Making Potassium Chlorate

[mrjeffy321]

I am trying to make some Potassium Chlorate (KClO3) by reacting bleach (NaOCl) with Potassium Chloride (KCl). I got this idea from this site:
http://www.fryingcolors.com/kclo3.html
I am trying to do the first method using the NaOCl and KCl.

I have followed the steps, kind of, and ended up with a dark browish percipitate. this is odd, since the reaction for this should yeild Potassium Chlorate, a white powder.

NaOCl (aq) + KCl (aq) --> NaCl (aq) + KClO3 (aq/s?)
add Potassium Chlorate to boiling/almost boiling bleach and get sodium chloride and Potassium Chlorate.

to save you some reading on the linked site, i'll tell you how it should be done, and then how I did it.

How it should be done:
-bring bleach to almost boiling (instructions say 1 gallon)
-add the Potassium Chlorate (instructions say 63 grams)
-continue to let it react untill you get it to a specific gravity of around 1.3 (as measured by a hydrometer)
-let it cool, put in refrigerator and let the Potassium Chlorate crystalize
-filter out the crystals
-repeat steps again with remaining liquid to be sure everything reacted
-then add the stuff you get out of the filter to distilled water (instructions say 56 grams/100 mL water)
-boil new solution
-evaporate the water, and collect the Potassium Chlorate

How I did it:
before I started, I decided to work out this reaction on paper, and the theoretical amounts of each substance i needed, so i based my figures on that, but even if i dont get a compleate reaction, i should still get something
-bring bleach to almost boiling (I used just over 1 liter of 6% bleach)
-add the Potassium Chlorate (i dont know any more how much I used)
-continue to let it react untill you get it to a specific gravity of around 1.3 (well I had a hydrometer, but I dont think it is very accurate, so i let it sit there for a long while, untill I was pretty sure it had reacted all it was going to do, but the number [approx.] I was getting on my hydrometer was 1.15)
-let it cool, put in refrigerator and let the Potassium Chlorate crystalize
-filter out the crystals
-repeat steps again with remaining liquid to be sure everything reacted

I am currently at this step, I havent gone this far yet

-then add the stuff you get out of the filter to distilled water (instructions say 56 grams/100 mL water)
-boil new solution
-evaporate the water, and collect the Potassium Chlorate

I dont know how much of a diference these last 3 steps will make, but I doubt that they will take my dark brown stuff and make it into good 'ol Potassium Chlorate, (unless im wrong, i dont know)
also, the vapor that is comming off this liquid solution while boiling and going out the exhaust suction, some of it is condensing around the grill plate and it is becomming a whitish powder, but then when I go to wipe it up, it looks much more yellowish on the paper towl I use, what is this stuff, in theory the only thing to evaporate in this reaction is water which last time I checked wont leave a residue behind.


I just though that maybe someone here could offer me insight into what is happening and, what should be happening.


just so you guys arent worried (to much) about my safety while doing this [this seems to always come up when I do something dangerous (thermite)] I will tell you that I know what Potassium Chlorate is capeable of, and I am doing the boiling with a ventalted exhaust near by, I wont be eating any of this either.

[chem_tr]

Hello, I will only discuss the redox chemistry of the reaction, maybe the reaction needs reviewing.

Cl+ + 2e- ---> Cl-
Cl- ---> Cl5+ + 6e-
------------------
3ClO- + Cl- ---> 3Cl- + ClO3-

We may even simplify it by subtracting the chlorine on the left:
3ClO- ---> 2Cl- + ClO3-

So, you should check the concentration of bleach; as you see in the redox reaction, three moles of bleach is needed to produce one mole of chlorate. Also, brown precipitates don't seem normal, please check the purity of your substances. Use distilled water as much as possible. If there are particles in your starting solutions, don't let them interfere with your business, just filter them off.

I haven't checked your concentrations, since we use SI units in Turkey, I am not familiar with gallons, etc.

Regards,
chem_tr

[thunderfvck]

http://www.wfvisser.dds.nl/EN/chlorate_EN.html#therm_starting

Check out that link and try using his procedure instead.

I'm inebriated at the moment so I'm unable to see why your procedure is wrong.

But assume that the link I provided will give you a procedure that WILL work (the guy who made the site is highly respected).

[Azrioch]

I'm inebriated at the moment so I'm unable to see why your procedure is wrong.


haha
:rofl:

[Gokul43201]

We really can't say much about the quantitative aspects for 2 reasons :

1. We don't know how much you've used (we could tell you how much to use, but it seems you've already figured this out)

2. Like you said, the problem seems to be not about how much, but rather about , "what the #$%^ is this brown/yellow stuff and where did it come from ?"

Okay, here's my five cents :

1. Do you buy KCl from a Chemical Supply or do you use some kind of Lo-salt ? If you buy from a chemical supplier, they might just sell you KClO3. If you use LoSalt, you might want to check on the other components. Most LoSalt is only about 70% KCl, so there's lots of other stuff.

2. There may be impurities from water or bleach. Why don't you use sodium chlorate (weed killer) instead of bleach ? I'm sure that's the more common approach.

3. Have you tried a basic flame test on your brown precipitate and your yellow condensate ? If you see colors other than lilac, that's a strong indication of impurity. Incidentally, potassium hypochlorite is a pale-yellow salt. Often, a little salt can be carried away by the steam ...depending on the size of the crystallites/particles - especially with vigorous boiling.


{Hmmm...first the thermite, then potassium chlorate. The word that comes to mind - pyrotechnics. I hope it's nothing more sinister than that.}

[mrjeffy321]

Procedure when using sodium hypochlorite
It is assumed bleach will be used, which is usually a 4% solution of sodium hypochlorite in water. If a less or more concentrated solution is used, adjust the amounts accordingly.
1. Take 1 liter of bleach, and place this in heat resistant glass or stainless steel container. Bring it to a boil.
2. Boil the solution untill only about 140 ml of solution is left. The exact volume is not critical, a deviation of 10 to 20 ml is acceptable.
3. Allow the solution to cool. If crystals form upon cooling, filter the solution after it has completely cooled. The crystals are sodium chloride and can be discarded.
4. In a separate container, prepare a solution of potassium chloride. Dissolve 28 grams of potassium chloride in the smallest volume of water possible (about 80 ml). This can be done by dissolving the potassium chloride in about 90 ml of boiling water, and allowing it to cool. If crystals form, add some more water, boil again to dissolve the potassium chloride, and allow to cool again. If crystals form, repeat. If not, the solution is ready to use.
5. Mix the boiled bleach solution with the potassium chloride solution. A white precipitate should form. This is potassium chlorate.
6. Bring the solution to a boil and add water untill all potassium chlorate has dissolved.
7. Allow the solution to cool slowly. Crystals of potassium chlorate will form. Cool the solution to 0 deg C.
8. Filter to obtain the raw potassium chlorate. Rinse the crystals in the filter with ice-cold water. The product can be further purified as described below.

this procedure seems very similar to what I was doing, althugh the above procedure seems to need very concentrated solutions of both bleach and potassium chlorate, something that I am probably not getting close enough to.

I am getting my potassium chlorate from a salt substitute (walmart), but this isnt one of those reduced salt ones, this is suppose to be no sodium stuff.
and I am using bleach that starts out as 6% by weight.

I did try burning some of it, but I dont think anything happened, i just burned the remnents of it that I couldnt scrape off the filter, but i just think that the filter paper is what burned, not the brown stuff. I am now evaporating the water off the "cleaned" brown stuff, so once it is dry i will be done with all those steps, but I barely have anything to show for it.

[mrjeffy321]

actually, I think now I will try to do it the way that is in that link you gave me, with the high sconcentration solutions.

but I just cant figure out why I am getting some type of brown percipitate forming, could it be because I am not using a high enough concentration of something? or not getting it hot enough?
when I filter out the percipitate, I get (what looks like to me) a highly concentrated bleach solution, it smells like bleach and looks like bleach, just darker, and when I try to make more potassium chlorate using the same method with the "new" concentrated bleach, the same thing happens.

maybe I should incest in a good electronic hydrometer, not rely on the leaky, possibly broken, old battery hydrometer I had.

[mrjeffy321]

OK, last night I (tried) to make a very concentrated solution of Sodium hypochlorite, but I may have only partialy succeded.

I took about 1 liter of 6% chlorox bleach and boiled it until it was about at 200 mL, then as I was letting it cool, I added some tap water to try to redisolve some of this stuff that has come out of solution ( i dont know what exactly it is, possible sodium chloride?, or NaOCl that came out of solution?) then I let it cool some more. afterward I filtered the solution twice with a pair of coffee filters, an collected alot of dark k and some other stuff that could be sodium chloride (since I think when you heat the bleach, some of it becomes sodium chloride). so I now have a solution of around 300 mL of what should be concentrated bleach. I will describe the solution:
a dark yellowish color (similar to dark urin, especially when it was still warm)
it smelled like bleach

I didnt add anything else to the solution while it was heating, just let the steam evaporate away. the vapor comming off theoretically should be steam, H2O(g).

but all this brown stuff that was made is concerning me, what is it and why is it there? it is just like the stuff that I had when I was trying to make potassium chlorate the other way. and while boiling the bleach, it got very dark in color, almost pure black, a very dark bown, but then went back to the dark yellow when it cooled, leaving some type of percipitate.

[mrjeffy321]

Success, kind of

I have tried 2 trials, and I am preparing the 3rd trial now, here are my results:
trial 1 - used only a 6% blech solution and not very much KCl, I only get brown stuff
trial 2 - used much more concentrated bleach solution with much more KCl, and here I did get some KClO3 crystals, not much, but some
I tested to see if it was KClO3 by adding sugar to it and burning it, I couldnt get it to burn very easily without the sugar, but the flames resulting sure arent any regular sugar flames I have ever seen, very bright, light blue flames, burns very quickly.

trial 3:havent done yet - I will use MUCH more concentrated solution of bleach, and a saturated solution of KCl, so in theory, this should work best.
I wonder if I will need to heat the solution(s) to get them to react, or will room temerature work just as well? I probably will get fater, more compleate reults if I heat it.


Is there a point of maximum saturatation for bleach (NaOCl)?, were even if I try to get it more concentrated, I cant, i'll just be waisting my time?

[mrjeffy321]

OK, I am not totaly clear on how exactly I obtained this substance, my best guess would be from when I was making concentrated bleach and then filtered it to get the particles out, which I thought was sodium chloride but just for fun one night, I decided to test to see if it really was by trying to burn it with sugar like I did with the other stuff i had made, and to my surprize, IT WORKED. now I know this stuff just isnt sodium chloride anymore, and I think I got it from what was a relativly pure solution of what was bleach, I just filtered it out and dried it.
So now I have 2 substances, one I got in my "trial 2" described above using a more concentrated bleach solution and lots of potassium chloride and it burns with sugar to produce a white/light purple flame, so I would have to say that my first substance is potassium chlorate. my second substance I think I just got by heating up the bleach, getting it more and more concentrated and making more and more salt, then perhaps could the sodium chloride have reacted with the bleach and made sodium chlorate perhaps? my substance 2 burns with sugar to produce a much more yellowish flame.
(now remember these colors that are being described are my opinion of what color it is, which may be slightly flawed because I am color bind, but I other people who have witnessed my reactions describe the color similary)

I have looked up what color both sodium and potassium chlorate should burn like:

The most useful element in pyrotechnics that belongs in in the alkalies period is potassium. It is more common than lithium and does not produce a yellow flame like sodium. The strong sodium flame color easily washes out other and can contaminate other compositions to ruin them. The weak violet flame that potassium gives off is advantageous because it doesn't interfere with color production. It is rarely used by itself to produce purple, instead a mix of blue and red are used.


