50AE Posted June 3, 2011 Share Posted June 3, 2011 Soo, you want photos? http://img33.imageshack.us/img33/264/picture154i.th.jpghttp://img233.imageshack.us/img233/5251/kclo3crystals.th.jpg Link to comment Share on other sites More sharing options...
pyrojig Posted June 3, 2011 Share Posted June 3, 2011 Very nice !!! I have my cell running at 17A ( sadly my pics are not so pretty) Im using graphite . Im getting crystals that are over an inch in length.... They are very interesting for sure. I have been viewing Swede's blogs.... , great stuff !!!! That guy has some serious tools. I followed that link to the E-Bay page and found the source of cheap Ti MMO stretched screen for making anodes. Great price !!! EXPANDED TITANIUM MESH STRETCHED SCREEN MMO COATINGI see that he was using a spot welder ( or TIG)to attach the posts to the screen. .What is the best way to cut Ti btw? I was wanting to purchase some of these and make them for my cell... I would love to get away from carbon rods. Link to comment Share on other sites More sharing options...
hillbillyreefer Posted June 3, 2011 Share Posted June 3, 2011 Very nice !!! I have my cell running at 17A ( sadly my pics are not so pretty) Im using graphite . Im getting crystals that are over an inch in length.... They are very interesting for sure. I have been viewing Swede's blogs.... , great stuff !!!! That guy has some serious tools. I followed that link to the E-Bay page and found the source of cheap Ti MMO stretched screen for making anodes. Great price !!! EXPANDED TITANIUM MESH STRETCHED SCREEN MMO COATING I see that he was using a spot welder ( or TIG)to attach the posts to the screen. .What is the best way to cut Ti btw? I was wanting to purchase some of these and make them for my cell... I would love to get away from carbon rods. Thanks for the link pyrojig, just ordered up three anodes too. Seeing as I'm ordering stuff what should i use for a cathode? Don't have time to go back through the entire thread ATM. Link to comment Share on other sites More sharing options...
WSM Posted June 3, 2011 Share Posted June 3, 2011 Very nice !!! I have my cell running at 17A ( sadly my pics are not so pretty) Im using graphite . Im getting crystals that are over an inch in length.... They are very interesting for sure. I have been viewing Swede's blogs.... , great stuff !!!! That guy has some serious tools. I followed that link to the E-Bay page and found the source of cheap Ti MMO stretched screen for making anodes. Great price !!! EXPANDED TITANIUM MESH STRETCHED SCREEN MMO COATINGI see that he was using a spot welder ( or TIG)to attach the posts to the screen. .What is the best way to cut Ti btw? I was wanting to purchase some of these and make them for my cell... I would love to get away from carbon rods. The titanium used is CP (commercially pure) and is able to be cut with a fine tooth hack saw or other metal cutting saw (by power or by hand). Titanium does heat up while sawing. I would think water would cool it down without causing (much) trouble for the saw. You will enjoy nice, clean chlorate for a long, long time with the MMO (as opposed to the graphite). WSM Link to comment Share on other sites More sharing options...
WSM Posted June 3, 2011 Share Posted June 3, 2011 Thanks for the link pyrojig, just ordered up three anodes too. Seeing as I'm ordering stuff what should i use for a cathode? Don't have time to go back through the entire thread ATM. CP titanium is the optimal material of choice for cathodes when using MMO anodes. I usually try to match the cathode size to the size of the anode; and surrounding the anode with two cathodes (connected electrically outside the cell) gives optimum performance of the anodes. I find that as I'm working on different electrochemical cells, I re-read Swede's blogs occassionaly to keep myself on the right track. If you're interested in further reading, I can quote a lengthy bibliography of industrial electrochemistry texts and articles. Let me know. WSM Link to comment Share on other sites More sharing options...
