hillbillyreefer Posted August 20, 2011 Posted August 20, 2011 did the solution turn yellow? Yes the liquor turned yellow. After all the black crap settled it had a distinct yellow hue to it. 12 hours into the second run, with no signs of black in the liqour. Hopefully it stays that way.
WSM Posted August 20, 2011 Posted August 20, 2011 Yes the liquor turned yellow. After all the black crap settled it had a distinct yellow hue to it. 12 hours into the second run, with no signs of black in the liqour. Hopefully it stays that way. Don't forget, the mother liquor (potassium hypochlorite, etc.) has a slight yellow-green cast to it. Granted, any iron dissolved in there is going to turn things distinctly yellow to brown depending on the concentration (which is one reason I prefer pure titanium cathodes ). Keep up the good work . WSM
hillbillyreefer Posted August 20, 2011 Posted August 20, 2011 Don't forget, the mother liquor (potassium hypochlorite, etc.) has a slight yellow-green cast to it. Granted, any iron dissolved in there is going to turn things distinctly yellow to brown depending on the concentration (which is one reason I prefer pure titanium cathodes ). Keep up the good work . WSM I was going to add that it is the color of bleach. If I had to guess I'd say it is a combination of both iron and hypochlorite. Noticed this morning that the liquor is not bubbling as much as it was when the cell was first started. It may need a bit of a pH adjustment. I've found swede's rule of thumb, but I'm out of muriatic acid, anyone know if 90 % acetic acid would be acceptable?
oldmanbeefjerky Posted August 21, 2011 Posted August 21, 2011 im pretty sure the point of ph control using hydrochloric acid was to replace lost chlorine ions. As ausfire said, at a ph of around 10, chlorine pretty much stops leaving the cell. adding acetic acid will raise ph back to 7 or so, but unfortunately it will also start causing chlorine to begin bubbling out. it wont help, if anything it will make things much worse. Also, the second time round i ran the cell, it was and has stayed pure white, so the yellowing after filtering was definitely iron chloride, which explains why it was precipitating out and turning the cell black-brown
ausfire Posted August 21, 2011 Posted August 21, 2011 Oldmanbeefjerky, The point of pH control is to maintain conditions that favour more efficient cell reactions not to replace lost Chlorine ions. As for those guides you’ve read adding hydroxide to increase yield makes no sense to me. The only reason I can think of as to why someone would suggest this is to inhibit the initial reactions producing the Chlorine you can smell. Possibly so there dads can’t smell it? I think you ought to do a bit more research into the cell chemistry I’m talking about -Ausfire
oldmanbeefjerky Posted August 21, 2011 Posted August 21, 2011 (edited) come to think of it, most of the guides i read that say were for somewhat improvised conditions, or crude setups Edited August 21, 2011 by oldmanbeefjerky
WSM Posted August 21, 2011 Posted August 21, 2011 come to think of it, most of the guides i read that say were for somewhat improvised conditions, or crude setups A list of good references is: CHLORATE REFERENCES FOR FURTHER STUDY.pdf I own hard copies of these referenced volumes plus more current works. They aren't light reading but illuminate the complex nature of the reactions in our cells. The more you know the better you can do what we're trying here. Swede knew this and shared his learning curve in his excellent blogs as he progressed. He also went far because he had developed good machining skills and an understanding of several sciences in his other pursuits. It's too bad his interests took him elsewhere and he's not here to further learn from. None of us knows it all and we're all learning. Hopefully we learn from each other and avoid pitfalls along the way. WSM
WSM Posted August 21, 2011 Posted August 21, 2011 I'm serious about knowledge, as evidenced by the photo of a small part of the library. The loose leaf notebooks dwarf the hard covers, by the way... WSM
WSM Posted August 21, 2011 Posted August 21, 2011 (edited) A friend of mine (I didn't ask his permission to post this so he'll remain un-named until I have that permission) suggested recently to place a vapor trap in the venting system. He suggested this when he noticed a build up of salt where his system exhausts outside the structure he runs it in ! He now runs his vent tube into a 1 gallon glass jar and from there to the outside. The salty, moist air deposits the salt and some moisture in the jar before venting to the outside. He is free to reintroduce the salt (mostly KCl) back into the system, rather than let it damage the structure or kill the vegetation outside (chlorates are indiscriminate herbicides). His system is continuous so the salt recovery from the vent is more serious than from a batch system. For anyone contemplating a large cell or even a continuous system, this is just one more thing to consider. If you do this, I strongly recommend using a plastic lid rather than any kind of metal lid on the vapor trap jar. WSM Edited August 22, 2011 by WSM