I have also video taped the 2 substances burning on my computer, it is kind of hard to tell colors though becuase of the brightness of the combustion, but someone might be interested in seeing it, but I cant attach it becuase my 1.2 Mb file it too large, so here is a link to it on a geocities page:
http://www.geocities.com/mrjeffy321/chlorates

[mrjeffy321]

well no one seems to be reading this, or at least responding, but I will keep posting my status, for a while anyway, it helps give me a chance to rethink some of this stuff while writting it,


When I was making my concentrated bleach solution, I boiled down over a liter and a half of bleach to around 400 mL, so it should be extreamly concentrated, in theory. well as it was boiling, it did as I expected, made that brown stuff, then I filtered it, then continued boiling and no more brown stuff was made. I am concluding that the brown stuff is the result of some type of reaction that is occuring in the 94% other in the bleach (6% sodium hypochlorite, 94% other, not all water I suppose).then once its gone, it is gone. then when it started getting lower, I started seeing large buildups of a white crust on top, and globs of a while powder at the bottom of the pan, ( assumed it was sodium chloride), so when I got done boiling it, I filtered out the "salt", then let it dry. later I decided, "hey, what the heck, i'll test the "salt" and try to burn it with sugar like I would do with the potassium chlorate, and to my surprize, it worked (like I told you all in an earlier post, I assume the "salt" is actualy sodium chlorate resulting from sodium chloride reacting with the sodium hypochlorate).
but now lets get back to the concentrated bleach solution, if you can call it that, since it exibits almost no bleach properties any more, it doesn whiten fabrics, it doesnt smell like bleach (it smells like something familiar, but I just cant place it), it doesnt react like bleach, as a matter of fact, the only 2 reasons I once though it was bleach are because it was made from bleach and it had a dark yellowish color. what I am thinking now is that while boiling, some/most of the bleach was reacted and made oxygen gas and sodium chloride, then intern, that sodium chloride reacted with the remaining bleach to form the sodium chlorate, but leaving the bleach color behind. if you havent watched the videos I put up, I encourage you to, although it is hard to tell colors because of the brightness of the flame, you can (and me especialy since I was right there) see the color diference in the 2 combustions. I have also tried to make more potassium chlorate with that concentrated "bleach", but was unsucessfull even using highly concentrated solutions of potassium chloride.

[mrjeffy321]

I have now made some chloate (potassium I guess) using the calcium hypochlorite method. i found it to b less labor intensive than the bleach method, becuase I started out with my solutions at the correct concentrations allready and I didnt have to boil down and destroy the stuff that I needed in the first place. but that method is harder, since I dont have a good supply of pool shock (calcium hypochlorite) and it seems to be more corosive on my pan that I used than the bleach was.


I think I will try to do the electrolysis method not, even though I will like that one the least, but technicaly it is the most efficient and less labor intensive of the three.

[Marijn]

Man, your persistant, that's for sure!

What are you going to use the stuff for?
fireworks? amateur rocket-engine?

[mrjeffy321]

actually, you just listed my two main things I want to do with it, general pyrotechnics fun and model rocket fuel.



Man, your persistant, that's for sure!

well, yes, but mainly no one is really responding anymore, I just use this a a place where I can recount my experiments, and by doing this I kind rethink them in my mind so I dont loose any details later if I forget, plus is anyone responds, thats good too! but that hasnt happened in a while, the last 7 posts were mine. and maybe later on, month or years from now, someone else can benifit from my experiences if they are trying to do what I am doing. if anyone would like to contribute, by all means, join in.

[mrjeffy321]

OK, this is actually a question, not just an update on what I am doing now:

using this page for a source of ways to make potassium chlorate,
http://www.wfvisser.dds.nl/EN/chlorate_EN.html#therm_starting
it disscusses an electrolytic method that uses sodium chloride as an electrolyte in water, and then runs a current though the water to turn the sodium chloride in to sodium chlorate (from NaCl to NaClO3) because of a lenght series of reactions that are explained on the page.

my question is, could I not just take bleach (Sodium hypochlorite, NaOCl) and electrolysize that, since it is allready in an aqueaus solution, therefore only needing to add 2 oxygen atoms to the compound, rather than the 3 atoms using the other method. (from NaOCl to NaClO3?)

I have found out that normal cloroz ultr bleach is composed of:
6.00% sodium hypochlorite (NaOCl)
5.63% Sodium chloride (NaCl)
0.015% caustic soda/sodium hydroxide (NaOH)

it seems like this reaction in question would be perfect to make sodium chlorate becuase it will require less time/energy to add only 2 oxygen atoms (rather than 3) and it contains sodium chloride aswell for the old reaction, and the .015% sodium hydroxide wont last long anyway once everyting gets started.

will this work?

[mrjeffy321]

I would very much like to know if my idea from above would work, taking a shortcut by electrolysizing bleach insted of salt water.

I know bleach can be made by electrolysizing saltwater, but cant you just keep on going and make sodium chlorate too?

[mrjeffy321]

I have went ahead and electrolysized the bleach, and here is what happened:

I let it run for about 20 hours to get these results,
the solution has lost its distinctive bleach color, it is now much more clear after being filtered to remove the gunk produced as a result of the elctrolysis process. it isnt totaly clear like water, but if you arent carefull, you can mistake it for water.
the smell, it has a chlorinated smell, similar, but somehow more chlorinated than bleach normally smells like (probably because of all that chlorine gas produced), but it isnt a stong a smell.
it has lost most of it's bleaching property on fabric, still will somewhat whiten fabric, probably becuase it isnt totaly finished electrolysizing.

other than that, that is all to report for now, still wished I knew what I should be expecting fromt this.

I think when doing this, the pH should rise throughout the process, and the pH starts out at about 11.4 anywar, but in order for me to get effective results, I think I need someone around 6. but in bleach production through electrolysis, you want a high pH, is it possible I could be making MORE rather than less bleach? but this wouldnt be likely because of my results.

[mrjeffy321]

I have answered my own question about whether it will "save a step" by electrolysizing an aqueus solution of sodium hypochloite (NaOCl) insted of sodium chloride (NaCl) to make Sodium Chlorate (NaClO3).
the Answer: No, although i will end up making the same thing in the end, since oxygen is made while electrolysizing the sodium hypochlorite electrolyte (and let to escape from the system), it takes away precious energy that could be used somewhere else, but is insted lost. When electrolysizing the aqueus sodium chloride solution, very little to no oxygen is made, energy more or less goes into making the chorate. If you go and calculate the theoredical energy need for both methods, the sodium chloride method would need something like 6 fardays/mole of chlorate, and with the sodium hypochlorite method, it is something around 9 fardays / mole of chlorate.



I have disscussed this with a diferent, more knowlegible, chemestry teacher, and she is under the impress that I am doing the impossible, what I am trying to do (and the results I am getting) should not be happening, and I understands why she thinks this, because all the stuff I am using to make gthe chlorate and the chlorate itself is soluble in water (some of the substances more than others), but she thinks that everything will end up being dissolved and I wont get anything to precipitate out. and yet, experimentally, I know that I infact do, and the stuff that does percipiatate out, has properties very similar to that of the chlorates that I am trying to male (sodium and potassium chlorate).

[mrjeffy321]

like i said above, the chemistry teacher I talked to doesnt think that what I am getting is really chlorate, but rather some kind of hydroxide(thats what she says), but I think I am actually getting a chlorate based on the reactions that I can produce with the stuff I get and all the "people"/souces that I have with similar instructions on how to make it.

is there anything that I can do to prove/test what I am getting to see what it is, if it is a chlorate or not? I thought that flame test with sugar was pretty good proof, especially with the distinctive colors I saw, but is there anything else?

[chem_tr]

You may have obtained a peroxide, as it helped burning. You can try treating the solid you obtained with hypochlorite, and if it is chlorate, all of them might be converted to chloride, easily detected with silver nitrate.

[mrjeffy321]

You may have obtained a peroxide, as it helped burning.
a peroxide, I never thought of that, i suppose it may be possible, but I quickly looked up sodium and potassium peroxide (dont need to look up hydrogen peroxide for obvious reasons) and they are a pale yellow color and a yello/orange color respectively, not the while/off white that I am getting.

You can try treating the solid you obtained with hypochlorite, and if it is chlorate, all of them might be converted to chloride, easily detected with silver nitrate.
I know anything about that, isnt it all ready in contact with the [sodium] hypochlorite when it is being made, therfore if anything is going to happen, it would have already happened?

[mrjeffy321]

I was experimenting with the electrolytic production method, trying diferent voltages, currents, finding the built in resistance of my chlorate cell, and after just a few minutes of opperation, I get this white percipitate that accumulated near the bottom.
at first I thought that this stuff was perhaps copper chloride, since there was a little bit of copper wire exposed to the water between my power source and graphite electrodes, so I thought that the chlorine was reacting with the copper to make copper chloride, which is very very insoluble and thus settles to the bottom, and copper chloride is white, just like my percipitate.
then I covered up the copper that was exposed (to the best of my ability) so that only the graphite was the stuff conducting the electricity into the water, again, after just a few minutes, I get the white percipitate still.

So could this stuff be sodium chlorate, the stuff I am trying to make in the cell?
sodium chlorate is highly soluble (100g/100mL), and I do seem to making alot of this percipiate in a shor period of time, but then again I am using alot of current (it varried, but is mainly between 1.2 and 2.7 amps at somewhere between 4.5 to 7.5 volts), so that might explain the speed of production. and the sodium chlorate has to compete with the virtually totaly saturated sodium chloride solution (36g/100mL), so maybe it is producing more sodium chlorate than it can redissolve in the amount of water that is being left "empy" from the usage of sodium chloride. the percipiate is hard to remove from the water, it is almost totaly usless to use a coffee filter, it will just pass right though, the only way I can clean out the water is to decant the clear water off and let the stuff settle out.

what could this stuff be?

[mrjeffy321]

the more knowlegible of the two chemistry teachers which I ask about this stuff told me, very quickly and confidently after she learned that I was using tap and not distilled water, that that white fluffy percipitate was some of the impurities reacting in the water, and it just may be so, I tried electrolysizing the solution for an hour (as compared to only a few minuted as before) and got no noticible increase in the amount of percipitate, so it could be that I used up all the impurities and now it is just a pure sodium chloride/ate/hpochlorate.. (and all that other stuff that goes on in the cell) solution, or i just didnt look hard enoug at it.

[mrjeffy321]

OK, I did the electrolytic method for a while, I was going good and then some stuff happened (ie. I spilled the cup :cry: and wierd stuff happened to the voltage and current that baffle me as to thier cause, ...). anyway, I eventually deci9ded that I would continue on with the next step, which is taking the sodium chlorate I had just made and transforming it into potassium chlorate. I did the steps, ...., and anyway I filtered out the crystals I got, and tested them using my ol' friend a lighter and sugar, and I get a yellow (and some green) flame, which leads me to believe that what I made was actually sodium chlorate in the end, not potassium chlorate, even though I did add the potassium chloride to the mix and boil it (for a long time). but because there was some green, I am thinking that the green resulted from a small amount of blue flame (from the potassium chlorate) mixing with some of the yellow flame (caused by sodium chlorate) and also alot of normal, unmixed sodium chlorate yellow flame. it is kind dissapointing how little I got from all this electrysis work and I even have the wrong stuff!'


One question I do have, the liquid I got out of my electrysizer was relatively clear and the potassium chloride mixture was the same clarity, when I mixed them together (you guessed it) clear. but after I boiled it, it got much yellower and greener, like the color of liquid bleach. why would this happen?

[pack_rat2]

KClO3 can be made by passing Cl2 gas through a solution of a K salt, or by the electrolysis of a KCl solution. Actually, it's NaCl that is normally electrolyzed to produce NaClO3. KCl is then used to precipitate the KClO3, which is relatively insoluble. You can't make it just by mixing a hypochlorite and a chloride.

[mrjeffy321]

KClO3 can be made by passing Cl2 gas through a solution of a K salt, or by the electrolysis of a KCl solution. Actually, it's NaCl that is normally electrolyzed to produce NaClO3. KCl is then used to precipitate the KClO3, which is relatively insoluble. You can't make it just by mixing a hypochlorite and a chloride.
I dont know how familiar you are with my epic tale of experimentation I gave walked everyone through with the last 2 pages of posts and several weeks, but I have just most recently compleated alot of work with the electrolytic method with disapointing results, I was successfull (in making sodium chlorate), but still dissapointing none the less, even though it is suppose to be a more efficient a more recomended method of production.
In fact you can indeed making chlorate by mixing hypochlorate and chloride, I have done it, it involves a lengthy process of boiling and mixing, ..., but that has been my most successfull method so far.

I have not tried the method involving the chlorine gas, the use of chlorine gas was kind of a turn off as an option, but as I become more experienced (or reckless depending on how you look at it) in my handling of dangerous/semi-dangerous materials, like chlorine, I might decide to try it.

[pack_rat2]

I did a little checking on different ways of making KClO3...the bleach method works, but it doesn't involve a reaction between hypochlorite and chloride (as I thought, and knew wouldn't work); it's a thermal decomposition of hypochlorite. The purpose of the KCl is to provide K+ ions to precipitate KClO3 from the NaClO3 solution. This URL has a lot of good info:
http://www.wfvisser.dds.nl/EN/chlorate_EN.html#thermal

[mrjeffy321]

yes, I have seen almost that exact same page, most of the time when I refer to a spep in the process, I am refering to the instructions on that page. Using those methods, I just seem to get the best results using the decomposition method.

to make the thermal decomposition reaction between the hypochlorite and the potassium chloride, I would think it woudl work better/more efficently if I had a more concentrated solution of both substances, but manily the bleach solution(since it starts out at only 6%), but if I try to "boil" off some of that water and make it more concentrated, the bleach will decompose and be useless to me.

