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making potassium (per) chlorate


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Posted (edited)

I want to expose myself to as little MMO smoke as possible.

 

Me, too. I do my spot welds outside and stand upwind (and hold my breath ;)). Swede always warned about avoiding ruthenium fumes. Avoiding all metal fumes is probably definately a good idea!

 

WSM B)

Edited by WSM
Posted

Sorry my responses are a bit slower than normal, I'm lurking around the PGI convention (:D) and don't sit in front of a keyboard very often. Also the cell phone service works but it's spotty for typing a response. LOTS of fireworks, very little discussion of electrochemistry (:( :rolleyes: ;)).

 

WSM B)

Posted
C'mon, ruthenium isn't that bad for you. It holds a special place in my heart (probably both figuratively and literally. It intercalates DNA)
Posted

This would have been nice to know before i went and plasma cut my MMO, i filled the workshop with ruthenium smoke, and i certainly was breathing it.

this might explain my current fever.......

Posted (edited)

This would have been nice to know before i went and plasma cut my MMO, i filled the workshop with ruthenium smoke, and i certainly was breathing it.

this might explain my current fever.......

RULE NUMBER ONE: SAFETY.

 

Always protect your self from the unknown. If you do not know whats in it, it can hurt you or even kill you.

Edited by patsroom
Posted
Let us know if your eyes and/or skin get stained black or your lungs fill with fluid.
Posted
will do. at the time though i asumed it was titanium dioxide which i knew was harmless enough. well. when i cut the next sheet ill be sure to do it in the fumehood!
Posted

will do. at the time though i asumed it was titanium dioxide which i knew was harmless enough. well. when i cut the next sheet ill be sure to do it in the fumehood!

 

Hi OMBJ,

 

I'm surprised you didn't use the fume hood in the first place! If you have safety equipment why not use it? Metal fume fever is no joke; you can get really sick.

 

(What good are the piles of chlorate going to do you if you don't feel good enough to use them ;) :lol:.) Please take better care of yourself.

 

WSM B)

Posted

the plasma cutter has a special bench (also used for oxyacetylene cutting).

which has a grate on which you place the metal so there is nothing below it.

 

i would need a special setup to get the welding fumehood to suck away the burnt metal smoke from the plasma cutter.

also the cut only took 1 minute at most and i didnt notice the smoke until i was done. plus i had just done a cut with some steel as practice, and it made no smoke, so i saw no reason to even think of a fumehood.

 

"its a shame that error and consequence or the sight of indefinite consequence is the only thing that will change ones ways to the better "- J.P.Richter

Posted

You can measure easy big amps with a $5,- multimeter with a trick.

Get a 1 ohm 10W resistor when you buy your multimeter.

Attach one side of the resitor to the + of your powersupply, te other to your -.

Now the law of OHM (U = I x R) wil tell you you'll have about 5.2 amps (5.2 = I x 1) running.

Remove two times some insulation on your + cable, say 5cm apart.

Put your multimeter on uAmps and stick the two probes in the two bare copper places.

You will get a value, say 1.6. You now can calculate a factor, your factor (in this example 5.2/1.6 = 3.25).

Your $5 dollar 100 amp multimeter has been calibrated.

When using in a cell, say you read 7.3 uAmp, you do 7.3 x 3.25 = 23.725 which will tell you you are running about 23 amps.

This is by the way exactly how big amp meters work, there is no massive currenr running through a spool, it is done by a bridge, exactly as desribed above.

 

Hi pdfbq,

 

Thanks for sharing the "trick". I probably could have figured it out on my own, but it never occured to me to do so. Also it's nice to have it layed out for you so all you have to do is plug in your own numbers and out pops the relevent data. Thanks again :). (networking is wonderful!)

 

WSM B)

Posted

well, i gave up on that.

my 50A ammeter is on its way, probably 5 days away at most now.

i might consider that method when i go and measure how much power my MOT welder outputs, in amps.

Posted (edited)

I am currently considering getting some 3v-5v power supplies wholesale, to resell, what kind of maximum amperage should i be looking for. These are for the purpose of electrolysis power supplies for making (per)chlorate mainly.

most i found are about 20A-22A with the same amperage for 5v. is this good? or should i seek switchmodes with higher current capacities?

Edited by oldmanbeefjerky
Posted (edited)

I am currently considering getting some 3v-5v power supplies wholesale, to resell, what kind of maximum amperage should i be looking for. These are for the purpose of electrolysis power supplies for making (per)chlorate mainly.

most i found are about 20A-22A with the same amperage for 5v. is this good? or should i seek switchmodes with higher current capacities?