WSM Posted August 21, 2011 Posted August 21, 2011 The other day I was discussing some details of my plans for "The Monster" (the large continuous system I have on the back-burner till I figure out some more details) with an experienced and capable friend; and he expressed the opinion that with the larger electrodes (6" x 6.75" anode plus two similarly sized cathodes) I'm considering, plus the high amperage they can handle (about 150 Amps), that I'll have two problems:1) HEAT, and2) they'll produce about 7 Kilos a day! "Just how much chlorate can you use?", he asked me. A valid concern. I don't use 7 Kilos a year, let alone in a day! I never wanted to produce such quantities and would have difficulty giving away so much, let alone using it. The heat problem messes with the low energy consumption plan I had, too. The ideal system uses just enough energy to raise the RC to about 40oC and lets the passively cooled CC drop to under 30oC where the crystals drop out without an active cooling system. Hmmm , I may have to experiment with smaller electrodes till I come up with a balance between efficiency and economy (no small feat!). My original goal was a system that could produce a Kilo of chlorate a day. This could easily get out of hand (if it hasn't already). Another concern he expressed is how to handle the product once it's formed? Making the course crystals is one thing, but then you have to purify and dry them before you can reduce them to a usable particle size. That's a lot of handling. No wonder companies charge so much for it. They also have to package, ship and market it. It's a good thing I don't do this for a living; I'd be exhausted !!! WSM
WSM Posted August 21, 2011 Posted August 21, 2011 The point of pH control is to maintain conditions that favour more efficient cell reactions not to replace lost Chlorine ions. -Ausfire A very good point, and one that shouldn't be lost in all the discussion. In an uncontrolled cell, it takes 9 moles of electrons to make 1 mole of chlorate (at best). In a pH controlled cell it takes 6 moles of electrons to make 1 mole of chlorate. The CE in an uncontrolled cell is, at best, 55% to 60%. In a pH controlled cell, the CE approaches and can exceed 90%! Several amateurs have done it and proven the concept. Thanks for bringing this up. WSM
pyrojig Posted August 22, 2011 Posted August 22, 2011 A very good point, and one that shouldn't be lost in all the discussion. In an uncontrolled cell, it takes 9 moles of electrons to make 1 mole of chlorate (at best). In a pH controlled cell it takes 6 moles of electrons to make 1 mole of chlorate. The CE in an uncontrolled cell is, at best, 55% to 60%. In a pH controlled cell, the CE approaches and can exceed 90%! Several amateurs have done it and proven the concept. Thanks for bringing this up. WSM Iv'e gotta ask, but has anyone had luck doing ph control via 2x a day v.s. the timed drip sys? This site claims that once to 2x a day just isnt sufficient to maintain the ph and that the heavy load of acid all at one time is not too good of a idea. http://oxidizing.110mb.com/chlorate/reaction.html
WSM Posted August 22, 2011 Posted August 22, 2011 Iv'e gotta ask, but has anyone had luck doing ph control via 2x a day v.s. the timed drip sys? This site claims that once to 2x a day just isnt sufficient to maintain the ph and that the heavy load of acid all at one time is not too good of a idea.http://oxidizing.110...e/reaction.html Probably true, if you dump it in on top of the mother liquor (lots of chlorine would likely be released ). If you dispense it slowly under the surface of the RC as Swede shows in his blog, I think twice a day may just work. Testing with pH paper would prove it out, one way or the other and help you dial it in. If you try it, share the results . WSM
pyrojig Posted August 22, 2011 Posted August 22, 2011 Probably true, if you dump it in on top of the mother liquor (lots of chlorine would likely be released ). If you dispense it slowly under the surface of the RC as Swede shows in his blog, I think twice a day may just work. Testing with pH paper would prove it out, one way or the other and help you dial it in. If you try it, share the results . WSM DO you have the same problems with using paper to test? The liqueur seems to "poison" the paper due to its high salt concentration, and gives odd readings. I have found a way to kind of work around this by diluting the test sample at least 50% or more of pure water.
oldmanbeefjerky Posted August 22, 2011 Posted August 22, 2011 This has a simple solution, just slowly drip the acid into the cell. dont just splosh it all in one go, but rather, see if you can get it to drip in over a period of maybe an hour or so, like the dripping system for introducing fluids into people who have lost allot of blood.
