Work Log

Semi-unfiltered life updates in the moment barely useful to me. Do not take seriously or literally. Project specific updates are located on their respective posts.

22 Dec 2019

I wonder if graphite can be used as a DIY bubbler?

15 Dec 2019

When I added the metabisulfite solution to the THF/Acetone mixture, two layers were formed. I wasn’t really sure which was which, so I distilled the whole thing.

The mix yielded a fraction that boiled at approximately 66C (THF). The other fraction that remained in the flask didn’t produce vapor until about 100C, indicating the acetone-bisulfite product was left in the flask.

The distilled flask had a density of 0.888. THF has a recorded density of 0.8876. Woot!

It is clear now that the THF could be added to a sep funnel and the lower layer removed (acetone-bisulfite-water mix). A distillation of the top layer would yield substantially pure THF.

The THF mix will be set over calcium chloride to dry for a couple hours. Then distilled a final time.

13 Dec 2019

Extracted THF from Oatey X-15 shower liner glue. First the plastic monomer was precipitated with water. A full 16oz can was transferred to a larger container and about twice its volume of water was added. The resulting mix was allowed to settle. The THF, acetone, and water mix was decanted and then distilled using a water bath. Everything below 70C was collected.

The acetone concentration is between six and 25 per cent according to the sds. They are practically inseparable by distillation because of their 10C boiling point difference. The acetone was therefore precipitated as the bisulfite adduct using excess sodium bisulfite (50g in 100ml H2O).

12 Dec 2019

Yield of copper barium chromite is 14.5g.

10 Dec 2019

Started learning FreeCAD. Modeling has been a debilitating gap in my knowledge for a while. I chose FreeCAD because it is open source and based in python.

I ran a few HPLC separations of highlighter and market fluids. The injection is definitely working, but separation isn’t very good. I’m just using a 50:50 MeOH and H2O mobile phase at the moment.

I haven’t gotten the HPLC to interface with my laptop yet. Still working on a method there. With the Smartline 2500, I think an analog integrator is my only choice. The 2600, however, has the ability to transfer an entire chromatogram via serial. So, I might be switching out the 2500. I need to purchase some new ferrules.

Dioxane Synthesis

  • 600ml antifreeze
  • 70ml sulfuric acid
  • distill at 1 drop per second
  • combine distillate with 20ml sulfuric acid
  • fractionally distill: collect 84-94C
  • combine distillate with 80g KOH
  • stir overnight
  • collect top liquid layer
  • if still miscible, add an additional 40g KOH
  • stir over sodium metal overnight
  • distill
  • store over sodium to prevent peroxide formation

09 Dec 2019

Propylene carbonate is an interesting solvent (Jorne and Tobias 1975). Alkali metals can be electrodeposited from their salts using aluminum trichloride. In some cases, the aluminum isn’t needed (Li). Synthesis from propylene glycol and urea using a zinc acetate on activated carbon catalysts proceeds with good yields (Zhao, Zhang, and Wang 2004). It might be worth experimenting with.

PC is not compatible with graphite electrodes.

02 Dec 2019

I have been working on variations of the chloroform synthesis for a couple days now. A practical chemistry book from 1900 has some really great synths in it (Cohen 1900). One of them is a chloroform synth using “bleaching powder”. The book goes into more detail than the prepchem.org synth.

Commercial bleaching powder is approximately 40% available chlorine, whereas my pool chem is 56%. So I scaled the reactants accordingly and added a bit extra acetone because it is cheap.

I ran the reaction in a 1L RBF and used an addition funnel to add the acetone in slowly. I think adding 10% of the required acetone at the start and then dropping in the rest over an hour or so is the ideal. You get the initial kickstart to warm the mixture and then a slow distillation of chloroform as more acetone reacts. I am unsure whether this results in acetone loss due to distillation before it reacts.

This setup has been run several times with mild variations. Better stirring would be helpful. Even a 2" stirbar has trouble with all the precipitated calcium hydroxide.

I have around 250ml at this point. I would have like to have double this, but R&D takes so long…

29 Nov 2019

Finally calcined the copper chromite.

I think I want to try thermal epoxy for the lab chiller.

1-10 micron alumina seems like and appropriate choice (Lin, Bhatia, and Ford 1993).

6um (2400 mesh) alumina powder is $15 per pound.

So I have these culture tanks that I rescued from the dumpster. Sized 3-8 gallon. I’ve been pondering some projects using them lately and I think spirulina is a fun place to start.

Although… the clear, plate styles circulating systems look really cool and are probably more light efficient. Plus I have a bunch of polycarbonate sitting around. Here’s some good info

I think I like the flat-plate bioreactor. I could even build a system to encompass a “grow closet” to use the light that would otherwise be lost. Essentially constructing the walls of an artificially illuminated plant space with photobioreactors.

An attached bioreactor is a really cool idea (T. Liu et al. 2013). I have a lot of filter paper, but for mass adoption a substitute should be found. Maybe newspaper…

Built a second LED grow light for my parents. The first prototype currently resides at a friend’s aquaponics farm. It takes approximately 5 hours to assemble one unit at a materials cost of ~$130.

18 Nov 2019

Made some copper barium chromite. Calcination will come later when my fume hood isn’t full of flammable solvents.

17 Nov 2019

I ran out of ammonia solution yesterday. I figured I would try the urea hydrolysis method this time.

Mixed some hydroponic nutrient stock solutions. Part A consists of 159g Masterblend and 79g magnesium sulfate. Part B consists of 159g calcium nitrate. Each is filled to a volume of 1L and is 250x concentrated. For each liter of reservoir volume, 4ml of each stock solution is added. Each ml of stock solutions provides 159mg each of masterblend and calcium nitrate with 80mg of magnesium sulfate.

The nutrient addition is highly endothermic. More than 10 minutes of mixing is necessary for full dissolution.

The calcium nitrate was pretty dirty. Probably leftover limestone from manufacturing. I filtered the solution through cotton.

I noticed that Masterblend is not a homogeneous, pelletized product. Rather it is a loose mixture of various salts and chelates. I bet that small dosing is highly irregular due to this inhomogenous distribution. Just another reason to use stock solutions.

12 Nov 2019

Continued distillation of chloroform mixture. I had trouble with foaming last night. I could prevent this from happening by adding a few mls of mineral oil as an anti-foaming agent and turning the stirrer up to a 9. Portions are now 600ml each.

Once the distillation head has reached 65-70C, heating is stopped. The remaining slurry composed of various calcium chlorides, hydroxides, hypochlorite, and minimal VOCs can be dumped down the drain.

Total collected wet chloroform is 44.7g (67ml) or a yield of 83%. Definitely better to use excess acetone! 67 The lab chiller is working fairly well. I think a rework with a larger radiator, larger cold-side reservoir, and better thermal grease is in the future. Maybe even better current control to maximize cooling capacity.

Distilled some ethyl acetate (“MEK substitute”) to purify it. EtOAc is really nice to distill. Even at almost a continuous distillate stream, the vapor front barely reaches 1/3 of the way through the column.

11 Nov 2019

Large scale synthesis of chloroform:

  • 1L of water and 370g hth super hypochlorite pool chlorinator was added to a 3 gallon bucket
  • overhead mechanical stirring (a power drill) with a stainless stir rod (some pipe and bolts+washers) was started
  • after 5 minutes of stirring, 25ml acetone was added
  • after an additional 5 minutes of stirring another 25 ml of acetone was added
  • after 5 more minutes the water began to heat slightly and I began adding ice to cool the reaction
  • 25 ml of acetone was added
  • ice was added to keep the reaction temperature below 10C

After the reaction reached 5C, the whole mixture became very thick. I assumed this was calcium hydroxide precipitating out. I decided to test this by adding a bit of hydrochloric acid. To my surprise, green chlorine was released indicating unreacted hypochlorite in the mix. So I decided to add an additional 25 ml of acetone. The mix began to heat up again-another indication that an excess of acetone is necessary.

To be entirely sure I added another 25 ml of acetone bringing the total to 125ml added.

After stirring for 10 minutes with no apparent rise in temperature, stirring was stopped. The mix was allowed to warm to room temperature. It was distilled in 800ml portions.

10 Nov 2019

First real test of the TEC chiller by synthesizing chloroform-A reaction which must be kept cool.

Commercial bleaching powder contains approximately 40% available chlorine. My “hth super shock treatment” states “Minimum Available Chlorine … 54%” and has a calcium hypochlorite content of 56.44%.