 

Typically 5Vdc with the highest amperage available, is the way to go for a chlorate cell. The cell will take all the current it needs but all the voltage you supply. If there is a voltage control trimmer on the supplies, that is a plus.

 

For a perchlorate cell, try for 6Vdc or (a little) higher.

 

WSM B)

Edited by WSM
Posted
ok so 5v is the way to go, this is good, there dont seem to be many 3VDC sower supplies out there anyway
Posted

ok so 5v is the way to go, this is good, there dont seem to be many 3VDC sower supplies out there anyway

 

Unless you are trying for max efficiency - which is slightly higher than 3V IIRC, just forget (permanently) the 3V crap. Go with 5V, proven time and again. Get a cell going already...less talk more rock !!

Posted (edited)

My ammeter arrived today, so i got the cell running.

it doesnt seem to be going well

 

first problem is that there is allot of foaming with the potassium chloride. i suspect that it contains potassium carbonate, or is slight foaming normal for finely powdered potassium chloride?

 

also, i had to improvise contacts, so i got some 2mm copper wire and attached it to the cell electrode contacts. almost immediately it heated up so much it hurt to touch, but its probably just because of the fact i wrapped the wire around the titanium sheet (anode connector) and the 3x 3mm tinned wires (for the cathode which connect to a peice of stainless. im going to add solder to the contacts so i dont get this problem.

 

also, my fears of going over what the cell could handle in amperage are at rest, the ammeter reads 11-7A constantly switching from 7,8,9,10,10.5,11 over and over. with a bit of fiddling, 12A is the highest i can get the amperage to go, will it rise as the alkilinity rises or will it drop?

just out of curiosity, where does everyone attach the ammeter, the diagram i got with my ammeter shows that i must connect it to the negative (negative comming from the cell, going to the powersupply), is this right?

 

my cell isnt going as smoothly as i had first imagined. if i dont solder the contacts soon i fear it will melt over night

 

 

-edit-

 

i just soldered the contacts which raised the amperage to 12-9 which is good, now i hope it helps with the heating problem. this isnt with my permanent pvc cell since i still need 1 more peice before its done, and the lid i am using in the cell running atm, might melt away if those temps persist. if in a few hours they dont cool i will have a PC-fan blow them, and the cell, which might help control temperature slightly, the heat generated at the contacts already made the cell quite warm as heat transferred down through the anode into the cell.

 

-edit 2 -

 

its been running for a a few hours now and the current has dropped from 12A max to 9-8A max dropping as low as 5.6A, surely this isnt normal cell behaviour?

currently the cell has about 320g potassium chlorate dissolved into 1.5L of water. does anyone know what Amperage i should stop at?

tommorrow i will go get some hydrochloric acid from my mates house, and carefully bring the ph back to near neutral, using my ph paper, and ill scoop out that annoying frothy foam which keeps clotting up on the anode then falling off like ashes. ill do an acid test with the foam to find out just what exactly it is.

Edited by oldmanbeefjerky
Posted

also, i had to improvise contacts, so i got some 2mm copper wire and attached it to the cell electrode contacts. almost immediately it heated up so much it hurt to touch, but its probably just because of the fact i wrapped the wire around the titanium sheet (anode connector) and the 3x 3mm tinned wires (for the cathode which connect to a peice of stainless. im going to add solder to the contacts so i dont get this problem.

 

Hi OMBJ,

 

Heat = inefficiency. You need to devise a method to solidly connect the leads to the electrodes; then the heat at the point of connection will be reduced. Instead of wrapping copper wire around the cathode, try crimping a ring connector to the end of the wire, drill a hole in the titanium and use a stainless steel machine screw and nut to connect the electrical connection. If you do and it heats up, just tighten the screw and nut assembly a bit. If it heats after that, something else is going on.

 

Take a close look at the photo of the cell I posted and see how I did it. I used tubular titanium leads (on the electrodes) filled with solder and connected the ring terminal with stainless screws and washers after tapping the ends of the tubes. I also used heavy stranded copper wire leads to handle the current. My electrodes got warm but not enough to damage the plastic compression fittings holding the round leads.

 

WSM B)

Posted

its been running for a a few hours now and the current has dropped from 12A max to 9-8A max dropping as low as 5.6A, surely this isnt normal cell behaviour?

currently the cell has about 320g potassium chlorate dissolved into 1.5L of water. does anyone know what Amperage i should stop at?

tommorrow i will go get some hydrochloric acid from my mates house, and carefully bring the ph back to near neutral, using my ph paper, and ill scoop out that annoying frothy foam which keeps clotting up on the anode then falling off like ashes. ill do an acid test with the foam to find out just what exactly it is.

