Maserface Posted June 5, 2016 Posted June 5, 2016 Well, the way you know is by which you started with. If you find out how to turn a sodium cation into a potassium one, be sure to let us know 1
schroedinger Posted June 6, 2016 Posted June 6, 2016 (edited) Differentiating them is easy, if they are pure to a flame color test. Yellow Is sodium pinkish is pottasium a mix will be yellow. Here you could use a cobalt glass to check for pottasium (filters out the sodium yellow color). Else solubility is your friend. Just calculate how much water you need to dissolve your ammount of chlorate, if it is sodium chlorate (@20ºC). Now you dissolve everything in that ammount + 10% of boiling distilled water and let it cool down again (if you lose to much water to boiling, top it up). Now, if you get a lot of cristalls (normally flat flakes) cool down to 2ºC and harvest your pottasium chlorate. If you don't get cristalls, you have sodium chlorate. If justa little bit dropped out again cool to 2ºC a d harvest the pottasium chlorate and drive the water out of the liquor to get the sodium chlorate out of the solution. The pottasium will need propably two cycles tk get sodium and chloride free. Edited June 6, 2016 by schroedinger 1
Mumbles Posted June 6, 2016 Posted June 6, 2016 Differentiating them is easy, if they are pure to a flame color test. Yellow Is sodium pinkish is pottasium a mix will be yellow. Here you could use a cobalt glass to check for pottasium (filters out the sodium yellow color).Else solubility is your friend.Just calculate how much water you need to dissolve your ammount of chlorate, if it is sodium chlorate (@20ºC). Now you dissolve everything in that ammount + 10% of boiling distilled water and let it cool down again (if you lose to much water to boiling, top it up). Now, if you get a lot of cristalls (normally flat flakes) cool down to 2ºC and harvest your pottasium chlorate. If you don't get cristalls, you have sodium chlorate. If justa little bit dropped out again cool to 2ºC a d harvest the pottasium chlorate and drive the water out of the liquor to get the sodium chlorate out of the solution. The pottasium will need propably two cycles tk get sodium and chloride free. ???? If only http://www.louis-roederer.com/sites/default/files/images/bottles/cristal_2.jpg 1
OldMarine Posted June 6, 2016 Posted June 6, 2016 Hehe! Nothing better than a taste test! Just a faint hint of the soil of the Valley with a crisp, clear chlorate finish!
WSM Posted June 6, 2016 Posted June 6, 2016 Well, the way you know is by which you started with. If you find out how to turn a sodium cation into a potassium one, be sure to let us know Potassium chlorate has a monoclinic crystal structure and sodium chlorate has a cubic crystal structure (similar to NaCl). Besides that, the flame test will quickly tell which one or if both are there (I need to get another piece of cobalt blue glass ). WSM
OldMarine Posted June 6, 2016 Posted June 6, 2016 I'm convinced I'll absorb/adsorb something from these threads!
OldMarine Posted June 6, 2016 Posted June 6, 2016 As I think Mase was saying, wouldn't your beginning chems dictate your outcome? Would there somehow be an elemental shift? Never heard of that without a reactor core!
WSM Posted June 6, 2016 Posted June 6, 2016 (edited) As I think Mase was saying, wouldn't your beginning chems dictate your outcome? Would there somehow be an elemental shift? Never heard of that without a reactor core! I think he may be recalling memo's tendency to run sodium chloride to chlorate and then use metathesis to change it to potassium chlorate with KCl solution. We've mentioned starting with potassium chloride solution to him, but we're not sure he's tried it yet. The main problem is he's using a platinized titanium anode and we're worried he's going to destroy it at some point (especially with the high chlorides at the start of his runs). Unless memo proves the warnings false, we're expecting some day he'll tell us the anode is dead . If you only use one system, then the answer is simple. If you mix the materials and forget where you are in the process, then simplicity goes out the window. WSM Edited June 7, 2016 by WSM
WSM Posted June 6, 2016 Posted June 6, 2016 How do you differentiate between the two? From my experience, when you do the test with sodium chloride, the flame color is bright yellow; and with potassium chlorate it's whitish (off white?!). WSM
OldMarine Posted June 6, 2016 Posted June 6, 2016 How could the two be co-mingled? Wouldn't the precursors determine the output? Sodium in= Sodium product out. Right?
Maserface Posted June 6, 2016 Posted June 6, 2016 I'm sorry, I couldn't recall if memo had added potassium chloride yet, so I was (half jesting) that if he had run sodium chloride he would have sodium chlorate etc. Carry on, gents 1
Arthur Posted June 6, 2016 Posted June 6, 2016 There are books (big books) by Vogel, titled quantitative and separately qualitative inorganic analysis. The book started in about 1900 and is kept up to date. BUT older versions escape onto the web as downloadable files -big files! Once you need to check for presence of chlorate or perc you need Qualitative methods from that book Quantitative analysis will tell you how much of each you have present.
