Mild Updates

July 19-2018 {Everybody needs my time...

I found a leak in the still's top plate. so I soldered that shut and soldered on a length of pipe to cut down to the 45 elbow for the alcohol extraction. I'll need to make a custom arrangement for the deuterium processing, but it's looking pretty good right now.  I gotta drag out the other battery in order to start charging it as well. I still need to build the upgraded solar tracker, but that'll be later. for now I'll just charge the battery on the back porch. I really gotta make some progress on that. Tonight. I'm going to dedicate myself tonight to neutralize the next liter of acid and a bunch of other things. I gotta do the Acid tonight. If it works out then i should be able to just run with tank construction. the only one I gotta be careful about is the Acid one. I can't finish that just yet. I think I might add in a third pump for the carbonate solution. I think I'll hunt down/make a battery box for the U1 battery I have, as I feel like that's a better fit for now. I'll still drag the rest of the batteries out of the corner and put them back on the trickle charger. I'm going to really crunch on the code coming soon here. I'll dedicate that to tomorrow. }

July 23, 2018 - 

Hello there! I ran an initial test of the Still and things went WONDERFULLY! I managed to liberate somewhere in the ballpark of 500mL of somewhat contaminated Alcohol, It's contaminated enough to not burn, and the measurement is based off of listed volume of my container, because I still have more alcohol to liberate. But it's super clear! I had a tad over a gallon of dregs I'd collected, so I figured I'd go for broke and burn it all. There is a downside to this, it takes forever for the junk to heat up. Something I'll have to keep in mind later. Also, I think it will be pertinent to add in the big gauge thermometer in the side of the pot, but I'd like to do it a little differently,  I still gotta play with that, but I had the thermometer at the top, so I feel like I was boiling the water at certain places. If I can find one, I'll make a way to hang the thermocouple at the top 2" of solution in order to have a more accurate temperature setting. I also need to dig up the stainless steel waddings for the column. I know I should do copper to avoid galvanic corrosion, but I think I'll be fine for the time being, Besides, I already have them. The very next thing i want to do is make a dedicated cooling bath for this system. I'd like to be able to push a button and have the system purge a half-gallon of coolant so I can add fresh ice to the mix. That's a nice to have at this point though. I can jerry-rig that into place. 

I Neutralized the next liter of acid (finally) and things looked like they went off without a hitch, there's an issue I saw initially, and that was when I refrigerated the mixed solution, nothing seemed to precipitate. It's been in the fridge since... shoot... I don;t have the time with me... either two or four p.m. No, it was two because i checked it at three, four and seven. right. I'll check it when I get home today. 

UPDATE: 07/24/2018

I looked at the mix yesterday, and it is still completely liquid. It's thick, but it's still liquid, with no discernible crystals. I decided to take a chance and added in ~40mL (measured with a 250mL Graduated Cylinder) adn lo and behold, it fizzed. So, what can we learn from this? 

  1. Slow down and double check your measurements,
  2. measure everything twice.

So that's all I have for now, Just a simple update. 

Mid-Afternoon Updates

I've designed a basic basket for measuring the appropriate amount of Sodium Carbonate. I still gotta figure out how to empty it into the system, but that's one less thing i gotta deal with. I do have to allocate some of the carbonate to 3d filament dehydration, but that should be minimal.

I've re-worked the file for the flange dimensions. Turns out it was 9.625" in diameter. The Lose an Inch method is good, but only if you remember it. Pops says he wants to come to PS1 to look around. I can show him the ShopBot and I can make my couple of parts. I might just make them all together. I'll definitely do that if it's something I can swing. Hopefully I can get enough free time tonight to neutralize the next liter of acid and do a final test. IF that works, then I'll finish construction of the system and go from there. I figure I can make the two five gallon jugs my first ten gallons of distilled water. This way I should be able to run through my distillation apparatus fairly quickly. I do need to get some more stable plugs for storage. I still need to finish making the distillation stand, but that can come later. I'd love to figure out where I put the digital thermometer...  

