chlorate cell ?'s

[kiss]

Sorry for starting another thread on this subject, but the other chlorate thread has alot of info on elctrode material, cell body ect. At least the majority of the 30 something pages that I've read so far.

I have a small 600ml cell that has been running for roughly 4 and half days now. The solution contained within is jet black from the graphite anode/cathode. The cell when operating does not get very hot. Abit warm maybe...like a fresh brewed cup of coffee. My solution level after running for 4 and half days is roughly 550ml-500ml.

I'm thinking on moving on to the next step in the process, which would be to boil the solution for 15min. However since I have so little solution i'm abit worried that I might boil away the majority of my stock.

Would it be ok to add a small amount of water to this? If so how much water would be ok?

Some of the video's that I've watched on chlorate production using graphite show black sludge on the bottom of the cell. I'm not sure if i have this sludge or not. If I do, should this sludge be trashed, or thrown in with the boiling solution?

thx guys

[anapogeetoofar]

The black sludge is mostly graphite, you DON'T want that. Add more water, filter out the black crap, THEN boil. See the link below for more.

 

link

[ausgoty]

I suspect that when you turn the power off and let it cool down, you will see kclo3 crystals start to form and sink to the bottom.

 

My process is to let it cool right down, decant the electrolyte (you should have a layer of blackish crystals and graphite in the bottom), wash at least once (to remove any resiual chloride) by just covering the crystals in water and sloshing around. Decant again.

 

Now I add boiling water until it just disolves (needs a big pot sometimes), then boil for 10 or 15 mins. Pass this solution through a good filter to remove the graphite and you will have a lovely clean chorate solution. Evaporate this for the final product.

 

I don't usuall bother doing much with the initial electrolyte as it just goes back in and anything left comes out in the next run.

 

Have fun! Sounds like a pian but well worth it, especially if a kilo of chlorate is the end result.

[kiss]

A Kilo!!! Wow....I don't think i'd feel safe with that much. I'm a noob to this hobby so...

Well I think I've gone through the entire internet looking for anything chlorate related. I thought I've done this already, but I guess since it's go time I'm alittle concerned...ya know?

As it stands I filtered the electrolyte through 2 pre-wetted coffee filters 2x then added abit of water..(roughly 250ml), and boiled this for 20min. I then let it cooled just a tad, and then ran it through 2 more coffee filters upon the solution was very clear with a slight tint of yellow. At this point I took some kcl and made a saturated solution with water, and added vol. for vol. with electrolyte. I let this sit on my window sill for about 10 min. When i came back i notice small ...(very small) white particals scattered on the bottom. I wasn't sure if this is what i'm after or not, but i then put my jar in the fridge. Well it's been about an hour now sitting in the fridge, I'm not sure what the temp is...(to take a guess ..I'd say somewhere around 60f), but now I'm seeing very clear, flat, IMO large flake's piled on top of one another about an inch high on the bottom of a 1qrt. mason jar. My thinking is this is it! This is the stuff I've been reading about for the past month.....KCLO3! I'm sure it need to be cleaned up though.

Or perhaps this is something all together diffrent. If thats the case then no big deal. I think I've still learned alot, plus i can try again.

Now...if this does turn out to be the real deal, then i will start to take notes, and be much more precise with up coming runs.

I'll take some photo's when the camera is ready, you can tell me what ya think of this.

How long should this stuff stay in the fridge before i put it in the freezer?

[ausgoty]

A Kilo!!! Wow....I don't think i'd feel safe with that much. I'm a noob to this hobby so...

Well I think I've gone through the entire internet looking for anything chlorate related. I thought I've done this already, but I guess since it's go time I'm alittle concerned...ya know?

As it stands I filtered the electrolyte through 2 pre-wetted coffee filters 2x then added abit of water..(roughly 250ml), and boiled this for 20min. I then let it cooled just a tad, and then ran it through 2 more coffee filters upon the solution was very clear with a slight tint of yellow. At this point I took some kcl and made a saturated solution with water, and added vol. for vol. with electrolyte. I let this sit on my window sill for about 10 min. When i came back i notice small ...(very small) white particals scattered on the bottom. I wasn't sure if this is what i'm after or not, but i then put my jar in the fridge. Well it's been about an hour now sitting in the fridge, I'm not sure what the temp is...(to take a guess ..I'd say somewhere around 60f), but now I'm seeing very clear, flat, IMO large flake's piled on top of one another about an inch high on the bottom of a 1qrt. mason jar. My thinking is this is it! This is the stuff I've been reading about for the past month.....KCLO3! I'm sure it need to be cleaned up though.