WSM Posted June 3, 2011 Share Posted June 3, 2011 Hi 50AE, Thanks for the photos (nice pile of crystals !). They look very familiar (not unlike some I have stored in various jars, etc.). Keep up the good work. WSM Link to comment Share on other sites More sharing options...
pyrojig Posted June 4, 2011 Share Posted June 4, 2011 Thanks WSM.... I will give a hacksaw a run at it... What is the easiest way to attach the Ti leg to the MMO mesh in your opinion? I have access to a mig( not TIG) welder and maybe a spot welder... I can rig a MOT to spot weld if it becomes a need. I am excited to get clean chlorate v.s. messy filtering hot boiling kclo3 in solution to get the dang graphite out ... Not fun in my books..... Link to comment Share on other sites More sharing options...
WSM Posted June 4, 2011 Share Posted June 4, 2011 Thanks WSM.... I will give a hacksaw a run at it... That's what I used. What is the easiest way to attach the Ti leg to the MMO mesh in your opinion? Have someone else do it ! Seriously though, I believe spot welding is the most effective means I've seen. I use a spot welder bought from Harbor Freight Tools. I have access to a mig( not TIG) welder and maybe a spot welder... I can rig a MOT to spot weld if it becomes a need. Swede used a TIG welder to bond cathodes to leads but was concerned (justifiably) about destroying the MMO or exposing himself to ruthenium fumes by using the TIG for attaching leads to the MMO. He also expressed concerns about fumes during spot welding, but we both do it. I figured, "just hold my breath and go for it" (outdoors ).I am excited to get clean chlorate v.s. messy filtering hot boiling kclo3 in solution to get the dang graphite out ... Not fun in my books..... I completely agree. Good Luck! - WSM Link to comment Share on other sites More sharing options...
WSM Posted June 4, 2011 Share Posted June 4, 2011 .... I have access to a mig( not TIG) welder and maybe a spot welder... Hi pyrojig, I forgot to mention, I have access to a MIG also. I once considered setting it up to do titanium; that is, till I reallized that between the expense of getting a different bottle of gas and special CP titanium wire !!! I can buy a lot of other materials for what it would cost me to set up and start learning how to weld the electrodes together. I decided to spend my resources elsewhere. The Harbor Freight spot welders (both 120V and 240V versions) go on sale from time to time for about $150 US, which has turned out to be money well spent. I was also impressed it was made in America! That is, till I looked closer, and reallized it says "Made in Armenia"! Obviously, I wear glasses for a reason ... WSM Link to comment Share on other sites More sharing options...
Arthur Posted June 4, 2011 Share Posted June 4, 2011 Welding MMO to CP Ti hangers is best done with an adequate spot welder. Yes you could make one, but for less than 20 spots it may be cheaper to pay a welding shop to weld them to your spec. Link to comment Share on other sites More sharing options...
pyrojig Posted June 4, 2011 Share Posted June 4, 2011 Welding MMO to CP Ti hangers is best done with an adequate spot welder. Yes you could make one, but for less than 20 spots it may be cheaper to pay a welding shop to weld them to your spec. Thank you guys for the replies .... I probably will have a shop do it if a friend of mine doesnt have a spot welder.. I am lucky to know a handful of guys with shops and metal working goodies ...including a CNC machine . Dang what I I'd give for one of those ...!!! From searching many sites, Im really finding that making (welding)my own is the cheapest ....These things arnt that cheap sold in sets (cathode TI, and MMO anode) ..at least $100..For a GOOD set.. My interests are chlorate at the moment, and perch in the near future. Sure is an wonderful thing to be able to use electricity and salt to get a valuable oxidizer !!! Sweet simple chemistry with a high reward! Link to comment Share on other sites More sharing options...
