bikemaster Posted September 21, 2010 Posted September 21, 2010 And you are using 3v... If this is true, try a graphite cathode because your SS cathode simply suck...
WSM Posted September 21, 2010 Posted September 21, 2010 (edited) hello WSM,nice to meet ya. welll i'd love to be able to take a photo for ya, but i dont have the means. i posted this problem of mine on another forum, and one of the replys had said there might be a sense wire? i've heard of this before. however not on the 5volt side. i was under the impression that is most commonly found on the 3volt side. the poster had told me to hook up a pc fan as the load before my cell. does this make sense? the fan thats built in hasn't turned on at all since i cut the wires and grouped them. this unit was tested at the store and was find. i'm lost. heres another one for ya...... when i drop in my electrodes (5 volt side) plain water the unit seems to be working. if i do the very same thing but have a saturated solution of electrolyt the problem starts unless i use the 3volt side. Hi Kiss, The fan worked before you grouped the wires? Try ungrouping the wires, power it up and see if the fan operates. Also see what the outputs are (i.e., what's different with the PS before and after modification). The comments about many varieties of stainless steel are valid. Make sure you know which alloy you're dealing with (I vote for 300 series). Plain water is not as conductive as water full of ions (salt solution). The cell may be drawing down the output from the PS. A DC ammeter (paralleled with a shunt) in series with the output of the power supply (between the PS and the cell) will tell you if you are drawing current (and how much) when the system is running. If you are showing voltage but not current, there may be a problem with the PS or your wiring or both. See if you can work it out and let us know. WSM Edited September 22, 2010 by WSM
kiss Posted September 23, 2010 Posted September 23, 2010 hey guys...well i discovard somthing the other day. my fan is siezed. it must have been this way since i purchased it. i havn't had the time to do anything yet, but because of this fact to you think if i replace the fan that might problems would be solved?
bikemaster Posted September 23, 2010 Posted September 23, 2010 hey guys...well i discovard somthing the other day. my fan is siezed. it must have been this way since i purchased it. i havn't had the time to do anything yet, but because of this fact to you think if i replace the fan that might problems would be solved? Try to unplug the fan, just to see if the 5v is working. If yes, it will be a good idea to change the fan.
kiss Posted September 23, 2010 Posted September 23, 2010 Ok Bike, Sometime this evening i'm going to make some time and try to wire up another fan for it. However I did test to see if i could still get 5v, and i can. So maybe because that old fan was seized anew one might clear up my issue?! I guess i'll find out later on tonight right....lol. I'll report back when i find something out.....if i find something out. Hey...BTW, I just wanted to say thx to all for putting up with me asking these ?'s when I could be in the electronics forum. I didn't mean to high-jack the thread.thx 4 the help guys.
Arthur Posted September 23, 2010 Posted September 23, 2010 Judging by the recent European proposal to ban the consumer sale of pot nitrate chlorate and perc and the three lab acids the wisdom contained in this thread could soon become more important than you think.
kiss Posted September 23, 2010 Posted September 23, 2010 would someone mind explaining to me why the voltage of chlorate cells is roughly 4-5 volts? Why not 6 volts, or 12v, ect. I've read some many diffrent text files on the net(many with great info), but none seem to go into great detail as to why this voltage range is accepted?
Ralph Posted September 24, 2010 Posted September 24, 2010 Im really not going to explain this well (its been ages since I did electro chem) but it is like the voltage required to make the chemical reaction happen to reduce the water and to oxidise the chloride ions than to further oxidise the hypochlorite ions to chlorate ions kinda like the oposite of what happens in a battery (its why all those batteries (AA AAA D) all are 1.5v even though they are vastly different in size
WSM Posted September 24, 2010 Posted September 24, 2010 Given the observations of Arthur, I've changed the configuration of my experimental reaction chamber (RC) from a tall narrow tank to one shorter and wider. I used a 14" piece of green thinwall 8" PVC pipe and glued a piece of 1/4" PVC plate to the bottom and cut a piece of 3/8" clear PVC for the lid. A thin cut of the 8" pipe will serve to back up a silicone seal on the lid. I'm joining the EC to the RC with two 1" PVC unions modified by replacing the stock o-rings with Viton o-rings of the same size. A third modified 1" union will connect the RC to the CC. The goal is to determine if the basic concept is viable and see how the external EC will compare to the idea of an RC with the EC mounted inside. I will take photos and post them later. WSM
kiss Posted September 25, 2010 Posted September 25, 2010 hey guys,just wanted to chime in and tell ya's that my psu is working now. It turned out to be the fan. Funny thing is, i was getting ready to throw this thing out when i discoverd the fan was seized. So i replaced the fan with another one that i had around here, and bingo-bango my cell is bubbling away Now back to more important issue's....who's got a cup of coffee around here.
