making potassium (per) chlorate

[athlon]

I read somewhere that I shouldn't allow the chloride levels to drop below 30g/liter of electrolyte with MMO anodes. How can I know when the cell is beginning to get depleted of chloride?

Is there some guidance as to how many Ah I can let through per amount of solution?

 

By the way, I don't have any Home depot shops in sweden. I'm trying to find a retailer that sells KCl as fertilizer, hopefully I'll find a source because buying table salt gets expensive really quick.

 

/athlon

[ausgoty]

Ah, carmine, thats what I meant, doh! So thats the easiest way?

 

In a pinch you can use the fertiliser "muriate of potash" the stuff I have is KCl with a horrible oily red binder of some kind. I have to boil this with water and filter to get rid of the red gunk. It is cheaper in cash but not in time. I have made quite a bit of good KClO3 from it.

 

They say the anode bubbles a lot more when the chloride is gone, something about making oxygen from the water as there is nothing else left. I've never let mine go that far. Just get the KClO3 out when it looks like there is enough in there to make it worthwhile, resaturate and start again.

 

Sodium chlorate is a different matter. The way I did that was to eveporate a small quantity of my liquer every couple of days until the salt I obtained burnt "like chlorate should" when mixed with sugar. Not very scientific, but the NaClO3 I obtained seems to be quite effective and very orange!

[WSM]

I read somewhere that I shouldn't allow the chloride levels to drop below 30g/liter of electrolyte with MMO anodes. How can I know when the cell is beginning to get depleted of chloride?

Is there some guidance as to how many Ah I can let through per amount of solution?

 

By the way, I don't have any Home depot shops in sweden. I'm trying to find a retailer that sells KCl as fertilizer, hopefully I'll find a source because buying table salt gets expensive really quick.

 

/athlon

 

Hi Athlon,

 

You can tell when the chloride is getting depleated by the amount of chlorate that collects on the bottom of the cell. Changing power requirements is another indication (dropping current, rising voltage or both). One of our prolific bloggers, "Swede" has documented a lot about his electrochemistry experiments and his blogs are a great source of the information you're looking for.

 

Does Sweden have hard water? We do here in the Western US, and water softener use is common. If water softeners are used there, see if potassium chloride is available as a healthier alternative to the sodium salt. Good luck with your search.

 

WSM

[WSM]

Ah, carmine, thats what I meant, doh! So thats the easiest way?

 

Hi ausgoty,

 

I wouldn't say the easiest way, but certainly easier to obtain (it should be available from suppliers who sell biological stains for microscopy). The other two are a royal pain in the kiester to get , but effective in use.

 

 

WSM

[Bonny]

Hi Athlon,

 

You can tell when the chloride is getting depleated by the amount of chlorate that collects on the bottom of the cell. Changing power requirements is another indication (dropping current, rising voltage or both). One of our prolific bloggers, "Swede" has documented a lot about his electrochemistry experiments and his blogs are a great source of the information you're looking for.

WSM

 

When I had my cell running I just watched for the current to drop.. in my cell from >20A to <15A. I considered teh run done at that point. My MMO anode still looks new after several runs. I've run it even harder (to <10A) and it still looks great.

Hi ausgoty,

 

I wouldn't say the easiest way, but certainly easier to obtain (it should be available from suppliers who sell biological stains for microscopy). The other two are a royal pain in the kiester to get , but effective in use.

WSM

 

I use NPAA - very sensitive, but VERY hard to get.

[WSM]

When I had my cell running I just watched for the current to drop.. in my cell from >20A to <15A. I considered teh run done at that point. My MMO anode still looks new after several runs. I've run it even harder (to <10A) and it still looks great.

 

I use NPAA - very sensitive, but VERY hard to get.

 

I remember seeing the current drop at end-of-run, too. Thanks for reminding me.

 

I have all three reagents, but I'm just learning about the properties of NPAA, which looks very promising. I like the sensitivity of Indigo carmine and/or NPAA. Aniline hydrochloride is effective but I'm not thrilled with the toxicity issues with it (plus it doesn't keep well once it's mixed with the HCl).

 

Regards, Steve

Edited January 25, 2011 by WSM

[Bonny]

I remember seeing the current drop at end-of-run, too. Thanks for reminding me.

 

I have all three reagents, but I'm just learning about the properties of NPAA, which looks very promising. I like the sensitivity of Indigo carmine and/or NPAA. Aniline hydrochloride is effective but I'm not thrilled with the toxicity issues with it (plus it doesn't keep well once it's mixed with the HCl).

 

Regards, Steve

 

 

I'v only ever used NPAA. Swede's blog was a great tutorial on testing. Very easy to do and (from what I've read) very sensitive.

