making potassium (per) chlorate

[frank]

@ killerinc

There is no better Anode than Platinum. It is expensive and will wear out if you let the cell run too long.

 

 

@WSM

I had to edit my post above as the conclusion I came up with were TOTALLY WRONG.

 

The power error (30% of total power supplied to cell) is indeed varying with the current and you will need to monitor current (estimate the average as it varies from time of day, and from day to day) in order to estimate the error that must be subtracted from the kilo Watt meter reading.

This will be a pain and you will be back to needing a current meter on the cell and reading it (approx. twice a day (or more) and obtaining an average reading by calculation. (Just what we are trying to avoid).

The KAW system may be more accurate than obtaining current reading (current meter on cell) as per usual and averaging current reading (twice per day, say) and calculating Amper hours into cell from that figure. But the errors will be unknown. If you have a system set up and run it consistently (similarish current into cell each run) then the KAW will give you a figure you can work on but you are really just using it as a fancy timer.

 

A constant current into the cell is the way to go if you can set things up that way, with no need for KAW.

 

A KAW meter placed at the cell (after the PSU) would be OK with any setup as difficulties with the PSU then dissappear. You would need good heavy wires and good connections so that the Voltage accross the cell remains at a steady 5V. The KAW meters that can be purchased will not do this as they will not operate at the high current see at the cell.

 

 

 

Frank

[WSM]

has anyone seen these videos this guy makes it look easy he is using platinium anode and stainless cathode and says they give best results

http://www.youtube.c...h?v=kp4BoEam3iY

http://www.youtube.c...h?v=O1aWzrRBMjk

http://www.youtube.c...h?v=oziKdF2tYOE

 

I found it interesting he tested for perchlorate in the first video but neglected to test for chlorate. Swede made potassium perchlorate from potassium chlorate, it works but has it's problems. He tested his perchlorate for chlorate and found plenty. It wasn't till he neutralized the chlorate in his perchlorate that he felt comfortable using it for fireworks.

 

There is much more handling involved than appears in these videos. It's still good to see how others do things, though. Very nice glassware, by the way. If it were purchased new, the cost would be more than a decent power supply, I think.

 

WSM

[WSM]

It just ground as fine as I could in my new coffee grinder. No idea what mesh size, it was making it's own chunks while trying to mix it with the benzo. The benzo is also old, possibly as old as 100 yrs, it came from my great, great, grandfathers pharmacy. That said it was the consistency of icing sugar. The comp was Oztap,

I don't want to derail this thread. I'll start another one in the future to discuss whistle.

 

If you try it again, mill separately the benzoate and the chlorate as fine as you can get them, first. Next mix as normal. Test the whistle immediately, store the mix for a month and test again. It's a strange thing but sometimes whistle mix works better after it's been stored a while. I can only guess why, but I've observed this phenomenon in the past. Let us know how this works.

 

WSM

[pdfbq]

has anyone seen these videos this guy makes it look easy he is using platinium anode and stainless cathode and says they give best results

It is easy when you have a Pt anode. But, as WSM already stated, this guy did not test for chlorate (use indigo carmine) so his perc should be treated as if it was chlorate so whats the point making perc then?

Also, what I have read is that Pt is sensitive to low CHLORINE as well as low chlorate levels which means that gong from NaCl all the way to NaClO4 is a bad for your expensive Pt anode.

By the way, I don't understand the demi water thing, especially if you use cheap KCl salt. It's full of 'things' other than KCl so whats the point in using ultra clean water when you are gonna pollute it massively.

[oldmanbeefjerky]

I agree. But i think, and this is just a rough guess, that there are salts like fluorides and such sitting in tap water which will slowly poison the anode. such salts are not often present in potassium chloride or sodium chloride, hence, it is safer and in rare cases, you can get many unexpected salts and minerals in your unsuspecting tap water by sheer chance.where i live the a tree has accessed the pipe for a certain tap, though now fixed, last year, whenever i wanted water from the front corner of the yard to fill my dog waterbowl up, i had to wait 30 seconds because after 10 seconds in the water would turn brown and mucky for 20 seconds. and even so, the MSDS which MUST be accesible for that product, will tell you whats in it. essentially making the contents of tap water unknown.

 

You know its funnny when you think about it but, if you want water for your cell and dont want to buy distilled water, just leave a bucket out in the rain, and there it is! clean pure demineralized (if you live in a place free of acid rain) water!