[pack_rat2]

The NaOCl should be as concentrated as possible, I'd think. And the KCl concentration would be unimportant, since the Cl(-) doesn't participate in the reaction to form chlorate. The reason I say that is that Cl(-) has a full octet of outer-shell electrons. It's the most stable configuration for chlorine, and it's not going alter oxidation number easily (it can happen by electrolytic methods). It's the thermal decomposition of OCl(-) that produces the ClO3(-), and the addition of K(+) causes KClO3 to precipitate out.

[mrjeffy321]

well the concentration of KCl might be unimportant in the reaction, but if you have a less then concentrated solution of KCl, then whrn you add it to the NaOCl, it will dilute the sodium hypochlorite solution more than necesary, idealy you would not want to add any extra solvent than necesary.

perhaps a way to increase the concentration of the NaOCl, without decomposing it first is to SLOWLY evaporate the excess water away, boiling it gets it too hot, but if you let it heat up to just maybe 20-30 degrees above room temperature, then it will evaporate away more quickly than just leaving it out in the open, and theorectically, since NaOCl is compleatly soluble in water, no mater how much you evaporate, nothing will come out of solution(but this is hard to believe).

[pack_rat2]

...but if you have a less then concentrated solution of KCl, then whrn you add it to the NaOCl, it will dilute the sodium hypochlorite solution more than necesary...
Note that you're not (ideally) adding KCl to a hypochloritel solution--the NaOCl, or most of it, should have been converted to NaClO3. I think the best approach is to take the most concentrated NaOCl sol'n you can make and thermally decompose it to NaClO3. Then dissolve the stoichiometric amount--plus some extra--of KCl in the minimum amount of water possible, and add it to the previous solution.

[mrjeffy321]

and thermally decompose it to NaClO3.

When I heat up and boil the hypochlorite solution, I am actually making sodium chlorate? for some reason I though I was making sodium chloride and oxygen gas (aside from the smell), that seemed to make more sense to me. but I do have experimental evidence to prove you are correct, some where, way up there in one of the ealier posts, I descibe a "mystery substance" that I believe to be sodium chlorate (you can ready my reasons on how I came to that conclusion if you can find the post) and I thought at the time that I had not added any potassium chloride to it (therefore keeping the sodium chlorate that I already had).
that would make perfect sense...I am destroying the bleach/sodium hypochlorite to make sodium chlorate.
Well, if that is true, than why the heck am I trying to keep it bleach for as long as possible with this slow heating idea, ...toss that out the window?


althought that solves one problem, maybe you can solve another I have had lingering.
when I first boil the bleach vigorasly for the first time, it starts forming this dark brown percipitate, I can filter it out, and I think it doesnt comeback if I boil the bleach again (dont remember exactly). I cant figure out what this brown stuff is, I asked clorox what the ingredients of their bleach were, and it didnt seem like anything unusual (although they never address the question concerning the brown stuff). the stuff wont react with anything that I have tried (ie. with the sugar that I react the chlorate with) and when you filter it out and dry it, it looks like rust almost.
any ideas?
what I could do is boil the bleach a bunch, and get the brown stuff out of it, while at the same time making sodium chlorate, so I kill to birds with one stone in that step, otherwise I have all this brown inpurity with my chlorate.

[pack_rat2]

I found some interesting info in a treatise on inorganic chemistry by Mellor. He doesn't mention decomposition of hypochlorites as a method for making chlorates, but describes the process in the hypochlorite section. Quite a bit of reseach has been done on it, mainly with the goal of PREVENTING it. Hypochlorous acid and hypochlorites undergo the following routes when they decompose: 2HOCl -> 2HCl + O2, 3HOCl -> 2HCl + HClO3. The first is the reaction that occurs when it produces bleaching action (oxidation by the O2) and is therefore the one usually desired. But I gleaned the following useful info... For a solution of NaOCl, chlorate generation is maximized at a pH of 7.13. Also, the presence of Na3PO4 is catalytic (he doesn't give a concentration, though). Other ions, including Cl(-) are catalysts, too, to a lesser extent. You might try starting with the strongest NaOCl sol'n you can buy (Clorox sells a high-potency version of their bleach that might be good). Then add ~1% Na3PO4 (just a wild guess for the amount), and adjust the pH with HCl (the sol'n will initially be very basic). You can get pH paper from any lab equipment supplier. Neutral to slightly alkaline ought to be good. You may have to be quick in checking the pH paper, since it will probably get bleached white pretty fast. As for the brown precipitate, it would have to be from an impurity or an unlisted ingredient. The presence of transition group cations (Fe, Cr, Mn, etc.) might do it, or it could be an organic. Be sure to do the boiling in a glass container; steel could add Fe.

[mrjeffy321]

As for the brown precipitate, it would have to be from an impurity or an unlisted ingredient. The presence of transition group cations (Fe, Cr, Mn, etc.) might do it, or it could be an organic. Be sure to do the boiling in a glass container; steel could add Fe.

(Fe, Cr, Mn, etc.), huh, well then a stainless steel pot wouldnt be the best thing to do it in, lol, that is what I have been using, that was originally my guess of what was causing it, but was dissuaded by many people saying, "O stainless steel wont react with it, that couldnt be the source of your problem, ...".

Can glass take the heat, obviously not normal glass, your talking about that special pyrex glass right, isnt that th stuff in measuring cups I think, where can I get some? would just any store have it in the kitchen/cooking section?

Quite a bit of reseach has been done on it, mainly with the goal of PREVENTING it

how funny.

OK I will put these new suggestions into practice and see what becomes of them.

[pack_rat2]

Pyrex glass is what I was thinking of. You can get all kinds of Pyrex bowls, pots, etc, made by companies like Corning, from department stores. Just one caution: even Pyrex can crack if it's heated too quickly by an open flame. So bring up the heat gradually.

[mrjeffy321]

Well, I still dont have any pyrex yet, but I did boil down alot of bleach and make another attemp at chlorate.
this experiment took place over about 2 weeks, so I dont really remember any more the exact amounts of everything I used any more, but I think I was around 1 liter of bleach (which I boiled down to around 600), and a bunch of potassium chloride.

I havent finished it yet, I havent filtered out the stuff at the bottom and dried it out, but here is the interesting part, I have this concentrated bleach solution, I boil that and add a bunch a potassium chloride, mix it up thoughouly,....wait, cool it down in my refrigerator for 2 days and see what percipitates, nothing!, not exactly nothing, but the only thing that percipitated was a coupld little impurity particles things that passed through the filter I used right after I boiled it, so I decide the filter that out and putit back in the refrigerator for another day, so I do.
the next day what do I see? a bunch a white granuals (and crystal looking things) at the bottom of the bottle, mind you all I did to it was filter it once to remove those tiny little umpurites, nothing else, it didnt even warm up very much while filtering it.
so now I potentially have some chlorate, and probably chloride, at the bottom of my bottle, why is it just not getting around to percipitating out, why not yesterday, or the day before?

[pack_rat2]

...[S]o now I potentially have some chlorate, and probably chloride, at the bottom of my bottle, why is it just not getting around to percipitating out, why not yesterday, or the day before?
I don't think there's any KCl, since it's too soluble. I think maybe it cooled down more, the second time, but I'm not sure.

[Dinner]

I am trying to make sodium chlorate (don't ask me why) by electrolysing a solution of table salt. I'm using a graphite anode and a stainless steel cathode. When I start electrolysing the solution an orange-brown precipitate forms (much like MrJeffy's). I looked at the ingredients of the salt I was using and it had Potassium Iodide in it! This, I think, would produce triiodide ions (and then iodine???) and is probably what causes the precipitate. Will this affect the formation of chlorate ions?

[mrjeffy321]

well the percipitate I got when trying to make chlorate through electrolysis was white, and I think we semi-determined that it was due to the impurities in the water (like floride, ...) and then it stoped occuring once all that stuff was used up and the water remained relativly clear.


for your table salt (mostly NaCl), there is indeed some potassium Iodide (KI) in it, but hardly any, I mean something around the order of .002% by wieght I think. so if you had a hypothetical amount of lets say 100 grams of salt dissolved in water, you would only have .2 grams of KI, and that is only about .0012 moles. so this is really, not very significant, not to say that it couldnt indeed be the cause of your problem, but I doubt that it is. plus, iodine/iodide compounds (at least the ones I know) are usually dark purple/blue/back, not orange-brown.


since you are using a stainless steel electrode (cathode) I am inclined to think that that is the cause of the percipitate, even though it is the cathode, it will corode slightly, but not nearly as much as the anode might.
I try to steer away from using any type of Iron (which includes(stainless)steel) in my electrolytic cells, it never ends well for the electrode.

try it with a graphite cathode as well as a graphite anode, and see if there is still some percipitate, also try using disstiled water insted of tap water if you arent allready doing that.

[mrjeffy321]

just an update on the status of that last batch of hlorate.

I had high hopes for this bacth, and it looked as if I was going to get alot (comparitively) this time, and when I dried it out, it looked good. but when I tested it...
yellow (and slight, barely noticcible green) flame, the tale tell sign of sodium chlorate. Not that I dont like sodium chlorate, but it is just not what I am trying to make, especially after I add al that potassium chloride to the mix, and then nothing happens. I really need to get some pyrex I suppose to try this.


speaking of pyrex, I was at the store today looking at some pyrex cups I could use, and they say specifically on them, "not to be used on stove top, breakage may occur". it this warning just for stupid people who try to heat up an empty cup over an open flame, or should I actually follow this because it will break if I try to boil bleach in it, I think it is the former, right?

[pack_rat2]

First of all, I should point out that the slightest trace of sodium ions will cause a yellow flame, and it will mask the violet of the potassium. Second, you say "green"...hmmm. I think that's from free chlorine gas that comes from undecomposed hypochlorite. What you have can't be NaClO3 if it precipitates out from any significant volume of water. NaClO3 is EXTREMELY soluble.

[mrjeffy321]

so your saying, the sodium will easily cover up the potassium color, even if I just have a little.
which makes that previous instance of the violet burning powder potassium chlorate all the more special because it must be very pure.

there is just a little green, the vast majority of the color yellow.

acording to MSDS, NaOCl solution is "100 % solubile in water", but that doesnt mean that when the water is evaporating off the crystals in the filter, some isnt left behind, although it is odd that there still would be NaOCl left, after all that boiling and reacting.

I was experimenting with containers I could boil my stuff in, I tried an aluminum soda can, and it worked surpisingly well, considering its very small surface area in contact with the stove. it didnt corode, although the thnk plastic film coating the inside did come off.

[pack_rat2]

I was experimenting with containers I could boil my stuff in, I tried an aluminum soda can...
Just be aware that NaOCl is a strong base, and bases react with Al to form aluminates, with the evolution of H2. If no gas bubbles form, you're OK. Those cans often have an invisible plastic coating which protects the surface.

[mrjeffy321]

and bases react with Al to form aluminates, with the evolution of H2.
O really, I didnt know that, cool, I learned something new today.
If no gas bubbles form, you're OK.
well no, hydrogen gas bubbles formed (that I know of), but hopefully alot of steam gas bubbles formed, hard to tell what it was, but the only danger I see of making hydrogen gas is the possibility of it combusting, and this isnt likely with the tiny amount I might have made.
Those cans often have an invisible plastic coating which protects the surface.
these do, although I think, not sure, that some of the coating came off while boiling, because it was bubling up from the can with all the gas forming around it, but I cant find any peices of it now.


I cooled that stuff down, and WOW, I got alot of crystals, filtered then and put it back into the refrigerator, and checked again, WOW, another large second batch, so I filtered those. they are still drying, so no word on how it will come out yet. but I dont think I want to use aluminum cans any more, for the reasons you said, but also because it can hold very much liquid and it had vertually no contacting surface area with the stove, so it takes forever to heat up, and a high center of gravity, as conpared to a pot for example (spills waiting to happen, not something I need). and I am now werry of using pryrex on the stove (because of its warning label descibed above), are there diferent grades/strengths of pyrex? some mroe suited for my purposes/laboratory pruposes?

[mrjeffy321]

A coffee pot seems to work for a pyrex substitute, if it isnt already pyrex (it doesnt say), i boiled alot of liquids in it, and I got alot of crystals, but I think the stuff I am getting now is less pure than what i was getting before.
the crystals are harder and dont crush into as fine of a powder as they once did, and it is harder to light.
I am probably boiling away too much liquid, so that the salts cannot dissolve and percipitate out too, that is what I am thinking.

