WSM Posted April 21, 2014 Posted April 21, 2014 (edited) Industrially, solubilities make sodium a necessity. For a home cell, we aren't constrained by the same requirements. Might as well try both and see if potassium is really too big of a hassle for you personally. Chloride to chlorate can be done with potassium quite well. I wonder if the potassium chlorate to potassium perchlorate is harder on the anode than sodium salts would be? For potassium chlorate, I subscribe to the KCl to KClO3 direct method. But due to the solubilities, it seems the best (or should I say, the easiest) route looks like 1) NaCl to NaClO3 and then 2) NaClO3 to NaClO4 and next 3) NaClO4 to KClO4. I believe the removal of sodium from the final product won't be as problematic as others have made it out to be. I'll try it and see . WSM Edited April 21, 2014 by WSM
WSM Posted April 21, 2014 Posted April 21, 2014 (edited) Ok I got a cell started to make sodium chlorate. I am using table salt because I can't really think of much else I could use... the problem is, how do I actually purify sodium chlorate? I think sodium chlorate has a higher solubility than sodium chloride so it means I have to put massive amount of salt in the cell before I get anything right?Also, it appears table salt has additives such as potassium ferrocyanide... others have trace amounts of potassium iodide. Are they a problem? Maybe. Perhaps Mumbles will add input here. I have pure sodium chloride to use (designed for salt water chlorination of swimming pools) and think uniodized table salt may also be available. Perhaps there are methods of purifying the table salt you have, to eliminate the unwanted ions . WSM Edited April 21, 2014 by WSM
WSM Posted April 21, 2014 Posted April 21, 2014 (edited) If you want to make perchlorate, it is better to do it with sodium salts. Potassium chlorate can be converted into perchlorate but the solubility for potassium chlorate is worse so it will be more challenging. I might try a batch and see how it works... Swede did this a few years ago and it was successful (proving it's possible). Read through his blogs. The question is, is it the best way?! I'm sure that depends on the individual. I've reasoned the best method for me to try is the sodium salts to perchlorate and then exchange with KCl solution to KClO4. The residue (NaCl solution) can then go into the NaClO3 system as "make-up" water. By using a vacuum filtration system to harvest KClO4 and following with a chilled (5oC) deionized water rinse; the removal of trace amounts of sodium is greatly simplified, yielding a "pure" product. WSM Edited April 22, 2014 by WSM
Mumbles Posted April 22, 2014 Posted April 22, 2014 I wouldn't worry at all about the iodine in the salt. There is a miniscule amount of iodide or iodate in iodized salt, that it's basically a non-issue. In a kilo of salt, you'll probably have around 50mg of the iodizing agent. Whatever it is will probably be oxidized anyway, and can be removed during recrystallization. If you don't want to deal with any additives, look for salt sold for canning or pickling. This doesn't have any iodine in it.
WSM Posted April 22, 2014 Posted April 22, 2014 (edited) Oké i tougth that you just want a make just naclo3. But for perchlorate is it better to use sodium. If you want to make it more pure. You realy have to boil it down. I did i a few Times in a oud cooking pot. With no problems. If I understand you correctly, I don't see the point in making sodium perchlorate for use in pyrotechnics since it's deliquescent. I only desire to make it as an intermediary to making other (more useful) perchlorates. Also, I agree with the sentiment (of others) in using borosilcate glass (lab glass) for boiling solutions of these salts, if needed. Metal pots will potentially add unwanted ions to the oxidizers. WSM Edited April 22, 2014 by WSM
WSM Posted April 22, 2014 Posted April 22, 2014 I wouldn't worry at all about the iodine in the salt. There is a miniscule amount of iodide or iodate in iodized salt, that it's basically a non-issue. In a kilo of salt, you'll probably have around 50mg of the iodizing agent. Whatever it is will probably be oxidized anyway, and can be removed during recrystallization. If you don't want to deal with any additives, look for salt sold for canning or pickling. This doesn't have any iodine in it. Thanks Mumbles. Do you think the potassium ferrocyanide could be an issue?