[Mumbles]

Being able to exclude calcium would be enough for me to use demineralized or preferably distilled water for my cell. Calcium chlorate, while not as bad as something like ammonium chlorate, is in that same sort of ball park. It is noted for being more sensitive than would generally be desired. Plus it just makes sense to introduce as little contaminants as possible, even if you're already getting a decent amount from KCl.

[WSM]

I agree. But i think, and this is just a rough guess, that there are salts like fluorides and such sitting in tap water which will slowly poison the anode. such salts are not often present in potassium chloride or sodium chloride, hence, it is safer and in rare cases, you can get many unexpected salts and minerals in your unsuspecting tap water by sheer chance.where i live the a tree has accessed the pipe for a certain tap, though now fixed, last year, whenever i wanted water from the front corner of the yard to fill my dog waterbowl up, i had to wait 30 seconds because after 10 seconds in the water would turn brown and mucky for 20 seconds. and even so, the MSDS which MUST be accesible for that product, will tell you whats in it. essentially making the contents of tap water unknown.

You know its funnny when you think about it but, if you want water for your cell and dont want to buy distilled water, just leave a bucket out in the rain, and there it is! clean pure demineralized (if you live in a place free of acid rain) water!

 

I use an RO (reverse osmosis) system in the house to purify the tap water for drinking and cooking, and when I tested it, it removed more than 95% of the dissolved solids in that water. I use the same water in my system and it works fine. It doesn't cost near what distilled water from the store costs (though I have some for special projects). As for the contaminants in the KCl softener salt, I'm not as worried as I would be if I didn't realize that nature cures the problem by crystallizing. Crystallization is nature's way of purifying compounds (not perfectly, but good enough for our purposes).

 

If your rain water is pure, keep the buckets covered till it starts to rain or they'll be full of dust, debris and who-knows-what. I think you'll be okay.

 

WSM

[oldmanbeefjerky]

I wont need to worry about dust. in the wetseason here, it rains everyday same time, so much so i could set my watch to it. the rain is so heavy that i could hold my cell container out from under my shade cover for 1 minute and it would fill up, not with the water washing off the cover but witht he actual rain it is that heavy.

 

Though for those of us withiut such regular heavy rain, that is a wise decision

 

 

[Bonny]

I'm going to have to give my mill and media a good thorough scrubbing and cleaning and the chlorate a good dessication before i mill it down into powder (lucky i have plenty of sodium hydroxide "lyeing" about ), i wonder how fine i should need to go? super fine dust or just icing sugar fine?

 

Get another jar plain and simple. The risk of having sulfur mixed with the chlorate (and milling) easily outweighs the cost of another cheap jar.

 

Did you wash and purify (recrystallize) the chlorate first? It should be cleaned and neutralized (ph). That is the first step BEFORE using, to remove any chloride and/or whatever could be trapped in there.

[oldmanbeefjerky]

Get another jar plain and simple. The risk of having sulfur mixed with the chlorate (and milling) easily outweighs the cost of another cheap jar.

 

Did you wash and purify (recrystallize) the chlorate first? It should be cleaned and neutralized (ph). That is the first step BEFORE using, to remove any chloride and/or whatever could be trapped in there.

 

 

Im getting around to recrystallizing the chlorate, but i thought i should wait until after my next batch before i do that. i have found when crushed the crytals feel slightly moistend.

First though i need a pot of somesorts strictly for boiling chemicals. i am stuck as to what kind i should use. though i aim to get a pyrex glass pot or a proprly enameled pot. the better question is which of the two can i find

[Bonny]

Im getting around to recrystallizing the chlorate, but i thought i should wait until after my next batch before i do that. i have found when crushed the crytals feel slightly moistend.

First though i need a pot of somesorts strictly for boiling chemicals. i am stuck as to what kind i should use. though i aim to get a pyrex glass pot or a proprly enameled pot. the better question is which of the two can i find

 

 

I (think) a GOOD QUALITY SS pot will work. I use pyrex cooking pots. Go to a second hand store and have a look. You could probably find a few other useful utensils there too.

[oldmanbeefjerky]

Thanks for the reminder, i almost completely forgot about the OP Shops for getting pyrex

[oldmanbeefjerky]

LASERRED is selling MMO mesh again, just thought i should let you all know!

 

I am going to buy some now explicitly for the purpose of reselling them with titanium connectors attached. There's something about his mesh that just makes me euphoric! I hope he isnt sprinkling them with crack

because the moment i saw the listing in ebay i was compelled to by two sheets without even thinking. but it was money well spent in my opinion!

Now i just need more titanium plates...............

