Monday, December 31, 2012

Ethanol 3 (mead)

Day 1 (Dec 31): Started new batch of mead: 24oz of honey in 1gal. Some problems.
- It appears to have been too much honey, since not all of it dissolved.
- The red-star yeast again failed to "head", but again was anarobic within 24 hours.
Day 3 (Jan 2): Fizzing like mad. Far more effervescent than soda. All trace of excess honey is gone.
Day 5 (Jan 4): Same state.
Day 8 (Jan 7): Still going strong. 1 bubble (at least 1cc) every 10s or so. Rate could be twice that.
Day 10 (Jan 9): Fizzing waned yesterday, and continues to wane today. Large yeast sediment at the bottom of the container.
Day 12 (Jan 11): Weak effervescence, significantly clearer solution.
Day 17 (Jan 16): Still bubbling very slightly. Looks almost like apple juice clarity-wise.
Day 22 (Jan 21): Faint effervescence still present. Probably done within 1-2 days.
Day 27 (Jan 26): No fiz for two days. Decanting. The substance is as clear or clearer than storebought apple juice. Sp Gr: 0.994
My vinometer (not a very accurate measure) says it's about 15% alcohol by volume, which is 12% by mass.

Saturday, December 29, 2012

Potash 2

Another run, this time being more careful to filter insolubles, not crystals being formed. Yield 7.6%.

Sunday, December 23, 2012

Glycerin 1

I attempted to create glycerin today using some "suspect" lye (a brown powder produced from potash rather than a white one from the store) and some beef tallow.

I melted the tallow in a pot, and mixed in double that volume of water, in which I had dissolved a half mole of lye. A white fluffy-looking layer immediately formed on top of the mixture, which I suspected might be a soft soap. But when I tested it, it was still very greasy, and very alkaline.

I set the whole mixture aside and let it cool. This took a surprisingly long time. (I think the alkali was still doing its thing and generating heat) After a bit I put it in the fridge to accelerate the cooling. Later I returned to find no glycerin layer at all, and a strongly alkaline and greasy layer where I had expected to find soap. I mixed in enough vinegar to neutralize the mixture, and set it aside to settle again. Two hours later there were still only two layers, when I had been expecting three.

I suspect I either used an inappropriate amount of lye, or that the lye was contaminated.

Lye 1

I attempted to make lye today, with questionable results.

I mixed 1/2 mol of quicklime in water, and got the expected:
  1. Sizzling reaction
  2. Exothermic reaction heated water
  3. Flocculant result
I then added 1/2 mol of slightly suspect potash (it's brown rather than white, see potash discussion) and got pretty much what I expected: a chalk precipitate and a slightly brownish liquid. I had used a lot of water, so the boil-down took forever. I stopped when I had maybe twice as much fluid as it would take to dissolve a half mole of lye, and transferred the liquid to another vessel, figuring that the precipitates so far would be something other than lye. Boiling the remainder dry gave a dark brown paste, then powder. It was highly alkaline.

Saturday, December 22, 2012

Quicklime 2

This time around it was 50g of chalk in and a couple hours on "high" in the kiln. 28g of lime came out. Since the ratio of molecular weights of calcium carbonate to calcium oxide is 100:56, that is dead on correct. Huzzah.

Day 14: in a clay pot with a loose lid, it appears to have reverted completely.

Potash 1

I was on the verge of just buying some firewood and burning it in a convenient fireplace (rather a waste because it's summer, and quite warm) when I was struck by an idea: I wonder if that wood-fired pizza place down the street does anything with their ash? Indeed they did not, and while I did get a strange look or two, I walked out with about 35lbs of ash and charcoal ends.
  • I filled a big stainless steel (not aluminum!) pot with 8lb of the mixture (about 1/3 full)
  • I topped it to 2/3 with water.
  • I stirred it thoroughly with a wooden spoon
  • Immediately large chunks of charcoal floated to the surface, and I picked them out and discarded them
  • I left the rest to sit for a while, coming back to stir it occasionally
  • After an hour, the top was covered with small unburnt wood & charcoal, which I strained off and discarded.
  • I used a ladle to dip out the clear fluid from the top of the container
  • I added more water, stirred, and repeated the process after another hour.
  • After 2 more repeats of the process, I had about 2L of potash solution
  • I discarded the wet ash
  • I put the liquid in some glass oven trays and dried it
The potash liquor (direct from the ash) is a honey-to-dark-brown color, and the potash is light brown (more like sand than salt).