I like the idea of also making propionic acid at the same time as chloroform, so I will be using MEK instead of isopropanol, acetone, or ethanol.

There isn’t a lot of info on the amateur synthesis of chloroform from solid hypochlorite. This video shows a 50L flask being used to synthesis liters of chlorine at a time from solid hypochlorite. Even with mechanical stirring and a jacketed cooler the reaction still got out of control.

There seems to be a large discrepancy between various syntheses in molar escess terms. Some have hypochlorite excess and other use excess methyl ketone. I will run this reaction on a half molar scale based on calcium hypochlorite.

  • 127g calcium hypochlorite as hth super chlorinator (56% hypochlorite) is added to a 1 L flask
  • 600ml H2O is added
  • 24 g (20ml) of butanone is added over the course of 15 minutes in 5ml portions

After the whole of butanone was added I waited for something to happen. After half an hour, nothing appeared to change. I removed the flask from the ice bath. The solution felt warm after another half hour. I put the flask back in the ice bath. After an hour or so I decided to try and filter it. A fritted filter produced a clear filtrate, but no immiscible layer. I could smell the chloroform in the white filtrete. So I put everything back in the flask and distilled the chloroform instead.

The resultant chloroform was rinsed with dilute sodium hydroxide. Total yield is 11ml of wet chloroform or about 42%. Further trials are needed to determine if any increase in yields is possible with varying reactants.

I think I prefer the cold household bleach method. At least, I think the ease of separation makes up for the cost and waste. I will dilute the rest of pool chlorinator and phase separate the chloroform.

Pssshhht. I just checked the price of calcium propionate on ebay. It’s only $17 for a pound. Totally not worth the time to isolate it myself. Distillation from Ca propionate and sulfuric acid is much easier. I will be using acetone for chloroform synthesis in the future.

09 Nov 2019

Ha! So I was about to disassemble the chloroform cell and I noticed some liquid in the exhaust tube. I rinsed the tube out with some distilled water and lo! an immiscible liquid was recovered. Only a couple drops were recovered, but still. The chloroform cell is not a complete failure.

As suspected, the chloroform was simply being carried away by the exhaust gas. Without a really great cold trap, this seems to be an insurmountable problem.

05 Nov 2019

The chloroform cell has been running for 15 hours and 45 min. The current is down to 850 mA. The total current input was about 15 amp hours. 0.34 KWh has been consumed according to the Kill-a-Watt. Water bath was maintained at wet-bulb temperature (a fan blowing over the water’s surface) averaging about 20C for the duration.

Unfortunately, no separate layer was present. :(

04 Nov 2019

Trying the electrolytic chloroform again. This time with a cooled, sealed cell using isopropyl alcohol.

To a quart canning jar was added 600ml H2O, 120g NaCl, and 35ml 70% propan-2-ol (25ml propan-2-ol). The cell is sealed and the output is directed to a bubbler (gas washing bottle) to view the flow and trap any evaporating solvents. With the better connected and stabilized electrodes, 3.3V was able to pass 1.1A to start.

Three hours into electrolysis and the stainless cathode is rusting away. Not excessively but it will not survive mass production. The reduction potential of acetone must be lower than stainless since the original cell did not have this problem. I will replace the cathode with some titanium after this run is over.

There are also leaks through the electrical connections due to the small pressure head in the system. Nylon washers should be used instead of stainless next time.

25 Oct 2019

After 26 hours and 29 minutes using a total of 0.53 KWh, no liquid has separated. I could definitely smell chloroform, but still…

At the end, the amperage had dropped to around 500mA. I suspect this was due to the slow increase in pH from the hydroxide being produced (3 moles per mol of generated chloroform).

Oddly enough, the PF of the system hovered around 0.6, i.e., really terrible. Probably because such a small amount of power was being used for such a large power supply.

Using an average of 600mA, the total power delivered to the cell was around 14 amp-hours. This should have produced something… Alas, my cell was likely loosing too much chloroform to evaporation. I shall try again using a closed flask instead of a semi-sealed beaker.

24 Oct 2019

After about 14 hours, no immiscible liquid has separated. I will continue running it until something happens.

23 Oct 2019

I came across a reference for making chloroform from acetone using electrolysis. (Teeple 1904) I can’t resist attempting it.

The original paper calls for platinum electrodes. Since this is essentially a chlorate cell with acetone, I will be using MMO instead. The paper suggests 6 amps per square decimeter (60ma per square cm). With a total of 8-10 amp*hours needed to generate a small layer of chloroform which can be separated by pipette.

Therefore, for a decent run time (24 hrs) I will need to use 300-400ma requiring 5-6 square centimeters of anode. The mesh anode material I have uses 2mm titanium wire. For each wire of the mesh this means 0.6 square cm for every 1cm of length. For a submersion depth of 5cm, this requires a little less than two wires’ worth of anode. Excellent

I think I will cut a six wire anode to be safe. Platinum can take a lot higher current densities than MMO. Also, cutting titanium sucks. So I’m going to make the anode kind of large so I can expand production later.

Since this is just a test run, I will make the electrical connection using stainless steel bolt situated in one of the mesh holes. Spot welding a titanium bolt would be better. We’ll get to that later.

Initial Test

To a 400ml beaker, 200cc of water, 40g of sodium chloride, 8cc of acetone, and a stirbar are added. A MMO over titanium anode and a stainless steel cathode are added with an approximate separation of 5mm. Voltage is applied and the anodes adjusted until a current of about 700mA flows (3.3V). Current is measured across a 0.22 Ohm resistor in series and power consumption is measured with Kill-a-Watt meter. The whole apparatus is covered in plastic wrap to minimize solvent loss.

The whole setup is run for approximately 12 hours to reach 8 amp-hours.

21 Oct 2019

A few months ago I acquired a bunch of HPLC equipment from the local university dumpster. Over the last few days I have been setting up a full system with the help of a friend. Everything seems to be working. The column I also found in the dumpster seems to be for a higher pressure system. As long as I keep the flow rate under 0.8ml, however, the max pressure is not exceeded.

The next major hurdle seems to be obtaining control software. There’s an open source chromatogram analyzer called OpenChrom, but no such software for control.

30 Sep 2019

Distilled some diethyl ether and heptane yesterday from car starter fluid. It took all day to distill 3 bottled. It would have been faster if I had larger glassware instead of having to process them piecemeal. I should look online for that brand with “50% ether” for a better yield. Still… its less than $20 per liter EtO.

Now on to hydrochloric acid. I’m about out of the stuff I made several years ago from salt and sulfuric acid. This time I will be distilling muriatic acid. I combined 600ml of hardware store acid with 400ml of di water and distilled.

17 Sep 2019

Some sort of brown precipitate has formed overnight in the disodium terephthalate solution. I will filter again to remove. My fritted glass filter is getting a little dirty… time for another piranha solution bath.

I bet the solution could be further decolorised using activated charcoal for increased purity if necessary.

The leftover bits of mostly unconverted PET are drying now so I can get an idea of the conversion.

9.9ml solution taken from 1L total. Approximately 2ml of 31% hydrochloric acid is added to precipitate terephthalic acid as a white solid. Filtered [Filter Tare = 12.39g] and rinsed with di water. The whole filter was dried on a hotplate resulting in 0.55g of white, powder terephthalic acid.

That means the entire solution contains ~55g of recoverable terephthalic acid. 24.34g of unconverted, sand-like material was left over. So of the 81.1g (0.42mol) of reacted PET, only 0.33mol was produced giving a molar yield of 60% and a conversion of 79%.

  • M.W. PET subunit = 192.2g/mol
  • M.W. terephthalic acid = 166.1g/mol

16 Sep 2019

PET to benzene synth continued yesterday for an additional 10 hours bringing the total to 14 hours. I brought the temp up to 180C for the final 4 hours of so and it definitely increased the conversion rate. After cooling last night I added about 200ml di water to precipitate all the terephthalic acid. There was definitely some fluffy white precipitate. :D

The mix was heated slightly to facilitate filtering. Filtrate was rinsed with di water. Several times. Filtrete could be dehydrated and reused, but it would contain significantly more ethylene glycol from the decomposition.

Sodium hydroxide solution (about 80g NaOH; 2mol) was added to dissolve only the acid (producing disodium terephthalate) and leave behind the unconverted PET. A lot of water was needed to dissolve the whole thing. At first, the entire 150ml volume of my filter was full, but with repeated washings (10+) that volume was reduced to less than 25ml. Phew! When the volume was 150ml I had thought the experiment had failed. With every washing my hopes of a successful reaction get a little higher.

