athlon Posted December 16, 2011 Posted December 16, 2011 I wash the precipitate after scooping out with about 1,5 liters of ice cold water. Then I dissolve it in about 1 liter of boiling water that I let boil for 15 minutes, filter and let cool. Now I scoop out the precipitate again and wash with ice water. Usually this last washing goes pretty fast due to no fluff, but this last time it took ages. I did a test about a week ago where I let the precipitate dry directly after scooping out and weighed to see how much of it I loose in the recrystallization process and the amount went down from 388g to 280g, so I guess there was about a third Sodium Chlorate. I have bought a shop vac this summer that I have been thinking of using, just need to find some info on how to... Wonder where that carbonate would be from then? Tap water? I have used tap water every time with no problems earlier though.
WSM Posted December 16, 2011 Posted December 16, 2011 How do you seperate the potassium chlorate from the sodium chlorate using a mixed salt as feedstock?Filters clogging is expected if you have a lot of (carbonate?) contamination. You might want to try and devise a buchner funnel setup. I have one that uses a shop vac for suction.I cut the top out of a 20l pail to fit a plastic strainer, and siliconed it in. I added another hole for the shop vac to attach with a pipe extending down into the bucket. I use coffee filters for filtration. Do you wash your chlorate after scooping out? Using a 100 or 200 mesh screen should help take away a lot of the crap. The water could then be filtered and reused if you want later.As for the electroode, try cleaning with HCl. If the contaminant is a carbonate or some other alkaline material, try treating with white household vinegar. since you're using sodium salts, the resultant acetates would be very soluble and easily washed away. I agree about treating the electrode with hydrochloric acid. In fact, good MMO can handle it very well and most usual contaminants can be removed before you use the electrode the first time. A lot of us are using laserred's MMO for electrodes. Swede mentioned several times about treating it with HCl to remove a brown smut (iron I suspect) before using it and I have done the same thing more than once. Also, after spot welding leads to MMO mesh, dipping the electrode in HCl for +- 1/2 hour will usually remove copper residue left by the welder tips on the weld points. Just let the electrode soak in full-strength HCl and then rinse with clean water. I usually flush the used HCl down the toilet when the process is finished (no worse than drain cleaner). WSM
WSM Posted December 16, 2011 Posted December 16, 2011 I wash the precipitate after scooping out with about 1,5 liters of ice cold water. Then I dissolve it in about 1 liter of boiling water that I let boil for 15 minutes, filter and let cool. Now I scoop out the precipitate again and wash with ice water. Usually this last washing goes pretty fast due to no fluff, but this last time it took ages.I did a test about a week ago where I let the precipitate dry directly after scooping out and weighed to see how much of it I loose in the recrystallization process and the amount went down from 388g to 280g, so I guess there was about a third Sodium Chlorate.I have bought a shop vac this summer that I have been thinking of using, just need to find some info on how to...Wonder where that carbonate would be from then? Tap water? I have used tap water every time with no problems earlier though. Do they fluoridate the water where you live? If so, I wouldn't use tap water for your cell. Fluorine will poison your MMO and render it useless over time. I use either distilled water or water filtered through a reverse osmosis filtering system (which removes 95%-97% of all dissolved solids in my tap water) for making my salt water solution. In many parts of the world, the local water department will add different things to treat the water at different times of the year for whatever changing conditions they encounter in their system. Fluorides are added to promote dental health (they say) but should be avoided in electrochemical cells. Just more things to consider... WSM
pyrojig Posted December 16, 2011 Posted December 16, 2011 Do they fluoridate the water where you live? If so, I wouldn't use tap water for your cell. Fluorine will poison your MMO and render it useless over time. I use either distilled water or water filtered through a reverse osmosis filtering system (which removes 95%-97% of all dissolved solids in my tap water) for making my salt water solution. In many parts of the world, the local water department will add different things to treat the water at different times of the year for whatever changing conditions they encounter in their system. Fluorides are added to promote dental health (they say) but should be avoided in electrochemical cells. Just more things to consider... WSM Heesh ..., I have used tap water for years..... I never considered they may put flouridate in the water ..... Thats not cool. Anyway to find out real quick?
athlon Posted December 16, 2011 Posted December 16, 2011 No fluoride in the drinking water and very low calcium content as I have checked that before when asking regarding water for my aquarium. Here's a shot of newly milled batch of chlorate:
WSM Posted December 16, 2011 Posted December 16, 2011 (edited) Heesh ..., I have used tap water for years..... I never considered they may put flouridate in the water ..... Thats not cool. Anyway to find out real quick? The fastest (easiest) way I know is to call the water company and ask them. I'm sure several tests are available but I'd have to study the matter before I could find suitable ones to share. WSM Edited December 17, 2011 by WSM
Bonny Posted December 18, 2011 Posted December 18, 2011 I have bought a shop vac this summer that I have been thinking of using, just need to find some info on how to... Look up buchner funnel and you'll get the idea, it's pretty simple. As long as the air being sucked into the "bucket" by the shop vac has to go through the filter then it will work.