[pack_rat2]

Remember that NaClO3, which is what you're making by the decomposition of NaOCl, is very soluble. So is KCl. When you add the KCl sol'n to the NaClO3 sol'n, the relatively insoluble KClO3 precipitates out. You want the initial NaClO3 and KCl solutions to be as concentrated as possible (though not super-saturated).

[mrjeffy321]

I seem to be getting very good at making a chlorate that burns yellow now, I can make batches of around 10-15 grams at a time of a fine white powerder that burns yellow (and just a slight tint of green).

With another two batches under my belt that work as described above, I am really getting good at this, with less than compleate satifaction.
It is obviously not pure enough (or the right type) to burn the correct color, and it is rather time and space consuming to make it. Also, as a matter of interest, i took a quick trip out to the power meter outside and checked to see how significant a dent in the electric bill my electric stove is making now that it is running much much more than it is ever used, and a surprizingly fast and noticable change in the spin of the dial.


What about this as a way of purifying the product, set the crushed powder in a finter and slowly pour a small amount of cold water over it (volume of wate varies with amount of chlorate), the cold water wont dissolve much chlorate, in theory, and should remove the sodium, chlorine, ... impurities that is present.
This idea is similar to the suggested process that was given in the instruction of making the chlorate, but I am afraid of loosing to much in the process due to it dissolving away, despite its low solubility.

[Sparkee]

Hi,new member here! I have had some success with chlorate production by electrolysis using an old computer supply and carbon arc rods. Most of the information I gleened from the web. Visser's site being one of them,another site was rouge science(no longer available???) The power supply, the amount of solution, how many rods,etc... all were contributing factors. To the amount and how long it took to process. Not to mention that once you obtain the NaCLO3?? a double replacement reaction is necessary to obtain KCLO3. One of the test I used was combining the dryed KCLO3 with powdered sugar and adding a small amount of H2SO4. If you get a reaction the concentration is supposed to be above 20%Caution!! It will happen fast! In your face fast if proper care is not taken! If I can be of help let me know. If the Chemistry is wrog please excuse me as I'am an Electrican not a chemist.

[mrjeffy321]

Hi, glad you decided to contribute to my thread.
you probably havent read all my prior posts on this subject, but I did try the electrolysis method once, but I became very discurages with it due to the long hours of just waiting for it, ..., then I started having problems with the current jumping from high to low and then nothing at all, then I burned out some power supplies and ruined some batteries, and to top it off, I spilled the jar loosing half the solution! I had some really bad luck, and I didnt like just wasting all that hydrogen (I used to make and collect alot of hydrogen a few months ago for some hydrogen detenations and for my fuel cell I buil, before I upgraded to some real explosives), and I also has problems with the (graphite) electrodes and the wires attatched to them clouding up my solution.
but it is nice to know that, with a little luck, other people seem to have great success with it.
One nice thing I found was a program on the internet that would save me a lot of time a guess work, insted of me working out how much salt, ... how long to run the cell, ..., you just input your starting conditions into the program, and it will compute it for you.
I do want to go back to the electrolysis method again, that is the more efficient and less labor intensive way of doing it(and cheaper), but I am currently out of supplies to do it with, I burnt out my last good power supply I can afford to loose, I still need to work out a better method for the electrodes, and Idealy for easily capturing the hydrogen gas (but that isnt necesary, just something that would be nice), and I need a way to measure the current, I have a multimeter but it wil only go up to 200 mA, I dont want to wait that long so I prefer full amps when I do it, I borrowed a ammeter from school and I kept that for a long time so I dont want to impose on them again to borrow something, especially now that they will be using it soon.


Tell me, were you very successful making chlorate, how much did you make? in how big of batches? any other advice?

I'am an Electrican not a chemist.
well, I fancy myself a physicist before a chemist, not that I am an expert at that either.

[Sparkee]

I used a 2 Gallon container, 1600g of NaCL in a saturated solution,8 carbon arc rods that were connected with magnet wire to the cathode,some stainless steel hard ware for an anode. the power supply was one that I picked up at a discount computer store for $10.00. I ran it at 5v and 6 A for 300 Ah keeping the liquid level constant with addition solution. I cut off the bottom of one of the containers and drilled 8 holes around the perimeter and one in the middle. I suspended it from some fiberglass unistrut above the cell. I had the voltage and ammeters from various demo jobs that I had done. If I can locate the pic's I could show you my set up. I was actually quite pleased with the yeild I dont recall the exact figures it was well over 500g. And turned out some great flash powder. My aim was and is for homemade fireworks. (my sons birthday is July 4th.) I have had modest success with that
I too had several tries fail, disentagrating electrodes, power supplies failing,just to name a couple. But, persistance won through! I have since deconstructed my cell as have made enough for my purposes. I will look for my information and would be happy to share it with you if you like. There is nothing like a big BOOM especially when you made it your self.

[mrjeffy321]

I have to say, potassium chlorate is indeed very fun to, excuse the word, play with. I have made some pretty cool demonstrations for other people with the meager amounts I have, some of the good ones I video taped and edited on the computer which I hope to put on a web site one day soon.
Most recently, I made a "rocket powered car" using a glass jar and chlorate, it didnt work as I expected from the other tests, but I did succeed in moving the car 10 inches before it burst compleately into flames.


Your set up was much more advanced than mine, certainly using more solution and prioducing much more.
But I think I will give it another go, I just need to get a power source, I might have an old trash computer with a working power supply I can for this purpose, I will look into it.
Did you make an extra effor in your cell to control the temperature and pH to get maximum efficency? When you ran it, how big of a problem was the water clouding up and dissolving electrodes?
I would be evry interested in seeing the picture you have of your setup if you can locate it.

[mrjeffy321]

Actually, now that I look at the power supply I have, I would have no idea how to use it in my cell. I assume it would involve destroying it in terms of it can never be used in a computer again, but I wouldnt know which wires to use or which have what current through them.

[Sparkee]

Many apologies for not getting back to you sooner. If you look on your PS the connector that goes to the mother board will have a green wire with a black wire on either side. If you jumper the green with the black to the left of it you should have a fan kick on when you apply the AC to it. Then check the red and black for +5 volts if you have that you should be good to go for a Power supply. At the present time I 'am assemblying my set up so I can re-take some pic's that I cannot find. As to the temp and PH, I used a fish tank heater and was able to maintain a fairly constant 75C.for the PH in the AM I would add 10 or so cc of HCl. (Muratic Acid 30%)It seemed to work at keeping the PH within acceptable levels (7-8??) The Electrodes I purchased from a welding supply store. Around $25.00 for a box of 50. After soaking them for a couple of days in linseed oil. (To help against deteoriation of the Electrode.)Allow them to dry?? I took some Magnet wire (22 awg) and made a couple of wraps around the carbon rods finishing off with some hot glue covering the wraps.( Dont forget to scrape the wire before you wrap it.)This should get you a start. I will get the pic's in the next day or so as I get time.

[mrjeffy321]

If you look on your PS the connector that goes to the mother board will have a green wire with a black wire on either side.
I have looked at two, old computers' power supplys and I dont see any green wires, let alone any between any black wires.
I do have the casing and wires of another power supply (the 'guts' are gone though) and I do see the 3 wires you are speaking of there. I will tryu to get a better power supply tomarrow or at my next oportunity.

[mrjeffy321]

I have gotten a power supply that looks good.
I dont see any green wire between 2 blacks, but I think it will work anyway because on its sticker, it not only has the voltages and amps supplied, but also the color of the wire to get it from.

Here is what it says:
DC output: 235 W max
+3.3 V 15A (Brown), +5 Vsb 1.0 (Green)
+5 V 22A (Red) , -5 V .5A (White)
+12 V 8A (Yel) , -12 V .8A (Blue)
P.G. Signal (Orange), Ground (Black)
(+3.3 V & 5 V Total output 130 W)


If I look at the PS connector, I see these wires in this order (abbrevaited):
R = red, W = white, Blk = black, Blu = blue, Brn = brown, Y = yellow,
G = green, O = orange

Side 1,
R, R, W, Blk, Blk, Blk, Blu, Blk, Blu, Brn
Side 2,
Brn, Brn, Blk, R, Blk, R, Blk, O, G, Y

Obvioulsy my colors dont match up with yours, so I cant just 'find the green', which wires should I use? I really dont want to screw this power supply up, I was lucky to get it, I could really use your advice since you are an electrician.

another thing, lets say that I want to switch from diferent voltages/current from day to day (for various reasons), would I just use the +12 V wire and then the ground wire for example? or would I need to use the -12 V wire? but then there isnt a wire for -3.3 V.

[Sparkee]

I believe that you want the PG signal and it's associated wire Orng and Blk,try to jumper between them. You dont have to cut up the plug just insert the wire and turn it on. If that dosent work you could go ahead with the green and black I dont think you will damage anything as it would have to be on for that to happen(The LV side) I tried to hack an Apple Power supply,never did figure it out so I stripped it of parts. The PS I have I picked up at a used 'puter parts store for $10.00. They had about a dozen or so to chose from. I'm still gathering my set-up, I have used it or parts of it elseware on other projects. Idle hands...I'll get more out ASAP. Hope this helps.

[mrjeffy321]

I tested it out, and it looks like it doesnt work. I cant get any voltage through any of the wires. I tried the same thing on another power supply that I know is good and I can get 5 volts acros the correct set of wires (and 5 amps), but I cant use this power supply, I'll try to get another one tomarrow.

You said that you used electrodes, electrodes used for welding.
arent those made out of steel with some type of coating around them that is suppose to flake off? if you used those, wouldnt the water get really dirty and the electrodes would get eaten away, or am I thining of a diferent kind of electrode? this is what I was thinking about, it this the type you used,
http://www.msm.cam.ac.uk/phase-trans/2001/PICF0127.JPG

[Sparkee]

No, the one's in that link are not the correct type. The Electrodes I used are used for carbon-arc welding, appx. 3/8 or 1/2" Dia. 16" Long, they are carbon rods that have a copper foil coating on them. I have heard them called gouging rods. I believe the length is fixed but the Dia. is variable up to 9/16". Any welding supply store would have them. Also the copper coating peels off fairly easy once it gets started. I cut them in half and soaked them in a container of linseed oil for three days. I've heard of some applying vaccum to the container, I didnt and they seemed to work fine. They will erode! I think that I replaced mine at the 1/2 way point. They were looking spindley and ragged. Well good luck on the PS. If I can help let me know. I'm working on a spark gap for a coil I built. Have a good one!

[mrjeffy321]

I finnally got a power supply that will work, I went through about 6 different ones before I found one that I could use. it is a different type of power supply, but I am getting a good current out of it, although it does drop drastically when in water.
So now I'll give that a try

[Sparkee]

Great! The I(Amps) should change once you get it into a saturated solution of NaCl,And the proper electrodes attached.I'm going to try and attach a pic of what I have gathered together.Well, I have to shrink the file size before I can upload it. Once I figure that out I'll send it along.

[mrjeffy321]

OK, it has begun, the electrolysis chlorate making started at about 6 amps with a fully saturated 400 mL of water (before adding salt).
this brings up a question, if I want to know the volume of my solution, do I take it after I add all the salt to it, or use the volume of the plain water I had before.

before I had 400 mL of distilled water.
after I added all that salt, I have around 450 mL of salty salty water.

[Sparkee]

I believe that in order to achieve the correct saturation the solution needs to be brought to a boil and the NaCl added until no more will disolve into it. Once that is achieved you would obtain the required amount. How did you come out as far as electrodes are concerened?? I used a Stainless Steel config. of plates and 3/8" nuts and bolts for the + and the gouging rods - arrainged circling the anode. anything in the container or in the immeadite area is subject to damage by corrosion. So prepare for that. Also are you planning to run it 24/7 ? I did and had little problem doing so. I would take the appropriate measurements every 10 to 12 hours . I also ended up attaching an hour meter that aided in the recording of the actual Amp Hours the cell operated. All said and done I ran mine for 287 Ah. I tried a few different power supplies during that and found the computer PS to be the most reliable. Good Luck! Let me know how things are going.

[mrjeffy321]

Well, I have logged 36 hours of running time as of right now.

Here is my stort of the first 36 hours of operation.