The whole process smells bad. Not pyridine bad, but still bad. A typical choline/fish smell with a hint of burning. Undoubtedly the decomposition of choline chloride.

If terephthalic acid is the final result intended, 200ml of 31% HCl is added to neutralize and precipitate the terephthalic acid. As I am going for benzene, I am just going to take a sample and precipitate to get an idea of yield.

14 Sep 2019

Started a test on the conversion of PET to benzene using DESs.

  • 105.42g PET, powdered (~0.55mol)
  • tare weight 1L flask: 274.69
  • added 179g ethaline made previously
  • added additional 124g ethylene glycol + 139g choline chloride (2:1 mol)

The distillation of denatured alcohol continues. Distillation of ~1600ml in 2L flask takes an hour or two. The distillate above 78.1C is collected as nearly pure ethanol amounting to about 200ml for each run. After this run I believe I will stop working on this project. Denatured alcohol may be cheaper, but it isn’t worth it for the time involved.

I really need a second hotplate stirrer.

I placed an “order” from the US National Germplasm System for a few plants including coffee and tobacco. I’m specifically interested in secondary metabolite production in hydroponics. I’ve seen some posts about plants not tasting the same, so I wonder if that applies to alkaloids and similar.

20 Aug 2019

The vigreux column was a pain and didn’t pack very well. I decided to try the new stainless steel packing I made from washers. I didn’t have enough to fill the whole column, so I topped it off with the plastic rings.

16 Aug 2019

Further research leads me to conclude that methanol-ethanol separation requires more than a single run through my 300mm vigreux column. Fifteen to twenty theoretical plates are needed for their 15C boiling point difference. So I decided to try some polypropylene raschig rings made from cutting tubing.

12 Aug 2019

I obtained some denatured alcohol fuel from Menards a few months ago for $4 per gallon. From the sds (product code 834G1) I found that it contains 49.13% EtOH, 50% MeOH, and 0.87% methyl isobutyl ketone. I don’t currently have a use for the ketone, so I need a way to remove it.

I stupidly thought it could be precipitated with a small amount of water, but its solubility is 1.91g/100ml.

MEK can be adsorbed onto zeolites… Adsorption of MEK vapor onto zeolites.

MIBK can be adsorbed onto activated carbon with a capacity of about 33%. Since the v/v concentration is 0.87%, the total MIBK content of a gallon is approximately 33ml or 26g. Being conservative, 100g of activated carbon is required.

I poured approximately 70g of activated carbon directly into the denatured alcohol can and let it sit for 1hr. I decanted the solution and added the rest (30g) to sit for a further hour.

While this was soaking, I made a ground glass adapter to fit directly onto the can. The female joint was cut from an adapter that recently broke. The new diamond cutting wheels are amazing. Nothing goes to waste around here…

I had actually intended the female joint to be screwed into place between the lid and container, but the lip was too thick. Oh well, a little bit of teflon tape works just as well.

11 Aug 2019

Made some sodium silicate solution for refractory use today from crystal cat litter.

I also made some silicate for producing TLC plates:

  • 79.64g silica (all the ground, pure stuff I had)
  • 200ml H2O
  • 53.00g NaOH

08 Aug 2019

I’ve had Google analytics on this site for a while, but I forgot to enable it by setting JEKYLL_ENV=production. Doh!

Sodium production did not fair well. My hotplate stirrer doesn’t have a good magnet on it or something because it can’t handle all that magnesium without slipping. Essentially nothing was being mixed. I resorted to shaking the flask every few hours, but this was far from efficient. Also, the PP exhaust tubing clogged. I woke up this morning to the smell of burning mineral oil to discover the stopped had been blown off by the pressure. I let everything cool down and tried again. This time I used a flask with a proper ground glass joint and a larger stir bar. I also added another 20g NaOH to compensate for the crud left in the original flask. Hopefully nothing goes wrong this time…

My back is still painful. I think the pain can be downgraded from stabbing to dull, however. So that is progress. If only I would stop helping friends move in and out of apartments it might actually heal.

04 Aug 2019

Replicating NurdRage’s sodium production video. I don’t have any particular use for sodium at the moment, but it is an excellent synthesis.

01 Aug 2019

I’ve been having back issues for a couple months now. It has gotten serious as of the last few weeks. I suspect sciatica stemming from a herniated disc.

A few days ago I began to notice bruises on my thighs. After a bit of googling I determined that they are likely a side effect of low vitamin C. I haven’t been eating much citrus lately or even red meat for that matter. Combine that with intermittent fasting for the last week and a half and the large inflammation and you got yourself a scurvy. Low vitamin C certainly isn’t helping my back heal… So I will be supplementing C for a few weeks.

29 Jul 2019

I bet a decent shape memory allow can be made using US nickels…

26 Jul 2019

Nothing like a perfect SpaceX launch to brighten your day.

20 Jul 2019

Recovering the gallium from a chunk of aluminum I made over a decade ago using the NurdRage ether extraction technique.

Lots of work on the website.

19 Jul 2019

One of my dumpster diving adventures yielded 900mg of platinum wire: 800 of which is currently dissolving in aqua regia to be made into 10% Pt on Carbon catalyst.

05 Jul 2019

Started drying the copper chloride solution. For weeks now it has been sitting in my fume hood. I bubbled ozone through muriatic acid and copper to create copper (II) chloride. I’m hoping to use this to make anhydrous aluminum chloride by single displacement.

04 Jul 2019

Lots and lots of cleaning/organization.

03 Jul 2019

It’s really difficult to fit all my projects into a 12’x12’ room and a tiny storage shed…

02 Jul 2019

The last few weeks have been exhausting: Wedding, MVOR, Guatemala trip, MINK. Now back to science…

I have been reading about the history of psychedelics research because of their resurgence in treating mental disorders. I think there is ample opportunity here for someone to translate the science into effective treatment on Youtube or other social media platform. I bet a channel devoted to illustrating (but not actually performing) the chemical reactions needed for synthesis of these drugs would be very popular. Unfortunately, Youtube would likely demonetize any such channel.

Working on vapor phase nitration of paraffins. Seems like a refluxing system I had in mind will return the nitropropanes as well as nitric acid. I think I will have to do a single pass system, which would be wasteful. Perhaps nitrogen dioxide would be better?

Glidarc atmospheric nitrogen fixation: Finally got my big flyback from home. Tomorrow I will give it a test with the ZVS driver I bought on eBay. The idea is to build something similar to (Patil et al. 2016). I’m debating whether to just go with the simple Jacob’s ladder design that has been done by a few amateurs. I also want to try adding a DBD ozone generator immediately following the Glidarc chamber. I believe the ozone will help oxidize the nitric oxide.

One important point of the Patil et al. paper is that frequency is important for Glidarc efficiency. Every amateur build of a plasma nitrogen fixation apparatus has used low frequency (60 hertz) transformers. The paper found the highest energy efficiency at 8 kHz; the middle of their test range. I am not sure what the typical frequency of a flyback is, but it is probably better than 60.

5+5 is the typical winding configuration for the primary on flyback transformers.

15 Jun 2019

Finally ready to test the DES Ethaline (2:1 ethylene glycol:choline chloride) for some organic transformations. First test: decarboxylation of Vitamin B3 (Niacin) to pyridine. I decided on using basic copper carbonate because of availability. I’m hoping that the reaction will proceed faster and give better yields than traditional destructive distillation (32%) or the best amateur catalytic prep using copper chromite (86%) (Doug’sLab 2015).

To a 250ml flask:

  • 25g niacin
  • 6g basic copper carbonate
  • ~150ml ethaline

Heat flask to 50C to start decomposition. Obvious evolution of carbon dioxide happening. Stir bar broke free after about 10 minutes of heating. Continued ramping up the heat. At heating mantle set at 210C, significant distillation occurred at still temp starting at 56C. The mixture is at approximately 135C.

I should have analyzed the expected return of pyridine before I started. Quantitative yield would be ~16g pyridine. I was so disappointed when I only recovered about 15ml even though this is close to quantitative. I hope to do a scaled up version in the future. A copper chromite catalyst might speed the reaction.

14 Jun 2019

Performed a test run of the NMP distillation from the old CitriStrip.