oldmanbeefjerky Posted December 18, 2011 Posted December 18, 2011 where i live no test is necessary, the water wreaks of flurine and is thick like juice, which is odd considering that during this time of year we have a daily monsoonal rainfall great enough to cover the states water consumption 3 times, which is why the government last year actually dumped half the water reserves into the ocean as they were overflowing we had that much rain.may i ask are there any noticeable signs of damage i can find if ive only ever made 3 runs using flurinated water?or should i not bother? by the way, if your in australia and looking for cheap bulk KCl, look up "valueplus potassium chloride", youll get it at a reasonable rate and all their outlets , the cheapest being "vetnpetdirect" which is an online store i buy mine from.they also sell other chemicals like copper sulfate and sulfur at an OK price, at least for me as i divide and resell them.unfortunately i know no overseas brands. though in america it appears to be very cheap and easy to acquire of 20kg bags at most hardware stores.
WSM Posted December 18, 2011 Posted December 18, 2011 Look up buchner funnel and you'll get the idea, it's pretty simple. As long as the air being sucked into the "bucket" by the shop vac has to go through the filter then it will work. The use of buckets and a shop vacuum sound like an interesting "field expedient" method. To separate the chlorate crystals from the cell liquid, I'm working on a similar idea. Having used the vacuum filtration method in laboratory work for many years, I'm partial to using a Buchner funnel with lab-grade filter paper. My plan is to build a bench-top Buchner funnel from large bore PVC pipe and PVC plate (see the PVC Ball Mill barrels made by oldguy for an idea of how it could be done) and draw the solution down into a 20 liter Pyrex carboy for later recharging with salt and using in the cell. By applying a vacuum the filtration goes very fast and rinsing the crystals with chilled D.I. water is trivial. I would show a diagram but all I have available is a rough hand sketch (most of this design is in my head). When I get around to building the thing, I'll show a photo of the setup. WSM
WSM Posted December 18, 2011 Posted December 18, 2011 where i live no test is necessary, the water wreaks of flurine and is thick like juice, which is odd considering that during this time of year we have a daily monsoonal rainfall great enough to cover the states water consumption 3 times, which is why the government last year actually dumped half the water reserves into the ocean as they were overflowing we had that much rain.may i ask are there any noticeable signs of damage i can find if ive only ever made 3 runs using flurinated water?or should i not bother? by the way, if your in australia and looking for cheap bulk KCl, look up "valueplus potassium chloride", youll get it at a reasonable rate and all their outlets , the cheapest being "vetnpetdirect" which is an online store i buy mine from.they also sell other chemicals like copper sulfate and sulfur at an OK price, at least for me as i divide and resell them.unfortunately i know no overseas brands. though in america it appears to be very cheap and easy to acquire of 20kg bags at most hardware stores. Hi OMBJ, If your water supply is that rough and it rains that much, have you considered using rain water? A simple cistern can be hooked up to a raingutter downspout from the roof of the house, and supply most of your cell needs. I read an article about damage to DSA anodes from fluorine and other contaminants. I'll try to find it and post it. If I travel to OZ, it'll probably be for a short stay (vacation); but if I move there I'll look up those sources . In the US, a few hardware and grocery stores handle it as (sodium-free) water softener salt in 40 lb (+- 18 kilo) bags. I like the reference to veterinary supply stores for KCl. I hadn't thought of them as a source; Thanks !
WSM Posted December 18, 2011 Posted December 18, 2011 Hi OMBJ,If your water supply is that rough and it rains that much, have you considered using rain water? A simple cistern can be hooked up to a raingutter downspout from the roof of the house, and supply most of your cell needs. I read an article about damage to DSA anodes from fluorine and other contaminants. I'll try to find it and post it.If I travel to OZ, it'll probably be for a short stay (vacation); but if I move there I'll look up those sources . In the US, a few hardware and grocery stores handle it as (sodium-free) water softener salt in 40 lb (+- 18 kilo) bags. I like the reference to veterinary supply stores for KCl. I hadn't thought of them as a source; Thanks ! I don't recall where I got this; either here on APC or on Science Madness, but here it is: mmo_poison.pdf WSM
oldmanbeefjerky Posted December 19, 2011 Posted December 19, 2011 I think you got this from oxidizing.110mb, i swear ive seen this file before. Also i think ill try that, honestly ive never considered it before. also, the amount it rains here, i wont need to use water washing off the roof, a whole bucket will fill up easily in 5 minutes of rain here.Unfortunately i wont have a chance to try it out because i go to victoria tomorrow.