Or perhaps this is something all together diffrent. If thats the case then no big deal. I think I've still learned alot, plus i can try again.

Now...if this does turn out to be the real deal, then i will start to take notes, and be much more precise with up coming runs.

I'll take some photo's when the camera is ready, you can tell me what ya think of this.

How long should this stuff stay in the fridge before i put it in the freezer?

 

So you are going the sodium chlorate to pot chlorate route?

 

It is far easier to just electrolise a solution of kcl then the chlorate just drops out of solution as it is produced. No worries about sodium contanination that way either.

 

My procedure above is for processing an electrolised kcl solution, not too sure the best way to go about the nacl route. Sounds like you are ont he right track tho, the crystals you describe sound like kclo3.

[NightHawkInLight]

A Kilo!!! Wow....I don't think i'd feel safe with that much. I'm a noob to this hobby so...

Well I think I've gone through the entire internet looking for anything chlorate related. I thought I've done this already, but I guess since it's go time I'm alittle concerned...ya know?

You realize chlorate isn't dangerous on its own, just like any oxidizer it only becomes flammable when mixed with a fuel. You should however be very careful any time you use it. Comps made with chlorate are MUCH more sensitive than nitrate based comps. Black powder would be very unlikely to be ignited by a hammer blow, but any chlorate composition that I've ever used could be. Do not use it in fireworks until you have experience using nitrates and perchlorates in a hundred or more devices.

 

Also, do not even bring it into the same room with your other chemicals or you may contaminate them and make them more dangerous, or even worse, unpredictably dangerous.

[kiss]

Understood Nighthawkinlight...

So is this stuff safe for me to put into the oven to dry? Or should i let it sit out to do that?

[Ralph]

yes so long as you concider what its in carefully (use something like borosilicate glass) and not iron or aluminium (they may be oxidised) and if it starts to melt (I highly doubt would happen in an oven as this occurs at close to 400 degrees) you have it to hot

[NightHawkInLight]

Understood Nighthawkinlight...

So is this stuff safe for me to put into the oven to dry? Or should i let it sit out to do that?

I believe chlorate has a slight toxicity to it, but if I remember correctly it's not much. As far as whether or not it is in danger of igniting, it is perfectly safe. It will not burn on its own, even if you hold a torch to it. It's about as flammable as table salt.

 

Keep in mind that if you dry it in an oven, some particles may contaminate the oven and sensitize anything else that is ever dried inside. So overall it is worth taking the extra time to dry it outdoors or in a place other than your usual work area.

Edited September 30, 2010 by NightHawkInLight

[inonickname]

If you live in a damp or humid climate (or a cold one) then instead of leaving it outside you can use a sealed container with a desiccant such as magnesium sulphate. If set up well it will dry in no time. Squeeze it dry in some kitchen paper towels first, which will get rid of a lot of the water. Misting some ethanol over it will also speed up the drying time. A water/ethanol mix is much more volatile than pure water, and will dry quicker. Lastly, you could set it under a lamp to dry.

[kiss]

UPDATE:

Well it's been afew days since my lasy post on this subject, so let me fill ya in.

I put the xtals in a pyrex baking dish and tossed it in the oven for about an hour on 200f. Watching this like a hawk...mind you! Afterwards it was pretty easy to see what was dry and what wasn't. Once this cooled to room temp., i coverd with a paper towel and afew rubberbands. Today i decided to scrap up the xtals with a plastice spoon, and put it on my scale. The total came in at 28grams. It's not a hugh amount, i know. But I started thinking as to why so little. True the cell was running for roughly 4 and half days, but i didn't mention that i would shut the cell off and clean the electrodes before going to work. So in a nutshell...at roughly 6pm i would turn the cell on, and then shut it off around 7am. I did this for 4 days. On the 4th day ...(somewhere in the middle), i decided to start with the boil. So i'm calling it 55hr of total time the cell was operating. Is 28g ok for this amount of time?