taiwanluthiers Posted April 22, 2014 Posted April 22, 2014 I think the ferrocyanide is used as an anticaking agent or something... I guess as long as they don't put sodium flouride in the salt it would be fine. I guess the concern with turning potassium chlorate into perchlorate is low chlorate concentration causing anode damage, but what Swede did was boil the water beforehand, and the heat of the cell keeps solubility up (Pot. Chlorate is quite soluble at high temperature) I mean Swede used platinum anode which is much more susceptible to being damaged than LD. By the way how goes the initial test with your slightly damaged Chinese LD?
pyrojig Posted April 22, 2014 Posted April 22, 2014 I think Taiwanluthiers made a point that answered your Q in a round about way WSM. ....The Use of the platinum seems more prone to degradation than the LD in a low chlorate Sol. Im sure if any chloride is present then the damage is far greater. I would imagine this to be even more true as WSM stated when the power is off , and the liqueur can attack the electrodes .
WSM Posted April 22, 2014 Posted April 22, 2014 I think the ferrocyanide is used as an anticaking agent or something... I guess as long as they don't put sodium flouride in the salt it would be fine.I guess the concern with turning potassium chlorate into perchlorate is low chlorate concentration causing anode damage, but what Swede did was boil the water beforehand, and the heat of the cell keeps solubility up (Pot. Chlorate is quite soluble at high temperature) I mean Swede used platinum anode which is much more susceptible to being damaged than LD.By the way how goes the initial test with your slightly damaged Chinese LD? I've gone so far as to gather the materials for a "quick and dirty" test (the LD anode, a piece of CP titanium sheet for a cathode and 500g of reagent grade sodium chlorate). I think I'll use a 4 Liter beaker (borosilicate glass) for the experimental cell and a 6Vdc power supply. I imagine it will run for a couple days or possibly more. I hope to photograph the parts and document this test. WSM
WSM Posted April 22, 2014 Posted April 22, 2014 I think Taiwanluthiers made a point that answered your Q in a round about way WSM. ....The Use of the platinum seems more prone to degradation than the LD in a low chlorate Sol. Im sure if any chloride is present then the damage is far greater. I would imagine this to be even more true as WSM stated when the power is off , and the liqueur can attack the electrodes . You're right about the platinum anodes, but I'm not very experienced with the PbO2 anodes yet. As for the negative effect on electrodes when powered down, this is true for chlorate cells. I'm not certain about perchlorate cells, since the electrolyte is primarily saline and not as potent (corrosive) as the chlorate cell electrolyte. I could be wrong, but I'm sure we'll soon see! WSM
taiwanluthiers Posted April 22, 2014 Posted April 22, 2014 By the way how does the presence of sodium chlorate affect the solubility of sodium chloride? Would it be safe for me to just keep adding solid sodium chloride to the cell and topping up with water as needed?
WSM Posted April 22, 2014 Posted April 22, 2014 By the way how does the presence of sodium chlorate affect the solubility of sodium chloride? Would it be safe for me to just keep adding solid sodium chloride to the cell and topping up with water as needed? I'm not sure of the effect adding solid NaCl would have in the NaClO3 solution. Since the process consumes water, I think adding an NaCl solution makes more sense, but if you try adding dry salt, tell us how it goes. WSM
taiwanluthiers Posted April 22, 2014 Posted April 22, 2014 I realize the process consumes water but I don't think it does so fast enough
pex Posted April 22, 2014 Posted April 22, 2014 This is my cell. Tomorrow i gonna fill im with naclo3.