I've almost completely cleared out the space for the fine-tuning distillations, so all that's left is the neutralization system and the big boiler. I still need to solder the elbow onto the condenser. but I probably wont run a distillation until Thursday night. I will definitely be measuring volumes tonight. Assuming that all works out I should be long outta dregs. I should really make that a smaller container... I might have a gallon in there by now, but I kinda doubt it. Once I get that taken care of, I can get te bucket for more acid and run things again. i'm thinking of insulating a toolbox and using that as an all in one cooling unit. but i gotta figure out which one will be sufficient. If i can, i'll run one apparatus off of the tiny little water pump that i should probably ensure is actually working before i get things going. On the wildly ambitious chance that it is, i can run both apparatus off of the same chiller. I hope this is the case. If it is then there is hope that i can get through all of the water in quantitatively very little time. I might be able to 3d print a fill tube of sorts. what would be ideal is another 500mL flask with a double neck, but we'll suffer through this first. One thing is for sure, the sooner i can get my station set up, the sooner science starts happening. If i can effectively run this process, then i shall be able to mass-produce deuterium oxide. 

Now, I know what comes next. Once I get this system down, where do I go from there? Automation. If I can get like... 5 little 500mL stainless steel stills, each with their own thermocouple and heaters and everything, then I should be able to make this in the background! that would be really exciting for me. I have crude designs to make an automatic drain for the battery acid and should therefore only need to send it through the filter and even that could be automated to some extent. I think the very next step, that i could start tonight, is to test 3d printed float designs in the acid. although, I suppose I could just use a bobber... I'm going to explore that option. as it would be a great, inexpensive method of adding a float to something that would rarely if ever touch acid. 

that only leaves me with the neutralization issue. i suppose the simplest method would be to prepare a batch of solution in something like a 5 gallon container. I don;t think that would be too difficult, i would just need 8 kilos of sodium carbonate, and being as i bought 22 of them, i should be fine... volume... i didn't think about the volume... 3153cm^3... that is just shy of a gallon... to prep five gallons....Plus it bubbled and foamed a tad, so there;s other things at play here. however if i can work out the ideal math for it, then i hsould be able to... i need ot consult some textbooks here soon... i;m confusing even myself.

 

Just Shy of a Week Later

Alrighty then! Where are we? Not a whole lot further physically, but a whole lot further planningly. I've tested my calculations that the 423g of Sodium Carbonate will dissolve in 1.5L of water. I tested this by measuring out the Sodium Carbonate on a scale and adding it to a clean 2.5 gallon bucket, then taking an industry standard 1.5L SmartWater bottle and upending it into the bucket. While not the most accurate of measurements, I did mark the side of the bottle initially and will be double checking the volume here soon. The results were conclusive: It did dissolve, Now I've let it sit, as the dissolving managed to raise the solution temperature by quite the noticeable amount. I was mixing with a gloved hand and did not have a thermometer handy (foolish, I know,) And everything dissolved after a moment in the elevated solution temperature, I'll be going back to examine the cooled solution and make sure everything works. The main reason for the hand mixing, is that the solution turned cloudy and the bucket is opaque-white, so there was little chance of me seeing any kind of major dissolution. 

Aside from the mild progress, I did get my 250mL Graduated Cylinders in, so I can measure the acid in a timely manner. I didn't realize this when I ordered it, but the cylinders come with a cleaning brush! So winning there! I'll double check the measurement theory more accurately here this week. If the system works out, I'll be able to make the volumes of all three containers. Also, i'll be able to properly test the chilling method of crystal removal. I'm excited to know that the initial design works, the issue with this method is volume. I have at least 10 gallons of saltwater to clean up, and after i'm done with this next liter, it'll be somewhere around eleven. adding the acid in dry is honestly probably the best overall idea, but i'm not sure it's really feasible on the automated scale. Plus there'll be no simple chill for salt removal style of system. I do intend on processing the water prior to processing the crystals, as i know that will be a pain. If my calculations are correct with regards to the (error 312: Notes at home) g/L salt still dissolved in the chilled water, i should be able to clear out the main couple of buckets with little difficulty. I might be able to just re-fill the boiler after each initial distillation without actually having to remove the salt deposits in between... I still have to find a gasket for that... The internet is a wonderful place, but i wish people would post a walk-in price per unit for one John Smith. As I have zero business deals with any of these companies, so i'll most likely be paying top dollar for a science project. 

