Paper 1

I have only a couple days before I leave on my trip, and I wanted to get something else done before I left, so a quick attempt at paper seemed reasonable. This may seem more craft than chemistry, but filter paper is important later on, so I'm including it here.

Raw materials: Dry grass, Potash, Water
Tools: A boiling pot, heat, a screen 

So here's the dry grass. It's really dry. It's been sitting in a box for weeks or longer, waiting for a project to come along. Originally it was going to be compost carbon, then weaving material, but finally it has become paper pulp fiber.

1 meter stalks of dry California grass

Step 1: Remove the nodes

I am not really sure why this is necessary, but all the small-scale references insist on it. I expect that if you're doing large-scale crushing or boiling the nodes break down by themselves, but on this scale it's worth doing the pruning.

Break the grass up into lengths with no "inter-segment nodes". That basically means break off the little hard parts where branches or leaves come out. Here is a piece of grass with two nodes circled

Grass with nodes circled

And break out the nodes completely, leaving just the stem bit

Grass stems

I am very slow, so after 50 minutes, I had a single thick handful, which I deemed a half liter or so.

A handful (~500ml) of straight grass stems

Step 2: Prep the Alkali

50ml Potash

WARNING: Do not use aluminum containers when working with alkali. Hot alkali, under the right conditions, can burn right through aluminum. When combined with boiling water, flames, and caustic solutions, this can be bad. Use glass, ceramic, or stainless steel containers.

I made a solution of 50ml of loose potash in 1 gal of water.

Step 3: Boil

The handful above contains more than a little woody stem (not wanted) as well as dirt, dust, and other detritus we want to get rid of. Boiling in alkali will separate all of these things for us as well as preparing the fibers themselves. If we were going to bleach the paper, this is the point where we'd do it. I didn't have the materials, so I skipped that step and just did the boiling.

I had the stems in the alkali while it came to a boil. After about 30 minutes of boiling, the scent of the steam changed from grassy to distinctly sweet. I held it at a boil for 60 minutes total, replacing the water as it boiled away. After that hour I took it off the fire, poured off the alkali and replaced it with fresh water.

Step 4: Rinse and Crush

This is pretty straightforward. I'm trying to separate the fibers from the rest of the stuff without making them too short.  I used a round wood stick against a flat wood surface, and the stems split and mashed immediately. Even though the stems were still rigid, the fibers themselves were extremely pliable and soft. The integrity of the stems as a whole was entirely an artifact of their geometry as a tube. During the rolling, some individual fibers got caught on the rolling stick and wound themselves up along it providing a very nice yarn which could be removed with a fingernail. The average fiber length at this point was quite long: over 8 cm.

Step 4a: The plan changes

The length of the fibers and the fact that they weren't crosslinking (they were staying parallel) gave me pause. I took the stems out and they bent and flattened easily, but the individual fibers stayed attached to their bretheren on the stem until something else snagged them.

I decided to alter the experiment mid course: I cut maybe half of the fibers to a length of about 3 cm using a knife and reboiled them in plain water, hoping that this would separate them and let them entangle/mat/felt more.

Shorter fibers boiling

Still not convinced

I took handfuls of the fibers and crushed them between two rocks, hoping to see something that looked like paper. Either this is going to take much longer than I expected (multiple hours) or the fibers are way too long. Perhaps more research is in order.

More saltpeter math - I am enlightened

Rationale

Nitrates are enormously useful compounds, and this blog is about simple chemistry, so investigating simple methods of producing them are extremely relevant.

Conclusions

FIRST: Despite far too many bad internet references about making gunpowder out of urine, I have finally figured out why nobody gives instructions on how to do it. It is, for the most part, impractical.

SECOND: If what you're looking for is soluble nitrates, it's far easier to use "normal" composting materials like grass clippings and animal products than to try to leverage the urea in urine directly.

The investigation

After doing the math on the saltpeter yield and after a lot more research on the composting process, I have decided to take another whack at figuring out what it would take.

Target values

Ideal hot, nitrifying composting seems to occur near a C:N ratio of 25 and a moisture content of 40-60%. If there were nothing in the mass that wasn't nitrogen, carbon, or water, the ratios might look like: 40% water, 57.7% carbon, 2.3% nitrogen.

Raw Materials

To produce 1 kg of soluble nitrates, we need 140g of nitrogen. Targeting a C:N of 25, we need 3.5kg (25 x 140g) of carbon. Since straw and sawdust are still 20% moisture, we would need 4.375kg of that material to provide the right amount of carbon to balance out the nitrogen. To get 140g of nitrogen from urea, we need  32L of urine, which is essentially 100% water.

Material	Urine	Straw or Sawdust	Total
Nitrogen(g)	140	0	140
Carbon(g)	60	3440	3500
Water(g)	32000	875	32875

That would leave a moisture content of 90%. (32875g water vs 36515g total mass)

AHA!

