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.