Since potassium carbonate and sodium carbonate are both white crystals, I assume the brown stuff is some sort of impurity. I tried dissolving the potash in alcohol, to no avail. Neither the potash nor the brown component dissolved in it. Other people seem to have had the same problem:

at Caveman Chemistry
at Alchemy Forums

Some agricultural forums talk about "red" potash, containing iron impurities. Ferric sulfate has a sort of pinkish-brown color, but is "negligibly soluble" in water. Ferric nitrate is a very light pink. Iron carbonate is exactly the right brown color, but is totally insoluble in water (as are most carbonates). Ferric chloride has a variety of interesting characteristics (it's yellow, or green, or pinkish-purple) and it's soluble in water. So the mystery continues.

Monday, November 12, 2012

Ethanol 2 (mead and cider)

Started two liters of mead and 1 gal of hard cider. Both were bubbling within 8 hrs.

Progress Report

Day 11: Bubbling almost completely stopped. Poured off & sampled.

Friday, October 5, 2012

Vinegar 1

I took 300mL of mead and separated it from the rest. Placed it in an open 1 gallon glass jug and shook vigorously to oxygenate
Day 2-4: Shaken vigorously daily and left in necked open bottle.
Day 5: decanted into and out of a beaker to measure the volume (listed as 300mL above)
Day 14: Still smells of alcohol rather than acetic acid. Shook again to oxygenate.
Day 16: A little mold on surface. Shook the entire bottle (mixing mold into the alcohol) to oxygenate.
Day 28: The scent has become considerably more vinegar-y.

I am reminded of some old pieces of pottery my grandmother kept: large, cylindrical glazed containers with 5-8 gallon capacities, with no lids whatsoever. She called them vinegar jars, and I'm left wondering if they didn't lack ceramic lids because they were meant to be covered with cheesecloth, allowing oxygen in but (perhaps) not mold. I'll have to look into that.

Friday, September 28, 2012

Quicklime 1

I gathered 60g of chalk (more or less pure, dry calcium carbonate)
I put it in the kiln (cone 05) for 8 hrs at top temp

  • The result weighed 34g
  • That is almost exactly the 33.6g we expected
  • The remainder may be unconverted chalk, absorbed water, or reabsorbed CO2

Sunday, September 23, 2012

Saltpeter 1 (human urine)

I gathered
  • 4.4L of peat moss
  • 4.4L of pumice pea-gravel
  • 2L of urine
  • 2L of water
  • 2 ceramic garden boxes
I put a 50/50 mix of moss and pumice in each garden box
I poured 1L of urine into one of the boxes, and 1L of water into the other, and labelled them
Conditions are warm and dry outside