I started out with my good power supply (I think an 'AT' Power supply, the kind that has a switch that actually controls the AC power to it, not just some 5 volt DC signal). I was getting around 7-8 amps out of it, but the problem was that as it would run, the amps would slowly increase, by about .6 amps/hour. It didnt take long (just about 1.5 hours) for it to reach the 9 amp max that this particlar power supply would support at that voltage, and it would shut itself down. so I had to continually reset it, nut atleast I was making good progress.
I decided to let it run over night, ...., I woke up the next morning, and I dont know what exactly happened but it had turned itself off (probably overloaded), and when I went to turn it on again, I noticed that there were considerably less bubbles being mad than before, and the rather notible hum of the fan was barely audible. I switched it off, and then back on again, and now it is compleately dead, I cant get anything out of it, which is really frustrating considering what I had to go through to get it and the other uses I was using it for besides chlorate production.
I did however have one of those (PS?) power supplies that I was testing before that I could get one wire working on it, so I switched power supplies. now I am getting a remarkibly steady current of about 1.58 amps (low volts, only around 4 v), that I can and have left for the past 18 hours, relatively uniterupted.

So anyway, I broke one power supply (I hope it comes back to life, that was a really rare find for me to get that, and it was useful for othe things), and now I am using a very steady power supply, but with low current and low volts. at this rate it will take another week atleast to get done.
If only I could figure out how to get the high amps out of this working power supply, it claim to be able to go up to 25 amps, but I would be happy with 10 since thats as high as my ammeter can measure, but all I can get us 1.58.

That hour meter is a good idea, it measue what is really important, the total amps that are going into the cell during the whole trial, that was you dont have to be concerned with keeping a log of what the amps are in a log (like me) at each interval.

As for electrodes, I am using some faily dense peices of graphite blocks I had sitting around the house for a while, they seem to be working very well, under the 7 amp power supply, they made the water very dirty, but using the 1.58 amp power supply, they water is staying clean for now (I filtered it when I changed power supplies).

[Sparkee]

Try varying the distance between or or one block deeper than the other that is one way to adjust I,.through the resistance of the cell it self. You may also want to try a peice of stainless steel wire or ??? for your Cathode. Did you look for the 5v/25A through the pin connector? the case it ground just start probing until you ID all the 5v pins then try them out. I also know that surface area of each is important. Do you know of visser's site reguarding chlorate/perchlorate production? He has done all the Math and is really quite good in his information.http://huizen.dds.nl/~wfvisser/EN/chlorate_EN.html Try that I'll see if I can find some more of those link's.My Email is jchv46m@msn.com I can send you a couple of files if you have an adress.

[mrjeffy321]

I have the electrodes spaced in a way that maximizes the current through the cell (they are very close together).

I will keep playing around with the power supply and try to get a better current out of it, but I dont know how successful I will be, I have went through all the wires before. All I can get are a coupld 5 v wires, but not the 5 v, 25 amp wire, but if I can get it, it will be a happy day indeed.

I am very impressed with how long I can leave this cell going, under the current conditions of around 1.58 amps, and not have to mess with it, I has pretty much been running constantly every since I started using this power supply, Slow but steady might be better than having the reset it every 2 hours.

my email address is mrjeffy321@yahoo.com if you want to send me those pictures.
And es, I have seen that page, it has been very helpful in figuring out how to produce chlorate, I have used it as a guide for both electroytic and decomposition production.
This site is good too I have found, it has a strong enphasis on electrolytic means of production:
http://www.geocities.com/CapeCanaveral/Campus/5361/chlorate/chlorate.html

[mrjeffy321]

That information you sent me was really, good, thanks. I will be reading over that for a while.

An update on my current cell:
I have now crossed the 110 hour marker, it has been running constantly (with only very short daily breaks to add HCl) for the past 87 hours at a fairly constant 1.58 amps. before that it was running at more amps and/or with more frequent breaks. I figure that I have about 130 or so more hours to go before the NaCl gets to about 10% concentracion, and that is when I should stop by. but I might quit early, say in around 50-60 hours, to see how it went and get my results this weekend, I am not sure what I will do yet.
Lately the efficiency has dropped since I was only able to add HCl once a day, so that adds some time to what I need to do.

I must say again how impressed I am with all that information you sent me, and how well designed your chlorate cell was.

[dauphin115]

Hi
Some weeks ago I started to plain my Chlorate/Perchlorate cell, the next week (I hope!) I will must to recieve the material for anode and catode, I found a very little expansive system for pH control, Is a system of Hanna Industries, this system is used for pH control in acquarium, the misure system and probe cost about 175 €,if we want, we can to see this system at http://www.hannainst.com/downloads/instr/istr981411r5.pdf I found a seller in italy http://www.acquaingros.it/edisplay/cat339.htm#36
This system have exit contact for controlling device, I would to build a solution tank for HCl with a valve commanded by this exit (I think that it's not hard to build this).
I project my cell with level control of elettrolite solution and a current monitor.
The problem for me in this moment is the power supply; I have some Pc transformers, but, how we know, this transormers don't have an costant current output, I looked other web site (www.geocities.com\CapeCanaveral\Campus\5361\chlor ate\chlorate.html ad example) and I try to understand the exactly goals but I need to know more about this.
I have very little experience about this topic, but I understand (I'm a chemist but my job is fireman) they are no topics/matters in italian language so if we have some advice about this I please we if you can to help me (transformer modifications or extra circuit).
All my new experience I will share with we.
Thank you very much!
Best redgards

[mrjeffy321]

That is a good idea about using a fish tank pH adjuster to keep your cell's pH controlled, but a little expensive for most hobbiest I would imagine (or at least for me).
As for your problem with getting a constant current out of your computer power supply, I had a similar problem when I was using an (I think it is called) AT power supply, where the power control to the computer actually turns on/off the power to the power supply. this type of power supply will give you lots of current, but I found that it also will fluxuate alot while you leave it running. Then, due to circumstances beyond my control, I had to switch to another type of power supply, I think called an ATX power supply, where there is a contant 5 v comming out of the power supply to the computer, and the button that turns on/off the computer controls that. Using this type of power supply (far more common to find now-a-days i think), I can get a much more constant current, I think it remained constant for well over a 100 hours of continous running for me, untill the condidtions in the cell began to change drastically, but it was a relitively low current though.

I have just finished my first real attempt at using an electrolytic cell to produce chlorate, I havent yet dried out the potassium chlorate, but so far the results look really good, and I'll decribe everything in more detail here later when it dried and I can get measurments of everything.

[dauphin115]

Ok, thank you for your information, about ph controller if you want I can to send you a file that I found on www about homemade pH controller, is without temperature compensation but if your cell have a control temperature you can calibrate this contorller at your temperatur's cell and all is OK, you only need to buy a pH probe (I think is impossible to homemade this probe), I'm sorry but is in Italian language, if you have problem with this language I'm very happy to help you, if you try to search on Internet about "pH controller" or controller pH" you can find some projects about this specially in amateur website of person that like aquarium hobby.
Hi Emiliano

[mrjeffy321]

sure, I would love to see some plans on how to build a pH controller.

I have compleated "trial 1" of my chlorate cell, dried and weighed the chlortate and tested it. Here are my results:

-mass of NaCl I started out with: 145 g
-volume of distilled water (before addeding chloride): 400 mL
-Throughout the test, I was just assuming 60% efficency, so
Total amp hours needed:460 ah
-I stopped the cell early, so I only ended up supplying 335 ah
-theorectical mass of sodium chlorate produced (at 60% efficient): 133 g
-after adding the sodium chlorate to potassium chloride to convert to potassium chlorate, max possible yeild of potassium chlorate: 153 g
-actual yeild of potassium chlorate: 109 g
-success %: 71.2 %
-actual calculated efficency would be 71.2% of 60%, : 42.7% efficient

So overall, I am pleased that I made so much in one batch, given that it took 2 weeks to make it, but I am dissapointed in the low % yeild, I though I was estimating conservativly when I said 60%, afterall I was trying to control the pH, but I ended up getting only 42.7% of what I would have gotten with 100% efficency, I wonder what the efficency would have been had I not added HCl periodically. I doubt that there is another 50 grams still in solution, I tried going back and boiling more water out to see if I could get any more, but only chloride percipitates. The over all quality of the chlorate is acceptable, it isnt as pure as I like, but that is more my fault than the cell's. I kept fairly good records of the current, volts, and calculated resistence throughout the 161 hour trial (with large gaps between record takings). There were however some reasons for its low overall efficency that I can account for, the long gaps between aditions of HCl, I wasnt home to do it and watch over it all the time, it was outside, in the cold, so it lost alot of heat to the environment, at one point, I over diluted it by accident when adding more water to make up for the amount that was lost, early on, I didnt realy have good way to gauge the pH (I still dont, I just have to asume it is neuatral when the HCl doesnt make it fizz any more), and other things that might have happened when I wasnt around.

I have started another trial, this time with tap water (500 mL) with 180 grams of NaCl, using 2 cathodes and 1 annode. I am getting about the same current, it varries slightly from 1.57 to 1.60 amps, but is fairly constant around 1.58. This cell I plan to let it go for the whole (or a very high percentage) of its total time needed to convert 90% of the chloride to chlorate, which I figure to be around 650 ah.

[dauphin115]

Very well!!
I know that is very difficult to control current efficency I read more and more on www about this, they are some experimental setup for chlorate cell, I read about electrode position into cell, anode on the bottom and catode on the top (anode under catode) the Cl2 gas that are formed at the anode to go up and "meet" the OH- that are formed at the catode, this setup help the formation of chlorate (not more but..), stirring the solution is another way to increase the current efficency because help the dissolution of Cl2 gas.
pH controller:
about this, the probe measure the concentration of H+ ions, the output of probe is a measure in mV that the pHmeter convert in pH value, I don't know more about this but I know that the presence in solution of ionic/cationic species don't influence the mV value ( it depend only on H+ concentration) so is possible to measure the value of mV (with sensible mV meter) and build an apparat that add in the cell HCl if the value of mV change.
The current efficency is more influenced by the value of the pH and you can obtain a good current efficency value only if you control pH.
I have a question for you; You use chlorate for your experiments or use it for preparation of perchlorate?
Hi Emiliano

[mrjeffy321]

For right now atleast, I use the chlorate I make for experiments (pyrotechnic, rockets, ...).

[Sparkee]

Glad to hear that it produced for you! Please let me know how your devices turn out. In my case I was able to achieve some spectacular results. One problem was getting the Al processed to a fine enough mesh. If it is not you end up with a fountain instead of a "BANG". BE CAREFUL!
Check out this link for PH/MV/T meters, WWW. Grainger.com

[mrjeffy321]

In the mean time, while we wait for my current chlorate cell to compleate, here a question about contruction of the cell.

I know you, Sparkee, made a pretty eleborate cell with lots of electrodes and a cover and it looked very well made.
My cell isnt quite so big, I am reluctant to make an eleborate cell just yet before I can pretty much perfect my process I will use and before I gather the materials needed (and get a better power source).
Right now, what I have is a plastic penut butter jar, about 5 inches tall and 3 inches wide. As my electrodes I use 3 (2 cathodes, 1 on either side of the annode), made of recangular chuncks of graphite. This basic system seems to work well, but my main problem, which I didnt get into before on my last trial (probably because it was outside), is that the copper wire I use to connect the power supply to the electrode gets corroded very easily and breaks off, this breaking the circuit. I have alot to prevent this, I have wrapped it in tape, then I covered it in hot glue, then I covered it in some rubber cement type glue, then I covered it with both glues, then I got some water putty that dried hard around it and used that, and in all cased, with in 24 hours (many times less) of continous running, the wire corrodes and needs to be replaced. the problem is occuring because of the chlorine gas being made at the annode that is rising up and corroding the copper, it seems to get through any barrier I give it, eventually.

Any suggestions on how I can prevent this from happening, or at least delay it much longer?

[pack_rat2]

...What about this as a way of purifying the product, set the crushed powder in a finter and slowly pour a small amount of cold water over it...
I've been away for a little while due to the holiday season, but now I'M B-A-A-ACK...! ;) As for purification, the accepted method is recrystalization. Heat up water to the boiling point and dissolve as much KClO3 as it can take, and a little more. Pour off the clear solution and cool it down. Pure crystals of KClO3 will precipitate out. Just keep doing that until all the KClO3 has been processed.

[mrjeffy321]

Hey, it has been a long time.
But wouldnt this method inevitibly leed to the loss of lots(7g/100mL) of perfectly good KClO3?
For example, if I decided to purify 100 grams, I would need to use about 1.4 Liters of water to dissolve all of it and I would get very little back.
Or is the idea insted not to redissolve it, but rather just get it wet and thus dissolve the impurities?


Any suggestions on the electrode problem?