MrB Posted June 6, 2016 Posted June 6, 2016 (edited) If you add an after filter to the RO system (with the right kind of resins) you can turn the RO into DI water (0 dissolved solids) and run much cleaner electrolysis operations. I'm considering doing that myself (I only hesitate because of the cost). Again, check eBay, for aquarium supplies. They have "cheap" canisters for ion exchange media as granulate, and usually bulk granulate is cheap as well. Don't pay extra for color-changing stuff. (Truth be told, i don't know if non color-changing stuff is still a thing.) B! EditI say again, since i keep returning to that recommendation for various supplies./Edit Edited June 6, 2016 by MrB
WSM Posted June 7, 2016 Posted June 7, 2016 (edited) I just submitted Homegrown Oxidizers Part Fourteen to the PGI Publications VP, for addition in one of the upcoming Bulletins. It describes my travails during the last few months, getting to where I am now with the sodium chlorate cell. Things keep running, and according to one of my associates in the effort, he expects it'll have to run a month and a half before it's complete (he actually estimated 45 days with a quick mental calculation) ! We'll see if he's right and how well things go... WSM Edited June 7, 2016 by WSM
WSM Posted June 9, 2016 Posted June 9, 2016 (edited) One problem I've noticed with the larger sodium chlorate cell is that with a short PVC vent riser (about 12" or 30 cm high), there was a lot of condensation of hot electrolyte slowly dripping from the opening at the top. I thought using a longer piece of 1/2" PVC pipe for the vent riser would allow the vapors to condense in the tube and reflux back into the cell. That didn't work, but did the same thing. I remembered something a friend did to his cell which had a similar problem. He made a vapor trap out of a large glass jar. I cleaned up a one gallon (3.785 liter) glass pickle jar and modified a 4" PVC pipe cap, adding two 1/2" NPT ports; one for a vent and the other for an input from the cell. Next I ran some clear vinyl tubing (1/2" ID) from the top of the cell lid up to the input port of the vapor trap The old 12" vent tube was connected to the top-most exhaust port in the pipe cap lid of the vapor trap. This setup works very well, in fact, a lot of the vapors condense in the vinyl tube and reflux back into the running cell. It's working so well there's hardly any moisture collected in the bottom of the jar (and no moisture dripping from the exhaust vent at all!). I wonder if the clear vinyl tubing radiates the thermal energy away that much better than the hard PVC pipe?! WSM Edited June 9, 2016 by WSM
WSM Posted June 10, 2016 Posted June 10, 2016 The vapor trap is still working well and has very little collected moisture in it. The bulk of the moisture is refluxing back into the cell. I'd call it a success! WSM
WSM Posted June 10, 2016 Posted June 10, 2016 Two days ago, after I assembled and installed the vapor trap, I also prepped the salt reservoir with modifications so it will operate properly. My hope is to set it up so it will feed the hot electrolyte through the salt crystals (replenishing the chlorides) and return to the cell, without dragging salt crystals along. We'll see... WSM
WSM Posted June 10, 2016 Posted June 10, 2016 Yesterday afternoon, I connected a peristaltic pump to the salt reservoir (refitted with more fiberglass filters) with white Viton tubing. I plugged it into a switched outlet, opened the valves and turned it on. The pump slowly filled the reservoir with hot electrolyte and then trickled the recharged clear liquor back into the cell. Success! I let it run for 12 hours, switched it off and closed the valves this morning. I'll study the results and effects of this setup later on. I love it when things come together! WSM
WSM Posted June 10, 2016 Posted June 10, 2016 A good friend and fellow electrochemist, suggested my sodium chlorate experiment is practically a continuous system. I believe he's right. It's designed to run consistently and produce sodium chlorate. While some is harvested, more brine is added to the cell OR more salt is added to the depleted electrolyte, and the system keeps going. Regardless, it's an experiment and I'll see how far it'll go. WSM
WSM Posted June 10, 2016 Posted June 10, 2016 sounds like it is working good....It's definitely looking promising, but I haven't harvested anything yet. My friend and fellow electrochemist thinks it'll produce several kilos per month. We'll see... WSM
WSM Posted June 12, 2016 Posted June 12, 2016 (edited) The sodium chlorate experiment is still running (about 375 hours [>18,000 AH], so far). I've modified the salt replenishment system so I can drain the salt reservoir for servicing and salt filling. IMGP7908.MOV The attached file is a video of the peristaltic pump and it's plumbing plus the PVDF filter housing used for the salt reservoir, all running and doing the job of trying to keep the chloride level topped up. So far it's working well. WSM Edited June 12, 2016 by WSM
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