[athlon]

I have now started a test cell containing about 1.5 liters of water saturated with table salt 69% KCl and 31% NaCl. I use a graphite anode from a lantern battery and about 5 cm is immersed in the solution. For cathode use I found a stainless steel spoon. The electrodes are spaced about 5 cm apart and a current of 250mA is delivered to the cell.

 

Anode surface area is about 9.5 cm² and at the oxidizing site I found out that about 30mA/cm² is regarded as enough for graphite so that it does not erode.

This won't keep any temperatures to talk about and I hope that's not a problem as with 5V that is only about 1.2W of energy.

 

I have already gotten a white precipitate at the bottom, I can not tell if it's chlorate or something else though and the electrolyte seems to be clear of any graphite particles so far.

Cell runtime is about ~15h.

 

Anyone correct me if I'm wrong about my calculations.

 

Edit: Energy was way off, 6W was used when I was trying to dial in the Amps at the beginning and the cell got ~1.2A

 

/athlon

Edited January 26, 2011 by athlon

[WSM]

I'v only ever used NPAA. Swede's blog was a great tutorial on testing. Very easy to do and (from what I've read) very sensitive.

 

All true. Swede's thoughts the last time I heard from him were methanol for the NPAA solvent and HCl for the acidifier (with the added benefit of being relatively clear compared to H₂SO₄). He also mentioned getting the test solution percentage down to 1-2%, though I think the added sensitivity at 3% NPAA makes up for being "wasteful" of the expensive (and hard-to-get) reagent.

 

WSM

[WSM]

I have now started a test cell containing about 1.5 liters of water saturated with table salt 69% KCl and 31% NaCl. I use a graphite anode from a lantern battery and about 5 cm is immersed in the solution. For cathode use I found a stainless steel spoon. The electrodes are spaced about 5 cm apart and a current of 250mA is delivered to the cell.

 

Anode surface area is about 9.5 cm² and at the oxidizing site I found out that about 30mA/cm² is regarded as enough for graphite so that it does not erode.

This won't keep any temperatures to talk about and I hope that's not a problem as with 5V that is only about 1.2W of energy.

 

I have already gotten a white precipitate at the bottom, I can not tell if it's chlorate or something else though and the electrolyte seems to be clear of any graphite particles so far.

Cell runtime is about ~15h.

 

Anyone correct me if I'm wrong about my calculations.

 

Edit: Energy was way off, 6W was used when I was trying to dial in the Amps at the beginning and the cell got ~1.2A

 

/athlon

 

Excellent start. Keep up the good work. How did you connect the electrodes to the power supply? Usually beginners use alligator clips; I know I did. When you get to larger or higher power systems, try to get "bolt together" connections to avoid wasting energy as heat rather than current into the cell (a tip from an electrical worker) .

 

WSM

[athlon]

I used nichrome wire on the positive pole wound tightly around the graphite, so that I could limit the current to the cell and a rather large clip, the size of automotive battery charger clips, on the cathode.

When I get my MMO anode I'll be designing the connections better. I'll just have to find a container that better suits a larger amount to be produced.

I have this meter connected between my computer power supply and the cell.

 

Hopefully I have found a source for KCl, I get the answer Wednesday next week. I've been busy calling all fertilizer dealers around here!

 

Will be excited to see what my small cell actually has produced, hopefully there's some potassium chlorate in there.

 

/athlon

[Bonny]

I have now started a test cell containing about 1.5 liters of water saturated with table salt 69% KCl and 31% NaCl. I use a graphite anode from a lantern battery and about 5 cm is immersed in the solution. For cathode use I found a stainless steel spoon. The electrodes are spaced about 5 cm apart and a current of 250mA is delivered to the cell.

 

Anode surface area is about 9.5 cm² and at the oxidizing site I found out that about 30mA/cm² is regarded as enough for graphite so that it does not erode.

This won't keep any temperatures to talk about and I hope that's not a problem as with 5V that is only about 1.2W of energy.

 

I have already gotten a white precipitate at the bottom, I can not tell if it's chlorate or something else though and the electrolyte seems to be clear of any graphite particles so far.

Cell runtime is about ~15h.

 

Anyone correct me if I'm wrong about my calculations.

 

Edit: Energy was way off, 6W was used when I was trying to dial in the Amps at the beginning and the cell got ~1.2A

 

/athlon

 

Great start athlon. You'll find production VERY slow using so little power, but it's all about experimenting.

 

All true. Swede's thoughts the last time I heard from him were methanol for the NPAA solvent and HCl for the acidifier (with the added benefit of being relatively clear compared to H₂SO₄). He also mentioned getting the test solution percentage down to 1-2%, though I think the added sensitivity at 3% NPAA makes up for being "wasteful" of the expensive (and hard-to-get) reagent.