  • Dilute CitriStrip with same volume of distilled water
  • stir for several minutes to ensure all NMP is dissolved in the water
  • filter through glass or polyester fiber (slow process)
  • let settle overnight
  • filter again through filter paper or cotton
  • distill under vacuum (water aspirator distills NMP at ~150C)

12 Jun 2019

I call the Liqiud Creosote test a bust: It is too dilute to be useful.

11 Jun 2019

Currently running a distillation of the Meeco’s Red Devil Liquid Creosote destroyer attempting to recover “acetic acid glacial”. It is not looking good. Of a total 600ml, 50-100ml distilled below 100C. I am still collecting at 100C.

10 Jun 2019

Worked on the strawberry wine project.

06 Jun 2019

Finished construction of a TA4 snr based temperature controller. I needed something that was more accurate than my other Rex C-100 based one. I also bought a Pt100 RTD probe for more accurate readings. The autotune function on the TA4 is really nice.

28 May 2019

Applied single-part epoxy to the inside of the fume hood.

Put a magic eraser wrapped in foil in the oven at 500F too see if that was sufficient temperature to carburize it… it is not.

27 May 2019

Finally started rebuilding the fume hood. It is hard to rebuild when you barely have room to walk let alone rotate several 2’x4’ MDF boards around.

Next time I am buying all my building materials from Home Depot. The Menards boards were up to 1/4" off dimension and several degrees out of square. They gave me a lot of trouble: Not worth a few dollars in savings.

I did, however, manage to stumble upon a potential source of glacial acetic acid. “Meeco Liquid Creosote Remover” has “acetic acid, glacial” listed as its only ingredient. I can’t find a SDS anywhere. I will run some tests to make sure when my fume hood is functional again. It was only $10 for a quart.

I’m not excited about the loudness of my exhaust fan. I am currently using a permanent magnet leaf blower driven with a standard dimmer. This is convenient because I can adjust the speed to match the danger of the experiment. It can really move some air. Unfortunately, the designers of leaf blowers aren’t too concerned about loudness.

25 May 2019

How about we mix plaster of paris with vermiculite to form a castable, insulating refractory? It seems that calcium sulfate (anhydrite) decomposes above 1200C (Newman 1941). This is perfect for use with vermiculite which decomposes at around 1100C.

Mixed a test batch of verm:plaster insulating refractory. 500ml verm + 250ml water (mixed) + 500 ml plaster. I added to my greased 4x8 inch mold and let it set for 1 hr before dislodging and drying in the oven at 350 for 1hr. It only formed a 1" thick brick but it seems pretty stable. The plaster I used is a mix of calcium sulfate, carbonate, and silica. If these bricks hold up, I will try it with a more pure product.

Apparently the reason for the DIY refractory community abstaining from vermiculite is that it “absorbs water and when heated will crack the refractory”. I’m not sure where this idea came from. Perhaps backyard metalcasting? The author states that vermiculite is added to potting soil to retain moisture and this makes it unsuitable for refractories. This doesn’t mean it is hygroscopic. Perlite has about half to two-thirds the water holding capacity of vermiculite but it isn’t zero keensteading. As with any water based refractory, a burnout period is required before use. I suppose we will just have to see how it holds up.

24 May 2019

I woke up this morning at 6am, unable to return back to sleep because of back pain. I need to fix this bed thing.

I have been neglecting my sleep for a long time now mostly because of cost. Why would I spend $500 on a mattress when I can buy and air mattress for $10? My back… that’s why.

I looked into ordering a mattress from Leesa primarily because I want to support one of the many creators I listen to/watch. The Skeptics Guide has a 25% off advert deal with Leesa so I tried there first. For a full sized mattress it was approximately $650. Not too bad, but more than I would like. I’ll find something cheaper and just donate them the money.

All of the mattress companies have diagrams depicting their various layers and features displayed proudly on their sites. They all seem to just be various densities of foam stacked upon one another. A cooling layer here. A support layer there. Meh… why don’t I just build my own.

Amazon has cheap mattress toppers available from 1-4 inches of many densities and materials. I’m a side sleeper and I get really hot at night. Especially when my significant other sleeps over. So I ended up buying a 3" latex foam and a 2" memory foam set. I’m not sure in which order I will put them, though.

One project I have had in the back of my mind for years now is a water cooled bed.

22 May 2019

Perhaps it is better to work at a small scale: shake flask culture.

  • https://www.thingiverse.com/thing:2983846

How about we use one-half of a disposable syringe filter for the bubbler? They already have appropriate sizes and are autoclavable… Nope: the filter material is thin and impossible to extract without damage.

Just bought ~$60 worth of wood to rebuild the fume hood. Half inch and three-quarter inch MDF for the walls and some eighth inch hardiboard for baffles. I plan on painting everything with some white single part epoxy I have and then sealing edges with silicone. LED lights would be nice.

21 May 2019

Looking into lab-scale bioreactor builds.

  • aeration: only SS brewing and alumina aerators are autoclavable
  • https://create.arduino.cc/projecthub/open-bioeconomy-lab/microbial-bioreactor-d7f61b
  • https://sites.google.com/site/opensourcebioreactor/

I really need to organize my projects better. I have 20ish going on right now and most of them are primarily in my head.

19 May 2019

Finished (mostly) the lofted bed frame. Attached a clothes hanger bar to the underside. Works quite well.

18 May 2019

I am practically useless if I take bacopa extract in the morning without breakfast. I assume that the same would happen with any supplement that is supposed to be taken with food.

I am currently constructing a bed loft. It shouldn’t be that difficult but I keep making simple mistakes. Drilling holes in the wrong place. Making cuts on the wrong side of the line. Just stupid stuff.

“Magic Erasers” are made from melamine foam. Carburization after inpregnation with graphene oxide would be fun to do. (Tjandra et al. 2018)

I have been researching plasma nitrogen fixation as a source of nitric acid for the amateur for a while now (nitric acid collection on Zotero). A new method got my attention: photocatalytic nitrogen fixation using carbon nitride/metal oxide composites (Mou et al. 2019). The process uses a DES composed of urea, melamine, and metal chlorides. The urea-melamine DES is capable of dissolving the metals quite effectively. Carburization produces a homogeneous carbon nitride/metal oxide catalyst that shows remarkable efficiency in photocatalytic ammonia production.

29 Apr 2019

Perchlorate electrolysis research. Lead dioxide or glassy carbon anodes?

  • seems like glassy carbon can be made from just about any carbon polymer (Pocard and Callstrom 1992)
  • perhaps a thin coating of some resin (e.g. urethane) onto gouging rods and vacuum pyrolysis to form a glassy carbon coated graphite rod?

06 Apr 2019

Researching truffle production. A summary of the info I have gathered so far:

Black truffles (Tuber melanosporum) can sell for $800-$3000 per pound. A single acre of oak or hazlenut trees can produce 25-150 lbs per year. That’s $20,000-$450,000 per acre per year. Maturation of a plantation takes 5-10 years. One particular site claims closer to 3 years to first harvest. A single stand can produce for 50+ years if properly managed. Infection by competing fungi seems to be a major killer of plantations. As many as half of startup plantations fail due to owner negligence or giving up. Infected seedlings can be purchased for $25-$75 each. Around 200 trees are required per acre. This is $5000-$15,000 per acre startup. Plus the cost of fertilization and application of agricultural lime (truffles life basic soil). I would prefer a method that doesn’t require so much startup capital.

Irrigation might be necessary. As will protection from freezing. Extended freezing temperatures could kill the truffles. Irrigation can be done only over the burn spots produced by developing fungi to reduce water usage.

Significant infection by competing fungi can occur by placing a truffle plantation in close proximity to established tree stands.

Perhaps I can do the inoculations myself. A company in the UK sells 100g sachets of truffle spore compost, which supposedly can be dumped around the roots of a tree to infect it. I wonder if I can buy a fresh truffle and extract the spores myself. Agar cultivation appears out of the question. Truffle mycelia require tree roots to propagate.

So I have a couple options. I can buy just a few infected trees and hope they can infect other trees by proximity alone. I can take a chance on the spore sachets. Spores can be obtained by crushing truffles directly.

31 Mar 2019

Mixed up a batch of choline chloride: zinc chloride DES. 1:1 molar ratio roughly (48g ChCl + 45g ZnCl2). ChCl is deliquescent and my container was apparently quite porous, so it was pretty wet. This made approximately 75ml. (Bagh 2014) uses ratios 1:1 to 1:3 so I’m not too worried about exact numbers.