WSM Posted September 26, 2010 Posted September 26, 2010 Given the observations of Arthur, I've changed the configuration of my experimental reaction chamber (RC) from a tall narrow tank to one shorter and wider. I used a 14" piece of green thinwall 8" PVC pipe and glued a piece of 1/4" PVC plate to the bottom and cut a piece of 3/8" clear PVC for the lid. A thin cut of the 8" pipe will serve to back up a silicone seal on the lid. I'm joining the EC to the RC with two 1" PVC unions modified by replacing the stock o-rings with Viton o-rings of the same size. A third modified 1" union will connect the RC to the CC. The goal is to determine if the basic concept is viable and see how the external EC will compare to the idea of an RC with the EC mounted inside. I will take photos and post them later. WSM I've begun to assemble the main components of my test/experimental continuous system: The EC is the smaller grey tank and the RC is the larger green tank (but you already knew that). I used 1" unions to join them plus the CC (not yet shown) which connects to the left of the RC, as shown. I'll keep working on it and show/describe the progress as I go. More later... WSM
WSM Posted October 17, 2010 Posted October 17, 2010 To facilitate salt solution preparation I made up a mixing vat from a tank fabricated from a piece of schedule 40, 12" PVC pipe with 1/4" PVC plate for the bottom and also the lid. The fittings on the top and bottom are connected to a peristaltic pump by way of the silicone tubing shown. It's not pretty but it sure gets the job done and can handle up to 8-9 gallons of salt solution. I simply mix the KCl nuggets into purified water and run the pump so the moving water does the mixing. Moving water can dissolve many times as much salt as still water (heating makes the water "move" also, but I'm depending on just motion) and that's the plan. I haven't taken a photo of the experimental system with the CC attached yet but will when I get it further along. More later... WSM
WSM Posted October 27, 2010 Posted October 27, 2010 I've begun to assemble the main components of my test/experimental continuous system: The EC is the smaller grey tank and the RC is the larger green tank (but you already knew that). I used 1" unions to join them plus the CC (not yet shown) which connects to the left of the RC, as shown. I'll keep working on it and show/describe the progress as I go. More later... WSM I've been very busy with work, family and home concerns until this past weekend (got sick and forced to rest and take it easy). I'm on the mend and starting to think about getting my concentric electrode test/experimental system going on a test run. I've done some calculations and given the surface area of the anode, it should handle up to 139 amps, max. The surface area from one of Swede's eBay MMO anodes (3" x 12") is 72in2 or 464cm2. Considering that I want it run at about 0.3A/cm2, That is almost 140 amps. These are maximum values and not likely to be reached by my experiment (without a lot of stress on the whole thing). I'm more inclined to start off easy with, say, 30A and monitor its progress from salt water to bleach solution in preparation for chlorate production. Oh, before you get excited about the math, Swede assured me the surface area is roughly twice the single side area (according to the manufacturers he's contacted) for the mesh anode material, which is good news for us and makes current calculations easier, too. I still need to plumb the system together and add in monitoring of the voltage, current and temperatures (RC and CC sections) as well as plumb the acid injection system to maintain pH in the RC. I also need to plumb the return pump which returns depleated solution to the RC from the CC, maintaining the fluid level in the RC. The CC will have float switches which will not allow it's fluid levels to vary outside of safe parameters (though the high level switch is more of a safety interlock than a control switch). The RC still needs to be plumbed with a vent as well as acid solution and make-up water injector ports, as well as a replacement salt solution port. When I find the