Arthur Posted November 8, 2015 Posted November 8, 2015 Use cheap pH paper or indicator liquid. learn to read it quickly! IMO it should be possible to predict the amount of acid needed -one of Swede's tables gives a figure in terms of vol of acid per amp hour.Once you have a prediction you can get closer to automatic operation, which reduces the number of pH tests required. Hopefully you can get to the point where at a useful current (5 - 50A) you can estimate the acid addition required and simply add some every hour to keep the pH in the right region then you can test every few hours and see how accurate the estimate was, and adjust the estimate.
MrB Posted November 8, 2015 Posted November 8, 2015 Wouldn't it be cheaper/easier to make a system the lifts the anode / cathode out of the cell when the power goes? A simple relay/battery system that operates a lift with a ratchet to prevent it from dropping back down until there is some human intervention, or, if one wants to go fancy, until the power is restored, and electromechanics are used to release the ratchet.B!
WSM Posted November 8, 2015 Posted November 8, 2015 It won't be solar powered.I've already ordered two pairs of 2x6" MMO+Ti electrodes from the Amateur Chemist. I have some time thinking about the whole setup Edit: My later thought comes to the measuring pH system. I'm aware that high-end probes have an astronomical cost, also that cheap meters get destructed and paper indicators get bleached. Any suggestions? It sounds like you're going to do a good job. Studying the system carefully and completely with all its various components well before you start may help you avoid many pitfalls, and aid you in creating a good design for your system and circumstances. If you post your thoughts and ideas here, we can offer ideas or suggestions which might be helpful. Arthur's right; dip the pH paper and quickly observe the color before it bleaches out. This is the least expensive method of pH determination I'm aware of (for use in chlorate cells), and it works well for me in most cases. Good luck in your efforts and please share the results with us. WSM
WSM Posted November 8, 2015 Posted November 8, 2015 (edited) I just think it's more trouble than it's worth. Having a system to switch over to main power as soon as the sun stops shining seems like additional complexity, not to mention solar panels are expensive. Also the current output will be unsteady, something needs to be done about that. You'll need a big battery for this, which is another cost item.Nothing is free. If your goal is potassium or sodium chlorate; I agree, it's a lot of bother. Just set up a cell and run it, plain and simple. If you're interests are in the process and expanding the understanding and development of a system with improvements, by all means try these ideas out and report the results here. The whole discussion about solar cells is a study of power systems, and is just one option (and probably nowhere near as efficient as other options). Along with photovoltaics, one could consider wind power as a source. Both are considered "green power", but have distinct drawbacks; including requiring battery backup systems for continuous supply of electric energy. On this planet, our least expensive supply of electric energy is hydroelectric systems. Whatever your prime mover happens to be, a generator needs to spin in order to produce electricity. That electricity (alternating current) needs to be reduced to a useful level of electromotive force (voltage) and rectified to direct current (DC) of the correct amperage for the demand of our cell(s). The simplest approach is to get a dc power supply, plug it into your available power source, apply it to your electrochemical system and wait for the results. The rest of it (the power discussion) is "tilting at windmills" and, unless acted upon, a waste of energy and a distraction. WSM Edited November 9, 2015 by WSM
WSM Posted November 13, 2015 Posted November 13, 2015 (edited) I did a flame test of my homegrown potassium perchlorate (from the LD cell) and the results weren't as good as I hoped for. Let me explain; first I made a solution from a sample of Swedish potassium perchlorate (vintage material used as a high purity reference) and did a flame test with a Nichrome inoculating loop in the clear blue flame of a Bunsen burner (running on propane). The result, as expected is a pale lavender flame, indicating potassium (and with no contaminants). Next, I tried the same test with a solution of my homegrown potassium perchlorate. I see the pale lavender flame, but it's not a pure as the Swedish material. I suspect a bit of residual contaminants remain. I see that a single quick rinse with cold distilled water isn't quite enough rinsing to completely remove contaminants from the freshly made potassium perchlorate crystals. I think I need to be more thorough in my washing of the fresh crystals to completely remove sodium and other contaminants from the perchlorate for it to be truly "pyro ready". I'll post more as my research continues. I know if industry can do it, we can do it. We just need to be thorough and take no short cuts. WSM Edited November 13, 2015 by WSM
Arthur Posted November 13, 2015 Posted November 13, 2015 Form my long ago lab days at uni, sometimes you have to wash several times -even sacrificing yield, to get good purity. However if you are sensible with washings they can simply be returned to the system for further electrolysis. Ultimately having high grade perc for colours is great, maybe some of the lower grade perc that flame tests yellow can simply be used for bottom shots.