The light has come on. Given the urea content of 32L of urine, we only need 3.5kg of carbon to get the ratio right, but the water content is beyond all reason. That's probably why no one documents urine as anything other than a "de minimus additive".

Forcing the issue

Presuming the 32L could be reduced (boiled down?) to 1.625L (20-to-1 reduction) without loss of nitrogen, the numbers would add up more like
 

Material	Urine	Straw or Sawdust	Total
Nitrogen(g)	140	0	140
Carbon(g)	60	3440	3500
Water(g)	1625	875	2500

Which gives a moisture content of 40%. (2500g water vs 6140g total mass) Close enough.

So if the presumption is valid and you had to do it this way, you'd do something like:

1. Reduce volume of urine to 5% original
2. Add 2.3-3 times (by weight) straw or sawdust
3. Mix and compost it

Nota Bene

Most of the "municipal water purification" references on the web (which also deal with nitrifying bacteria) have an end goal of anaerobic denitrification so the organic nitrogen is ultimately expelled as inert nitrogen gas. In this case, the high water content is no problem.

More practically

Follow the instructions from numerous sources which use fruit, vegetable, and fresh green plant matter. It produces the same nitrates, but doesn't require boiling urine.

References

• Composting at LSU
• Composting at University of Idaho
• Composting at WebLife.org

Acetone 1 (honey + chalk = acetone)

My longest chain to date:

• Honey + Water + Yeast = Mead
• Mead + Acetobacter = Vinegar
• Vinegar + Chalk = Calcium Acetate
• Dry distilling Calcium Acetate = Acetone

Acetone could be used to thin or strip paints, but I think the most likely use is as a recoverable solvent to extract oils from seeds. That would indeed be a labor boon.

Notes:

1. My original vinegar was made from mead, and thus contained a variety of compounds beyond simple acetic acid. I distilled it, and got a very clear product.
2. It takes a surprisingly large amount of chalk to slake a relatively small amount of vinegar.
3. The drying step is by far the longest part. I used a glass pie pan in a 200ºF oven. It took hours.

Procedure:

1. Add chalk to vinegar until fizzing stops
2. Add 10% more chalk than you have already added
3. Add 100% more water by volume
4. Filter the mixture to remove undissolved chalk, leaving a calcium acetate solution
5. Place solution in a shallow bowl and apply gentle heat. (Over 160ºC would break down the acetate)
6. Collect the calcium acetate
7. Dry distill the calcium acetate producing acetone.

Results:

• The calcium acetate came out a little dusky rather than totally white.
• The distilled acetone came out light brown, but smell and application to styrofoam confirm acetone was present
• Much of the solid remained unchanged

Caveats:

Acetone is a List II Substance

Saltpeter math

Nitrogen: The math

From Wikipedia: 

• Grams of urea in a liter of urine: 9.3
• Molar mass of urea: 60g
• Molar mass of potassium nitrate: 101g

Break out the Unit Factor Analysis manual...

So to get 1kg of Potassium Nitrate, you would need about 32L of feedstock.

Glycerine 2, Soap 1

New attempt:

• 380g tallow
• 5 oz water
• 86g store bought lye (WAY too much due to miscalculation)

1. added the lye to the water and let it cool.
2. melted the fat completely and let it cool for a minute or two
3. combined the two and mixed lightly
4. poured into a glass container and set aside to cool overnight.

Result: still an unseparated emulsion in the morning.

Tallow on the scale

Lye and Water Mixture

Melting before adding lye

Unseparated result

After 24 hours it was still pretty much a homogeneous gel, so I "remade" it:

1. melted it over a stove
2. added a cup of water (to aid in melting)
3. added a cup of vegetable oil (to balance the excess lye)
4. left to cool in the metal pot I did the melting in

Result: Really granular/void-filled soap, but definitely soap.

I also collected about a cup of water and a couple ml of cloudy glycerin

The soap was still really granular, and when I squeezed it I got a lot more glycerin. So I divided it into three balls and wrapped them in cheesecloth, then pressed them. This produced dryer soap and more glycerin, but not much more water.

Next note: Decanting two separated liquids is hard without the right equipment. I think that if I were doing this at scale I'd probably find it useful to make some specialized equipment

Day 6: The balls of soap are still in their cloth and still very slick. I think they're still exuding a bit of glycerin. But they do work as soap.

Day 20: The soap is now hard enough to be considered ready

P.S.
Lye is hard to find these days. Went to 2 hardware stores, a supermarket and 2 drugstores. No dice. Ordered it from Amazon instead. Easy.

Nitrogen from composting

Posted nitrogen-fixing question to four composting forums:

• Garden Web
• Helpful Gardener
• Dirt Doctor
• Permies

But no particularly applicable experience/data. It seems like I'm asking people about the right problem at the wrong scale. I shall look elsewhere.

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.