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Lux Natura
09-29-2017, 04:19 PM
Having calcined wood to ash and extracting and purifying the salts, I proceeded to capture dew in the evening throughout the spring and summer.

Had around 200 grams or so of salts to work with initially.

I saved the liquid that was on top of the salts in the early mornings and still have that.

Throughout the summer, the salts did get contaminated - little bugs got in, and dust and whatnot. So I decided to see what would happen if I tried to purify those salts using repeated recrystalization. I did not weight my initial amount, but it did appear to be close to the 200 grams that I had in the spring when I began.

After each recrystalization, (basically just dissolve in distilled boiling water, let cool, and crash out in the fridge) I get less and less salt coming out - mind you the crystals are exceedingly pure.

Wondering where the salts are magically disappearing to, I even tried to evaporate off the waters that remain after crashing out the crystals in the fridge - but that water evaporated away to nothing.

Now, in my current recystalization, I have maybe 1 gram of worth salt floating around in my cold solution. After I filter those off - and evaporate away the water, there will be nothing left. The water evaporates away without leaving any of the crystals.

So where did they all go? Close to 200 grams of the crystals have disappeared throughout the purification process, and they were not left in the water either.

My only thought is that somehow through the process of heating and cooling, they became volatile, and just escaped that way.

Anyone experience something like this before?

z0 K
09-29-2017, 11:12 PM
Having calcined wood to ash and extracting and purifying the salts, I proceeded to capture dew in the evening throughout the spring and summer.

Had around 200 grams or so of salts to work with initially.

I saved the liquid that was on top of the salts in the early mornings and still have that.

Throughout the summer, the salts did get contaminated - little bugs got in, and dust and whatnot. So I decided to see what would happen if I tried to purify those salts using repeated recrystalization. I did not weight my initial amount, but it did appear to be close to the 200 grams that I had in the spring when I began.

After each recrystalization, (basically just dissolve in distilled boiling water, let cool, and crash out in the fridge) I get less and less salt coming out - mind you the crystals are exceedingly pure.

Wondering where the salts are magically disappearing to, I even tried to evaporate off the waters that remain after crashing out the crystals in the fridge - but that water evaporated away to nothing.

Now, in my current recystalization, I have maybe 1 gram of worth salt floating around in my cold solution. After I filter those off - and evaporate away the water, there will be nothing left. The water evaporates away without leaving any of the crystals.

So where did they all go? Close to 200 grams of the crystals have disappeared throughout the purification process, and they were not left in the water either.

My only thought is that somehow through the process of heating and cooling, they became volatile, and just escaped that way.

Anyone experience something like this before?

Wood ash will give you several fixed salts depending on what wood you used. If you calcined the wood ash then extracted the water soluble salts with distilled water you will get mostly potassium and sodium carbonates in the water. Magnesium and calcium carbonates in the calcined ash are not very soluble in distilled water.

Once you set out the water soluble salts to deliquesce in nightly dew the salts will be exposed to small amounts of ammonium nitrate and other things including acids in the air dissolved in the dew. They can change the chemistry of the salts. Plus you had contamination with insects and other things. Insects can produce some powerful enzymes further altering your mix of salts.

It is very difficult to volatilize the water soluble fixed salts. The process you used dissolution and evaporation will not cause potassium carbonate to volatilize. It is hard to say what will happen when you alter the materials in the matrix with contamination.

You say you still have the liquor that was on top of the salts. What is the pH of that liquid?

Lux Natura
09-30-2017, 01:50 AM
What is the pH of that liquid? 12-13.

One thing I did notice, when the salts have hot distilled water added to them, there is much fizzing and bubbling. It settles down at the point where all the salts finally are dissolved.

Realistically, I know that using recrystalization has diminishing returns with ever purer yields, but it boggles my mind that ultimately all this salt has disappeared.

theFool
09-30-2017, 08:50 AM
May I ask, how many times did you dissolve and coagulated the salts? (approximately)

Potassium, sodium and calcium salts that are found in ash cannot become volatile at such low temperatures. I doubt also if there have been discovered any kind of volatile compounds of those elements according to chemistry.