 

I'm kinda scared having this stuff. I guess it was the challenge that kept me going. To see if i could ya know? I'd much rather be dealing for perchlorate for the safty side of things. It's been a great learning exper., but i guess it's just to incompatiable. Not alot of uses. I made a one gram batch of H3...(70/30....KCLO3/W.pine char.) I didn't grind the KCLO3 very well. I'm not sure just how much abuse it can handle. But the charcaol is like dust! Out of this one gram batch i made very small piles, and ignited them on a stone plate.

Some of these piles lit-up with ease, while others were just a tad stubborn. Could this be from not grounding down the KCLO3 enough?

I noticed it burns with xtreme light! Red in color...this ok too?

 

 

[Arthur]

Have you read the whole of http://oxidizing.110mb.com/chlorate/chlorate.html and have you read the whole of Swede's blog on here. Both are complimentary reading and both very reliable and accurate. LOTS of research in literature and LOTS of practical work has gone into each of these resources, which have been willingly offered to the web community by their authors.

 

"In a typical Amateur cell you will get 0.00596 grams Chlorate formed per minute per Amp. "

[WSM]

I'm kinda scared having this stuff. I guess it was the challenge that kept me going. To see if i could ya know? I'd much rather be dealing for perchlorate for the safty side of things. It's been a great learning exper., but i guess it's just to incompatiable. Not alot of uses. I made a one gram batch of H3...(70/30....KCLO3/W.pine char.) I didn't grind the KCLO3 very well. I'm not sure just how much abuse it can handle. But the charcaol is like dust! Out of this one gram batch i made very small piles, and ignited them on a stone plate.

Some of these piles lit-up with ease, while others were just a tad stubborn. Could this be from not grounding down the KCLO3 enough?

I noticed it burns with xtreme light! Red in color...this ok too?

 

 

Hi Kiss,

 

There are many uses for chlorate but they depend on judgement and skill. No need to be afraid of it, just learn its nature and respect it. The crystalline potassium chlorate can be handled like any other pure salt; you can grind or mill it with no great concern. The operative word here is pure. if certain substances are present, chlorates can/will become friction/impact sensitive. This is where chlorates got their bad reputation.

 

Chlorates really shine in the hands of skilled pyrotechnists when used for color stars and are known for brilliant colors and large flame envelopes. The best smoke compositions utilize the low ignition temperature and cooler burning rates of chlorate to perform correctly in not destroying the smoke dyes. H-3, when mixed with NC lacquer, can be used for the pyrogen base of electric matches very well. The list goes on and on.

 

If you are careful not to let any contaminants get into your chlorate, go ahead and grind or ball-mill your chlorate crystals to powder. Never grind or mill a chlorate mixture, but chlorate by itself should be okay.

 

The "red" color may be from the violet spectral emissions from the potassium. I, too, have noticed that in burn tests of chlorate mixtures. It sounds like you've got the right stuff. Try letting your cell run 24 hours a day without interruption; it will be happier.

 

WSM

Edited October 4, 2010 by WSM

[Arthur]

Please think carefully about the used filter papers, paper saturated in chlorate will be quite flammable. Look out Whatman GF A It's a glass fibre filter "paper", But it really doesn't like being folded so a buchner funnel is best.

[patsroom]

I truly do not wish to start a new thead in chemistry. But I have a burning question.

I know that lead dioxide anode is used in producing perchlorate , but there is a site that says they have Lead oxide anode for perchlorate producing. I wonder if they mean dioxide or can lead oxide make chlorate/perchlorate?

I know this is just a little bit over the subject matter here but I think that this is the most current veiwed site on the subject to production cells.....Pat

[patsroom]

Well I did manage to contact the site I was talking about. It was a mis-print and should have been PbO2 anodes on Ti mesh, so I just decided to order 5 of them will sent them the payment tomorrow as we got the price down a little from last years dealing with them..... We well see how it goes.....Pat

[kiss]

Well i've been away for a few days, but during my time away, i've managed to re-xtalize my kclo3. I lost abit of the weight, but the return product looks like window glass clear! This may sound abit strange, but i thought the stuff wasn't going to get much cleaner, after watching it in the fridge. However the xtals are wickedly clear this time around.