Mumbles Posted December 19, 2011 Posted December 19, 2011 What you're smelling from your water is NOT fluorine. They do not add it in a volatile form. I also somehow doubt you've ever smelled real fluorine. It's not the same as chlorine, just as bromine and iodine have their own unique odor. It's probably from chlorination. Ask or find out for sure if your water is fluoridating. Going off of a hunch or invalid belief is not going to tell you for sure.
WSM Posted December 19, 2011 Posted December 19, 2011 I think you got this from oxidizing.110mb, i swear ive seen this file before.Also i think ill try that, honestly ive never considered it before. also, the amount it rains here, i wont need to use water washing off the roof, a whole bucket will fill up easily in 5 minutes of rain here.Unfortunately i wont have a chance to try it out because i go to victoria tomorrow. You know, I think you're right. Thanks. Good luck in Victoria. WSM
WSM Posted December 19, 2011 Posted December 19, 2011 What you're smelling from your water is NOT fluorine. They do not add it in a volatile form. I also somehow doubt you've ever smelled real fluorine. It's not the same as chlorine, just as bromine and iodine have their own unique odor. It's probably from chlorination.Ask or find out for sure if your water is fluoridating. Going off of a hunch or invalid belief is not going to tell you for sure. I believe you're right about it being chlorination. If over-chlorinated, boiling the water for a while will drive off excess free chlorine (for drinking purposes, but a chlorate cell won't mind extra chlorine as long as the pH is right). The normal rate for fluoridation is between 0.5 and 1.0 ppm depending on region and temperature. An exception would be natural fluoridation from minerals in the region the water came from (and then a fluoride reduction plan might be used). I agree, asking the local water department about fluoride levels is better than guessing about the levels (besides, they're probably proud of their service to the community and glad to divulge the details of their water quality). WSM
oldmanbeefjerky Posted December 23, 2011 Posted December 23, 2011 well, if not rain i would use distilled water for my chlorate as i care about my electrodes.also, where im from, not only is there a very high level of chlorine, but also natural minerals as well. distilled water is very cheap and rainwater is free and in the excess, if my house survives the upcomming cyclone, ill use rainwater in my next big batch which i hope will have a kilo or so.
WSM Posted December 24, 2011 Posted December 24, 2011 well, if not rain i would use distilled water for my chlorate as i care about my electrodes.also, where im from, not only is there a very high level of chlorine, but also natural minerals as well. distilled water is very cheap and rainwater is free and in the excess, if my house survives the upcomming cyclone, ill use rainwater in my next big batch which i hope will have a kilo or so. Excellent! Good luck, OMBJ; and let us know how it goes . WSM
WSM Posted December 27, 2011 Posted December 27, 2011 I've been away visiting Family for the Holidays (Man does not live by pyrotechnics alone; he needs to cultivate his audience, too ). I hope to get around to some trial runs with my continuous experiment before too long. One major stumbling block is building a shed to store and run my experiments in so uninvolved persons or animals don't come in contact with hazardous materials or equipment. I like sleeping indoors, and that situation may be jeopardized by my life companion if one of our grandchildren or pets should be harmed by any of my "foolishness", so I need to limit access to it. Some have suggested running it indoors but, like Swede, I don't like seeing my expensive and hard-won tools turn brown !!! So... my best option is building a small garden shed, electrifying it and running my experiments outside where no one needs to see or smell it. I don't anticipate any complaints from my neighbor since his pool already produces chlorine smells enough for both of us... and I expect no one will really notice my contribution, if I keep it within reason . I'll continue this discussion later... WSM
WSM Posted December 31, 2011 Posted December 31, 2011 (edited) NEW TOY! I got myself a 200X digital microscope, and what do I use for a test? Electrodes, of course! I first photographed the surface of a DeNora MMO electrode: Next I photograph the surface of laserred's MMO material that I cleaned with HCl: Then it occurs to me to get a photomicrograph of the surface of patsroom's LD anode: The surface of the MMO looks vaguely like the text book views except the amount of magnification isn't high enough to clearly show the "cracked mud" appearance in those books. But the LD, Wow! It looks like shiny gray gems or crystals. It looks like what I imagine a hard crystalline beta form should look like, not the brown porous alpha form. I also took a microscopic video, but the file size is enormous and I'm not sure if I should post it. This digital microscope is a fun tool. I wonder what else I should use it for? WSM Edited December 31, 2011 by WSM
athlon Posted December 31, 2011 Posted December 31, 2011 Looks nice! Have been thinking of getting one of those myself, for soldering smd components, if it doesn't get in the way.Does it have different grades of magnification? Live view on the monitor?