ideal mix, I hope to combine (if possible) the make-up water with the replenishing salt solution for a well balanced system (Man, this is getting more complicated than running a saltwater fish tank or reef !) Part of the reason I've designed my experiment with a wide, long and shallow crystalizer is to allow the system to crystalize the product with passive, rather than active cooling (which should be much more energy efficient; electricity is high priced here), plus I don't want to "babysit" my system with constant daily fiddling. Once it's running normally, ideally I only have to harvest my crystals once a week or twice, tops. After I settle on a final design for a continuous system and build one, I plan to work on the Holy Graile of actively controlling the pH without killing the sensor. I have a pH controller designed for saltwater aquarium use I'd like to adapt to the purpose but need to protect the sensor from the hostile environment of the RC/EC while still getting real time pH level reads and active control of the acid injection to maintain the ideal range of (6.5-6.8). Wish me luck! I said it before, it's amazing how complicated a simple idea can get! WSM
WSM Posted October 31, 2010 Posted October 31, 2010 (edited) I just calculated the volumes and ratios of the experimental system. The fluid level of the electrode chamber (EC) is 0.74 gallons (2.8 liters); and of the reaction chamber (RC) is 1.476 gallons (5.58 liters) and the high point of the crystallization chamber (CC) is 5.96 gallons (22.58 liters). That makes the total maximum fluid level 8.176 gallons (30.946 liters) if my measuring and math are correct. The approximate ratios are=EC:RC:CC1:2:8 The 4:1 ratio between the CC and RC closely matches the ratio I calculated for weekly harvesting (which was a guess, but testing the system should tell for sure). I've dusted off the power supply Swede sold me and powered it up. It reads 3.94 Vdc output and 0.00 Adc (of course, no load yet) but has the potential to feed the system ~100 Amps according to Swede. I rigged the power supply with two digital meters (voltage and amperage) for following the power demands during operation. I'm connecting the PS to the EC using 2 AWG welding cables for minimal resistance. If this supply is too much for the system, I'll fall back to my bigger supply which has outputs of 0-10 Vdc and 0-150 Adc and dial the whole thing in from there (I have much larger welding cables for the bigger supply). There is a third option; the 5Vdc 60 Amp supply I bought on eBay this spring. It ought to be a chlorate producing workhorse! I'll have to add more later, I have to go help my Grandson carve pumpkins... (Happy Halloween). WSM Edited November 1, 2010 by WSM
chemid Posted October 31, 2010 Posted October 31, 2010 (edited) Hi guys, this is my setup. MMO coated mesh titanium anodestainless steel cathode5v @ 20 amp computer psu. Im taking KCL and trying to get CLO3. After I run this for a week and get the crystals at the bottom, how should I filter it? Should I run the hot mixture through cofee filters, pour ice cold distilled water over the white crystals, dump the water at the bottom then have the crystals usable? Or should I ice the entire mixture first, run it through coffee filters, and then pour more ice water through it? The filtration is where I'm getting confused. Edited October 31, 2010 by chemid
WSM Posted November 1, 2010 Posted November 1, 2010 (edited) Hi guys, this is my setup. MMO coated mesh titanium anodestainless steel cathode5v @ 20 amp computer psu. Im taking KCL and trying to get CLO3. After I run this for a week and get the crystals at the bottom, how should I filter it? Should I run the hot mixture through cofee filters, pour ice cold distilled water over the white crystals, dump the water at the bottom then have the crystals usable? Or should I ice the entire mixture first, run it through coffee filters, and then pour more ice water through it? The filtration is where I'm getting confused. Hi Chemid, I've had great luck scooping wet chlorate crystals out of the cell with an aquarium fish net (about $1 or so at Walmart and it keeps my