WSM Posted June 5, 2011 Share Posted June 5, 2011 Thank you guys for the replies .... My interests are chlorate at the moment, and perch in the near future. Sure is an wonderful thing to be able to use electricity and salt to get a valuable oxidizer !!! Sweet simple chemistry with a high reward! True, but like I said before, " It's amazing how fast a simple idea can get complicated..." Have fun (I do)! WSM Link to comment Share on other sites More sharing options...
hillbillyreefer Posted June 5, 2011 Share Posted June 5, 2011 CP titanium is the optimal material of choice for cathodes when using MMO anodes. I usually try to match the cathode size to the size of the anode; and surrounding the anode with two cathodes (connected electrically outside the cell) gives optimum performance of the anodes. I find that as I'm working on different electrochemical cells, I re-read Swede's blogs occassionaly to keep myself on the right track. If you're interested in further reading, I can quote a lengthy bibliography of industrial electrochemistry texts and articles. Let me know. WSM Thanks for the offer, on the articles, unfortunately my chemistry classes were all prior to the invention of the electrochemical cell, lol. I'll read through Swede's blogs and start figuring out my cell. My main question was what material to use for the anode? Would lead plates out of a lead acid battery work? Been meaning to ask what your favorite wsm cartridge is? Link to comment Share on other sites More sharing options...
WSM Posted June 5, 2011 Share Posted June 5, 2011 (edited) Thanks for the offer, on the articles, unfortunately my chemistry classes were all prior to the invention of the electrochemical cell, lol. I'll read through Swede's blogs and start figuring out my cell. My main question was what material to use for the anode? Would lead plates out of a lead acid battery work? Been meaning to ask what your favorite wsm cartridge is? The cleanest anode (and longest lasting, so far) appears to be MMO on titanium. I thought of LD on battery plates, also. Sadly, no, they won't do what we'd like them to do. I've done .22 LR the most (lots of cheap fun !). I keep thinking I'd like to get a 45-70 like a friend of mine has, though a stainless-steel .44 cap and ball is nostalgic AND easy to clean . (or did I misread your question ?) WSM Edited June 5, 2011 by WSM Link to comment Share on other sites More sharing options...
hillbillyreefer Posted June 6, 2011 Share Posted June 6, 2011 (edited) The cleanest anode (and longest lasting, so far) appears to be MMO on titanium. I thought of LD on battery plates, also. Sadly, no, they won't do what we'd like them to do. I've done .22 LR the most (lots of cheap fun !). I keep thinking I'd like to get a 45-70 like a friend of mine has, though a stainless-steel .44 cap and ball is nostalgic AND easy to clean . (or did I misread your question ?) WSM Thanks for the answer on the plates. Didn't think it would work, but had to ask. You can't go wrong with a 45-70 in a modern rifle, light loads for plinking, then load her up almost to 458 winchester for hunting big bears and moose. They are a lot of fun. Ahh heck they are all fun, cap and ball revolvers are a hoot. I've had the priviledge of firing a few, always good for a giggle. Now back to reading and talking about perchlorate. Edited June 6, 2011 by hillbillyreefer Link to comment Share on other sites More sharing options...
dagabu Posted June 6, 2011 Share Posted June 6, 2011 *In no way related to chemistry* I love my 45-70! Its a single shot, 1000 yd veneer tang site, hand cast 500gr, gas-checked bullets. Steel butt plate lets you know who is in charge. I love to go to the range with several rifles and let others shoot a few rounds from my Ruger custom 10/22 that we call the Daisy Picker then from my single shot .223 then the .45-70. The .22 with a 1" bull barrel barely moves when fired from a bipod, the .223 has a nice push when fired and the .45-70 kicks like a friggen mule! Now, back to crystals, -dag Link to comment Share on other sites More sharing options...