[Sparkee]

Having the cover on my set up helped ,also I used magnet wire (26 ga.) you might try shrink tube also. On the end of the electrode where the wire attaches I used hot glue and shrink tube for some protection and tried routing the wires up and away from any obvious problems. At about the halfway point of the process I did replace all the electrodes as they were eroded to the size of pencil lead. I didnt have any of the wires corrode. I think that having the tight fitting cover helped by allowing me to route the chlorine gas away from any problem areas. Make no mistake corrosion will be an issue! I had mine set up in my shop even with an exhaust fan I still had problems. Anything that was not stainless steel was affected. Several of my hand tools in the vicinity have a nice layer of rust. I still find chloride/chlorate accumulated in places when the humidity is high. From that I learned that when next I run a cell it will be outside.

[mrjeffy321]

I find I get best results using a combination of hot glue on the bottom and this runnery type glue called, "goop" on top. Right now I added a middle layer of wax to see if that will do any good, but the jury is still out on that.
I think I will try to set up some type of lid to divert the gasses away, but this will be hard considering how low to the water leve the wire is. it might be a better idea if I just redesign the whole cell, but I wanted to wait before I did that until I got at least one reliable, high amperage, power supply I can count on now breaking, otherwise I'll have to wait years to get a bucket of NaCl(aq) turned into NaClO3.

[Chronos]

You can buy the stuff at the grocery store. It's called lite salt.

[mrjeffy321]

The 'lite Salt' you are refering to is actually a mix of Sodium Chloride and Potassium Chloride, thus containing less (lite-er on the salt) "salt" than normal salt. But I would need pure Potassium Chloride, no sodium chloride (that is just a by product of this reaction), so I use something called, 'NoSalt', also at the grocery store, but a tad more expensive.

by the way, the wax idea worked terribly.

[pack_rat2]

Hey, it has been a long time.
But wouldnt this method inevitibly leed to the loss of lots(7g/100mL) of perfectly good KClO3?...Or is the idea insted not to redissolve it, but rather just get it wet and thus dissolve the impurities? Any suggestions on the electrode problem?
You just say the solution you have at the end of the purification, until your're ready for the next batch. Sure, you'll always have some left over, but if you keep making it, that amount doesn't increase. And you MUST dissolve it in order to purify it, since the impurities are locked into the crystal structure. As for electrodes...platinum is what's recommended! I bet you just loved to hear that. I've read something about stainless steel and carbon rods, for those of us who aren't rich.

[pack_rat2]

I posted a link on the thermal method; it also has info on electrolysis. Here it is, again:
http://www.wfvisser.dds.nl/EN/chlorate_EN.html#thermal

[mrjeffy321]

platinum is what's recommended!
I, no problem, I will just reach into my vault and pull out a couple bars.
I am unsure on how well platinum would work, or for that matter silver or gold (what about nicrome wire?) would work almost as good, but would a platinum electrode work perfectly with no corrosion or erroding? or would it eventually. I was under the impression that no matter what I used, it would get corroded but at diferent speeds.

Saving the water used for purification, good idea. But then it gets complicated if you want to do a batch a diferent size than the amount of water you have, .. time to get out the measuring cup and esimate what is dissolved already.

Does anyone know what the average purity of KClO3 is without purification, through either method (if there is a diference)?
Then once it is purifies, doesnt it get to be pretty close to 100%


Sparkee [or whoever wants to answer], a while back (many posts), you said that you used an "hour meter" to help you measure the total amhours into your cell. I was looking around, considering getting one, but I dont really know what to look for, I found a wide range of styles, prices and desciptions. I foun something called an hour meter, but it is used to meaure the time elaped on electrical motors and what not and I am unsure if it is the same thing you had. also, there seems to be specifcations on the voltage that the hour meter uses, does this matter if my cell is not within the hour meters range?
example of what I found:
http://amos.shop.com/amos/cc/main/ccn_search/st/%22hour%20meter%22/sy/productsx/ccsyn/260/prd/8197242/ccsid/324920718-20893/adtg/02100541

[Sparkee]

It was (is) just a standard analog hour meter using line voltage. Run in series with your power supply line side. The one I use came off an old compressor control panel that I demo'ed a while back. I set it up so that when I switched on the power supply it would engauge a relay and begin recording. Through this I also ran the heater ( aquarium type) so that when I performed the daily maintainance(Ph,etc..) that the heater would also shut down. If you happen to forget to un plug the heater when you pull it out bad thing's can happen. The glass tube encasing it will shatter exposing the element and you have 120v exposed. Not good! I admit that my setup was probably over done. Had a lot of time on my hands. But, What the heck keeps me out of trouble.Let me know if I can be of help. The one your link showed is DC I suppose it would work. Mine ran off 120v so I was able to keep it farther away from the cell (corrosion,etc...)

[pack_rat2]

"...[Y]ou said that you used an 'hour meter' to help you measure the total amhours into your cell...."
If you can't find one or can't afford one, you can do it the old-fashioned way. Put an ammeter in series with the circuit, and make a note of the current. Then, at periodic intervals, check the current and record it. For each interval, calculate the average (sum of the current at the beginning and end of the period, divided by 2), then multiply that value by the length of the time interval. Then add up the values of all the intervals for the total. This method isn't as accurate as using a meter that measures current*time continuously, but it should be more than adequate.

[mrjeffy321]

that is essentially the way I do it now, but it is so time consuming, keeping all those records of what the current was at each interval.
also, when I cant tend to it all the time (like when I goto sleep), alot of times it stops because of some problem, and i never know when to estimate the stopping time was. if I can find one cheap enough, it think it would worth it to me convience wise to get one.

I am roughly into my 440th amp hour on my second trial of my chlorate cell, only about 210 more to go.

[mrjeffy321]

OK, it is finsished after long last, my second trial is done, the Chlorate has been extracted, dried, and weighed.

Stats:
-Started with 180 grams of NaCl
-dissolved in 500 mL of water
-should have taken 650 ah to convert 90% of it at
-estimated 55% efficency (what I estimated it would be from the begining)
-I ran it for the full 650 ah, by my log (which inclues soem rounding, but more on that later).

Theoretical maximum amound of KClO3 that could have been made by convering 90% of the 180 grams of NaCl: 272 g.

Actual yeild: 140 grams
% success: 51.5$
Actual efficency: 28.3 %


This is pathetic, I am ashamed of these results, it is stuff like this that makes me think I forgot a decimal somewhere because this is horrible!
I let this cell run for the entire month of Feburary to get the 650 ah needed, then I spend a week extracting it and letting it dry, crush it up and weight it, and all I get is a measly 140 grams, (just a small jump from my last cell), and I should have theoritcally gotten 272 grams.
sure is alot compared to how much I used to be making, but I spent so much time on this, changing electrodes, keeping careful logs, adding HCl, ...... and something must have gone terribly wrong for me to get only 28.3% efficency, I could have done nothing and got better than that. I did do some rounding and estimating, but I dont think this could have made that huge an impact on my results.

This really makes me want to redesign my cell, but there are so many complications, I dont know where to start.
if/wheh I redesign it, its main purpose would be to produce chlorate, but I also want to be able to collect/divert all the gasses (speratly) that come off the electrodes.

[redwraith94]

mrjeffy321: Boiling bleach decomposes it from 3 x NaClO to 1 x NaClO3, 2 x NaCl

Platinum electrodes can be used, but they have to be uber pure, even .01% rhodium/some other similar group metal will give the electrode a set service life...this is considering electrodes that are usually copper core, niobium alloy 1st plating, then platinum over-plating (usu ~100-250 microns thick or so)

Graphite works fine, and they are much cheaper, I just got a quote for platinum clade copper rods. 2 x rods 1 foot long each with a 100 micron plate 1/4 inch full diameter...90 dollars US...too much money for an electrodes w/ ~5,000 hrs service life? lol.

Finally, don't be ashamed of your results. A big thing that comes into play for electro-chemistry is current density, temp, ph etc. You really want fairly large electrodes for your setup. I am doing research right now, because I am also looking to make a Chlorate/sugar/Ammonium sulfamate/dye based smoke bomb for the fourth.

[Letda]

hey guys, im new at all this so dont judge me right away. I'v been researching how to make the potassium chlorate for about a week now w/o actually doing a lab. I'v read everything that had been posted, but im still a little lost. I was just wondering if one of you could break down the steps in lame'ns for me. I run an IQ of 147, knew frued before i knew freud, but chem.... i sometimes wonder. If anyone can talk one on one with me to help me understand i might be of some value to your conquest. Just E'mail me at -letda13@hotmail.com-. otherwise ill be reading up on your findings and starting my experiments my self. Ill post everthing i find i promise :)

[mrjeffy321]

Hello, I have been researching/making potassium chlorate for about 9 months now, so I have gotten plenty of experience by now.

Do you have any specific questions, or do you just want general information on the process(es).
Like redwraith94 mentioned, this is a popular time to start making KClO3, only about 2 weeks left until the 4th of July (and all the homemade fireworks that go with it [taking all necesary precautions of course]).
If you want to make alot of Potassium Chlorate in a short amount of time, I would go with the decomposition of hypochlorite method (boiling bleach), but if you have more time and are patient enough, the potential for gain using the electrolytic method is much greater. I myself prefer the electrolytic method, but I have been plagued by bad luck with it also, using hypochlorite is certainly provides much quicker results (and some might consider it easier).
I actually have a batch of KClO3 drying right now.

[Letda]

I guess I’m kinda of an unusual person, I’m a psychology major with a weird fascination with astrophysiology and aeronomics, so I guess I’m not trying to make "just" fireworks for the 4th of July but I want to use concepts from these basic principles to further my know how in such matters....

So, when boiling the bleach, do you just boil until no liquid is left or do you get the crystals before that, and are they what I need in pyrotechnics? And I’m totally unfamiliar with electrolytic, is that just like putting a positive charge on one end of the cup and neg. on the other end??? As you can see, at 17, I think I'm a little behind, I was too cool to take chem. serious in school.... how sad huh!

[mrjeffy321]

The bleach boiling method is easiest to understand.
Bleach is a solution NaOCl (sodium hypochlorite), and generally it has alot of other stuff in there too, I know that clorox bleach is 6% NaOCl, 5.63% NaCl, and .015% NaOH, and the rest it is just inert stuff and/or water. All you are concerned with right now is the NaOCl.
When you boil bleach, the NaOCl decomposes to form NaClO3 and NaCl,
3NaClO --> NaClO3 + 2NaCl
Sodium hypochlorite is very soluble in water (100 g / 100 mL), but sodium Chloride not so much by comparison. So the trick is getting the maximum possible amount of NaClO3 dissolved in the smallest amount of water possible and not have very much "other" stuff in solution, like NaCl.

This page,
http://www.wfvisser.dds.nl/EN/chlorate_EN.html#therm_starting
gives instructions on how to make chlorate both using electrolysis and thermal decomposition of hypochlorites.

You will see in those instructions that you are suppose to boil 1 L of 4% bleach down to 140 mL. If you do the math (and I have), you will find that this is alot more than is really necesary to hold the amount of NaClO3 you will have left after decomposing the NaOCl. The reason is because there is all that other stuff in solution too. Actually, in practice, if you follow those instructions, there will be NaCl comming out of solution even before your done boiling.

Anyway, so now you have a solution of NaClO3 and some NaCl. But you wanted KClO3, not NaClO3!! to turn the sodium chlorate into potassium chlorate, you can use a double replacement reaction between the NaClO3 and KCl. The potassium ion will push the Sodium out of the NaClO3 and replace it, and then the Na ion will join up with the Chlorine ion,
NaClO3 + KCl --> KClO3 + NaCl

After you do this, you should notice a white percipitate forming. This because unlike NaClO3, KClO3 is not nearly as soluble, not even close.
But to maximize yeild, we want to get all the KClO3 out that we can, so we cool the solution down to just around 0 degrees celcius, and then filter out the percipitate, which will be mostly KClO3 and some NaCl.


The Key to the whole reaction is that bleach (NaOCl) will decompose and form NaClO3, which can them be turned into KClO3.

the electrolytic method is much more complex, but is explained in the web page provided above.

[Letda]

I understand this alot better than before, so thnx. But, where do you get potassium chloride, is that the salt substitute? and is the NaCLO3 worth anything in that form or must the Na be replaced with the K?

[mrjeffy321]

I buy my Potassium Chloride as a salt substitute, called, "NoSalt", there are also salt substitutes (I think called "LoSalt"), but these also contain a large part sodium chloride, you want to get the one with as much potassium chloride as possible.
Sodium Chlorate is in itself worth something. It will react very similar to KClO3, but because of its high solubility, it is hard to extract. alot of the time in chemical formulas for pyrotechnic things, KClO3 and NaClO3 are interchangeable.