[pdfbq]

Being able to exclude calcium would be enough for me to use demineralized or preferably distilled water for my cell. Calcium chlorate, while not as bad as something like ammonium chlorate, is in that same sort of ball park. It is noted for being more sensitive than would generally be desired. Plus it just makes sense to introduce as little contaminants as possible, even if you're already getting a decent amount from KCl.

I understand what you are saying but when you buy cheap KCl you have no clue what's all in there, it can contain lots of CaCO3, at least that is what I think.

 

I have a question: Is Ca(ClO3)2 in small amount in solution dangerous? When making perc one has to destroy the NaClO3. I guess you'll destroy the Ca(ClO3)2 as well then but I'm not sure.

Edited August 30, 2011 by pdfbq

[oldmanbeefjerky]

i know very little about calcium chlorate, but form what i do know. its easier to remove form solution that would be potassium or sodium.

calcium chlorate will readily exchange its chlorate ion or a carbonate ion. so just add in a bit of potassium or sodium carbonate solution and problem solved.

after that filtration will cleans your cell of calcium.

 

i think i heard of a method somewhere in a txtfiles entry on a the complex sciences of chlorates. i got bored and ignored it mostly, but it did say ,you can remove calcium and lead in a similar manner by using sulfuric acid and perchloric acid, which apparently will only target the calcium and lead compounds, but it sounded a little off, so i stoppped reading, plus i got bored and was looking for quick ismple methods of making chlorates (at the time i was 14 and had no idea about science or anything, i still thought CO2 plus water made sulfuric acid, and that sulfur carbonate was used in stink bombs)

[WSM]

i know very little about calcium chlorate, but form what i do know. its easier to remove form solution that would be potassium or sodium.

calcium chlorate will readily exchange its chlorate ion or a carbonate ion. so just add in a bit of potassium or sodium carbonate solution and problem solved.

after that filtration will cleans your cell of calcium.

i think i heard of a method somewhere in a txtfiles entry on a the complex sciences of chlorates. i got bored and ignored it mostly, but it did say ,you can remove calcium and lead in a similar manner by using sulfuric acid and perchloric acid, which apparently will only target the calcium and lead compounds, but it sounded a little off, so i stoppped reading, plus i got bored and was looking for quick ismple methods of making chlorates (at the time i was 14 and had no idea about science or anything, i still thought CO2 plus water made sulfuric acid, and that sulfur carbonate was used in stink bombs)

 

That's right, industry used to remove calcium chlorate by addition of dilute sulfuric acid, which will turn the calcium in solution to calcium sulfate (gypsum) which is insoluble and drops out. It is then filtered out and the remaining solution is calcium free. If you already have perchloric acid, making potassium perchlorate is trivial (react it with an appropriate potassium salt in solution and the potassium perchlorate crystallizes out). It's easier than making it electrolytically.

 

WSM

 

edit.: A solution of potassium sulfate should do the same thing without having to handle the corrosive acid.

Edited August 30, 2011 by WSM

[hillbillyreefer]

My cell is outside, over the last week our ambient temperatures have been swinging 15-25C daytime to night. In the mornings there is a heavy buildup of crystals on the electrodes. I've been pulling the electrodes out, scrapping them off and starting the cell back up. I have not been diligent in watching the cell temperature, but last night it was at 36C this morning 27C. I'm estimating around 75g of chlorate on the electrodes. Edited August 30, 2011 by hillbillyreefer

[oldmanbeefjerky]

ooh, nice!

fortunately i have been blessed with constant tempuratures of 28-30 all through the day and night.

Though without AC, it is a curse!

Edited August 30, 2011 by oldmanbeefjerky

[WSM]

My cell is outside, over the last week our ambient temperatures have been swinging 15-25C daytime to night. In the mornings there is a heavy buildup of crystals on the electrodes. I've been pulling the electrodes out, scrapping them off and starting the cell back up. I have not been diligent in watching the cell temperature, but last night it was at 36C this morning 27C. I'm estimating around 75g of chlorate on the electrodes.

 

I wonder if bubbling air though the cell wouldn't stir things up enough to keep the crystals from collecting on the anode? It might be worth a try.

 

WSM

[oldmanbeefjerky]

I suppose that might work, but it might leech additional chlorine from the cell.

 

in my opinion, there should be a structure of somesorts in the cell for the chlorate to grow on, something that will be more favourable, but what could it be made of?