 

WSM

 

I used isopropyl alcohol.I mixed it at about 2% (maybe 3%), and also used HCl as the acidifier. A test I did using a 500ml (IIRC) solution of commercial perc showed no chlorate. When I added a grain (not weight) of chlorate it was detected by the NPAA - which would indicate much less than >1% chlorate can be easily detected.

 

I used nichrome wire on the positive pole wound tightly around the graphite, so that I could limit the current to the cell and a rather large clip, the size of automotive battery charger clips, on the cathode.

When I get my MMO anode I'll be designing the connections better. I'll just have to find a container that better suits a larger amount to be produced.

I have this meter connected between my computer power supply and the cell.

 

Hopefully I have found a source for KCl, I get the answer Wednesday next week. I've been busy calling all fertilizer dealers around here!

 

Will be excited to see what my small cell actually has produced, hopefully there's some potassium chlorate in there.

 

/athlon

 

To limit the current, move the electrodes farther apart. Keep in mind as the solution heats up the current will increase a bit. As noted by WSM, bolt all the connections together. You can build a great cell by simply using a 20l plastic pail from the hardware store. That's what I use.I was easily making batches of 5lbs or more, running 20-25A into the cell. For KCl, look at the hardware stores. It's commonly used as water softening salt. You should be able to get a 50lb bag for $10-$20 I think.

Edited January 26, 2011 by Bonny

[WSM]

I used isopropyl alcohol.I mixed it at about 2% (maybe 3%), and also used HCl as the acidifier. A test I did using a 500ml (IIRC) solution of commercial perc showed no chlorate. When I added a grain (not weight) of chlorate it was detected by the NPAA - which would indicate much less than >1% chlorate can be easily detected.

 

To limit the current, move the electrodes farther apart. Keep in mind as the solution heats up the current will increase a bit. As noted by WSM, bolt all the connections together. You can build a great cell by simply using a 20l plastic pail from the hardware store. That's what I use.I was easily making batches of 5lbs or more, running 20-25A into the cell. For KCl, look at the hardware stores. It's commonly used as water softening salt. You should be able to get a 50lb bag for $10-$20 I think.

 

Hi Bonny,

 

What percent is your isopropyl alcohol? My preference would be 99% if I used IPA. Methanol was suggested and I like it's low moisture content. Perhaps shellac thinner (denatured ethanol) would be another good candidate? Swede got a positive indication using NPAA with as little as 10 ppm of chlorate, which is very good. The indigo carmine is supposed to be more sensitive than that! I see a contest brewing...

 

If anyone knows where I can get 50 lbs of KCl for $10, let me know quick!!! Home depot was the lowest local source at $14 per 40 lbs up to a month ago. Two days ago I noticed that since then it was raised to $20 for the same bags. Potassium salts seem to be on the rise in a dramatic fashion, right now. I don't know what's going on, and if it's not just the US economy, but an international condition, it would be wise to stock up before it gets worse .

 

 

WSM

[Bonny]

Hi Bonny,

 

What percent is your isopropyl alcohol? My preference would be 99% if I used IPA. Methanol was suggested and I like it's low moisture content. Perhaps shellac thinner (denatured ethanol) would be another good candidate? Swede got a positive indication using NPAA with as little as 10 ppm of chlorate, which is very good. The indigo carmine is supposed to be more sensitive than that! I see a contest brewing...

 

If anyone knows where I can get 50 lbs of KCl for $10, let me know quick!!! Home depot was the lowest local source at $14 per 40 lbs up to a month ago. Two days ago I noticed that since then it was raised to $20 for the same bags. Potassium salts seem to be on the rise in a dramatic fashion, right now. I don't know what's going on, and if it's not just the US economy, but an international condition, it would be wise to stock up before it gets worse .

 

 

WSM

 

The isopropyl I used was indeed 99%. I'm sure denatured alcohol would be fine as it is (generally) denatured with methanol.

I have some indigo carmine, but have not tried it. Wasn't methylene blue another indicator? I've been "out of the loop" for awhile and all my notes are packed away somewhere ATM. Also, do you have the link for the former cape canaveral site?

 

As for the KCl, it's been a few years since I bought any. I've got 40+ lbs of chlorate waiting to be converted or used up, so I'm in no rush to buy any.

[WSM]

The isopropyl I used was indeed 99%. I'm sure denatured alcohol would be fine as it is (generally) denatured with methanol.

I have some indigo carmine, but have not tried it. Wasn't methylene blue another indicator? I've been "out of the loop" for awhile and all my notes are packed away somewhere ATM. Also, do you have the link for the former cape canaveral site?

 

As for the KCl, it's been a few years since I bought any. I've got 40+ lbs of chlorate waiting to be converted or used up, so I'm in no rush to buy any.