11 Mar 2019

I will be away from home for about two weeks and unable to work on any projects. Gotta make that money…

03 Mar 2019

Racked the strawberry wine today. Gave it a taste test as well. Pretty good… Still carbonated a bit, but tasty nonetheless.

Finally settled on LEDs for a grow light.

28 Feb 2019

Day 3 of acetic acid distillation. Recovered an additional 110ml water. All of this work for 15g of glacial acetic acid??

27 Feb 2019

Day 2 of acetic acid distillation. Recovered about 120ml of water from the system. It took almost 10 hours of distillation to get that much. I started with 300ml of 5% acetic acid.

I watched a video just now on Why FYRE Was Never Real - Wisecrack Vlog. I had no idea that there are people whose main purpose in life is to take Instagram photos and share them. I can understand those who garner followers to attract advertisers and the income that they bring. But fame for fame’s sake? What does that even do for you? I suppose I am too much of a pragmatist.

Made a hydroponic herb garden today from parts around my house. It uses a small fountain pump to move water from the reservoir at the bottom of the bucket to the three restricted drip emitters. The media is 25:75 vermiculite:coco coir.

Hydroponic herb garden
Hydroponic herb garden

I had some trouble with the first drip emitters. I used a circular length of polypropylene tubing with holes poked in it. Of course the holes got plugged. Even after rinsing the media several times and wrapping the pump in several layers of polyfill stuffing. So I switched to drip emitters.

Looking into plastic as a viable column packing material for low temperature distillation. Polypropylene seems an acceptable choice for ethanol:water mixtures (Adogbo and Ayodele 2013). Nylon is also resistant to ethanol and has an appropriately high boiling point. Both plastics can be bought as small tubing and cut into “raschig” rings. Nylon absorbs water though. Plastics probably wouldn’t transfer heat a well as most other materials. Considering you can buy a pound of ceramic raschig rings on eBay for $14, or just use stainless scrub pads this doesn’t seem worth it.

26 Feb 2019

Today I would like to look into a minimal cost, nutritionally complete diet.

Food replacements (e.g. Soylent, Huel) are a possibility, or rather their DIY counterparts.

Constructed a makeshift dean-stark trap using basic glassware and round bottom flask with a distillation arm. My fume hood isn’t tall enough to incorporate the whole setup, so it is sitting in front. Since this is only ethyl acetate, water, and acetic acid, I don’t need much in the way of fume0 extraction. Also, the temperature controller box is working perfectly.

Diethyl ether might make a better drying agent, but I don’t want to deal with the hazards associated with it.

The whole process takes a long time to complete. I anticipate several days for a full gallon jug to yield approximately 180g of glacial acetic acid. Just a guess… about $0.75 for the electricity and ~$5 for the gallon of vinegar = $120 per gallon. That doesn’t include the time invested or any inevitable losses of ethyl acetate or vinegar. Glacial acetic acid routinely sells for ~$50 per gallon on eBay. Obviously not the most economical. Once running, the system requires very little intervention. Just emptying the water trap and refilling the boiling flask with new dilute acid ever few hours.

Alternatively, one could use calcium chloride to cause an equilibrium inversion and distill out the acetic acid directly (Garwin and Hutchison 1950). A huge number of theoretical plates is necessary though. At 60% concentration of calcium chloride, it might be possible to distill the vinegar using my equipment. It would still require something like 20 plates. 304 Stainless isn’t good enough for high concentration acetic acid (316 is fine). Maybe a diy spinning band column using magnetic bearings at the bottom…

The relative volatility of regular acetic acid:water at 5% concetration is something like 1.01 and you would have to distill all that water first. That requires hundreds of plates and a lot of time. With 60% CaCl2, its close to 1.61 requiring 15ish plates. (Berg 1992) Still… you would lose a lot of acetic acid.

Best just to buy sodium acetate and distill over sulfuric acid.

25 Feb 2019

Experimenting with ethyl acetate as an azeotropic drying agent for dilute acetic acid. Ethyl acetate - water - acetic acid distillation

Works well enough for a single pass. Now I just need a dean-stark trap…

Column packing material: apparently glass beads don’t have enough surface area. Many people use stainless steel scrubbing pads, but those aren’t entirely inert. Cutting slices from pipettes is too labor intensive.

21 Feb 2019

Made a PID temperature controller box today for about $20. PID temperature controller box

Made from a cheap Rex C-100 PID controller from China and a GFI outlet. Those PID regulators come with a 40A SSR and a thermocouple. For $15 you really can’t beat it. The box is from an old computer power supply. I used a receptacle instead of hard wiring so I can use it for all kinds of equipment. From sous vide to lab furnace. I even bought a second controller for additional devices if I need it.

22 Jan 2019

Plant propagation techniques

  • hydroponic
    • droplet sizes
    • rockwool: use mineral wool insulation in place of Grodan cubes
  • simple

12 Dec 2018

I’ve been bingeing Stargate Atlantis lately and I’ve noticed one thing in particular. Every member of the Atlantis team has one job and one job only (apart from support staff). They don’t have to worry about making food or paying for medical care. They don’t have to worry about the majority of cleaning including their clothing. They wear practically the same thing everyday and it is expected of them to do so. Everything apart from the problems in their respective fields is completely taken care of. I wish I had the means to make that happen for myself. Even better would be to have to means to provide that for the entire human race. Maybe this is why I am drawn to being one of the first to colonize mars.

30 Nov 2018

Crypto bot trading

The problem is invariance. Every AI/bot trader I have seen used static prices and maybe some technical indicators to train. But a stock price isn’t based on whether its $300 or $3 (except in a categorical penny stock vs. blue chip sort of way, but that data is included in the volatility). What I’m talking about is the same mechanism by which a person recognizes the same graphical trend between stocks and over time (e.g., resistance levels). Or put another way, the absolute number of seconds since the epoch doesn’t matter, but the day of the week certainly does. The key is finding the appropriate invariant parameters, or better yet creating an AI that can. Since the latter has been the subject of research for decades and not likely to be solved quickly, I am forced to stick to the former.

Some of the more advanced crypto bots use the order book which can be useful. An interesting technique is to determine the total number of new book orders placed per unit time. That might be incorporated.

When a trader looks at a chart, what do they see?

  • up/down trends
    • is the current price above or below the price(s) of the last time period
  • what did the stock do at this previous price? (resistance level)

How to format data input to be invariant?

  • prices are not based on absolute values
    • inputs should be percent change from the previous time period(s)
    • time periods should scale: kind of like a fractal, self-similar on many levels

Hard coding some day trading strategies? E.g. resistance level:

  • locate similar prices in the historical data
  • determine if support or resistance level
  • if support: predict a bull market
  • if resistance: predict a bear market

I envision a network of regions that each have a prediction on future prices. Output: [(price1, time_delta1, certainty1),(price2, time_delta2, certainty2),…]. Alternatively, the output can be (price_delta1, time_delta1, certainty1). The predictions are combined based on their certainties and orders executed appropriately. Regions can be intermixed, but that may be more complicated than necessary at the moment. A region can be as simple as extrapolation from the EMAs or as complex as a whole deep learning AI. The regions are curated based on performance and replaced as necessary.

Instead of prices, the input will look like [+0.23,-0.1,-0.15,…]. Basically a price delta.

20 Nov 2018

  • More mHTM work

19 Nov 2018

  • Worked on mHTM porting to python 3 code

12 Nov 2018

  • Started to get back into using Anki more effectively
  • I would love to build a anki app that organizes cards based on classes and functions:
    • a function is a card set which certain aspects can be modified, but the card serves the same purpose
      • e.g. learning how to add: 5+5=10 is the same function as 3+6=9
      • the numbers don’t matter; only the function
      • only a single card is presented to check if a function is known
      • the next presentation of a function is a different card from the set
      • cards can be generated on demand if the function is something a computer can deduce
      • works for the function add but doesn’t work for plural form of the word:
    • a class…

Note: upon further reflection, this sort of thing will naturally sort itself out by virtue of the rating system. If a card is easy to remember because it is based on a shared function, the user can simply rate it as easy to remember.