oldmanbeefjerky Posted June 8, 2011 Share Posted June 8, 2011 (edited) Nice job WSM! One thing about my chlorate production. Each time I refill the cell with fertilizer KCl, bubbles are evolved and then an... ughhhh, disgusting smell. It's not chlorine, it's not an irritating odour, it's like something sweet, shit, and vomit are mixed together. It almost made me puke infront of my cell today. And then, a white foam like from someone's mouth appears on the surface, making the thing even more.. unattractive. Also, this KCl seems to be acidic, it lowers the pH a little bit. well, if you havent used lab grade 99.95% pure or higher, chances are a little organic ion, such as citrate and somesuch may have found its way into the solution.my current batch of chlorate i have going , which i am simply experimenting, using lead electrodes from an sla, started to sting of rotting fish or rotting rat (those who have smelt dead mouse or rat will know what i mean),turns out that the container i was using wasnt washed out properly from when it was used to make some hmtd, and the hexamine, apparently formed hexance according to my friend, and started making the smell which could be detected from more than 3 m away. my point being, is that the smell could be from any organic forms of potassium mixed up with the chloride. all of these will form an acid upon electrolysis if they have access to hydrogen gas, i think, and these acids would certainly increase the ph. -edit- my cell, began to make the smell right after it began to make a very large amount of foam , just thought i should mention it -edit- ide hate to double post so ill just this this here. im pretty sure, actually quite certain, that its possible to make lead dioxe electrodes by the electrolysis of lead acetate and copper acetate, in the same way you can using lead nitrate and copper nitrate. a guy managed to do this, heres a quopte from him:"get 100 grams of water soluable lead (lead nitrate, or lead acetate)get 60 grams of water soluable copper (copper nitrate, copper acetate, not chloride PbCl is insoluable in water) mix chemicals with distilled water and 2 drops of dish soap (surfactant, it makes a smooth coating)mix until fully dissolvedwith a amperage limited power supply attach your graphite electrode to the positive and a piece of copper to the negative.the copper ions take less voltage to reduce therefore they get priority to the cathode forcing the lead ions to the anode where they are oxidized to lead dioxide (solid) you should limit the amperage to as low as possible 2ma per square cm worked well for me. rotate the electrode 90 degrees every 15 minutes for 2 hours minumim. (after 2 hours I had 10 grams of PbO2 deposited on my graphite electrode.good things come to those who wait" its easy to make, just make/get yellow lead oxide, then place it into vinagar, and wait a few days, then you have lead acetate. electrolyse it, along with copper of the same kind, which shouldnt be too hard to make, and there you have it, lead dioxide plated electrodes.i also read elsewhere you can use lead scrapeings, and react with vinagar, but it takes months to make.i think citrate may work also. i added citric acid into a electrolysis cell where i was trying to convert red lead back into dioxide and lead, and within 12 hours, half of the lead settled on the bottom of the jar had attached itself to one of the electrodes, making a massive 300g lead sponge, i dont know if it was dioxide or not. on my australian (queensland) based chemical supplies site, i am currently stockpiling, i think i might sell lead dioxide kits and lead dioxide electrodes. what would you people who are unable to make lead dioxide electrodes but need them, be willing to pay for the acetate kits or pre built electrodes? Edited June 8, 2011 by oldmanbeefjerky Link to comment Share on other sites More sharing options...
WSM Posted June 8, 2011 Share Posted June 8, 2011 Welcome oldmanbeefjerky, Interesting thoughts about the agricultural KCl. I also like the ideas expressed about using alternate materials to plate LD on conductive substrates. Do you know if the lead dioxide is alpha or beta form? It's my understanding that we seek the harder, crystaline beta form, though I've seen reports of plating the porous alpha form then the beta form over that. These things would be good to know, rather than take a "Well...I think so" approach (especially if one were to go to all the trouble and expense of setting this up). If you can't find or buy LD anodes, making them is the only option left if you're determined to use LD. oldmanbeefjerky, where do you hail from? I wouldn't mind having another source of materials if the shipping isn't cost prohibitive . WSM Link to comment Share on other sites More sharing options...
