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Lux Natura
09-14-2016, 11:56 PM
Night after night, I had placed my salt out to collect the dew, always draining off the oil in the morning.

After I had about 1/2 liter of oil, not knowing what to do with the now mushy salt mixture, I left it on a shelf.

After about a month, I started to see the salt climb the walls.

2 months later, the salt had reached the top lip of the pyrex dish.

At this point, I checked on it daily, just because it seemed there was action afoot.

One day, I found a puddle on the shelf below the pyrex - and in that puddle was a single nearly perfect crystal.

Taking this crystal out of the puddle and drying it, I placed it in a flask, and it is now starting to effloresce.

Interested in seeing what other changes can occur, I have devised a pelican style setup, from which the salt can climb out and then drop back into that which it climbed out of to see if that which climbs out will change over time.

From a bit of thinking about it, what I have come up with is that the pressure inside the matrix of the original salt was lower then the vapor pressure - hence it took on water. This makes sense, as in the preparation of it I cooked off all the water. Placing it outside, it takes on humidity.

Afterwards, out of that water, was born something that had a higher internal pressure than not just the moisture in the air, but the very liquid it was swimming it. So it climbs out. Then it dries off, and even now, it seeks to dry itself even further. Maybe as the molecular lattice is formed, it traps water, and as the lattice contracts, it seeks to expel that water. Even after it has expelled enough water to form a nice crystal, it keeps contracting, forcing more water out and turn white powdery. One way or another, there is some action that drives moisture out - maybe a heat, but it's a slow growing process. Certainly I had not seen this had I not waited many months for it to develop.

To taste, the second salt has much more of a bite than the first. It does not dissolve in water either, so I have not gotten around to comparing pH. I have yet to see what it dissolves in and will test in alcohol.

I am interested in researching more about this - and if people have such experiences, or can suggest texts to look into that talk about these kind of things.

For what it's worth, knowing what the cation of my initial salt was, no other salts I have come across in my research fit what the new salt is. Ideally it should be a simple thing to figure out, but in practice it doesn't line up. As if there is something else in the air that is an anion or something similar that just is not chemically defined in the scientific literature. It may not even be the "cation" based salt anymore either - but I will do some flame tests just to see.

JDP
09-15-2016, 12:23 AM
Night after night, I had placed my salt out to collect the dew, always draining off the oil in the morning.

After I had about 1/2 liter of oil, not knowing what to do with the now mushy salt mixture, I left it on a shelf.

After about a month, I started to see the salt climb the walls.

2 months later, the salt had reached the top lip of the pyrex dish.

At this point, I checked on it daily, just because it seemed there was action afoot.

One day, I found a puddle on the shelf below the pyrex - and in that puddle was a single nearly perfect crystal.

Taking this crystal out of the puddle and drying it, I placed it in a flask, and it is now starting to effloresce.

Interested in seeing what other changes can occur, I have devised a pelican style setup, from which the salt can climb out and then drop back into that which it climbed out of to see if that which climbs out will change over time.

From a bit of thinking about it, what I have come up with is that the pressure inside the matrix of the original salt was lower then the vapor pressure - hence it took on water. This makes sense, as in the preparation of it I cooked off all the water. Placing it outside, it takes on humidity.

Afterwards, out of that water, was born something that had a higher internal pressure than not just the moisture in the air, but the very liquid it was swimming it. So it climbs out. Then it dries off, and even now, it seeks to dry itself even further. Maybe as the molecular lattice is formed, it traps water, and as the lattice contracts, it seeks to expel that water. Even after it has expelled enough water to form a nice crystal, it keeps contracting, forcing more water out and turn white powdery. One way or another, there is some action that drives moisture out - maybe a heat, but it's a slow growing process. Certainly I had not seen this had I not waited many months for it to develop.

To taste, the second salt has much more of a bite than the first. It does not dissolve in water either, so I have not gotten around to comparing pH. I have yet to see what it dissolves in and will test in alcohol.