 

Hi Bonny,

 

Methylene blue solution is a test for perchlorate. A weak solution of methylene blue is prepared with distilled water and a drop in a test solution sample will turn purple if perchlorate is present. Nitrates and chlorates don't interfere. I'll have to look for the Cape Canaveral site and post it later. If not, I may have a copy of parts I can send.

 

WSM

[Arthur]

With Sweede not currently contributing to the forum, does anyone have a current supplier of electrodes, Given a Ti cathode source, I'd like to find anode sources too. There's a UK supplier of electrodes near me ( about 2 miles!) BUT they only supply small Pt electrodes which are a bit pricey for playthings!

[WSM]

With Sweede not currently contributing to the forum, does anyone have a current supplier of electrodes, Given a Ti cathode source, I'd like to find anode sources too. There's a UK supplier of electrodes near me ( about 2 miles!) BUT they only supply small Pt electrodes which are a bit pricey for playthings!

 

Hi Arthur,

 

We have suppliers of MMO anodes here in the US. What type or size are you looking for? Maybe one of us can get one to you to try out?! Let us know.

 

WSM

[frank]

Hi,

 

The address of the CapeCanaveral (or geocities) site in now http://oxidizing.110mb.com/

 

If looking for Anodes for making Potassium Chlorate you could try Manganese Dioxide. They last months in a Potassium Chlorate cell if used at around 50mA per square cm.

 

How is Swede?

 

 

 

 

[WSM]

Hi,

 

The address of the CapeCanaveral (or geocities) site in now http://oxidizing.110mb.com/

 

If looking for Anodes for making Potassium Chlorate you could try Manganese Dioxide. They last months in a Potassium Chlorate cell if used at around 50mA per square cm.

 

How is Swede?

 

Hi Frank,

 

Welcome and thanks for the link. As for Swede, We don't know (haven't heard from him since last July or so). We hope he's okay and just occupied with other projects.

 

Have you made MnO₂ anodes? How did you do it (and thanks in advance for sharing )?

 

WSM

[WSM]

There are MMO on titanium mesh pieces available on eBay right now at very low prices. See items:

 

260727268167 and

260728266798

 

Even the smaller of the two sizes will run at up to 150 amps. With two cp titanium cathodes (one on either side of the anode) and a decent power supply, enough chlorate could be produced to provide an active amateur pyrotechnist all he needs and surplus. I see the surplus supplying a perchlorate cell.

 

I have bought from this supplier before and he ships quickly and at reasonable rates. Again, I'm not connected with him in any way except as a satisfied customer .

 

Enjoy.

 

WSM

[Bonny]

There are MMO on titanium mesh pieces available on eBay right now at very low prices. See items:

 

260727268167 and

260728266798

 

Even the smaller of the two sizes will run at up to 150 amps. With two cp titanium cathodes (one on either side of the anode) and a decent power supply, enough chlorate could be produced to provide an active amateur pyrotechnist all he needs and surplus. I see the surplus supplying a perchlorate cell.

 

WSM

 

Personally, my main goal has always been perc, my surplus will be used as chlorate.

I've got at least 30lbs of chlorate waiting for conversion. My "shop and lab" are currently in boxes due to renos. I've got about 5-10lbs of perc that just needs a little more cleaning. I've already fried two Pt anodes, and will hopefully never need another, I've got a nice lead dioxide anode waiting to be tried...

[WSM]

Personally, my main goal has always been perc, my surplus will be used as chlorate.

I've got at least 30lbs of chlorate waiting for conversion. My "shop and lab" are currently in boxes due to renos. I've got about 5-10lbs of perc that just needs a little more cleaning. I've already fried two Pt anodes, and will hopefully never need another, I've got a nice lead dioxide anode waiting to be tried...

 

I've always planned one thing at a time, first chlorate and then perchlorate. I don't need it, but I enjoy the challenge and get great satisfaction from the thought of being self-sufficient.

 

I haven't produced any salts in over two years, but plan to run my experimental cell as soon as I can and record as much data as possible during its operation. With the lessons learned there I'll move on to "the Monster" and see what it can do (original goal was one kilo per day, but I'm afraid it will do more).

 

I have an LD anode too. I want to do a trial with it as soon as I can repair some shipping damage on it.

 

WSM

[athlon]

Anticipation, the anticipation! I could not wait any longer as I'm too eager to see what my little cell has produced for me. Had to hot filter the liquid once to get rid of the carbon particles and now the liquid is cooling in a bucket of snow.

[athlon]

So, here's the yield:

[Peret]

So, did you use a manganese dioxide anode for this batch? It appears to have a slight potassium permanganate tint to it, or perhaps that's just in the camera.