Anyways, I got the lit knocked off of the old tank. I was rushing and the edge is wasted, but it's reasonable and salvageable with some fancy welding. I still need to knock the hole in the lid for the stack and figure out what I'm going to do about that emergency blow valve thing. I may have to hire one of the other guys at PS1 for that... 

Oreilly has sheets of coolant-safe gasket materiel that are 16x36 ish that a buddy of mine is setting aside for me. $10 and I can use it for so many gaskets!!! Can't wait! Eventually I'd like to re-make the still into something a little more cleaning friendly, but we can't all be perfect... we can, however, all get very interesting ideas... More on that once I flesh them out a little...

So where does this leave us? Well, Today will be some cleaning and acid neutralization. along with grabbing the gasket material and proper tank dimensions. Once I get all of that together, I'll grab the first x-wing stave dimensions and head up to the great white north and run a set of parts out on the CNC. That will probably be later this week. What i think i'll do between now and then, is finally run the dregs through the still and finally attach the 45 to it. Then I can call it finished for a while. As soon as I can I'd like to get the major flange sections cut out on the Johnson Bandsaw. So I may take all of the metal I have with me to the cnc and just do an hour's batch job out there. Maybe, if the material works out well, i can cut out a couple of simple trusses out of the cross sections. And whaddayaknow i'm mixing projects again!

Anyways. I'm gonna work on math and code and see you all later!

Weekend Progress

We got a lot in this weekend, the still is so TINY!!! I cleaned up the condenser and riser Saturday night over Rambo, so we'll get that soldered together here soon. The rest of the still only took me an hour to actually construct. Cleaning took about twenty minutes, and the main body has a tiny neck on it so I couldn't fit my fist in it. I'm not too worried about that though; especially since the first run will be alcohol anyways. I'll grab the electric stove element and give that a crack here sometime. I started the Glue Up of the Reaction Vessel which has gotta be cleaned and cut, along with the sodium carbonate container, but before I do either one of those, I need to do a test mixing of the right quantities of Base to water in order to confirm volume, and I'd like to do another test for neutralization ratio's as well, as I got an interesting precipitate at the bottom of the first batch. I can also confirm that the green precipitate from the earlier experiment is due to the stripped galvanization, so it's probably a combination of zinc and iron, if I had to guess. Regardless, I'll be working on extracting that once I get a clear off the water, as I can use it for Zinc electroplating. 

I still need to remake the base on my filtration apparatus, and design the v2 of it. But that will require some CNC work and a plastic injection machine, neither of which I have at the moment. I have expectations to pump the acid using air pressure, however, I'm a little wary on this method's accuracy. However, it would be the simplest version to implement, and the code would be a breeze. I do feel that a pump would do better, but to find one durable enough for the job and cheap enough to be considerable would be a trick all in itself. I would like to explore that idea in the future for the pocket version, but for now, I think I'll stick with gravity and cutoff valves.

I also started the construction of a new lab bench on the basement sink! I had a section of 3/4" plywood I cut to fit the space roughly, I still need to make the center support and location stuffs, so that should be nice and quick. I have a sheet of plate glass that i'm using as the primary surface, so that's there, the camera will be able to clamp directly to the face of the lower shelf, and i can keep the Alconox and Spray Bottle on the small corner of the shelf. I also found the 2.5 gallon buckets I needed for the dump container, now all I must do is make an appropriate lid for it. This sounds like an excellent laser project! 

I'm starting work on the code, and it's going to be very long. I guess, maybe not so, but longer than blink, and that's long to me so far, so it's time to make 1's and 0's! 