I am interested in researching more about this - and if people have such experiences, or can suggest texts to look into that talk about these kind of things.

For what it's worth, knowing what the cation of my initial salt was, no other salts I have come across in my research fit what the new salt is. Ideally it should be a simple thing to figure out, but in practice it doesn't line up. As if there is something else in the air that is an anion or something similar that just is not chemically defined in the scientific literature. It may not even be the "cation" based salt anymore either - but I will do some flame tests just to see.

Your "salt" might just be absorbing some gas from the atmosphere and changing its properties and composition. For example, potassium carbonate gradually absorbs carbon dioxide from the atmosphere and becomes potassium bicarbonate, which is non-deliquescent. The absorption of carbon dioxide (even though the composition of this gas was not quite understood at the time) by several substances was the subject of the classic chemical researches of Joseph Black, in his "Experiments upon Magnesia Alba, Quick-Lime, and some other Alkaline Substances":

https://archive.org/details/experimentsuponm00blac

Lux Natura
09-15-2016, 01:46 AM
Your "salt" might just be absorbing some gas from the atmosphere and changing its properties and composition.

Yes, that is what I am thinking as well, although I'm not able to find what it can be changing into using either what I know should be contained in the atmosphere, and the crystal lattices / angles. It may be possible that there are hydrate forms of salts that are just not listed online due to them having little industrial / chemical / economic usage and having a low decomposition point. A resource such as something that list the crystal types of all compounds that have XYZ elements in their structure would aid greatly to narrow down what, if anything, is being captured, but I don't think such a resource exists online.

I'm thinking that this process, of the salt changing by capturing and giving off, can be continued, although at times something may have to be done in order to allow the salt to undergo this change, whether it's dehydrating it, heating it so that some weak bonds can break down, etc.

Thanks for the link - I will add it to the weekend reading list!

Andro
09-15-2016, 05:22 AM
Lux ~

This new salt:

Does it mix with oils, like essential oils?

Does it now dissolve in alcohol?

Does it now dissolve in non-polar solvents as well, such as Di-ethyl ether?

Have you checked its sublimation temperature?

I have friends here who have made similar experiments and who sent me images which coincide with what you are describing, but I never did this one myself. The salt 'climbing' is interesting...

Philosophical
09-15-2016, 10:36 AM
I am reminded of St Dider, although this is only my impression from what you have shared.

http://i67.tinypic.com/2zgwy1t.jpg

They will see in the practice of the work 2 parabolic rivulets, who confounding [or mixing] themselves together, give Birth to the triangular stone

Lux Natura
09-16-2016, 07:14 PM
Lux ~

This new salt:

Does it mix with oils, like essential oils?

Does it now dissolve in alcohol?

Does it now dissolve in non-polar solvents as well, such as Di-ethyl ether?

Have you checked its sublimation temperature?

I have friends here who have made similar experiments and who sent me images which coincide with what you are describing, but I never did this one myself. The salt 'climbing' is interesting...

Does not mix with oil.

Does not mix with water.

Dissolves in my own homemade alcohol (85%), and when it dries, all the water is thrown out around the salt in a ring in small droplets.

Dissolves in non polar very easily.

I don't have the setup to test for sublimation, but a standard lighter flame (around 900C from online sources) does not sublimate it.

Makes me wonder... where is the salt climbing to? It can climb up, then down. Seem to just want to spread out actually. I wonder, given a large enough surface area, how long until it stops climbing away, and at that point what kind of changes will it undergo? I still think the climbing is related to it escaping from moisture.

Philosophical
09-17-2016, 12:02 PM
Hmm based on the above it seems as if it is not the salt I thought it was but interesting nonetheless (At least based on my understanding of the matter which is admittedly limited). Care to share a picture?

JDP
09-17-2016, 05:28 PM
I don't have the setup to test for sublimation, but a standard lighter flame (around 900C from online sources) does not sublimate it.