WSM Posted August 22, 2011 Posted August 22, 2011 DO you have the same problems with using paper to test? The liqueur seems to "poison" the paper due to its high salt concentration, and gives odd readings. I have found a way to kind of work around this by diluting the test sample at least 50% or more of pure water. What a coincidence, that's what I was going to suggest. I believe Swede did something similar to test chloride concentrations with those expensive test strips he bought. One of the concerns wasn't salt poisoning but the hypochlorite "bleaching" the pH test strip material before you could get a good "read". Let me know how that works for you. It's one bridge I haven't crossed yet. WSM
WSM Posted August 22, 2011 Posted August 22, 2011 This has a simple solution, just slowly drip the acid into the cell. dont just splosh it all in one go, but rather, see if you can get it to drip in over a period of maybe an hour or so, like the dripping system for introducing fluids into people who have lost allot of blood. Again, Swede's method of letting the dilute acid diffuse through small holes cross-drilled in PVC pipe under the surface of the cell liquid made sure nothing was "dumped in", causing a rapid release of chlorine gas. Rather, any developed chlorine remained in solution where it would do the most good. WSM
oldmanbeefjerky Posted August 22, 2011 Posted August 22, 2011 What a coincidence, that's what I was going to suggest. I believe Swede did something similar to test chloride concentrations with those expensive test strips he bought. One of the concerns wasn't salt poisoning but the hypochlorite "bleaching" the pH test strip material before you could get a good "read". Let me know how that works for you. It's one bridge I haven't crossed yet. WSM I immediately thought that boiling out the hypochlorite to read the ph would work, though that would lower the ph slightly , and give an inaccurate reading, wouldn't it.
WSM Posted August 22, 2011 Posted August 22, 2011 I immediately thought that boiling out the hypochlorite to read the ph would work, though that would lower the ph slightly , and give an inaccurate reading, wouldn't it. That doesn't sound like a good idea. Diluting a known quantity a measured amount would be more accurate I believe. WSM
patsroom Posted August 22, 2011 Posted August 22, 2011 (edited) This has a simple solution, just slowly drip the acid into the cell. dont just splosh it all in one go, but rather, see if you can get it to drip in over a period of maybe an hour or so, like the dripping system for introducing fluids into people who have lost allot of blood. I think that this may inspire some ideas. It is a little dated. Random Discussion & Chat Let's Take this Outside - place to discuss side topics in others' form Posted 06 December 2009 - 10:51 PM I am glad that you made it here and I see that your ideal would keep the two solutions from mixing.I been working on a test as well and the two solutions are in contact with each other. I truly believe that if the two liquids are of different gravities and the heavier on is on the bottom that they would not mix either. The opening of the bottle I am using is like about 5/8 of an inch, the liquid has not mixed any farther than when I first started the test. I glad to see you are testing this as well as it will help in the old ideal about using a drip system to dose a chlorate tank.I am hoping to go in the direction of making a complete holding tank with a pump using a homemade solenoid that will deliver the solution in the proper amount over a time period. The PDF showns what I am thinking. Attached File(s) Dosing_Delivery_Concept.pdf (6.69K) Number of downloads: 4This post has been edited by patsroom: 06 December 2009 - 11:14 PM Edited August 22, 2011 by patsroom
WSM Posted August 22, 2011 Posted August 22, 2011 I think that this may inspire some ideas. It is a little dated.Posted 06 December 2009 - 10:51 PM I am glad that you made it here and I see that your ideal would keep the two solutions from mixing.I been working on a test as well and the two solutions are in contact with each other. I truly believe that if the two liquids are of different gravities and the heavier on is on the bottom that they would not mix either. The opening of the bottle I am using is like about 5/8 of an inch, the liquid has not mixed any farther than when I first started the test. I glad to see you are testing this as well as it will help in the old ideal about using a drip system to dose a chlorate tank.I am hoping to go in the direction of making a complete holding tank with a pump using a homemade solenoid that will deliver the solution in the proper amount