11 Nov 2018

Learning Programming Languages

  • start by accessing which libraries/functions are most commonly used
    • github analysis

09 Nov 2018

Had a dream last night that I disappointed my parents regarding school. Figures. Really changes your perspective. #journal I noticed over the last couple weeks that I am getting fat. Starting keto again seems like a good idea. I was still working on the farm the last time I really got into ketosis. I suffered from headaches all the time because of it. #journal

  • been researching a lot of cyber security lately

30 Oct 2018

Lost in the infinite #journal

28 Oct 2018

  • Elijah’s Quick Whiskey turned out ok
    • the color was a deep red-brown; darker than most whiskeys
    • the taste was acceptable; it was still 40% ethanol…
    • I don’t have much to compare it to, since I’ve never drank from a bottle of whiskey that costs more than $20
  • I would like to build a large food dehydrator…

25 Oct 2018

  • attempted the first test of quick aged whiskey yesterday
    • 720 ml 40% alcohol from sugar wash
    • previously used ozonolysis, carbon filtration, (Shinnosuke Onuki et al. 2007) and 4x distillation to purify
    • made sure to remove 10ml of the head to limit methanol
    • mixed 300ml azeotropic ethanol with 420 ml H2O
    • added 10g of apple wood chips; broiled in the oven for 5 min to simulate the charring of barrels
    • 1 hour at 120C/15 psig in mason jar with lid closed tight
    • let cool
    • the color is quite nice; a light brick red
  • Second run through the autoclave today
  • Finished the CO2 scrubber yesterday
    • bubble air through solution
    • NaOH + CaOH + CO2 -> NaOH + CaCO3
    • sodium hydroxide is an absorption catalyst through the production of sodium carbonate
    • calcium carbonate precipitates for easy removal

16 Oct 2018

  • looking into making aged whiskey very quickly
    • UV irradiation (possibly with catalyst + heat) to catalyze the breakdown of lignin into aromatic compounds
    • heat (possibly lower intensity photoirradiation) to catalyze the synthesis of more complex aromatic compounds
  • could probably make whiskey from the lignin in cardboard or newspaper ;)

Aged Whiskey

  • Extraction phase
    • fluctuating high temperature and pressure of ethanol and oak barrel material
    • maybe sonication? -> probably not scalable
    • maybe requires oxygen? (probably not)
  • Irradiation phase
    • UV irradiation (280–300 nm (Lanzalunga and Bietti 2000)) to catalyze lignin degradation
    • ozonation? -> no; leads to overoxidation
  • Alternate until finished
    • use opacity as an indicator of extraction efficiency or completeness

13 Oct 2018

  • some password work
    • I would like to publish my method of generating and securing passwords, but that would make me more vulnerable

10 Oct 2018

  • more tesla coil work: getting close to first light

08 Oct 2018

  • more tesla coil work
  • My sleep schedule has been really weird lately. I still get around 8 hrs of sleep per night, but I tend to fall asleep around 3-4am –not exactly a typical sleep schedule. I’ve spent more time that I should have watching Star Trek TNG over the last few weeks #journal

20 Sep 2018

  • more tesla coil work

19 Sep 2018

  • Picked up a pattern and material for a pretty sweet red dress for the Larryville RDR

18 Sep 2018

  • ScanTesla output was jibberish… :(

17 Sep 2018

  • ScanTesla output file is 22GB… I need to load it onto my server for analysis
    • the original program is supposed to output the best config, but for some reason it didn’t work
  • I would love to rewrite ScanTesla to include elements from JavaTC and some evolutionary algo stuff
    • Stated work on converting some equations in the literature to python code
    • might need to learn more numpy to make it efficient

16 Sep 2018

  • soldered SMD chips to UD2.7c board
  • worked with JavaTC a bit to determine the right secondary coil form

30 Aug 2018

I spent all day yesterday fixing my laptop OS. It started with a simple upgrade that I had been delaying for several weeks. For some unknown reason, the update failed but didn’t roll back the changes. So I was left with a half functioning 18.04 system that failed to log in after I rebooted. Fortunately I had backed up my drive the day before. I made an extra copy of my home folder just in case. So I figured this would be a good opportunity to try out Qubes. Six hours later, I still hadn’t been able to get it to work. I was able to get into the text installation menus, but couldn’t get encryption to work due to a known bug. I’m fairly certain the problems I was having were: A) Nvidia graphics and B) PCIE related. I tried every grub flag that I found on the internet… must have rebooted a hundred times. Finally I gave up on Qubes and settled on a clean install of Ubuntu 18.04. After much fiddling with grub flags I got it to work.

27 Aug 2018

  • more work on the server
    • setting up kvms for tor services
    • I might relocated some of the other services mentioned in the server post to kvm for security
    • need to generate some certificates
    • need to work out the interfaces and forwarding
  • messed with some security settings in Tomato
    • turned off pretty much all logging -> will need to reenable them as I do more research into their pen testing usage

21 Aug 2018

  • Meal Planner

20 Aug 2018

School has started again: terrible drivers are a tolerable evil in exchange for the library staying open later than 5pm. #journal

  • more remailer website work

19 Aug 2018

  • ScanTesla finished but didn’t output anything -> time completely wasted
  • continue work on remailer
    • choosing a theme and relearning css

18 Aug 2018

  • made another batch of Play Hard
  • worked on the remailer website

17 Aug 2018

  • more meal planner app
    • learning about graph databases (Neo4j 2015)

16 Aug 2018

  • continued distillation of DMSO
    • had some kind of light brown liquid in the receiving flask, possible suck back from the pump?
    • I’m dumb. I released the vacuum but the system was still warm and as it cooled it sucked the vacuum oil into the flask.
    • going to have to redistill
  • I still want to make a meal planner app…

15 Aug 2018

  • researching urea hydrolysis for ammonia production
    • urease?
    • not available to buy
    • extract from vegetable matter? -> seems like a lot of work
  • production of sodium by DES
    • using aluminum? -> energetically favorable by 1250 kj/mol
    • still need anhydrous metal chloride
  • Hydrogen peroxide sterilization
    • vacuum chamber
  • Started distilling DMSO from 90% cream -> PITA
    • vacuum distillation at around 90C with direct heating

10 Aug 2018

  • more server: plex

Last night I was a part of a conversation about work. One of my friends was considering a promotion. He would be transitioning from working somewhat independently to managing a dozen people. Essentially the discussion boiled down to how much his happiness was worth to him. Everyone in the room agreed that their current work situation was not ideal. The descriptions ranged from “I don’t hate working there” to “I really hate my job”. These are highly skilled workers, mind you. I saw how these people, whom I admire, just hated work or at the very least thought of it as a necessary evil. I never want to be that way. #journal

09 Aug 2018

  • more server

08 Aug 2018

  • reinstalled Ubuntu 18.04 LTS on the server (again)
    • gave a write-up of the setup

07 Aug 2018

  • more site work
    • changed fonts: more simplistic

06 Aug 2018

  • worked on this site
  • TODO: correct image alignment of post graphical abstracts

05 Aug 2018

  • haven’t been feeling the best lately; had my first migraine in something like a year yesterday #journal
  • ethanol brewing has successfully yielded more than a gallon of ~80%
    • the distillation column didn’t separate as well as I hope- I suspect the small entrance hole (1/8" pipe) was too small
    • I overloaded the column and contaminated the liquor with copper. Doesn’t matter since I’m not drinking it and I’ll be running it through an all glass system for the final distillation
    • added come charcoal to remove some impurities- mostly worried about methanol

27 Jul 2018

  • ethanol brewing is slowing; since this is entirely for chemistry, I’ll let it ferment to completion
  • hopefully I will test my pressure cooker still soon
  • I broke my 1m chromatography column yesterday :,(

26 Jul 2018

  • A lot has happened; I’ve been too busy to update here :(
  • Started a test on ozone sterilization for ethanol production on Monday?
    • I originally wanted to do a side-by-side test of ozone versus placebo, but I messed up the procedure. So I just sparged ozone in both 5 gal carboys to make sure it was feasible in the first place. Plus, I am almost out of abosolute ethanol for the lab. I will have to make a fractionating column to distill it.
  • Urea evaporation went poorly. The original solution is perfectly clean, but attempting to boil 2.5 gallons of liquid outside that emits ammonia is difficult to keep clean. Also, I neglected to check whether the latex rubber tubing I used as a gasket was compatible with ammonia. Spoiler… it isn’t. So now I am recrystallizing the urea just like I would have done with cheaper fertilizer grade.
  • The gym bet failed. Partly because my partner wasn’t able to start the bet and partly because it is just too much of a time commitment. Even 30-45 min per day seems excessive. I made it a week without interruption but decided to end it after that. For now, I do a few sprints or quick foot ladder drills in the morning. Just enough to get my heart rate up and that seems to be working.
  • The DES one-pot recovery hasn’t worked. My guess is that the total solubility of metals in DES is lower than water so I need a greater volume. Something I can easily look up. I started with 1/10 mole choline chloride:1/5 mole ethylene glycol. Roughly 10 mL of solution. A small crystal of iodine was added. I added a sim card for the gold content. The plastic card warped and the iodine color was lost over a day or so, but the gold bits of the card seemed only slightly degraded. I added more iodine but after several days the sim card remained unchanged. I could use more DES or I could electroplate the solution. If all the metal has dissolved in the DES, electroplating will give pure metals. If I recycle the solution by electrolysis and dissolution simultaneously, the metals will plate as impure alloys or even metal sponge.
  • The vermiculite furnace failed: the whole thing practically crumbled. The strength of the material wasn’t high enough to allow removal of the form. If I had used a metal form, I could have either left it there permanently or calcined the entire thing before removing it. Wood just couldn’t handle high enough temperature even just the drying stage. I’ll just have to use a metal bucket or similar next time.