How about just improvising one? All you need is a small sample of the salt (say, a couple of grams) and then put it inside a large test tube, like say this one:

https://www.indigo.com/glassware/test_tubes/big-tube-glass-test-tubes-25x200mm-55910R.html#.V916QE0rK1s

Hold it with test tube tongs, like this:

http://images.slideplayer.com/28/9396311/slides/slide_16.jpg

Then just get a Bunsen burner (which I suppose you already have) or a propane torch and gradually heat the bottom while holding the test tube at an angle, like this (you might want to use a yellow flame first, then gradually move on to a blue flame by regulating the air-gas mix):

http://classes.kvcc.edu/chemistry100/Lab08/pictures/08.jpg

Since test tubes are cheap, you can afford to sacrifice them, so don't be afraid to make the bottom of the test tube red hot, to the point where the glass starts to deform from the intense heat. If there is any sublimable substance in your "salt" it should volatilize and partly condense on the upper parts of the test tube that are furthest away from the heated bottom.

Lux Natura
09-17-2016, 06:08 PM
Hmm based on the above it seems as if it is not the salt I thought it was but interesting nonetheless (At least based on my understanding of the matter which is admittedly limited). Care to share a picture?

Attaching pictures, but they are not showing up it seems?

http://i.imgur.com/IT7ZKOr.jpg That the crystal that originally crawled out of the soup. About 5mm by 10mm (1/4 inch x 1/2 inch). Flat top and bottom, with 60 and 120 degree angles. The corner i chipped off handing it and tasting it. You can see the stuff that is drying out from it (the white stuff bottom left, there is some more but the camera does not capture it). Under the microscope it is tiny needles or hairs for the stuff drying out. Might be a nitrated form due to the needles, but the taste is wrong for the nitrate. Tastes much more like the hydroxide version, but it's not a hydroxide either.

http://i.imgur.com/YhKkULp.jpg This is the stuff in the pyrex crawling out. I've set up so what crawl out of the top one is thrown back into the bottom one. These sat there for at least 2 months before the salt climbed far enough to get to the lip. This salt tastes actually pleasant and nothing like the crystal that crawled out of it initially. Might be a bicarbonate, but it tastes a bit sweet and round and muted actually. That wet spot on the wood to the bottom right is where the puddle first jumped to, and then went around the wood and dripped down on a container below that shelf, and in that is where the first crystal grew, but that all happened overnight.

Nitrate form and bicarbonate form makes sense, just based on what is in the atmosphere / contained in dew, but not according to checking out what those forms are supposed to look like and how they ought to behave and taste.

I still have all the oil saved, and im going to use that now, to further create another combination. Somehow the idea of only using what the salt captured and allow it to cycle some more makes sense to me. Maybe it can go into the oil, and something new will crawl out!

The dark color is actually from an accident I think. For the first 30 cycles it kept pure, but then somehow it turned dark. I think maybe some dirt got thrown into it? I cleaned it the best I could at the time, but it's still there.

Lux Natura
09-17-2016, 06:33 PM
JDP -

At some point around where the glass is maybe halfway to melting, lots of white smoke comes out - it shoots out of the test tube.

At the point where the glass is red hot and deforming, the salt has thrown off everything it can, and is brilliant white powder. On the inside walls of the vessel are two things: a clear liquid that looks exactly like water (but is obviously not, as the temperature is above 1000c), and a red oil. If I tip the test tube back up after removing the flame, the liquid runs down and you can hear the hiss as it meets the salt, but the oil sticks to the side.

After it has cooled, the water again leaves the salt and sits on the side of the test tube. The red oil turns to an orange waxy looking thing and it spreads out on the inner walls. The wax is very easy to remove.

Andro
09-17-2016, 07:49 PM
Attaching pictures, but they are not showing up it seems?

Lux,

The image URL you tried to post was not correct (it needs to end with an image suffix, such as 'jpg', 'png', 'bmp', 'gif'). Please go to your image link again, right-click on the image and select : 'Copy image location' or 'Copy image URL'. This way, you will receive an URL that ends with .jpg. This is the link that has to be used for the image to show. Also, please make you pics smaller and upload them again, because the current ones are huge for a forum... Also, please do not hesitate to contact us with any further logistical issues...