[Letda]

so let me make sure im understanding this. When you boil the bleach, you get NaClO3 crystals after filtering the liquid, or is the liquide the NaClO3?

[mrjeffy321]

by boiling bleach, you make NaClO3 AND NaCl.
Since NaClO3 is so much more soluble than NaCl, most (or all) of the crystals that percipitate out will be NaCl, and the NaClO3 will remain in solution.

Then when you add KCl, you make KClO3 and NaCl. this time NaCl is much more soluble than KClO3, so most of the percipitate is KClO3 and then NaCl remains in solution.

[Letda]

Thnx,i just bought everthing 10 mins ago so ill be testing everything tomorrow, ill let you knogw how things o. thnx for all of the help.

[Letda]

well, my first run was a complete and utter failure....all i got was a bunch of brown and black stuff. I filtered it out, added the KCl and recooked...same thing...and i got no noticable crystals the first time? i guess ill start round two here in a bit...any suggestions?

[Letda]

ok, i managed to get KCl pure crystals using the boiling process, but i dont know how the bleach is suppposed to work, i boil and all i get is a bunch of brown and balck crap. no crystals form, im i boiling to much or not enought or what?

[mrjeffy321]

Are you following the instructions in the link I provided a couple posts back,
http://www.wfvisser.dds.nl/EN/chlorate_EN.html#therm_starting
I found if you follow these instructions pretty closely, you will have very good results, although some deviation can be made to see what works best.

You should boil the bleach in a pyrex / heat resistant glass container optinumy, definatly not metal.

[Letda]

i was using metal, it said stainless steel on the site if i remeber right. i guess ill get glass then. Ill get back to you when i use the glass.

[mrjeffy321]

I used to use stainless steel, and I kept getting some brown stuff in the mix while boiling. At first I thought it was a product from the reaction, although I couldnt explain what it was, and now I realize that it was most likely Iron Oxide being made when the bleach oxidized the Iron in the pan (my first clue is when it ate throught the pan and I had a big hole in it).

Glass is definatly best, although you need to be more careful with it. I use a old coffee pot that can take the heat.

[Letda]

i just bought some glass bake-ware, hopefuly if i dont heat it up too fast it wont shatter. I mean if all else fails... I have on old coffee pot of my own so i can further follow in the steps of my mentor...lol.

you wouldn't happen to have anymore vidoes would you? I'm curiuos to see what you've been doing with 9 months supply. =)

[mrjeffy321]

Any more videos? how did you know about those?....o wait, I remember posting those 2 videos to show the difference in flame color of the two batches of KClO3.
I do have a few more of some interesting stuff I did with the KClO3 (ending dramatically on Febuary 18th), but they are too large to show.

Now, I mostly just use it in small (less than 50 grams) pyrotechnic things. Right now, my stock pile is a little less than 200 grams of KClO3. Hopefully I can get my electrolytic cell up and working again.

[redwraith94]

I was going to try the electrolytic cell myself, but after reading one of the links that you posted mrjeffy321, I decided to do the bleach method instead. I have tried the electrolytic methid before w/ Sodium chloride, and never was able to spend money for proper electrodes, so it always ended up something that I wasn't happy with. I just bought a gallon of the cheapest bleach that I could find. I'll keep you guys posted on how it goes.

[Letda]

well, i just wanted to let you know the glass worked wonders and i got exactly what i was looking for but....in the midst of all of my happiness, while cooling off....it shattered. i was so disappointed to say the least. Now i cant find anything anywhere to use thats glass and can go on the stove. if you know of anybrand or place to buy it i would be more than happy to hear about it.

OH, and good luck to you redwraith94, its kind of a pain in the butt, but im sure youll have no promblems once you get going.

[mrjeffy321]

but....in the midst of all of my happiness, while cooling off....it shattered.
Oh no, I feel your pain.

Like I said before, I use an old [easily 15 to 20 years old] coffee pot, and as long as I treat it carefully, it works very well. Now-a-days, I dont think they make coffee pots as good as used to, alot of the ones I see say specifically not to boil water in them, and others NOT FOR STOVETOP USE.
Supposidly, Pyrex brand glassware is good for this type of thing, but even that must be made in different "Grades" of heat resistivity because all the pyrex I see in the store has that "Not For Stovetop Use" warning on them.
there are laboratory glassware peices designed to withstand high temperature conditions, that might be a possibility.

[Letda]

My experiments are going to be post-poned for today at least, and probably tomorrow due to an unexpected direct assult from the flu virus...lol. but, not to worry, progress will presume soon enough and you'll know all aoubt it.

[redwraith94]

Normal glass is mostly SiO2 (Silicon Dioxide) with alot of other impurities/color additives as well. Pyrex has B2O3 (Boron Oxide) as an additive.

The thing is that B2O3 expands ALOT less than normal glass (SiO2 + whatever...Na...K...Ca...etc.) so the more Boron in the glass, the less it expands when heated, and the less it contracts when cooled. Since the glass moves less it produces much less internal stresses, which is why lab grade pyrex can usually be heated w/ a propane torch, or a bunsen burner w/ no problems @ all.

http://cgi.ebay.com/ws/eBayISAPI.dll?ViewItem&category=26237&item=7526217836&rd=1&ssPageName=WDVW

This is one that I will probably buy when I get paid since it will hold an entire gallon of bleach @ one crack. I am not sure if this can be used stove top though, I will have to check w/ the seller first, and you probably should too if you go to buy it.

[mrjeffy321]

You want to boil an entire gallon of bleach in one batch?
When I use the boiling method to make chlorate, I usually use 1300 mL of bleach (which is all my coffee pot will hold without overflowing when it boils), and it takes quite a bit of time to boil all the excess water away and process the remains. From when I begin to heat the bleach, until when I put the KClO3 solution into the freezer, it takes about 4 hours. Given most of the time is waiting for the liquid to boil and then cool down, but an entire gallon, WOW, someone is patient.

[redwraith94]

Yeah, if you think that is patient, wait till you here how I made my first batch. I actually used a pyrex glass bread pan (not lab grade) and put it in the oven until all of the water boiled off. I had to do six batches for the entire gallon.

[mrjeffy321]

So, Letda, have you gotten any results yet, give up, still sick?


A [long] while back in this thread, I think I mentioned something about a program thatr could calculate the run time of an electrolytic chlorate producing cell. The program I am/was refering to is here (at bottom of page),
http://www.geocities.com/CapeCanaveral/Campus/5361/chlorate/table54.html
As great as this program may be, I think it leaves alot to be desired, so I decided to make my own.
Here is the link to a web site that you can download (283 KB) my program's install file so you can test it out yourself, I assure you it is safe, there is no virus, spyware or anything bad, it is totally safe.
http://www.geocities.com/platapus453/Chlorate_Cell_Setup.zip
I would like for you all to test it out, tell me what you think of it, and possible give me some sugestions on how to improve it.
I personally think my program is wonderful just as it is, but I am looking at it through the eyes of a programmer and I marvel at some features I added that are taken for granted or expected in programs today.

***please note, since this program was written in Visual Basic .Net, it requres that your computer have the .Net framework (version 1.1) installed on your computer, which can be downloaded free from Microsoft***

[Cesium]

Alright, I have joined the quest to make potassium chlorate. I have decided to do the electrolysis of NaCl and then precipitation with KCl. I have a small batch precipitating now and I think it is working. Assuming I get KClO3, what ratios do you suggest for burning it with sugar? Anybody else try any cool things?

And also, How do you "manually" find out the amp-hours? I think I can only measure volts.

Thanks in advance.

[mrjeffy321]

I personally like the weight ratio of about 3 parts Chlorate to 1 part sugar (sucrose), or to be more precise, 2.86 KClO3 to 1 C12H22O11.
The more complete of a combustion you set it up to have, the cleaner it will be (ie. less smoke), you dont want too much/any excess sugar because when/if that starts to burn, it makes alot more smoke and leaves a dark residue behind.
I have tried lots of "cool things" with KClO3, many of which included rocketry [notice the past tense]. Then on Feburary 18, 2005 (a date etched [or rather exploded] in to my memory), I found out how dangerous the stuff could be.


Measuring the amp hours through the cell is very critical, it will determine how long you should run the cell and how much Chlorate you can expect to get. There are two basic method of measuing amp hours, either directly with a meter (an amp hour meter, which I tried and failed at building [unless someone with electrical skills wants to help :wink: ]), or indirectly through taking measurements and keeping a tally. Since I dont have a meter, I have been forced to do it the hard way, measure the current (amps) through the cell with an ammeter, then from that, I estimate an average current for that period of time, which I then can get my amp hour reading from. It is a hassel if you want to do it correctly. The more readings you can take, the more accurate you will be, and when you have to estimate, round down, not up, it is better to put too many amp hours through the cell than not enough.
I recently had an idea about using a watt hour meter as an amp hour meter substitute. Since power (watts) is equal to Volts * Current, and watt hours is power * time (time being in hours), if you divide watt hours by the average voltage through the cell, you should get amp hours. But I cant find any watt hour meters that will measure DC current in a reasonable price range.

[Cesium]

I have a multimeter and it only measures volts and ohms. Guess I need to buy an ammeter now.

I am guessing that the current changes by itself as more chlorate is produced. Otherwise you wouldn't have to keep on recording values. If you have a constant source of power and the cathode-anode spacing remains the same, the current wouldn't remain the same also?

[mrjeffy321]

Using Ohms law,
V = R*I
Volts = Resistance * Current, if you can measure volts and ohm, then you can determine the current.
However, I dont trust multimeters to measure resistance for me, ESPECIALLY through an electrolytic cell. I would recommend getting yourself an amp meter (preferable one that can meaure high currents, atleast a couple amps).
In a perfect world, the resistance through the cell would remain the same and that would make things much easier. But in reality, the resistance depends on many things, electrolyte concentrate (the solute and solvent will varry as the cell ran), temperature of the cell, temperature of the wires, ... .
The current will change all the time, atleast in my cell it does, sometimes you'll be lucky and it will stablelize for a while, but most of the time it will fluctuate (not drastically, but enough to make a difference).
What is your power source? Make sure it can handle outputting several amps of current if you dont plan on waiting a month for the cell to be finished, the higher the current, the less time you have to wait.
Side Note:
I ran my cell for the entire month of Febuary (1st through 28th, not continous mind you), I put 653 amp hours through the cell, and I made a total of 140 grams of NaClO3, which gave me an efficeny of 28.3%, quite pathetic. I hope to hear some better results from you.

[Cesium]

Yes I have read extensively about your successes and failures. You sure have stuck with it though!

My power source is a battery charger for a drill. It's great because I get a constant flow going without batteries dying and whatnot. It gives 3.5 volts, no clue how many amps. I read on one of the sites that was linked here that 3-4 volts was recommeded.

What do you think about using several anodes and cathodes? Wouldn't the amperage increase by using 2 or more power sources connected to different sets of electrodes in the same cell?

Also, what color is your solution normally after you have run it for a day or so? On one unsucessful attempt it was brownish-yellow because of all the saturated chlorine and hypochlorous ion (I think). This time it was pretty much clear with particles of graphite flowing around.

Thanks again for all your help!

[mrjeffy321]

Yes I have read extensively about your successes and failures. You sure have stuck with it though!
I like when people appreciate my work, it makes all the log taking and number tallying worth while. I seem to have become somewhat of an expert on a certain, specialized, topics here.

The power souce is outputting just the bare minimum need for the reaction to occur,
"The supply must be a DC supply with a current capability of at least what you want to run the cell at and a voltage above 3.5 volts (more if you are making perchlorate)." - source (http://www.geocities.com/CapeCanaveral/Campus/5361/chlorate/powersup.html)
So technically, it would work. Keep in mind, as I said before, the more amp the better, and current is dependent on voltage (V = R*I), so assuming the resistance in the cell stays roughly the same, the higher the voltage, the higher the current. I use a computer AT power supply, I switch back and forth from using the +5V (gives me about 2.5 amps) and +12V (gives me about 8.0 amps) outputs. In this type of cell, I dont thinking having an over voltage will hurt any (until you get down to less than 10% chloride, then you'll start making per Chlorate).

Using more electrodes will increase the current since the combined surface area on the electrodes is greater. I use carbon-graphite electrodes which erode away slowly through use. It is good to have a very low current to surface area density on the annode (+) in order to slow the erosion, however the cathode (-) doesnt seem to erode at all, or atleat non-noticeable amounts. So using several annodes will help reduce the current density, but it will also help distribute the chlorine production thoughout the cell, thus increasing the amount of chlorine dissolved in solution. With less of the chlorine escaping into the atmoshere (besides making it better for you), it will dramtically increase efficency. I wouldnt recommend using multiple cathodes, I dont see the need, if you have the spare electodes, use the for extra annodes if anything (or spares for when one is used up).
Uisng more than one power source on the same cell is tricky and I dont recommend it. For one, it is easy to burn out a power supply that way (I have done it), also, it doesnt seem to help that much I find. You would only need to have one ground connection to one cathode, but then you could have multiple annodes connected to the outputs of several powers supplies, but this makes the total current harder to measure.