Saltpeter and control troughs, environment
Day 1

Day 2:
  • Both are "wet"
  • Conditions remain warm and dry
  • Turned the containers
Day 3:
Both are "damp".
  • I added 1L of urine and 1L of water to the respective boxes
  • This was a mistake. This was far more than the urine box could absorb, leaving a pool atop the moss
  • I turned everything
Experiment (urine) and control (water) troughs
Day 3
    Day 5:
    • Still small pool in urine box
    • I removed 1/3 of the "water" moss/gravel mix and put it in the "urine" side
    • Turned everything
    Day 6-10
    • Turned every other day or so
    Day 12:
    • Everything dry
    • Added another liter to both containers
    Day 13:
    • Turned earth.
    • It's obvious now why they called it 'black earth'... even when dry it's much darker than the watered soil
    Day 16
    • May have observed the "white crust/crystals" mentioned in some texts
    • Almost completely dry, no odor whatsoever
    • Added another (4th) liter of urine, making it very wet... not quite pooling.
    Day 17:
    • Turned earth, very very wet. Maybe need to switch to 5 day cycle?
    Day 18:
    • Ditto. Looks like we need to slow down delivery. 
    It appears that the timing (20-ish days) was short but reasonable, that the aeration was reasonable, but the carbon content may have been too low, and the containers neither large nor sufficiently insulative enough to maintain the required temperatures for rapid decomposition. Future tries should:
    1. Scale up the carbon content (sawdust, straw, etc)
    2. Add all the urine at once
    3. Make some concession to keeping the mass temperature high.

    Friday, September 21, 2012

    Ethanol 1 (mead)

    I started this on Friday, 21-Sep-2012.

    Pretty much directly out of "Caveman Chemistry" for this one:

    * 16oz (300cc) of honey
    * 1500mL water
    * 1 packet of yeast
    * Wake the yeast with water & sugar
    * Mix in 2L drink bottle
    * Cap

    Progress Report
    Check regularly! The book says "check every day" I'm pretty sure that if I had waited for 24 full hours, the bottle would have burst. There was a slight exhalation after 8 hrs, and after 16 it gave a serious "pop", then foamed & frothed for a couple minutes.
    Day 2: Airlock (bought a cheap plastic "inverted cups" airlock and a rubber cork)
    Day 4: Bubbled more or less continuously for 2 days (so far)
    Day 7: Still bubbling away.
    Day 12: Bubbling seems to have stopped. Will check again tomorrow.
    Day 13: Bubbling completely stopped. Decanted.

    Nota Bene
    The ambient temperature throughout this endeavor has been on the order of 80 degrees F, sometimes warmer. This is around 10 degrees warmer than is recommended, which may account for the rapid transtion into and out of carbon dioxide production.

    Monday, September 17, 2012

    Tallow 1 (beef fat)

    My local market advertises "hand trimmed meat", so I asked the butcher if I could have some of the trimmings. He was happy to oblige, for no charge! I got 40 oz of mixed trimmings.

    I estimate the composition at about 40% hard fat, 50% soft fat, 10% connective stuff.
    • I chopped it as best I could into cubes between 1cm and 1in in size. The connective tissue I just tossed in straight.
    • I added 60oz of water to the fat, and boiled it (low boil) for several hours. Suprisingly, it didn't make much of a change in the fat.
    • I set it aside for the evening
    • I boiled it more vigorously for 2 hrs in the morning, and it clearly began to separate.
    • I kept a little water in the bottom of the pot the whole time, but it boiled away rapidly, so I was replacing it fairly frequently.
    • After another 2 hrs, the fats seemed to be mostly dissolved.
    • I set it inside a sink with cool water, and once it was cool, I put it in the fridge overnight.
    • The next morning I broke the tallow cake and emptied out the water underneath, which was crowded and clouded with various material
    • I cleaned the pot, put in some more water, tossed the tallow chunks back in, and repeated
    • The tallow came out cleaner the second time, as did the water
    • A third pass was yet better

    I've become convinced that a little judicious scraping of the water-side of the tallow cake does a lot to improve the purity of the next iteration of the cake.

    Beef tallow in pot, and showing detritus
    First rendering

    Before, rendering, after: less detritus
    Second rendering

    A light scrape after the 3rd render made the 4th one dramatically whiter.

    * MATERIALS 40 oz beef trimmings, 2-4 gallons of water.
    * PROCESS I did 4 renderings, including the initial one.
    * PRODUCT The tallow stayed soft at any temperature above refrigerator temps (40 deg F) which is a bit of a bummer.
    * YIELD I ended up with 19.5oz of tallow from my initial 40oz "beef trimmings" sample. Not sure if that's good, bad, or typical.