 

Once your cell is set up and running correctly, a rule of thumb is to shut it down when the original (starting) current drops to 50%. Then you can harvest the chlorate for processing, recharge the cell with salt and start again.

 

More running time (after the current drops to half) is harder on system components and yields little more chlorate.

 

WSM B)

Posted (edited)

OMBJ,

 

As WSM said, use bolts to secure the connections nice and tight. The amperage usually uincreases as the cell heats up, until it stabilzes at the running temp. I'm not sure the size of your cell, but if you pump too much current into a small cell, the solution might get too hot.

 

The amperage can be increased by moving the electrodes closer together.

Edited by Bonny
Posted (edited)

well,

 

the cathode cable got exposed and corroded away, though it wasnt the souce of the foam. i will boil the solution, to remove chlorite, then i will filter it through an old shirt, as not to melt a hole through it like my past two experiences with chlorites and shirts then i shall resume electrolysis with two titanium cathodes, instead of stainless steel.

 

i wonder though, will it be ok if i use two cathodes which each are about 48cm2 with my anode which is 99cm2?

Edited by oldmanbeefjerky
Posted

well,

the cathode cable got exposed and corroded away, though it wasnt the souce of the foam. i will boil the solution, to remove chlorite, then i will filter it through an old shirt, as not to melt a hole through it like my past two experiences with chlorites and shirts then i shall resume electrolysis with two titanium cathodes, instead of stainless steel.

i wonder though, will it be ok if i use two cathodes which each are about 48cm2 with my anode which is 99cm2?

 

If the copper got into the mother liquor you may want to discard this batch and start fresh (copper chlorate contamination can result in dangerous reactions where you don't want them). The two cathodes roughly equaling the surface area of the anode sound like a good idea. I would wire the cathodes parallel to each other and be sure to isolate the electrical connections (leads) from the mother liquor (cell solution) to prevent a repeat of the last one.

 

WSM B)

Posted

WSM..

I have to say thanks for your inspiration. I hope youll forgive me for bumping in here, but your advise on the spot welder was a good one... I tried the cheap $20 spot welder attachment for a arc welder , and it did nothing but burn and imbrittle the TI. I managed to get a halfway weld with it, but it was a waste of $. I just purchased the 115V pincher style spot welder, and it worked like a dream......! Almost effortless. One thing that I have learned is Ti needs to be absolutely clean and acetone washed before a weld to achieve a great bond.

Thank you again .

Pyrojig

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post-10746-0-41995200-1313543953_thumb.jpg

Posted (edited)

If the copper got into the mother liquor you may want to discard this batch and start fresh (copper chlorate contamination can result in dangerous reactions where you don't want them). The two cathodes roughly equaling the surface area of the anode sound like a good idea. I would wire the cathodes parallel to each other and be sure to isolate the electrical connections (leads) from the mother liquor (cell solution) to prevent a repeat of the last one.

 

WSM B)

 

The tinned wire crimped and bolted to the cathode wasnt in the water the chlorine gassses just weakened the already brittle wire which would have been a few bends away from snapping. i highly doubt any copper got in, and if it did, it would be less than 0.2g tops!

 

this is the first and last time i ever use wiring inside the cell. outside is fine, but never again inside. from now on ill just spotweld titanium plates to the electrode (should i ever make more).

 

also, the setup you described, you mean have one cathode on either side of the anode right?

 

 

-also, i just received the msds for my potassium chloride, and i was puzzled, because it says the only contents were potassium chloride and 0.5% sodium chloride. nothing out of the ordinary which was insoluable. meaning that the foam is definitely a product of potassium, most likely carbonate, i hope.

Edited by oldmanbeefjerky
Posted
What source of water did you use to dissolve the potassium chloride?
Posted

i just used tap water, since i was just throwing together a cell since i finnaly was able to. should i use deminieralized water instead?

 

i just wasted 3 hours of effort , a peice of filter paper and a good stainless steel pot in removing the precipitant.

the pot is now full of little eroded holes, after my mum insisted we just let it sit for 30 mins. the solution turned dark brown, and had eaten small holes in the pot upon my return.

the chlorite somehow dissolved the iron in the pot to make iron chloride, which as soon as i ran the cell, formed black iron oxide, which gave me a big fright since i thought my anode was producing the mess, since the water was clear when i begun , well actually it was yellow i asumed it was aqueous chlorine though, since all my past cells went yellow over time.

anyway, i am going to start a fresh batch now. and this time ill use boiling hot water instead of cold water to dissolve the chloride.

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