In my opinion you should replicate the experiment in order to confirm that the result cannot be attributed to a mistake.
Then, write down the details of how one could replicate it and give it to interested people (if you find any). In case they succeed too you will have a confirmation of the new discovery.

z0 K
09-30-2017, 04:26 PM
12-13.

One thing I did notice, when the salts have hot distilled water added to them, there is much fizzing and bubbling. It settles down at the point where all the salts finally are dissolved.

Realistically, I know that using recrystalization has diminishing returns with ever purer yields, but it boggles my mind that ultimately all this salt has disappeared.

You might consider distilling the liquor pH 12 -13 in a water bath to expose the salts dissolved in it. By collecting the distillate water in a receiver you can then take a pH reading to see if anything distilled over with the water.

The crystallization process you have described separates out water soluble salts. The less soluble ones will precipitate out when the water is cooled. The more soluble ones will remain in the cold water. Salts from biomass can be processed in many ways depending upon what your goals are. Wood ash is not a rich source of potassium carbonate. Fixed salts do not evaporate away but if you leave them exposed to sunlight and wind, weather and wildlife many things can happen that you probably did not witness.

Ghislain
10-01-2017, 06:23 AM
If you distill and capture, without any loss, your material, then weigh it at all stages and see if there are any discrepancies.

Ghislain

elixirmixer
02-04-2018, 08:45 AM
I just found evidence that at about 180degs Celsius, there is in fact some volatilization of the alkaline salts. Which makes me wonder what could be achieved at higher temps??

Today is my first attempt to make some standard volatile salts of tartar just from sage ashes and sage essential oil. See how we go...

Lux Natura
02-08-2018, 04:53 AM
There is the argument that salts do not volatilize, and we can look at chemistry to understand why, but there are other methods of salt transport which would end with the same result but work through a different pathway, giving the same end result.

I've been watching my salt jar for the last few months, and that's the conclusion I have come up with. Slow, long term volatilizing and redepositing further along the glassware at room temperature, without any evidence of salt crawling up the sides or anything like that. There are plate tectonics in my salt flats, but it takes months to see any changes. Ridges and mountains are forming. Must be some pressure gradient acting upon it, but literally the only inputs are the light it gets (sits on a window sill) and minor heat fluctuations during the day.

Who knows, maybe I will wake up one day and it will have rearranged itself into something closer to its true nature.

elixirmixer
02-08-2018, 05:13 AM
I had a pH strip go purple from the steam of my evaporating salt solution when at high temp and on their second wash, so reasonably pure.

I still failed making my volatile salts though and it was a very sad day. In fact I wish I hadn't replayed because its just reminding me of the pain.....

Dragon's Tail
02-08-2018, 05:18 AM
Half a pound of salts is A TON vs what I'm normally working with. Have you been measuring what's dropping out of solution by drying and weighing? Are you using enough water for them? If you are trying to get potassium carbonate, i've found that it's best to filter the solution while hot and then recrystallize from that, one of the common "impurities" drops out on heating, which I call "the dark serpent" because of the way it looks in the bottom of a mason jar. Once it appears, I evaporate off a bit more, and then filter hot before going to the next drying step. This saves a couple solve et coagulas.

Lately, I haven't been trying for purity of potash because I believe some of those other things, particularly the magnesium compounds, may be important.

I also have to disagree with Zero a bit. Hardwoods have fairly high concentrations of potassium carbonate, and magnesium salts are decently soluble (I forget if that's the chlorides or the carbonates with that ion). I'm doing a small batch right now from leftover charcoals that I purified from my fire pit at the property. I filtered them from the ash, washed and dried them in the sun, and then ground them into a carbon powder that calcines without any smoke indoors where I am now. But I've also had to leech them over and over, and getting the "salts" completely extracted from the calcium carbonate and silicates is taking a while. Over half a gallon of distilled water gone through so far (me and my small batches)

When you say 200g EM, are you talking about ash? Because from wood that would yield about 20g give or take of actual salts. A lot of it is going to be glass and chalk that are not soluble. ... EDIT: unless you MAKE them soluble ;)