I've been messing around with very small batches of H3...(i make up 1gram and sepperate).. and i'm not overly impressed! Very bright burning, but somehow not as fast as i thought it would be. Maybe i'm watching to many flash powder clips? I don't see this being used for lift, but what do i know. I'm sure if it were to be contained then that would be another story. Any ideas, or thoughts?

Patsroom--- Keep us informed on your progress.

[WSM]

If you are careful not to let any contaminants get into your chlorate, go ahead and grind or ball-mill your chlorate crystals to powder. Never grind or mill a chlorate mixture, but chlorate by itself should be okay.

 

 

Hi Kiss,

 

When I said the above statement, "Never grind or mill a chlorate mixture", I mean a mixture of chlorate and a fuel. In rereading it I saw how that could be misunderstood. Chlorates can be milled with compatible salts or fillers without concern, but please do your homework and be sure the candidate materials are indeed compatible, first. We wouldn't want you to learn they weren't compatible "by accident" !!!

 

WSM

[kiss]

Hey... i understood what you ment. But thanks for clearing that up.

Well i found a pretty decent method of grinding this up. I still don't own a ballmill....(have all parts needed though....accept TIME), so i used the good ol' method of the druggies. Lay-out a peice of paper and put kclo3 on top, and then another paper, and used a large socket to roll/push, crush, ect. Comes out like dust! Since i've started using this method i've noticed a VAST improvment of my H3 comp. Still doesn't seem to be as fast as flash powder, but pretty darn close Now this stuff seems like lift powder. Ignites much better and alot more consistant too. To be honest i'm pretty surprized at how much grinding it down has that much of an effect. Not to sound lame....I know it would have a big effect of course, but i just didn't think it would be like this. It's a night and day diffrence!

I made a couple of 1 and a half gram salutes, that turned out nice. Not a hugh booming force but certainly enough to grab attention. I gave myself a pat on the back, for my victory. This comp. is so basic...(IMO), that it lends itself,...almost begs to be made. With the exception of the goofballs who would only abuse it.

Speaking of goofballs....

I have to admit that i did mix-up a small 1 gram batch w/ roughly 4-5% of sugar added. What i noticed right away was the ignition was VERY easy. I guess you would call this as being more sensative(sp?). If you don't know....when i mix-up my small 1 grammers, i sepperate it further for testing. ergo,...1 gram would give me roughly 15 small piles that i use to play with. Just to see how things work out. Now that i'm grinding in this matter i don't think i'll be using sugar again. After 35 years, i kinda fell in love with my fingers ya know? They fit me just perfect.

I have my cell running again. This time around i started directly with KCL. I'm not so sure it was a good thing or not. Using KCL has shown me my flaws in my cell through the salt build-up around connections, ect. Sodium Chloride doesn't do this, but hey...I guess it's better know anyway.

Sooner or later i will get around to posting some photo's.

[patsroom]

The anodes are here today 4 inches x 4 inches square. They look good. I think I will sell the one I do not need.

picture 3.BMP

Edited October 13, 2010 by patsroom

[bikemaster]

Wow!

What was the price?

I am waiting to see what will be their performances!

[patsroom]

Wow!

What was the price?

I am waiting to see what will be their performances!

 

 

I am thinking about $55 USD plus shipping and handeling

I am hoping to get Swede help soon to test for me if he would?

 

Mumbles this is the wrong place for this discussion I'm sorry I will move to the other forum when I can

(The Agora).If you need, go ahead and delete this one I would understand.........Pat

picture 4.BMP

Edited October 14, 2010 by patsroom

[Updup]

I am thinking about $55 USD plus shipping and handeling

I am hoping to get Swede help soon to test for me if he would?

 

Mumbles this is the wrong place for this discussion I'm sorry I will move to the other forum when I can

(The Agora).If you need, go ahead and delete this one I would understand.........Pat

 

 

Those look pretty nice! Also, Have fun hunting!

[WSM]

I'm looking forward to hearing how these LD anodes hold up in practice. I rather pay a few bucks than jump through detailed plating hoops if I don't have to. Can we get these LD anodes on a continual basis or are they a one-time deal ?

 

WSM

[Bonny]

I'd also be interested as my experience with Pt anodes has been ...mixed. made some perc, but cooked the anodes, and they are pricey.