hands from smelling like bleach), then put them in a compatible fine mesh fabric sieve over a glass bowl. Rinsing the crystals with chilled distilled water is a good idea plus save the rinse water for make up water in the next run. Swede uses the bucket filters used for biodiesel manufacture to separate and wash his crystals and I think that's a great idea (see Swede's blogs, an excellent source of good ideas). Coffee filters are a fairly cheesy substitute for real lab filter paper. The best setup would be a vacuum filtration setup with a buchner funnel, real filter papers and a source of vacuum (even a water aspirator would work). I know a man who uses a salad spinner with a fine (synthetic) fabric liner in it all set in a small plastic washtub as a "poor-mans- centrifuge" to remove moisture from his chlorate crystals. If you ice the "entire mixture first" you might drop out KCl with the KClO3 and that would not be good (self made contamination!). If you need greater clarification of any of my suggestions, please ask (I'm not always as clear in my descriptions as I think I am ). Good luck and have fun!!! WSM Edited November 1, 2010 by WSM
WSM Posted November 1, 2010 Posted November 1, 2010 If you have a need for distilled water (and who doesn't?) and have a Target store in your area, check out their grocery section. I was pleasantly surprised to see it in 1 gallon bottles and on sale! My wife is still questioning why I need six gallons of distilled water (She's right, maybe I should have gotten more!!!). Walmart also has 1 gallon bottles of distilled water available, shop and compare prices. For most of my electrochemical experiments, I'm using water purified through a kitchen RO (reverse osmosis) system which is proving to remove ~95% of the dissolved solids in my tap water (from ~400ppm in tap water to <20ppm in the purified water). Swede just uses his tap water, and considering the contaminants already in the KCl water softener salt and hardware store HCl, he's probably right. For pyrotechnic uses, 99% purity in the final product is usually acceptable (that's 100,000ppm allowable contaminants, Yuk!) by Mil-Spec standards. Crystalization is an excellent method of purification (nature's way) and does a very good job of separating what we want from what we don't. My main concern is since we are re-using the rinse water and mother liquor from the cell, are we concentrating the contaminants in our systems? We are, but the crystalization is removing them from our product. Given this reality, I believe we need to limit the number of cycles we put the water through, cut our losses at some point, dump the old solution and start fresh with new. Experimentation is required to determine the best limits to set (Where's Swede when you need him? Maybe I'll have to step up to the plate on this one ). By careful rinsing of our crystals with chilled purified water our product purity is usually 99.9% if we're careful. That's closer to reagent grade than the technical grade material usually used in pyrotechnics. The number one contaminant in commercial chlorate is KCl. If that's the worst we should be okay using our chlorate directly. My ultimate goal is to create feedstock for a perchlorate system (actually it's learning how on a DIY basis). My actual need for KClO4 is low but my need for practical knowledge on producing it is considerable, and my main motivation! It's impressive how small a system will provide more oxidizer salt than most amateurs can use in the normal course of experimenting . WSM
Mumbles Posted November 1, 2010 Posted November 1, 2010 It's probably worth noting that while KCl may seem like a benign contaminant, it has actually shown to be a sensitizer for chlorate compositions. The thought is that it forms small amounts of KClO and/or KClO2, which are much more reactive. At the levels in your product though this is probably not a very big issue. What other contaminants would you expect to be in the HCl and KCl? I would maybe expect some iron in both, and bleach or chlorine in the HCl. I could maybe come up with some spot tests for the iron for you to see if things are concentrating.