[hillbillyreefer]

<br />I wonder if bubbling air though the cell wouldn't stir things up enough to keep the crystals from collecting on the anode? It might be worth a try.<br /><br />WSM <img src='http://www.amateurpyro.com/forums/public/style_emoticons/default/cool2.gif' class='bbc_emoticon' alt='' /><br />

<br /><br /><br />

 

It would probably work. I kind of like it, it gives me a bit of Chlorate to experiment with. I love instant gratification.

[oldmanbeefjerky]

well i think ill try it on my next batch. i Have a 3v pump laying about here somewhere, and my cell is currently dissolving its absolute maximum capacity.

 

------edit-------

Ive found it and i dont think i like how fast it is bubbling air through the cell, im going to have to be very careful about how i seal up the hole the tube is going through to make sure the seal doesnt break so that the second vent tube is still going to be venting away all the unfriendly gasses, and that they arent simply going to leak away through the gaps.

 

It is also rather noisy too, so im either going to have to sound proof it the way i did my old ball mill which was putting it in a box and cover with blankets , or im going to have to run it once an hour for 15 minutes run the pump by timed relay.

neither of which i look forwards to, but find is completely necessary to run my cell without stopping half way to clear the built up chlorate before continuing

Edited September 1, 2011 by oldmanbeefjerky

[WSM]

well i think ill try it on my next batch. i Have a 3v pump laying about here somewhere, and my cell is currently dissolving its absolute maximum capacity.

------edit-------

Ive found it and i dont think i like how fast it is bubbling air through the cell, im going to have to be very careful about how i seal up the hole the tube is going through to make sure the seal doesnt break so that the second vent tube is still going to be venting away all the unfriendly gasses, and that they arent simply going to leak away through the gaps.

It is also rather noisy too, so im either going to have to sound proof it the way i did my old ball mill which was putting it in a box and cover with blankets , or im going to have to run it once an hour for 15 minutes run the pump by timed relay.

neither of which i look forwards to, but find is completely necessary to run my cell without stopping half way to clear the built up chlorate before continuing

 

One method used to encourage better fluid movement within the cell is to design it with tall, narrow electrodes that will stir the cell naturally with "hydrogen lift" as the cell runs. Another help is to leave a 100mm to 150mm air gap above the liquid in the cell to help things vent and settle before they leave the cell. Of course. this idea works better in larger cells with a lot more activity.

 

I'm using an aqurarium air pump for the air bubbler. They are typically fairly quiet because they're designed to run indoors where folks don't need any extra noise. A bubble stone or something similar would help break up the big bubbles to smaller, more gentle bubbles to stir things up. It would be ideal if the air being pumped was as warm as the mother liquor so cool air wouldn't promote crystal growth on the end of the air tube, and jam it shut.

 

Just some thoughts...

 

WSM

[hillbillyreefer]

Ambient temperature this morning was only 5C, the cell has cooled to 15C. The buildup on the electrodes has been decreasing since it first started cooling. I assume because the saturated solution, is much less dense, since the cell has cooled by 20C. the weather is supposed to warm up by about 12C over the next couple of days. It will be interesting to see what happens. An insulated cell ma be needed.

[oldmanbeefjerky]

One method used to encourage better fluid movement within the cell is to design it with tall, narrow electrodes that will stir the cell naturally with "hydrogen lift" as the cell runs. Another help is to leave a 100mm to 150mm air gap above the liquid in the cell to help things vent and settle before they leave the cell. Of course. this idea works better in larger cells with a lot more activity.

 

I'm using an aqurarium air pump for the air bubbler. They are typically fairly quiet because they're designed to run indoors where folks don't need any extra noise. A bubble stone or something similar would help break up the big bubbles to smaller, more gentle bubbles to stir things up. It would be ideal if the air being pumped was as warm as the mother liquor so cool air wouldn't promote crystal growth on the end of the air tube, and jam it shut.

 

Just some thoughts...

 

WSM

 

oh i wont be worrying about the hose getting jammed. i already know how i am going to tackle thta problem, and that is that if i am going to leave it running continuously , i am going to make sure the tip of the hose is never actually submerged in the water.

i am going to put the tube pointing down, through a fat sealed peice of pvc, and it will catch the air keeping the tube out of water. also, because the air is going from a small tube to a big pipe (figuratively) pressure will be able to build up, in there should the chlorate somehow magically block the pvc pipe section. the pressure will build up and the air will force off the crystals.

WSM, do you actually use a bubbler stone? i was considering getting a new bubbler stone anyway soon, since i need to keep my live bait alive longer when fishing (its a portable aerator) and that i could use it in the cell. but i decided not to since i thought that it would be eaten away by the chlorate cell, or do they work?

If my current plan failes, i do like to have a backup.