of the current in a logbook to spot any trends!

Most computer supplies automatically shut down when over loaded. Only "modern" ones have +5V output greater than about 20 -25 Amps. The more modern supplies also have an output of +3.3 Volts at upto 10 -15 Amps.

The use of a resistor in the circuit is to lower the current (Amps) through the cell, this will at the same time lower the voltage across the cell. The sum of the voltage across the cell and the voltage across the resistor will equal the supply voltage! The voltage from a computer supply is constant (they are constant or fixed voltage supplies). Ideally you want a constant current supply, but that's another story...:D
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[*] posted on 9-12-2007 at 09:31


Simple: my present PSU is not an ATX. I haven't used one for some time, opting instead for what amounts to a homemade battery charger.

ATX supplies are fan cooled and are good so long as the load current is within ratings.

For your cell, you might use a (5V - 3V) / 4A = 2/4 = 0.5 ohm series resistor, rated for more than (5 - 3) * 4 = 8 watts. 10, 12, 15 and 20W power resistors are cheaply available in this value.

To load the unused outputs (mainly the +12V (yellow to black), and if you disconnect +5V from the cell, you might want an additional load on that line as well), about 5W is fine: from the 5V output, a 5 ohm, 5-10W resistor will suffice, while from 12V, a 20-30 ohm resistor will suffice.

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[*] posted on 11-12-2007 at 10:08


Hi
Constructing a new electrolizer, well actually just wanted to brag, check it out
5.5 liter, 8 anodes and 8 cathotes, all graphite


[Edited on 11-12-2007 by hashashan]
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[*] posted on 11-12-2007 at 11:25


Hashashan - I see you are still using "old fashioned" graphite (gouging rods), haven't you switched over to the "new - fangled" Co oxide (spinel) anodes yet..... :D

What is it built from - looks like plumbing fittings, I've thought about that, but I usually use bottling and pickle jars. At least you can see whats going on inside. How much current are you going to put through it!
That looks like a good EFFICIENT design, unlike a 10 litre, 12 rod cell I put together a few weeks back. My cell really needs some stirring. I really put it together, just to produce some bulk chlorate, as I am starting to run out. It can bubble away in the background. I wrote up the following item, but never got around to posting it:

--------------------------------------

........ Well, contrary to my comments about "filthy gouging rods" and wanting to try out MMO pool chlorinator electrodes, I have decided to first have a go at a relatively large sized chlorate cell. This is because I still have a couple of boxes of cheap gouging rods left and I also have several containers of chloride/chlorate "liquor" left over from recrystallising etc. that needs to be recycled.

My previous largest cell was about 4 litres, so I have decided to have a go at a "Tim (12AX7)-sized" 10 litre cell, based on an old plastic paint tub. This should be capable of processing at least 3.5Kg of NaCl as well as the old solutions.

The cell is sealed and the lid has 12 (9.5mm) gouging rods mounted through it. The rods are held in place using waterproof cable glands and "o" rings. One advantage of this design is that the used gouging rods can easily be removed and replaced, by unscrewing the gland. The "o" ring seals in gasses and fumes and prevents corrosion of the electrode electrical connections

The stainless steel (SS) cathode is constructed from an old cooking pot which I had bought some time ago for processing chlorate solutions, etc. But being made in India it only lasted for about a week before holes appeared and it started leaking. The handles were drilled off, and the base was cut off using a jig-saw with a metal cutting blade fitted. It conveniently fits nicely inside the paint pail witha bout a 10mm gap around it.

The vent tube is 6mm ID PVC tubing fitted similarly to the gouging rods, but using the next size down cable gland.

Image 1: Main components, SS cathode, plastic pail, lid with gouging rod anode assembly.
Image 2: Details of anode electrode connections and mountings.
Image 3: Close up, showing cable gland, gouging rod and "o" ring.
Image 4: SS cathode, in position and wired up.

[Edited on 11-12-2007 by Xenoid]

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[*] posted on 11-12-2007 at 11:46


I like your cable gland idea, Ill need to find some of those. I just use hotmelt glue :)
and no need for the electric connection, I just soldered my wires to the copper.
Didnt want to use SS because of possibility of chrome ions running loose, and I do want to use that chlorate later in a perchlorate cell with the PbO2 anode.
The tube really is a simple 6 inch PVC pipe
And I still dont know how to make a good lid to it, this one is just going to sit over it, not really a lid .... more like a cover.

about stirring, I was planning to however my magnetic stirrer went in flames :D while making my PbO2 anode I had a little fire so still need to fix it, or maybe to make a new one
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[*] posted on 11-12-2007 at 11:52


Nice and large. What kind of power supply do you have lined up for that?

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[*] posted on 11-12-2007 at 12:20


@ Tim - if you are referring to my cell, I'm using that 48 amp halogen lighting transformer power supply I put together, it's in the "PSU" thread. I'll probably run it at 24 amps, ie 2 amps per rod.

@ Hashashan - unfortunately those cable glands are quite expensive, to save money, I bought the next size SMALLER. I cut off the internal sealing bits, drilled them out to 9.5 mm and fitted "O" rings. This also means they don't take up so much room! Although expensive, they should last a lifetime.

I've thought long and hard about the stirring, it will really make a difference with a bulky cell like this. I did some experiments with a rare earth magnet attached to an old microwave fan motor, spinning a conventional lab stirrer bar. It worked, sort of, but then it meant I had to make a stand. I've also looked at various other magnetic stirring designs. I have even considered using the fan motor with a long rod coming down from the top. This is partly why the project is "on hold".

That grey plastic sewer pipe, you can get screw on lid fittings, with "O" ring seals and also simple endcaps, I have considered this as a design from time to time. A bit like the combustion chamber of a "spud gun".

Looking at your design again! Doesn't that lid or cover actually fit INSIDE the pipe - in other words, shouldn't the rods be going through it the other way!
Hot glue sealing should be fine, I've used epoxy in the past, it holds up quite well.

[Edited on 11-12-2007 by Xenoid]
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[*] posted on 11-12-2007 at 14:31


Ill use a modified PC PSU(just making it Voltage controlled)
I couldnt find a lid. This lid wont fit in Its the same diameter .. so It was meant to be exactly in this direction.
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[*] posted on 11-12-2007 at 21:00


Hello Hashashan,

Do you intend to treat the rods with Linseed oil or some other stuff.

Dann2
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[*] posted on 12-12-2007 at 04:56


nope, I dont have the patience for that.
Ill electrolyze till the anodes erode
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