oldmanbeefjerky Posted June 9, 2011 Share Posted June 9, 2011 well, currently i am in the northern territory, but will soon be moving too makkay, which is an hour north of brisbane, or brisbane suburbs.i thought it would be a good idea to make a pyrotechnics chemicals buisness in the northern territory, as nobody has access to such chemicals, which is silly considering its the only state in which public use of fireworks is even legal!when you say, where do i hail form, i take it you mean where am i more specifically, the answer, as mentioned before, will be makkay, but currently i am in darwin. unlike all the other australian chemical suppliers in general, i wont be shipping by courier unless absolutely neccesary, which some people think is, for chems like copper nitrate for some stupid reason, its safe enough to send by international mail, but not locally by air, which is almost guarranteed to be sent by freight trucks going across australia.so shipping wont be all that much, at most ide say it would maybe cost $3-6, $1 for packing, and 2-5 for actual shipping costs for up to 500g. and about 2-3 extra for international shipping . the actual lead and copper acetate , ide be selling very cheaply, maybe $5 for 100g, depending on how much it costs me to make, which wont be much as i have an unlimited amount of lead, and know where to bulk buy highly concentrated vinegar as acetic acid.the reason ide sell kits is because of the high costs of shipping electrodes, which would be $5 in australia and $9-12 internationally, per 2 electrodes.once i find somewhere though that i can get the kind of lead sheet i desire, i may experiment with making LD electrodes by electrolysis of sulfuric acid with two lead electrodes , in which the sulfuric acid is a catalyst , meaning that i can make as many lead dioxide electrodes as i want and i wont loose any precious acid. lastly, i am quite certain that the lead dioxide is beta, if made from the acetate, and pure water is used. but i cant be sure until i make it myself. as soon as my batch of lead acetate is done, i will make a LD electrode, and if it i alpha, i suspect that it would be spongy yes? or it would fall apart during electrolysis? so it shouldnt be too hard to figure out. though the guy who told me did say that it has been used to successfully make sodium chlorate with not much corrosion. Link to comment Share on other sites More sharing options...
WSM Posted June 9, 2011 Share Posted June 9, 2011 well, currently i am in the northern territory, but will soon be moving too makkay, which is an hour north of brisbane, or brisbane suburbs.i thought it would be a good idea to make a pyrotechnics chemicals buisness in the northern territory, as nobody has access to such chemicals, which is silly considering its the only state in which public use of fireworks is even legal!when you say, where do i hail form, i take it you mean where am i more specifically, the answer, as mentioned before, will be makkay, but currently i am in darwin. unlike all the other australian chemical suppliers in general, i wont be shipping by courier unless absolutely neccesary, which some people think is, for chems like copper nitrate for some stupid reason, its safe enough to send by international mail, but not locally by air, which is almost guarranteed to be sent by freight trucks going across australia.so shipping wont be all that much, at most ide say it would maybe cost $3-6, $1 for packing, and 2-5 for actual shipping costs for up to 500g. and about 2-3 extra for international shipping . the actual lead and copper acetate , ide be selling very cheaply, maybe $5 for 100g, depending on how much it costs me to make, which wont be much as i have an unlimited amount of lead, and know where to bulk buy highly concentrated vinegar as acetic acid.the reason ide sell kits is because of the high costs of shipping electrodes, which would be $5 in australia and $9-12 internationally, per 2 electrodes.once i find somewhere though that i can get the kind of lead sheet i desire, i may experiment with making LD electrodes by electrolysis of sulfuric acid with two lead electrodes , in which the sulfuric acid is a catalyst , meaning that i can make as many lead dioxide electrodes as i want and i wont loose any precious acid. lastly, i am quite certain that the lead dioxide is beta, if made from the acetate, and pure water is used. but i cant be sure until i make it myself. as soon as my batch of lead acetate is done, i will make a LD electrode, and if it i alpha, i suspect that it would be spongy yes? or it would fall apart during electrolysis? so it shouldnt be too hard to figure out. though the guy who told me did say that it has been used to successfully make sodium chlorate with not much corrosion. G'day. Unfortunately, I'm in the US (lower left coast) and the shipping is an issue. Too bad, I'm always on the lookout for new suppliers (especially locally). It's good to have alternate sources though. Keep up the good research ! The information gleaned from such work will benefit us all (any photos yet?). Who knows, maybe I'll give the acetic acid plating salts method a try?! Thanks for sharing, oldmanbeefjerky. WSM Link to comment Share on other sites More sharing options...