Lux Natura
09-17-2016, 07:58 PM
Thanks for the help Andro. Got them working!

z0 K
09-17-2016, 08:30 PM
JDP -

At some point around where the glass is maybe halfway to melting, lots of white smoke comes out - it shoots out of the test tube.

At the point where the glass is red hot and deforming, the salt has thrown off everything it can, and is brilliant white powder. On the inside walls of the vessel are two things: a clear liquid that looks exactly like water (but is obviously not, as the temperature is above 1000c), and a red oil. If I tip the test tube back up after removing the flame, the liquid runs down and you can hear the hiss as it meets the salt, but the oil sticks to the side.

After it has cooled, the water again leaves the salt and sits on the side of the test tube. The red oil turns to an orange waxy looking thing and it spreads out on the inner walls. The wax is very easy to remove.

From your description of the test tube firing I can see you have stumbled onto something interesting. If you have more of the material about 200mL volume or more I suggest you dry distill it to collect the sublimate and water and oil you observed in the test tube firing. The best way to go about that is to use a kiln with a horizontal port. Place your flask inside and attach a receiver on the outside. You will need to cool the receiver in ice.

Also from the photos you posted I can see the crystal material is growing from the mother liquor under it. This is a form a thin layer chromatography. It is possible that you have found another way to gather the philosophical principles necessary to make the Quintessence.

JDP
09-18-2016, 12:45 AM
JDP -

At some point around where the glass is maybe halfway to melting, lots of white smoke comes out - it shoots out of the test tube.

At the point where the glass is red hot and deforming, the salt has thrown off everything it can, and is brilliant white powder. On the inside walls of the vessel are two things: a clear liquid that looks exactly like water (but is obviously not, as the temperature is above 1000c), and a red oil. If I tip the test tube back up after removing the flame, the liquid runs down and you can hear the hiss as it meets the salt, but the oil sticks to the side.

After it has cooled, the water again leaves the salt and sits on the side of the test tube. The red oil turns to an orange waxy looking thing and it spreads out on the inner walls. The wax is very easy to remove.

Did any solid condense on the upper part of the test tube? In other words, did you get any sublimate? If not, then you might want to pursue further the investigation of what are the byproducts, as the previous poster suggests, by actually dry-distilling a larger sample of the salt to see if the volatile products can condense, perhaps into a liquid.

If you are going to use a kiln/furnace to heat larger glass vessels, though, take the precaution of coating them with a layer of refractory to prevent accidents that can happen when heating glass vessels too strongly. A very easy one is a mixture of either equal parts clay and sand, or 2 parts sand to 1 part clay (proportions depend on how "smooth" and "plastic" the clay you work with is), made into a somewhat sticky "dough" with water, and then you apply it on the glass flasks/cucurbits/bottles and let them dry for a couple of days before using. Should the heat be strong enough to cause the glass container to soften too much or even melt, this will create a refractory "shell" that will keep the glass "in" and not spill on the bottom of your kiln/furnace, thus making a mess of it. Like this:

https://distillatio.files.wordpress.com/2013/05/nitric-acid-making-cucurbit.jpg

See how the cucurbit that goes inside the kiln/furnace is coated by the layer of refractory paste, while the part that sticks out of the kiln/furnace does not need it and can be "as is". Then you hook up your condenser/s and receiver to the cucurbit/flask/bottle that is being heated.

Lux Natura
09-18-2016, 02:31 AM
JDP:

Thanks for the tips!

I will eventually look at larger scale dry distilling, but first I have a few more things I want to try with the salts that involve just ambient conditions. In my mind, once they have reached a point where changes stop occurring, then I will introduce things such as strong heat. Honestly at this point its just a matter of going by "feel". Like it's alive or something, and I don't want to subject it to conditions it cannot (yet) withstand.