WSM Posted November 1, 2010 Posted November 1, 2010 It's probably worth noting that while KCl may seem like a benign contaminant, it has actually shown to be a sensitizer for chlorate compositions. The thought is that it forms small amounts of KClO and/or KClO2, which are much more reactive. At the levels in your product though this is probably not a very big issue. What other contaminants would you expect to be in the HCl and KCl? I would maybe expect some iron in both, and bleach or chlorine in the HCl. I could maybe come up with some spot tests for the iron for you to see if things are concentrating. Hi Mumbles, Thanks for the input. I hadn't considered KCl to be a sensitizer and that's good to know. Any references? I suppose that makes good rinsing more of a requirement for safety than merely a good suggestion. Other contaminants? I was aware of the iron in HCl and some dark spots (of unknown) in the KCl. I was thinking my hard tap water may introduce some calcium and magnesium ions into my cell and chlorates of those metals aren't good either (hence my desire to use purified water to start, I'm hoping RO water is good enough). I'm happy to have any tests you care to share. I do have a few analytical reagents tucked away around here somewhere and don't mind using them occasionally to determine what I'm dealing with. It pays to work from a basis of knowledge rather than guesswork (safer, too!). Thanks for the offer. Are the spot tests qualitative or are they quantitative as well (that would be nice!)? WSM
Mumbles Posted November 1, 2010 Posted November 1, 2010 Well, the tests are quantitative depending on what kind of toys you have access too. A UV/Vis spectrometer makes things a lot easier. The quick test for iron is done by adding acidified Potassium Thiocyanate solution. Equal amounts of 10% w/v KSCN and 2M HCl are mixed just prior to use. A few drops of 3% hydrogen peroxide are then added. A brick red color indicates the presence of iron. It's dependent on Ferric iron, thus the hydrogen peroxide. I think this test is fairly sensitive.
dagabu Posted November 1, 2010 Posted November 1, 2010 Knock, knock... Hey, I just wanted to pop in and see what you all were doing. You guys are amazing, I cant understand a thing you guys post but I sure am impressed. One question before you push me back out the door into "neural typical" land, is the manufacturer of (Per) chlorates at all financially feasible?
bikemaster Posted November 1, 2010 Posted November 1, 2010 (edited) Hi guys, this is my setup. MMO coated mesh titanium anodestainless steel cathode5v @ 20 amp computer psu. Im taking KCL and trying to get CLO3. After I run this for a week and get the crystals at the bottom, how should I filter it? Should I run the hot mixture through cofee filters, pour ice cold distilled water over the white crystals, dump the water at the bottom then have the crystals usable? Or should I ice the entire mixture first, run it through coffee filters, and then pour more ice water through it? The filtration is where I'm getting confused. This is maybe the first time that you use your cathode, but with time you will notice black deposite create by the cathode... If you want a product clear from this oxide you have to recrystallized your product. This is the way I do it (I also have SS cathode): 1. Let you cell cool down ( Bring it down to 5C if possible)2. Screen the product through something that will catch the cristals but that will not take hours. (keep the liquor for the next run!)3. Dissolve the cristals in the least water possible. (with some more water because to much cristals will form during the filtration )4. Filter the solution through 2 coffee filters. (some cristals will form on the filter, but I redissolve and refilter it)5. Cool the solutions slowly to around 4C. (If the solution is put directly in the frige, you will trigger a flash recristalization and a lot of KCl will cristalize)6. Filter the cristals of KClO3 and try to have the less water as possible on them (this water is full of contaminant). Them rince them with cold distilled water. (Vacuum filter help a lot on this step)7. Dry the cristals somewhere there will be no contamination from the air. (outside in the wind is not good...)8. Simple observation. (It your cristal seem clean this is a good start, but if you can some contaminant on the cristal, you to restart from point 6...)9. Mill the cristals if you want powder! P.S. : Before disolving anything related with chlorate cell liquor, the will corrode metal.... If you don't want your parents on your back be careful (sorry but i don't know your age...) @DagabuIf I want to have chlorate to my door it will cost me over 10$/pound and even more for perchlorate...I don't know for other, but I buy 40 lbs of KCl for 12 $, water is free and I pay 0,07$ per KWh;)For the moment perchlorate cost a lot because anode cost a lot, but if we find a very good way to make LD anode it will maybe change!For sure we put a lot of time on this project and less on firework...But for a future chemical ingineer the experience worth a lot! Edited November 1, 2010 by bikemaster
Mumbles Posted November 1, 2010 Posted November 1, 2010 I forgot the exact source I read about the chloride sensitivity. I am reasonably sure it came from Principles of Pyrotechnics by Shidlovskiiy.
dagabu Posted November 1, 2010 Posted November 1, 2010 Well, maybe you guys can come up with a plug and play version some day so a dummy like me can pretend to make pot perc! Still, you guys ROCK!!
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