oldmanbeefjerky Posted June 10, 2011 Share Posted June 10, 2011 (edited) G'day. Unfortunately, I'm in the US (lower left coast) and the shipping is an issue. Too bad, I'm always on the lookout for new suppliers (especially locally). It's good to have alternate sources though. Keep up the good research ! The information gleaned from such work will benefit us all (any photos yet?). Who knows, maybe I'll give the acetic acid plating salts method a try?! Thanks for sharing, oldmanbeefjerky. WSM aw!another potential buyer swept away by the marshmellow avalanch that is the pacific ocian as for the lead oxide acetate mixture, itle take a few more days before i get any results, because my yellow lead oxide (the only kind i know will work for this), was derived by super heating the lead then blowing ir with air (lead oxide floats in a molten lead bath, so if air is passed through it, all oxidized lead will float to the top), which means it is infused in the lead metal. its my first time making it.but i will definately post some pics once the electroplating is all done. by the way, since oldmanbeefjerky is such a hasle to type due to its length, everyone can just call me ombj, even i do! p.s, litharge is lead oxide, yellow or red does not matter, though ide go with yellow Edited June 10, 2011 by oldmanbeefjerky Link to comment Share on other sites More sharing options...
WSM Posted June 10, 2011 Share Posted June 10, 2011 aw!another potential buyer swept away by the marshmellow avalanch that is the pacific ocian as for the lead oxide acetate mixture, itle take a few more days before i get any results, because my yellow lead oxide (the only kind i know will work for this), was derived by super heating the lead then blowing ir with air (lead oxide floats in a molten lead bath, so if air is passed through it, all oxidized lead will float to the top), which means it is infused in the lead metal. its my first time making it.but i will definately post some pics once the electroplating is all done. by the way, since oldmanbeefjerky is such a hasle to type due to its length, everyone can just call me ombj, even i do! p.s, litharge is lead oxide, yellow or red does not matter, though ide go with yellow Hi ombj,Don't be bashful, you can show photos of the process too . It'll probably be just as educational as the finished product ! Thanks for bringing the the whole notion of creating lead dioxide plating from the basic elements to light. I was thinking it had to be done with expensive and hard-to-get reagents, but I see you're starting with a much more basic approach. Good on ya . I can't wait to see the fine details! WSM Link to comment Share on other sites More sharing options...
oldmanbeefjerky Posted June 10, 2011 Share Posted June 10, 2011 thats what i was planning on, but i accidentally spilt my whole thing on the ground off the shelf. Im not used to using gloves, and doing things that require such precision .the only avaliable gloves i have , as my bulk order for latex gloves hasnt yet come in, are some thin leather gardening gloves, which i am rather clumsy in. anyway, im gonna take on a whole other method of making the lead acetate, because i have high purity hydrogen peroxide, im going to use peroxide and acetic acid together to make about 30-50 grams of lead acetate. apparently it only takes an hour or so to completely dissolve.this time though ill take pictures throughout the process. sorry mates, looks like your gonna have to wait a few more days before i confirm the results. Link to comment Share on other sites More sharing options...
WSM Posted June 10, 2011 Share Posted June 10, 2011 (edited) Hi ombj,Don't be bashful, you can show photos of the process too . It'll probably be just as educational as the finished product ! Thanks for bringing the the whole notion of creating lead dioxide plating from the basic elements to light. I was thinking it had to be done with expensive and hard-to-get reagents, but I see you're starting with a much more basic approach. Good on ya . I can't wait to see the fine details! WSM I can't wait to see the fine (and final) details !!! Sounds good, ombj! Keep up the good work, and do be careful . WSM Edited June 10, 2011 by WSM Link to comment Share on other sites More sharing options...
WSM Posted June 10, 2011 Share Posted June 10, 2011 (edited) Oops , Sorry about the double post WSM Edited June 10, 2011 by WSM Link to comment Share on other sites More sharing options...
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