WSM Posted April 23, 2014 Posted April 23, 2014 (edited) Hi pex, Looks good. Let us know how it goes. I can't seem to find my 4 liter beaker yet. I'll keep looking but I may have to use something else for the cell body. I did find a bottle of distilled water to use (I'm getting closer to being able to run the perchlorate cell). WSM Edited April 23, 2014 by WSM
taiwanluthiers Posted April 23, 2014 Posted April 23, 2014 (edited) I am still running a sodium chlorate cell. Not sure what is the rate of water consumption but it doesn't seem to consume water all that fast. Seems like chloride is getting consumed faster than that. The LD anode is in the mail, I will have to figure out how to make the cell itself. It will be a while before I have enough sodium chlorate to try however... maybe I'll start out with potassium chlorate. BTW I placed some potassium chlorate crystals on some sidewalk weed, and it's dried and dead. Now I need to figure out how to get it on vertical plants. Edited April 23, 2014 by taiwanluthiers
pyrojig Posted April 23, 2014 Posted April 23, 2014 Pex, I noticed that your cell is using alligator clips as a connector. There will be losses and waste of power to the electrodes . Heat will be one of these , and any oxidation will reduce the connection even further. If I where to suggest anything , it would be to bolt on your wire via connectors etc.. This will maximize the power delivered . @WSMYou do have a point there. on the electrodes , I was still in chlorate mode (thinking) I guess that the electrodes may be inert to the liqueur ......hmmmmm Guess your gonna have to get that 4l beaker and give it a go
WSM Posted April 24, 2014 Posted April 24, 2014 Pex, I noticed that your cell is using alligator clips as a connector. There will be losses and waste of power to the electrodes . Heat will be one of these , and any oxidation will reduce the connection even further. If I where to suggest anything , it would be to bolt on your wire via connectors etc.. This will maximize the power delivered . @WSMYou do have a point there. on the electrodes , I was still in chlorate mode (thinking) I guess that the electrodes may be inert to the liqueur ......hmmmmm Guess your gonna have to get that 4l beaker and give it a go pex, pyrojig is right about the alligator clips. Bolting the wires to the electrode leads is best. I like the rest of your setup though. I'm still having trouble finding the Pyrex (borosilicate glass) reaction vessels I would like to use for my perchlorate test. I may have to use one of my old PVC reaction chambers and see how it goes. WSM
taiwanluthiers Posted April 24, 2014 Posted April 24, 2014 PP seems to work just fine... I mean it works for chlorate.
WSM Posted April 24, 2014 Posted April 24, 2014 (edited) I am still running a sodium chlorate cell. Not sure what is the rate of water consumption but it doesn't seem to consume water all that fast. Seems like chloride is getting consumed faster than that. The LD anode is in the mail, I will have to figure out how to make the cell itself. It will be a while before I have enough sodium chlorate to try however... maybe I'll start out with potassium chlorate.BTW I placed some potassium chlorate crystals on some sidewalk weed, and it's dried and dead. Now I need to figure out how to get it on vertical plants. That parallels my experience with weed killing. If you mix the chlorate with some sort of sticky, water based gel, that might do the trick. WSM Edited April 24, 2014 by WSM
WSM Posted April 24, 2014 Posted April 24, 2014 (edited) As to the PGI articles I've been writing, I'm working on part 5, but just received the bulletin with part 3 in the mail today. Part 5 is about continuous systems and part 6 will be about perchlorate cells (if all goes according to plan). WSM Edited April 24, 2014 by WSM
pyroChile Posted April 24, 2014 Posted April 24, 2014 (edited) Hello! I have a question.. in this link (http://www.wikihow.com/Convert-a-Computer-ATX-Power-Supply-to-a-Lab-Power-Supply) shows that connecting the +5 v and +12 v are obtained 7v. Is it useful for perchlorate? How many amps would deliver that connection? =) Edited April 24, 2014 by pyroChile
WSM Posted April 24, 2014 Posted April 24, 2014 PP seems to work just fine... I mean it works for chlorate. That is an option. I also have access to PVDF materials I could form a reaction chamber from, but welding PVDF takes specialized equipment and techniques. Solvent welding of PVC or CPVC is much easier and may be the best option. We'll see... Thanks for the suggestion, taiwanluthiers. WSM
taiwanluthiers Posted April 24, 2014 Posted April 24, 2014 Just wondering, I'm using the +5v on the power supply for chlorate cell, but should the voltage be the same or higher for perchlorate cell? I really hate the fact that oxidizing.110mb.com is gone, it had so much information.
WSM Posted April 24, 2014 Posted April 24, 2014 Hello!I have a question..in this link (http://www.wikihow.com/Convert-a-Computer-ATX-Power-Supply-to-a-Lab-Power-Supply) shows that connecting the +5 v and +12 v are obtained 7v. Is it useful for perchlorate? How many amps would deliver that connection?=) Hi pyroChile, The article link is one I've seen, and 7Vdc is useful for perchlorate cells. The current delivery depends on the power supply and the configuration of the setup. I'm planning on using 6Vdc with my first experiments. Let us know how it works for you. WSM
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