Since I use carbon-graphite electrodes, after a day of running it, my solution is as black as the nigh (especially if I use high current most of the say). If I filter the carbon out, then I am left with a yellowish liquid that looks and smells like bleach, because it is. I can then boil that down to decompose the hypochlorite (which I need to do the take a pH reading with my litmus paper), and then it becomes much cleater - almost transparent.

Have you or anyone else had a chance to look at my program to calculate the running times for a chlorate electrolytic cell (mentioned about 6 post back)? I am eager to get some user feedback on it to see how I can improve it.

[Letda]

yeah, iv been gone a while...sorry. I have to admit i've almost given up. I have been through 2 more glass "pots", and they keep shattering on me...its extremely frusturating. I'll try again in a few more days, [i have to work mornings now...:-(...so]. and If i break another glass i think im going to try the electronic method....

[Cesium]

Nice work! I downloaded your program today. It's going to be really useful. There's no way I can really tell yet if it is accurate though. Once I get an ammeter, I am going to test it out. I'm going to see what my yield is and then calculate the efficiency of my cell using that.

[mrjeffy321]

I first got the idea for the program from this site (program link at bottom),
http://www.geocities.com/CapeCanaveral/Campus/5361/chlorate/table54.html
the two programs give the same ansers, so either we are both wrong, or both right.
In the program, I found out how much charge must be used to convert x amount of chloride to chlorate, I believe it is 6 faradays per mol of chloride converted, then it is simply a matter of adjusting for efficency (I think if you just leave the cell alone and not try to adjust pH or anything, you average about 50%, so that is the default efficency in the program).

[jeffomatic]

I make potassium chlorate by electrolyzing "diet salt". I use a 1 quart stainless steel kitchen pot with a glass lid that has a hole in the middle, left after removing the plastic knob. I made an anode holder that fits in this hole. I use battery carbon for the anode and a hefty battery charger for the source of DC. I mix a concentrated solution of the diet salt, then start the charger on the lowest (6 volt) setting. I adjust the depth of the anode to get 4 amps and let it run for 24 hours. The I filter the solution and boil it for a while and set it in the fridge. The potassium chlorate crystals will precipitate first. The solution decanted can be returned to the electrolyzer and more salts and water added for another batch. The crystals can be washed with ice water to clean them, then re-disolved in hot water, boiled and crystalized again to purify them.

The diet salt works great, it is a mix of half NaCl and half KCl. The only trouble is that it contains iodine too. It takes extra filtering, as it turns the whole solution dark reddish brown. I filter the iodide out with a cloth filter in a funnel, followed by a toilet tissue wad in a funnel to get more of it out. The iodine forms a dark brown glop which filters out reasonably well, but the filtered solution is still somewhat yellow.

Don't get copper or other metals in the chlorate because it can make it unstable. I only prepare it in small amounts because of the potential for instability. I store it in the fridge with a loose-fitting lid. Don't mix KClO2 with things until you are ready to use it, especially sulfur. Assume all mixtures using chlorates can be impact sensitive, so don't tamp them into any container. Read all you can about hazards and mixtures before messing with chlorates!

[mrjeffy321]

The diet salt works great, it is a mix of half NaCl and half KCl. The only trouble is that it contains iodine too.

Don't mix [KClO3] with things until you are ready to use it, especially sulfur.
I dont think using diet salt is the best idea, since you have both NaCl and KCl, you will be making KClO3 as you are electrolysizing the solution. Since KClO3 isnt very soluble, it should percipitate out, so when you filter the dirty solution, you should be loosing some of your product. I still think it best to use just plain (cheap) NaCl to make NaClO3 first....then turn it into KClO3.

You salt has iodine in it? I have got to get me some of that. No, more likely than not, it has Potassium or Sodium Iodide in it, and a very small percentage at that. I think ordinary salt has about .02% NaI by weight, I am not sure about your brand of diet salt, but I cant imagine it is too much higher since in reality, the body doesnt need but just a very little amount.
However you seem to be descirbing that you find iodine crystals/blobs in your solution, implying that there is alot of Iodine being make, perhaps from alot of NaI in your salt. Does it have a list of ingrdients or something on the side with the % of everything?

You shouldnt be mixing KClO3 with sulfur anyway, dont even bother being careful because you shouldnt put yourself in that situation.
But yes, you need to always becareful when mixing KClO3 with a fuel to burn with, but I have found that KClO3 and sucrose is reasonaby safe/stable to be stored (not that it is a good idea to make a bunch and let it sit just to test the theory). In other words, dont mix it until you want to use it.

[gravenewworld]

seriously, what is up with this thread? why doesn't it ever die?

[mrjeffy321]

seriously, what is up with this thread? why doesn't it ever die?
Its no longer a thread, it is more of a steel cable now that it has grown to 9 pages long, granted there are longer threads out there, but this one is my favorite for some reason.


And by the way, as long as I am posting, I might as well post some useful KClO3 info pertaining to my experiments.
I have run two more trials in a newly designed cell (actually 2 separate cells but the same design). I have the electrodes positioned at the bottom sticking up through the solution with an open top.
On the first trial with the new cell I had some...interesting...results.
I have 220 grams of NaCl in solution with 600 mL of water. I began assuming 55% efficiency, so I needed to put about 800 amp hours through the cell. Then about half way through the trial, something happened, I don’t know what, but I must conclude it had something to do with my graphite anode eroding away and the solution turned green-ish brown and it wouldn’t filter out. I ended the trial, and long story short I think I had some copper compound that was some how introduced. I ended up making 58.7 grams of slightly off-white colored KClO3 after 403.1 mp hours, giving me an efficiency of about 40%.

After the above trial, I found my cell leaked for some reason, so I rebuilt it new, using the same design, then only difference was that I made a slight change to the electrodes. I greatly increased the surface area of the anode (about double the previous SA) and soaked it in linseed oil for 5 days, let it dry and then installed it in the cell. I had much better results. I did a smaller trial so I could get finished quickly to see how well my changes worked.
I assumed 50% efficiency at the start, dissolved 80 grams of NaCl in 500 mL of water and passed 170 amp hours through the cell. This time the new anode worked wonders, much less (but still considerable) amounts of graphite powder was left in the water and less visible erosion was detected. I ended up making 56.2 grams of KClO3, giving me 43% efficiency. However, this entire trial was designed to be a very quick and dirty experiment to test the new cell and anode design, I didn’t even worry too much about pH control, I am very pleased with the results.

I usually don’t bother to purify my KClO3 after I filter the precipitate out of the solution the first time, causing it to burn with a yellow color (instead of the purple color it should have), but since I got an off-white KClO3 in the first trial I mentioned in this post, I decided to try it.
The color improved, it became much cleaner, but still not the snow white I am used to getting, and it still burned with a yellow flame, so apparently the purification process isn’t fool proof, but what I might do is take maybe 100 grams of the "good" stuff I have just sitting around and try to purify that. I would prefer the purple burning powder, but for what I use it for, the color doesn’t matter much.

[dx/dy=?]

Keep it up mrjeffry.

Your perserverance is inspiring.

[Cesium]

I'm wondering what thoughts anyone has on preparing KClO3 with K2CO3, described here: http://www.frogfot.com/synthesis/chloratedisprop.html

3K2CO3 + 3Cl2 ==> 5KCl + KClO3 + 3CO2

Ways of making K2CO3:

Fractionally crystallize K2CO3 from Na2CO3 and K salt or

5C12H22O11(s) + 48KNO3(s) => 24K2CO3(s) + 36CO2(g) + 55H2O(g) + 24N2(g)

HIGHLY exothermic and often does not go to completion.

Or make NaClO3 first from Na2CO3 then add KCl to get KClO3

Or can K2CO3 be purchased?

Thoughts, problems, or experience are appreciated.

[mrjeffy321]

I dont know anywhere off hand to get any Potassium Carbonate, but perhaps it could be obtained by heating baking soda (Sodium biCarbonate) to make Sodium Carbonate, water and Carbon Dioxide.
Then using a double replacement reaction with KCl, turn the Na2CO3 into K2CO3. Sound good?
I dont like the idea of burning Sugar and Potassium Nitrate to make K2CO3, for one because it is unnecesarily exothermic (it makes for an impressive reaction, but why burn something just to get the byproducts), also, as you stated, you are assuming the combustion is 100%, which we know it will not be, therefore you'll have a bunch of other stuff mixed in with your K2CO3

How do you propose to make and bubble the chlorine through the heated solution? This method seems a little complex and time consuming doesnt it, especially since you making 5 times the number of moles of KCl in the reaction as you are of KClO3.

if you try it, I would love to hear the results and your impressions.

[Cesium]

Mainly just throwing it out here because this thread is the ultimate source for all questions dealing with KClO3. I guess I am just frusturated with the difficulty in predicting the yields of NaClO3 by electrolysis of salt and the amount of variables that are involved. But then again, my power source is sucky and I still don't have a multimeter, so I haven't really given it my best shot.

Cl2 would be generated with sodium bisulfate (or any acid) and bleach. I did this as a test and it made LOTS of chlorine gas with tiny amounts of each reagent. If you ever need chlorine do this.

[mrjeffy321]

While I am thinking about it, let me just post my results from my recent purification of the "impure" KClO3.

I started with 100.0 grams of KClO3. it had enough [Na] impurities so that when it combusted with Sugar, it was yellow rather than violet.
I dissolved it in about 200 mL of boiling water, le it boil for a little while, then cooled it. Afterward, I stuck it in the freezer overnight only to find that it had frozen solid (which doesnt lend itself to easily filtering out the percipitate) so I had to thaw it and then cool it back down in the refrigerator and then briefly stick it in the freezer.
By the time I filtered it, the solution was somewhere between the highly scientific temperature range of "refrigerator" and "freezer" temperature.

I filtered it, dried it, and weighed the KClO3 extracted back out to be 81.5 grams. When I combusted it with sugar, the light it gave off was very bright more than anything really. There was still some yellow, but it had shifted considerably towards bright white and perhaps just the faintest of hints of violet. So I ended up loosing about 20 grams of KClO3 in order to make some slightly more pure, but hardly noticible, KClO3 cystals.

[Cesium]

I am happy to report that my first proper attempt at making potassium chlorate was a success. I pretty much used the most OTC methods possible so my cell wasn't too great. 70g NaCl in 200mL water with a graphite anode (from old lantern battery) and stainless steal (4" cap screw) cathode in a polypropylene container. Electrodes were usually around 2-5cm apart and I tried to keep the temperature around 40-50C. Electricity came from a computer power supply of course at 12V (way too much I know...should have hooked multiple smaller cells in series but I only thought of that three-quarters of the way through!) and the current averaged 2.11 amps. HCl was added once or twice a day, but I didn't bother to measure pH. The cell was run for 115.9 hours for a total 9.14 faradays; this corresponds to a 56% efficiency. Of course, the standard horrible and yucky way of logging the amps periodically was used to calculate the approximate charge. This was the only part of the process that was at all annoying...the rest was easy and quite enjoyable :approve:

The jet black solution filled with the graphite sludge of several anodes was filtered three times and then boiled to destroy residual hypochlorite. At this point I had a yellow solution (Fe+2) tinted brown due to collodial graphite that could not be removed by filtration. I added 65g of KCl (salt substitute) to 250mL of water, mixed the two solutions, boiled the mix down, and began crystallization. This crop of needle-like crystals were discolored yellow and green due to iron and chromium impurities, respectively (and probably some graphite too). I then redissolved and recrystallized them, washed them with ice-water, and dried them in a toaster-oven. I ended up with about 48 grams of a nearly perfectly white powder which is a 46% yield. Not too great, but I think I actually needed to run the cell longer.

This is probably the only section of my post that merits a response. The stuff burns with a nice lilac flame, but it tests positive for chloride ions when silver/copper nitrate is added (a white precipitate forms). The flame color, however, indicates that they are very few sodium ions in the product. I guess there could be KCl but doesn't make too much sense due to its higher solubility. There were some other impurities listed in the salt substitute (calcium or magnesium silicate and something else that I can't remember) so perhaps this is what is precipitating. Or else there are just so few Na+ ions in there that there are overpowered by the K+? This is doubtful because flame tests are very sensitive to sodium ions....odd.