WSM Posted November 14, 2015 Posted November 14, 2015 Form my long ago lab days at uni, sometimes you have to wash several times -even sacrificing yield, to get good purity. However if you are sensible with washings they can simply be returned to the system for further electrolysis. Ultimately having high grade perc for colours is great, maybe some of the lower grade perc that flame tests yellow can simply be used for bottom shots. If you mean to use (recycle) the rinse water for subsequent cell runs; then yes, that was my plan. I'm not against the idea of several rinsing cycles (despite the possible loss of some of the material) because the low solubility of potassium perchlorate will limit the total amount of those losses. I believe somewhere around 1.5% solubility at 20oC is expected, per rinsing cycle. I'll have to get back to you about how many cycles I think it will take. More than likely I'll have to test it before I can positively state how much is required. WSM
schroedinger Posted November 14, 2015 Posted November 14, 2015 WSM in my experince i got chloride free pottasium chlorate (tested with silver nitratr in nitric acid) after 3 cycles of recrystallisation. First two done with simple tab water third one done with distilled water. Maybe depends on your tab water, but my is quite clean. The last cristallisation process want to be left alone and happen slowly. Just turn of the hot plate and leave it alone. This way you get the big flake cristals with an average diameter of 1 cm. Like we know the bigger the crystals are the more pure they are and they grow bigger with alower cooling.
WSM Posted November 14, 2015 Posted November 14, 2015 (edited) WSM in my experince i got chloride free pottasium chlorate (tested with silver nitratr in nitric acid) after 3 cycles of recrystallisation. First two done with simple tab water third one done with distilled water. Maybe depends on your tab water, but my is quite clean.The last cristallisation process want to be left alone and happen slowly. Just turn of the hot plate and leave it alone. This way you get the big flake cristals with an average diameter of 1 cm. Like we know the bigger the crystals are the more pure they are and they grow bigger with alower cooling. I want to see if I can avoid boiling the solution, which would take a lot of water and energy (especially with potassium perchlorate [Very low Solubility]). If I can rinse off the soluble sodium contaminants with two or three rinsings of cold, pure water; it'll take a lot less energy to process the perchlorate. I can't imagine commercial producers of potassium perchlorate spending too much time and energy cleaning up their products. It would cut into their profits way too much. WSM Edited November 14, 2015 by WSM
r44astro Posted November 20, 2015 Posted November 20, 2015 I tried using cotton t-shirt for filter, the kcl3 adsorbed into it, won't do that again.
WSM Posted November 20, 2015 Posted November 20, 2015 (edited) I tried using cotton t-shirt for filter, the kcl3 adsorbed into it, won't do that again.That's true of most filters. I think glass filter papers and few others would be impervious to the effects of chlorate contamination. A good safety point is to keep dry filter papers (or other organic filter media) contaminated with oxidizers, in a closed metal container (outdoors, away from inhabited buildings) till they can be safely burned to destroy the hazard. WSM Edited November 21, 2015 by WSM
Arthur Posted November 20, 2015 Posted November 20, 2015 Whatman used to do two grades of glass filter circles GF-A and GF-B, I don't know if they still do. The A grade was faster than the B grade. They do NOT fold well try to use them in a buchner funnel. Papers used with oxidisers are very dangerous if allowed to dry.