over a time period. The PDF showns what I am thinking. Attached File(s) Dosing_Delivery_Concept.pdf (6.69K) Number of downloads: 4This post has been edited by patsroom: 06 December 2009 - 11:14 PM For pH control I believe the simplest and most elegant solution is the system developed by Swede and illustrated in his Blog: The T-Cell III - Evoluton He stated in a personal communication that industry used known concentrations of HCl added at regular intervals according to the current demanded by the cell. He wrote: "Industry has determined from the chemical reaction exactly how much HCl is consumed per ton, and the numbers do work. Once the cell is running, the delivery can be massaged to fine tune the pH, and once it's dialed in, it seems to be quite stable, more than I thought it would be. The HCl demand starts high and tapers off, and we came up with a general rule of thumb:0.057 ml of concentrated (32%) HCl per ampere, per hour, with the HCl delivery volume cut by 33% after the chlorate crystals begin to form." I have adopted his technique of a gravity fed metering system as the simplest and most energy efficient way to go, despite having the ability to accurately administer via a digitally controlled peristaltic pump. This is, of course, my own opinion. WSM
pyrojig Posted August 22, 2011 Posted August 22, 2011 @ WSM I have found the diluting to test to be the best most accurate option at this point. I just was wondering if others had the same issues I had with the testing strips. Im sure your right about the hyperchlorite being the issue in the poisoning . I do like the idea of the dispenser/diffuser tube that swede spoke of. I just am not sure how I want to set up a system (one that works like a washer machine timer) . I think that i will use it to operate a simple solenoid, with a dump valve that runs into a drip tube , that essentially goes into the cell. It will slowly drip over a timed period.
patsroom Posted August 22, 2011 Posted August 22, 2011 To bad Swede has gone AWOL from the forum. But he had his reasons and I believe they were good ones. WSM I know you been here adding to this forum for a long time (13 September 2009 - 09:09 AM ). And the information you have added has helped many here. That is what this is for and as always we look forward to hear from you.When Swede was here we were-or I should say "I was" looking for ways to add pH to the cells in a few diferent ways and as I said above that the ideal is dated. But it still stands as a way to control pH level. It is the live and learn thing that we all go thru with the help of our friends. I find that it has help me and I feel that it has helped other as well. There are afew other areas that information was added in the forums some good some bad but it is there if one is willing to look for it.
oldmanbeefjerky Posted August 22, 2011 Posted August 22, 2011 Yeah, its a shame that almost all the people who just "get it", are never there to help anymore.
WSM Posted August 22, 2011 Posted August 22, 2011 (edited) Yeah, its a shame that almost all the people who just "get it", are never there to help anymore. True enough. Swede added the most in a relatively short time, as did tentacles (who hasn't entirely gone, by the way). There are a few others who have added a lot to the body of knowledge, also. Most of my pyrotechnics experience is past-tense so I've thrown my efforts into electrochemistry, since I can research without alarming anyone (I live in town and can't just go out and shoot stuff off). So the years of study and research are beginning to gel and I'm actively (but casually) advancing in my practicing research in cells and accessories to produce high quality oxidizers on a small scale. Since about 2008, inspired by a pyrobin posting by Carl Tauch, I've spent most of my time designing and redesigning a continuous chlorate cell, built on a small scale, with the ultimate goal of producing perchlorates. The continuous chlorate cell will provide feedstock for a perchlorate cell. Why do I do it? Do I need the perchlorate? No. I enjoy the challenge and learning (I never let schooling interfere with my education). If it gets to be routine, I'll quickly get bored and move on to something else. That may be what happened to Swede; who knows? I have actually spent the bulk of the past four years slowly acquiring all sorts of expensive odds and ends to build an efficient continuous system and begin to prepare for the elusive second step: turn all that surplus chlorate into usable perchlorate. A tough challenge but every little success brings great joy. It's fun. WSM Edited August 22, 2011 by WSM
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