16 Jul 2018

  • TODO: fix graphical abstract size in css

13 Jul 2018

  • TODO: fix graphical abstract size: too big

10 Jul 2018

  • currently evaporating urea solution (Blue DEF) to get highly pure urea
  • still evaporating the zinc ammonium chloride solution; foaming is a major problem; probably better to buy it next time
  • made some iodine (Doug’s Lab Video)
    • for ionometallurgy (MChem 2013)
  • The conical flask I was making zinc chloride in cracked! I guess I really will have to buy it…

08 Jul 2018

  • DES’s are even more awesome than I imagined (P. Liu et al. 2015, Alonso et al. (2016))
  • applications to explore:
    • electropolishing of stainless
    • electrodeposition of aluminum
    • biodiesel manufacture
    • electrowinning of gold plating
    • organic synthesis of all kinds :)
  • further investigation of (Bagh 2014) revealed an electrochemical window of only 2.66-3.74 V for DES5 from 100-130C, so it makes sense that I was depositing zinc using 5V
    • make sure temperature is above 130C and voltage is <3.7V
  • Testing second batch (1/5 mol scale) of DES5
    • amine smell when attempting to dry >160C… definitely didn’t finish drying
    • attempting 3.3V 150C electrolysis using MMO/titanium anode/cathode; actual voltage is 2.66V;
    • saturated with at least 15g sodium chloride

07 Jul 2018

  • finished construction of the verm box
  • initial tests with DES resulted in precipitated spongy grey material onto the cathode
    • Two possibilities: sodium was being produced and reacting with residual water
    • zinc was being reduced from the DES because the voltage was ~5.0V which might be enough to break the Choline chloride: Zinc chloride bond -> will try 3.3V tomorrow
  • Started a second 1/5 mole scale using pure HCl this time
    • 16.28g zinc oxide + 15g H2O + 80g HCl 20.2% -> 41.7g ZnCl2*4H2O
    • reduced the resulting liquid to saturated solution; made sure white HCl fumes were gone
    • added 28g choline chloride
    • boiled to get rid of water; >150C
    • total weight of beaker + stir bar + DES = 69.5g
  • DES’s would make a great high temp heat transfer liquid instead of mineral oil or other flammable solvent
  • the first test was with a small piece of platinum wire + copper cathode; not much current flow; will try larger MMO anode + titanium cathode tomorrow
    • in order to make this a good video, I should try more readily available cathodes; carbon for starters
  • high index of refraction for DES5 (n = 1.5) (Bagh 2014) makes images appear larger than expected from a glass of water (n = 1.3)
  • TODO: add pic of DES index of refraction demo

05 Jul 2018

  • filmed starting construction of vermiculite refractory box
    • constructing the box is probably not the best
    • I should just suck it up and use a round metal former
  • synthesized zinc chloride 1/10 scale: 8.14g ZnO + 25g HCl 32% soln. + 5mL H2O
    • apparently anhydrous zinc chloride was used in the paper (Bagh 2014)
    • I added the requisite amount of choline chloride (14g)
    • Tomorrow I will evaporate it down. Hopefully the DES is enough to keep hydrolysis to a minimum
  • researched platinum group metals concentration in street dust

04 Jul 2018

  • filming during daylight
  • still working on getting the server back up and running
    • apparently OpenStack is only available for ubuntu16 and I installed 18 :(
    • trying to get it working…

03 Jul 2018

  • set up for filming using Hannah’s Nikon
  • need more light

02 Jul 2018

  • filmed parts buy for vermiculite lab furnace video
  • did a lot of cleaning of the workspace
  • 01 Jul 2018

    Deep learning Organic Synthesis

    (Coley et al. 2017)
git clone git@github.com:connorcoley/ochem_predict_nn.git
git clone git@github.com:connorcoley/rdkit.git
export RDBASE=$(pwd)/rdkit
cd rdkit/
mkdir build
cd build/
cmake ..
make
make install

30 Jun 2018

Roofing

  • Measure area of foot; add 10% extra for wastage
  • Ridge: a single 3-tab single cut into three covers 18 inches of ridge

Items Needed:

  • dumpster or large trash can
  • gloves
  • belts with nail holders?
  • knives
  • push broom
  • magnetic nail pickup

29 Jun 2018

  • Finished week 1 of workout plan

28 Jun 2018

  • Made Jafar costume.
Jafar and Iago
Jafar and Iago

27 Jun 2018

  • Research on AGEs for reddit…

26 Jun 2018

  • Day 2 of the gym bet successfully completed.
  • Still consuming at least 6 ‘salads’ per week. Still haven’t had a depressive episode. Longest streak in history for me.
  • looking at insulating refractory mixes
    • vermiculite with sulfuric/phosphoric acid chemical binder (Ekedahl and Veale 1959)
  • working on site setup

TODO:

  • fix website(s)
  • plan for upcoming videos
  • order chemicals for upcoming videos
  • write checklist for flaminglasrswrd work day

25 Jun 2018

  • Investigating motion capture software for possible inclusion of workout gifs to the food planner project (if I choose to add in workouts later on).
  • Investigating better hydrogen torch setup. A separator cell that doesn’t explode…
  • Started workout program and bet with Matt.

15 MAY 2018

I need to get back to work. Spent the weekend at my parents house. Partly for my brother’s graduation and partly for Mother’s Day. All my sibs were there. I didn’t get a headache this time… curious.

04 MAY 2018

Been a little off lately. Not quite to the point of depression, but certainly getting there. I’m sure my RescueTime and logkeys data will show how little I’ve worked the past 3 days. Further evidence for the Kale experiment started a little less than a month ago. I haven’t had any symptoms since I started except for now, exactly coinciding with a break from consuming leafy greens.

29 APR 2018

So I didn’t sleep last night. I “went” to bed at 4am and got up again at 5am without any actual sleep. Writing academic papers even informally on this blog is painstaking. I wish there was a IDE for journal article writing.

17 APR 2018

I tried to use <eatthismuch.com> yesterday. A mildly unpleasant experience. Don’t get me wrong, its an admirable site. It just has limitations, which in my opinion, are debilitating. I am now convinced I should write my own.

A few weeks ago I looked into writing my own recipe recommender system. When I located eatthismuch, I decided it wasn’t worth it (without even looking at the site in depth). Competition is not my strong suit. But, now, having actually reviewed the site, it doesn’t appear all its cracked up to be. They haven’t actually captured the semantics of recipes and food prep. The site just seems like a backend collection of if…then statements without any sort of knowledge. For instance, I told the site that I would prefer to eat the food ‘whole egg’ for breakfast. So when I refreshed the recommendations, the site gave me 1-2 whole raw eggs for breakfast. A human, of course, would recognize that input as saying that I would prefer to use eggs as an ingredient in my breakfasts. Of course, I could learn how to use the site properly, but I don’t want to do that. I want a recipe/food/meal prep program to have zero learning curve. Like a human whom you ask, “What should I make for dinner tonight.” Therefore, I would like to attempt a meal planning service.

14 APR 2018

A week of uninterrupted happiness and motivation. I can’t remember if that has ever happened to me. Since the last episode on April 5, I have been eating a salad composed principally of leafy green every morning. The hypothesis is that somehow nitric oxide is contributing to my happiness. But whatever the real reason this is working, I’m not going to stop with the breakfast salads.