WSM Posted November 20, 2015 Posted November 20, 2015 (edited) [quote name="Arthur" post="150925" timestamp="14Papers used with oxidisers are very dangerous if allowed to dry. ...but, oh so fun WSM Edited November 20, 2015 by WSM
Arthur Posted November 20, 2015 Posted November 20, 2015 We love things that burn, but not in an electrochemistry lab!
WSM Posted November 21, 2015 Posted November 21, 2015 We love things that burn, but not in an electrochemistry lab! Amen. WSM
pyrojig Posted November 22, 2015 Posted November 22, 2015 Its been awhile since i have contributed to the chlorate discussion ( lifes been very busy) . I find that burning the filter papers to be the best way of disposal as well as therapeutic. I dont like the idea of keeping dangerous fuel/ oxidizer mixes stored ( as in the case of contaminated filter papers . ) . Im glad to seee you guys keeping things alive around here . Wish I had time to contribute here , but i figure when winter months hit I may have a little more time to pitch in . .
WSM Posted November 22, 2015 Posted November 22, 2015 Whatman used to do two grades of glass filter circles GF-A and GF-B, I don't know if they still do. The A grade was faster than the B grade. They do NOT fold well try to use them in a buchner funnel. Papers used with oxidisers are very dangerous if allowed to dry. I guess I'm old fashioned, or just impatient. I only use filter paper in a Buchner funnel. Using it folded in a standard funnel is very slow and tedious. WSM
WSM Posted November 22, 2015 Posted November 22, 2015 (edited) Its been awhile since i have contributed to the chlorate discussion ( lifes been very busy) . I find that burning the filter papers to be the best way of disposal as well as therapeutic. I dont like the idea of keeping dangerous fuel/ oxidizer mixes stored ( as in the case of contaminated filter papers . ) . Im glad to seee you guys keeping things alive around here . Wish I had time to contribute here , but i figure when winter months hit I may have a little more time to pitch in . . Life is hectic here, too (been working 12 hour days, 6 days a week; and it's scheduled to continue into February!). I'm taking a few days off next week for the Holidays and hoping to catch up a little with neglected projects (if weather allows), we'll see... If I can, I'll try to get your revised bucket-cell electrodes assembled so your research can continue with it. I'm still slowly gathering high-tech bits and pieces for a couple projects of my own (I'll share more about those projects when they start to come together). It's a shame when life interferes with fun . WSM Edited November 22, 2015 by WSM
taiwanluthiers Posted November 22, 2015 Posted November 22, 2015 What is your job? Are you a retail manager?
WSM Posted November 22, 2015 Posted November 22, 2015 What is your job? Are you a retail manager? No, I'm an electrician working for a large public utility. WSM
taiwanluthiers Posted November 22, 2015 Posted November 22, 2015 I thought only retail managers work 60+ hours a week. Imagine the amount of work needed to manage a single Walmart... I see them come in on off days all the time.
WSM Posted November 23, 2015 Posted November 23, 2015 (edited) I thought only retail managers work 60+ hours a week. Imagine the amount of work needed to manage a single Walmart... I see them come in on off days all the time. We're working on upgrading our infrastructure which is good business (AND, may also be mandated by the Government), so we're putting in a lot of OT. It helps that it's close to the Holidays, and many of us are planning a nice Christmas for our families. It's a plus that we're paid hourly and not salaried! WSM Edited November 23, 2015 by WSM
pyrojig Posted December 4, 2015 Posted December 4, 2015 It's a shame when life interferes with fun . WSM )I hear ya there . lol . Ive been so dang busy too. As you could probably tell by my lack of posts. I look forward to getting back into the swing of things once winter slows things down.
50AE Posted December 4, 2015 Posted December 4, 2015 I wonder if magnesium chlorate can be made without worries with MMO electrodes? All this to synthesize barium chlorate. What are your opinions?
WSM Posted December 4, 2015 Posted December 4, 2015 I wonder if magnesium chlorate can be made without worries with MMO electrodes? All this to synthesize barium chlorate. What are your opinions? Not sure about Mg(ClO3)2 but I've heard of converting two moles of potassium chlorate to one mole of barium chlorate. If you're already making KClO3, why not try it that way? WSM
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