Short Ammendum: 07/10/2018

I took the neutralized sample out of the fridge, and the entire thing was crystals. Now, this was mixing the dry sodium carbonate into the acid, so in the final setup there should be another ~2.5L of water involved in this. Note, any residue inside the bucket is from the acid neutralization. The bucket was cleaned thoroughly with Alconox prior to experimentation. 

Plans for the weekend

We started to get stuff in yesterday, we got the stand clamps in, I may have to order more of those, but we got the mantle in, the thermometer for the still, and the parts for the WanHao. Another thing I got in was the Crawler model, so I can jump right back into that boat again! 

Regardless, what are we doing for the weekend. I'd love to get the large boiler cut apart, and have stuff tacked together. I hereby declare the steel body the boiler and the copper body the still, for clarity's sake. The Still is scheduled to get here today, so I want to have that fully assembled by the end of the weekend, and I'd love to give it a solid break in test by cleaning all of the dregs I've gathered. It should be somewhere around half a gallon once all is said and done. I'm so excited to get that outta the way. I might lose some of the older alcohols to that just to be rid of them.  I'll be selecting wood for the distillation supports, I'd love to get that all assembled soon. Once I get the plywood concept done I'll have to make the real one, but that'll be down the road some. 

Back to this weekend's plans:

  • Initial boiler prep
  • Make & Mount both storage vessels (A/B)
  • Select wood for dist. Stand
  • Build Still
  • Clear off destination location
  • Go shopping for missing tank pieces
  • 3d print gears - I'm going to have to make some adjustments on this, as the adapter will be ridiculously thin at this point. More on this dilemma later. 
  • Design and print adapter for gears

I'm going to stop there because that's already a lot. I'm pretty sure the still on it's own will be at least three hours or so. 

Holiday Progress

Hello there, Happy Belated 4th of July. 

We built the full-size stand yesterday and took stock of the pipe at hand. I heartily believe I have enough material on hand to get through 90% of the construction of this behemoth. I am already planning on shrinking the overall volume of the machine in order to save on materials and the like, although this will increase the time spent processing fluids. But the overall goal of this exercise is not to make processing fast, rather, efficient, and not labor intensive. I have place several orders for equipment and the like, but much of it still needs assembly or construction. I have measured out my distillation apparatus, and it comes in a shade under 18" in length. Io that's going to push the entire machine up to ~22" long. I'm planning on using some old lumber for V1 of the stand. when I get a solid concept down I'll order a strip of aluminum for the top and make a nice one. I have some old oak panels that might be of good use here. plus I can fill in the void with lead and make it rock solid!

Regardless of all of that, I need to have a functional setup. I've got enough pieces here to make a functional prototype. It'll be ugly, but in the case that it works, I'll actually spend money on the electronics. I might even invest in a custom board with extra battery-charging capabilities! Regardless, the next step will be the primary boiler creation. at least, during daylight hours. I have a lotta welding to do... I bought the battery boxes for the general charging this weekend, so that's another thing I have to construct. 

Alright, Next Step: Calculate acceptable volumes of reaction/containment vessels. Once I get those numbers, I can continue with construction. Here's a picture of all of the math:

IT's rounded somewhat heavily, in the "overcompensating" direction. But the long and the short of it is I need three lengths of pipe: 9.5", 15" ad 28" - Volume of water wise, the reaction vessel only needs to be as large as the volume of both containment vessels, so 24.5" and really you could make that 24 if you wanted to save a buck, but because I've seen this reaction in open air, I know that this reaction can produce a considerable bubbling effect, so I would like the extra few inches in order to save some fittings. All this means is I can finally make some models and cut some pipe. I may cave and buy a 2 foot length of 4" PVC... I only need 14" to have significant overhead for the reaction chamber. that could really save some space. I'll get it running well, eventually i believe i can cut this down to half a liter and a bleach bottle, so we'll spend money at that stage. Doing some math, if I have to go to the hardware store for endcaps, I'll just get the length of pipe, it's an extra $3 so i'd be buying 2 caps instead of 1, plus i already have some caps for the pipe. 