06 APR 2018

Feeling much better today.

I think I’ll move any conversations about AI to a separate page from now on.

05 APR 2018

Had a depressive episode this morning. Only just arrived at the library (3:30pm). Tested a hypothesis that this episode might be related to nitric oxide system. Consumed 6g of citrulline and 5-6 leaves of kale to test. Oral mouthwash last night and exercise depleted body stores of nitric oxide precursors. That intervention doesn’t seem to be working sufficiently. I have a constant need for comfort.

QOTD: How does the brain determine what inputs represent features and what are classes? Does it separate the two? Are classes disjoint? Features not so?

04 APR 2018

Why do we have short term memory?

Is it solely to organize actions into a specific order? A telephone number consists of numbers 0-9 but only the specific order is important. Altering the connection weights between any particular number and that sequence isn’t very useful. I.e. The fact that a particular sequence has a 9 in it doesn’t matter.

If you were to ask Alexa, “What time is it?” You don’t want the response to be, “1:26 PM the time it is.” Although technically correct (the best kind of correct), it is not the typical response and it doesn’t conform to the rules of grammar and syntax. Unless you asked Alexa to change her name to Yoda, of course. An example so simple is certainly understandable for humans because the time scale of the order switching is only a few seconds (within the human short term memory window). A desirable AI system should ideally be able to order an infinite sequence of events, which is obviously impossible.

Hmmm… it seems that visual imagination is competitive in space while auditory imagination is competitive in time. For example, when I think about how a particular object looks and activate its critical feature pattern, that object appears in my mind always in the center of focus. If I attempt to place that object in my periphery, my focus always snaps to it. I cannot simultaneously hold my focus at the center of the visual field and imagine an object in my periphery. I can, of course, imagine lots of different objects of varying complexity, but never two objects of a class. E.g. I can imagine a red circle and a blue circle but not both simultaneously. My mind’s eye flits back and forth between them, unable to make permanent changes to the appearance of either. Oddly enough, if the circles touch or overlap, I can imagine them as one shape (like a figure eight). In essence, visual imagination is competitive in space. An object is regarded as one if it is continuous in space, and only one object can be manipulated in imagination at a time.

Likewise, auditory imagination is competitive in time although this one is considerable harder to explain because I cannot express it in alternate dimensionality like I do with visual imagination.

03 APR 2018

I dreamed of Prolog last night. Do you know how hard it is to program in your dreams?

Designing Programs

Syntax, toy problem, blah, syntax, syntax, syntax, toy problem. That’s how the vast majority of “tutorials” on programming languages teach and the complete opposite of how one uses a programming language. To use a programming language (and any language for that matter), one starts with an conceptual idea of what one wants to explain or do. From there, a series of decisions are made to accomplish that goal. Instead of teaching tiny bits of syntax which have no inherent purpose to the brain, wouldn’t it be better to show the brain a new item that is actually useful? Teaching syntax is necessary, no doubt, but it shouldn’t be the first step in learning a language. E.g. Rosetta Stone and DuoLingo use the practical approach. A lot of online programs use the learn by example path, which is somewhat better. But they fail where you have to make actual design decisions later using the particular programming language. E.g. Why would one choose to use a set() over a dict() in python?

I’ve run into this problem headfirst while learning Prolog. Of the few tutorials on Youtube, none of them cover anything more than syntax. Github is full of practice problems from such and such a college course or book.

Fortunately, I’ve come across a book which might be of use for the particular area of Prolog. The Practice of Prolog (Sterling 1990) teaches how to develop a project in Prolog from start to finish.

02 APR 2018

Recently I have been learning about Prolog. I like the idea of pure declarative languages. The beauty of simply defining the problem and having the interpreter/compiler solve the problem is striking. It is quite different from my previous programming adventures in C++ and python. I stumbled upon a realization this morning: Backtracking in Prolog seems to be the exact mechanism that Adaptive Resonance Theory calls “Resonance and Reset”.

I’ve been going about this all wrong. I’ve been so focused on finding out all the ways the brain solves the problem of knowledge acquisition and use that I have neglected the reason why that problem had to be solved in the first place. The human brain has assuredly a vast number of features that help it solve that problem. A number of them are sure to be superfluous, redundant, and downright incorrect thanks to evolution. Trying to wrap my head around all the various features of the brain is nigh impossible especially since I currently believe there are emergent properties of the brain. A better solution might be to solve the problem of knowledge acquisition from first principles. I’m certainly not the first person to do this. Perhaps all of philosophy (and certainly Ontology) is in this pursuit.

For instance: Why did the brain develop grouping (e.g. a set of pixels on the retina are collectively denoted ‘square’)? By assigning a group, the brain can modify its internal state only once and have that change propagate to all affected members rather than modifying each affected member separately, thus saving energy.

So the question is: What problems compose knowledge acquisition and use? At first glance, knowledge accuracy and knowledge acquisition speed are a trade off. Knowledge that is applied to a set that is not completely consistent is known as a heuristic.

29 Mar 2018

[stream] What would my ideal schedule look like? I have attempted many times in the past to streamline my routine and plan my days (sometimes months) into the future. It never seems to work. Four days is my typical stretch. Then I revert back to my primitive, unscheduled self. Its a tiring routine in and of itself. I keep recalling something I read about Ben Franklin, that he would practice one and only one routine for a month before working up to another one. In the past, I have thought that he just doesn’t know how to push himself. But perhaps he really knew what he was doing? My track record of implementing change is practically nil. Perhaps the mind, no matter how excellent or effortful, just can’t handle that much change. Inevitably, something breaks down.
In other news, the fasting has somewhat failed. I think intermittent fasting has its merits. I certainly started out feeling much much healthier and my mood stabilized a bit. My memory mostly returned. The first day I skipped breakfast and lunch. I then only ate ‘dinner’ after I felt hungry for a couple hours. I made it to 4pm the first day. 5:30pm the second. By day four I didn’t even want to eat at 7pm. That is the problem that I am facing now. Last night I stayed up to 4am (a whole problem by itself) and I felt just insane hunger at 3am for some reason. I hadn’t eaten much that day because I felt no hunger. I would feel my stomach rumbling, but no desire to consume food. My calorie count is epically low over the last couple days. By my resting metabolic rate I should be consuming circa 3000 kcal per day. Likely I was consuming less than 1500 on some days. Certainly I am in ketosis. I attempted to counteract the low energy a bit by consuming more fat, namely bulletproof coffee. I am still consuming my protein shake thing.1 If I wasn’t so poor, it would also contain a lot more fat. The only fat I have used in the past in mixes like that is MCT oil. Solid fats would require more prep that I am used to doing. Perhaps I can add some olive oil instead. I tried that with the breast milk project and it doesn’t taste good. Today I had, in addition to BP coffee, a breakfast of microwaved broccoli with butter, salt, pepper, and mustard seeds (for the enzymatic conversion to sulforaphane). This was only sort-of breakfast since it was 1pm.
Let’s try an experiment shall we. I’m going to remove/disable social media from my phone. My big crutches are Facebook, Reddit, and Youtube. Combined I spend at least several hours per day on them. I don’t need that. The only part I might miss is the event updates on FB. I will still have email, text messaging, and snapchat. The last one because its the only way I seem to be able to communicate with one person in particular. I need to figure something out to minimize that distraction. Note: I’ve noticed that I can’t leave my phone facing up within my visual field… I see phantom LED notifications. Out of the corner of my eye it appears that the indicator LED on my phone is illuminated, but when I look closer nothing has arrived. Serious addiction.
I don’t think I can completely eliminate my cell phone. I did that once. For about 6 months I didn’t carry a phone because my old one broke down and I was too poor to buy another. As a consequence, I was freer, but I also lost contact. My mom was especially distraught. She wasn’t really on FB at that time and the few calls I did make to her were now nonexistent. Now, of course, she has a phone and is more active on FB. Similarly, I can’t forgo the laptop. I am a programmer by skill set. Not impossible, but practically untenable to be a programmer without a computer.
[/stream]

26 Mar 2018

21 Mar 2018kugelrohr

Made some updates to this site.

Footnotes

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  1. 500ml milk + 30g whey protein + creatine, ALCAR, NAC, TMG, citrulline, beta alanine, taurine, agmatine, ornithine, vit C, Mg, K, Zn, potato starch

  2. 18+ hr fast + fermentable fiber + high protein + vegetables: Testing the effect of fiber consumption on tolerability of intermittent fasting