WSM Posted December 31, 2011 Posted December 31, 2011 Looks nice!Have been thinking of getting one of those myself, for soldering smd components, if it doesn't get in the way.Does it have different grades of magnification? Live view on the monitor? This one was about $40 online from meritline.com with free shipping and I couldn't resist. It would get in the way as the focal point is right at the end of the unit. So far I haven't found a different grade of magnification with mine but the website lists a unit that does have a range of adjustment and an adjustable stand, but it costs about $100. It is live view on the monitor. The video of the LD anode surface allows you to see the crystal faces better since the surface isn't flat. Warning: this is a huge file: Patsroom LD Video.avi See what you think. WSM
Tesla Posted January 10, 2012 Posted January 10, 2012 I finally got my cathode and anode together. It's a mmo with a stainless steel shaft, and a stainless steel plate with a stainless steel shaft. I was unable to get them welded, so I used a stainless steel bold on each. My goal is to go from kcl to kclo3. Correct me if I'm wrong, but the method is to heavily saturate the water with kcl, find the optimal spacing for the anode/cathode, and stop the electrolysis when the current drops to half its original amount. Can anyone think of anything else I should be aware of before I fire it up?
pyrojig Posted January 10, 2012 Posted January 10, 2012 (edited) I finally got my cathode and anode together. It's a mmo with a stainless steel shaft, and a stainless steel plate with a stainless steel shaft. I was unable to get them welded, so I used a stainless steel bold on each. My goal is to go from kcl to kclo3. Correct me if I'm wrong, but the method is to heavily saturate the water with kcl, find the optimal spacing for the anode/cathode, and stop the electrolysis when the current drops to half its original amount. Can anyone think of anything else I should be aware of before I fire it up? What are you powering it with? I have a converted computer PS that pushes 30A at the 5v rail. It is a similar setup like yours, and I have found that the best spacing is 3" for that supply.The Amps will be high during the break down phase of the Kcl to Kclo3 so expect it to show over what the Ps is rated for for a day or few. My PS would run up to 34+ A during the first stage , then level out to high 20's for the mid run . I think that the prob you'll face is the SS bolt coming loose , and eventually rusting in the liqueur. This will lead to a really bad connection and loss of production . Your area of contact( ss arm to electrode) must be sufficient enough to transfer the current to the electrodes ,or else your wasting power that could be used to make chlorate. This is why welding is the best option bar none . Another thing I believe I see, is that your using hot melt glue to seal the posts with. It will fail within a few days. I have tried everything under the sun and still never got hot melt to hold for more than a week or two at most. J.B. weld was the winner. I ruffed up the bucket lid at the top and bottom where the electrode arm enters the cell, then liberally applied the J.B. weld to create a brace/ seal ( 2-in-1) effect. This method has proved to last 2-3months. The electrolyte liqueur is merciless. Salt creep is not your friend when it comes to connections !! So stop it while it is fresh. Also before I forget, make sure that your kclo3 is not going to create a "salt bridge" . This will short out the electrodes / killing your Ps in a heartbeat. Point being made;;;;;; always keep an eye on the height of the finished kclo3. I have a HomeDepot Bucket cell, and dont have to open it to see the build up. I just take a strong flash light to the opposite side of the cell, and it is transparent enough to shadow the salt levels/ line on the side facing you. By all means give it a run, and keep a eye on it every few days. Edited January 10, 2012 by pyrojig
pdfbq Posted January 10, 2012 Posted January 10, 2012 (edited) My experience is that clamping (using a bolt) works but I'm 99.99% sure your stainless steel on the anode will not hold. You need Ti. For sealing, probably only people in a certain country (probably US) can buy J.B. Weld. What I use is a 2 component glue (like J.B. weld) but sealed with silicon kit (the stuff for your bathroom)That will stay cool for a while in both chorate and perc cell Good luck Edited January 10, 2012 by pdfbq
mabuse00 Posted January 10, 2012 Posted January 10, 2012 I just got 2 MMO sheets from laserred.Say, did your stuff has this acid smell to?Mine also have some kind of “rust” on them, please see the pictures. What do you think? Is that OK? I’m too busy at the moment to try anything with them, my chlorate experiment certainly has to wait some time. Is there anything necessary to preserve them for some time?
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