Alright, well, I have a method for making the whole thing, filtration, neutralizing, and purification one clean and tight system. I'll look into that more later. Depending on the durability of PLA against concentrated H2SO4, I may be able to use old 3d prints for this system. how awesome would that be? I'll play around with that design later, as it should be able to neutralize at least half a battery's worth of acid at a time, but that varies from battery to battery, so i'll need a better metric than that. Regardless, that's a target for a later date, but how cool would that be? 

Back to the task at hand, I'll have to have the system feed fluid into the chamber automatically, so after a certain pressure raise... oh. Alright I gotta calculate out the pressure of fluid addition, glad I caught that now. So after 2 fluid additions, whatever metric that would be, if the pressure doesn't rise significantly, it'll immediately dump the system, that should help me out with keeping crystals out of the reaction chamber, god only knows how much of a nightmare that would be... I should make the top of the chamber accessible, just in case. Anyways, I've got an hour of downtime, so let me go model these things.

RoughRender.0001.JPG

Alright, looks like things work, barely. I can only neutralize about 3 liters of acid before I have to dump the bucket, but that's pretty good I think. I can get another couple of 2.5 gallon buckets and refrigerate them as soon as they're done and grow all of the crystals, IIRC they'd form within a day or two. I'm not sure if it will be necessary in the end, but I really wanna have as few potentially harsh chemicals inside the new still as I can. I should look up how much I can fill the bucket with crystals before I start contaminating things. I have no issue condemning a bucket to crystal duty as I build the new boiler. I have no interest in saving the paint on it at this time. maybe i'll copper plate the inside later... I'll definitely blast the inside to knock down the rust, at least initially. Anyways, time to go home. We'll see you later.

 

Day One Update

Alright, so where are we? I have begun modeling the parts in Revit for S&G, I'll probably finish the model by the end of the week. I've figured out a much simpler refill monitor, for the acid and base tanks: Toilets. I'm going to use microswitches tied to those tiny soda bottles and build vertical toilet tanks to monitor fluid level. So much easier than measuring pressure, especially because it wont fluctuate with outside press/temp.

I'm going to scale down my operation a bit. I heartily believe I can fit the entire structure into a 2'x4'x1' space, and I might be able to make that even smaller. I can't wait to get this thing up and running proper. I'm going to try to keep it as condensed as possible, so I'm planning, at this point, to have a 1 gallon (total) reaction vessel, with appropriately sized charging tanks. I'm going to use some more planning than I have in order to make this cost effective, but I believe I can make this entire system for less than $100. The structure is costing about $13, and more than one length of PVC is Construction Salvage, as well as the 5 gallon water jugs.

Alright, I'm getting a better sense of my scale now, I should be able to make things even smaller as a few of the models are based off of the old volumes. But the last major parts I need are some plastic rods. Because I'm trying to do this proper Sciencey like, I don't want to introduce metals or weird organics into the mix unnecessarily. I know one thing, tomorrow I build the full-size chassis. I've Got it! If I make the storage tanks 3" in diameter then I can use some 2" test caps for the floats! I just hope they're light enough. If not, I have some 3d printable buoys that should do just fine. I'll have to clear them first, If for no other reason than sealing. 

 

July Target

Alright, so the overview started to spill into this, so I figured I'd fill this in where I could.

The target for July is as follows: Get the holding tanks made/mounted, begin primary distillations, and get a prototype controller operational. Lay out specs for any remaining materials. 

Stretch goals for July: Get the V1 Controller installed, and install V1 standalone power supply. 

Alright, what does the target entail detail wise? I'm currently modeling the individual tanks and will be making a full-scale 3d model in the near future. It'll have as much detail as I deem necessary at this point, as I'd like to begin construction soon. I'll be going for the "cleanest design" at this point, but I'll probably change things up given the material at hand. I'll make a model of the final piece as things come. 

Now. I haven't yet talked about the PSU until this point. At the end of the line, I'd like to make this thing solar powered, as most of the electronics can be driven off of 12V or less. I'd love to make the array both modular, as I have several different sizes, and, ideally, solar trackable. This would be a fairly simple rooftop mounting with a camouflaged cable to calm down Pops. Hell, I bet I could install it without him noticing, initially. The only thing I'd like to do is get a shield of sorts, like Plexiglass, something to take a bit of impact before the cell does. I'll think of something acceptable, I'm sure. Anyways, that's going to take some more thinking than I have patience for. 

Overview

Alright, where shall we start? 

I started this project back in oh... summer sometime, in 2016... I've documented a lot of my work [here] so I won't go into too much detail, but the gist of it, is that I saw Cody Reeder extract deuterium, that he enriched, from old battery acid. I had a couple of batteries lying about, so I thought I'd give it a shot. after a little compulsiveness, I ended up with over 15 gallons of it... yeah... So I started to replicate the experiment, which by this time had become a STEM project at Morton College. I got familiar with more glassware than I could name offhand, and got pretty good at titrations, I think... Regardless, I collected everything and tried to purify the resulting water as best as I could, and ended up with a small, I think 30ml sample IIRC of water that - I still have to test - contains a higher content of deuterium. I'm planning on continuing this process in the near future, with proper testing when I get the chance. 

So that brings us up to today, I've let things slow down some, which may or may not be a good thing, I'm not sure yet. One of the odd things about the process I use { (H2SO4)aq + (Na2CO3)s -> (Na2SO4)aq + (H2O)l + (CO2)g } is the Sodium Sulfate. If you properly neutralize the acid, and let it alone, it crystallizes. The crystals are thin, needle, water-clear, geometric spears when they first form, only taking on a color if there is a contaminant in the solution, and if let dry, turn into a white powder that sticks fairly well to many surfaces. The crystals are quite brittle, and can contain a lot of water. they tend to settle on the bottom of the container, but are easily scraped out with any hard edged strainer.  that being said, if you let things go too long, and break the crystals by moving the container, then they have a distinct possibility of creating a crystal manhole cover. I have one that is approaching 2.5" (6cm) in thickness and produces a notable amount of concern for me. dealing with such a large sample may prove to be quite difficult. I have not checked the other bucket of product. 

I should refrigerate them... Refrigeration should create more crystals and therefore should help in keeping large crystals out of the new boiler I purchased from Clawhammer Supply. I have the 1 gallon unit, and that should be a great size for primary reduction. After that, I have a lovely 500mL Round Bottomed Distilling apparatus for the rest of the process. Being as we went through nearly a liter of material during the STEM trials, and ended up with less than a tenth of that, I feel comfortable losing the first two thirds of material I have, after salt reduction. I'll be saving it, for further testing, but my primary focus will be with the last third of material. 

So where do we go from here? I still need to actually receive and construct the boiler, and I still need to acquire a 500ml heating mantle. Once I have both of those, I have enough equipment to start, but I'd like to make a dedicated Distillation Stand where everything lines up well. I do feel the need to take samples of the accumulated liquid and run tests on them, so I think I'll hit up Walmart for some jars. 

So here's the shopping list, no particular order, in it's entirety: 

  • High Vacuum Grease.
  • Aluminum Bat: 3/8" x 1" x (12)" (Dist glassware stand)
  • Heating Mantle
  • Sample Jars
  • Stand Clamp things...
  • Threaded stand rods
  • Setscrews
  • spare joint clamps
  • Cooling bath
  • Burette
  • Indicator (need to check my notes.) 
  • PH Sensor would be lovely... there may be inexpensive hope for this yet!
  • a place to set up the automated neutralization. 

I still have "live" acid I need to deal with, and I have a metric shit-ton of NA2CO3 to use, and I still need to figure out what I'm doing with the resulting dehydrated salt... but yeah! I don;t wanna manually add the Sodium Carbonate by hand, so i'm working on an automated set up. Sounds like summer's gonna be fulla science! I'm going to work on the final neutralization set up here and get back when something happens.