Summary On First Liquid Stone Experiment

OK, I did this originally many months ago, then got caught up in things, and now it’s a lot later than I expected. That’s good in a way, as long term slow reactions have had time to operate, but bad in that I’ve not taken any measurements / observations in the middle.

As this was intended as a recreation of ‘my guess as what was likely to happen by accident’, it isn’t that big a deal in any case. It mostly just shows what is likely a bad way to do things, that might have stimulated the interest of some Egyptian Kid playing in the dross next to a shop and got somebody thinking about better ways.

Right now I’m packing things up (and have been for a couple of days) as I’m “between jobs” and that means I can’t carry the costs of a ‘bi-coastal’ lifestyle, so the Florida Rental has to go (end of the month I move in with a friend in their Florida house on a lake… so not exactly having a reduction in life style, just costs ;-)

At any rate, “the junk must go”, and part of it is this plate of samples that have been asking me to write a posting about them. Each is a paper cup with about 2 to 4 ounces (volume – heaping spoons, actually…) of stuff in them. Call it 125 cc or so. Some as low as 50 cc. They are all a light gray or white, so showing pictures of bland dirty white hockey pucks is unlikely to be informative. Instead, you will get a short description of what each was made from, and what it has become.

I will be saying one of the ingredients is Natron. It is commercial Sodium Carbonate (Arm and Hammer brand washing soda) but as natron was just natural Sodium Carbonate, I think that’s appropriate as it is close to the original material. I also found a source of “lime” that was a bit of a challenge. The garden shop stuff isn’t CaO, but a mix of some CaO and some Calcium Hydroxide (‘slaked lime’) as that is what was sold at the local stores. Most likely, fully “burnt lime” would be better, but as a first approximation of ‘lime on a crap pile’ having the mixed stuff is likely not too bad. But instead I used some more pure lime for this round. I found what looks to be real ‘burnt lime’ in the pickle and canning section of the grocery store as “Pickling Lime”, and that’s what I used for these small experiments. Clay was from a standard bag of clay based Cat Litter. Using specific kinds of clay would likely be better. Again, though, as a ‘quick test of stuff from a trash heap in old Egypt’, this is a reasonably common crummy clay. I also used some Diatomacious Earth (D.E. from here on out) as a silicon dioxide sample. I’d have rather used some quartz sand, but figured this was OK for a first look.

More detail on chemistry and methods than you might want from the original posting about this batch here:
https://chiefio.wordpress.com/2014/02/12/some-notes-on-geopolymer-cement-clay-bricks-unfired-and-diy/ Hard to believe it was a year ago, but it is.

All units are given in ratios. So, for a 1:1:2 lime:natron:clay you would use one “unit of volume of your choice” of the first two, and two such scoops of the last one. Eventually it would be better to use mass ratios, but I don’t have a scale right now. Typically I added just enough water to make a stiff paste, but some mixes had excess water and were a bit more soupy / slurry like (usually causes weaker cement). Once the basic evaluation is done, then a strength test (perhaps to destruction) by standing on each (about 2 inch) diameter puck will be done. Followed by a resistance to water test – i.e. does it crumble when soaked.

In no particular order, the mixes and my sensory evaluation:

1 Lime
1 Natron
2-3 Clay (by eye is not exact…)

Hard white lump. Surface rubs off as a white powder (might be excess alkali that turned to carbonate on the surface). Not a particularly dense stone, but usable (most likely for ‘light duty’). Does not fracture on light tapping on a hard surface. Broke in half when I stood on it, and then falls apart when placed in water. Broken face shows many clay inclusions of gray color. Clearly not enough alkali soaks into the clay grains to convert them outside the surface (so likely more clay dust and mixing would be better). When wet, the mass has a gray color like clay.

Enough to get the idea into someone’s head that “this stuff sets up”. Dumping some lime and natron on a natural clay surface or clay dust pile, that gets wet for just a while, would be enough to get someone started looking at ‘making stones’, even if fairly weak ones. From that, it’s time, experiment, and observation.

1 Clay
1 Natron
1 D.E.

Made a thin puck of about 2 cm height. On handling while still young, it broke into 1/2 and 2 x 1/4 chunks. Now, it is white and weak. Simple finger squeeze caused one of the 1/4 chunks to fly apart into crumbs. Not going to try the ‘stand on it’ test. While this clay was fully divided into more dust like particles, this mix has no strong alkali in it. Clearly neither clay nor D.E. binds much (at all?) in the weak base of Natron. You need more alkaline catalyst like lime or lye.

But even a negative result tells you things… Look to lye and lime (CaO) as the catalytic agents, or perhaps a bit of KOH from wood ashes.

90% Clay slurry
10% Natron / D.E. mix

This gives a puck that looks like it is mostly gray clay with a white layer on top (where the Natron collected as the water evaporated?). A fairly strong feeling puck (rather like an unfired brick) but friable to strong finger pressure. IMHO, just a clay brick with some D.E. scattered in it and some Natron floated to the top / mixed in. It simply turns to mush in water.

But this confirms that Natron alone is not enough, and that the ratio with clay is not having much effect between these two mixes. Clay makes nice bricks, but to harden it takes fire, or something stronger than natron.

1 Clay
1 Lime
1 D.E.

This was a small thin puck, made with excess water. It is a purer white, but very friable with low strength and crumbled getting it out of the cup and handling it. Lime is not enough to set up the D.E. into a solid. It does fall apart in water, but starts out so prone to crumble that it’s hard to say if the water makes it go much faster. Lime alone is not cutting it as a catalyst.

3 Clay
3 Shells (ground up sea shells for feeding birds)
1 D.E.
1 Natron
1 Lime

Makes an irregular puck. Surface prone to spalling and flaking, but some parts fairly hard. This was to test a low ‘catalyst’ level with lots of clay and carbonates. It might give the idea of a stone, but it is just not anywhere near a usable thing, really. I suspect that a very strong lye is needed to make silicates “go”, while the carbonates would work better as a classical Roman Cement kind of mixture. At any rate, a bit of natron and some lime on a pile of dirt (clay, limestone or shells midden, some D.E. or related sea muds) isn’t going to cut it. Though it might get someone started looking at the hard lumps and ‘trying stuff’.

It doesn’t turn to mush in water as fast as the others (I think the surface is a bit less permeable) but does soften and can be ‘mushed’ easily (showing a drier under layer). I could see folks making mud bricks finding that a bit of lime and sand might make them stronger and a bit more water resistant. A possible path for discovery to start.

Finally, the last one:

1 Lime
1 Natron
1-2 D.E.

Just checking to see if a large excess of ‘catalyst’ might make the silicon dioxide of D.E. do anything. This makes a very white, very solid puck, with a flake layer on the top (that tastes rather alkaline, and that when wet – flakes in hand not on the puck – didn’t break up easily but did feel ‘soapy’ so alkaline). About 1 inch thick. Once the top flakes are off, the puck itself is solid and not friable to the fingers.

Standing on it, the ‘rim’ where it was raised from wetting the paper cup, crumbled, but the puck itself held up. Some bits of the side surface show cracking. Water wetting gives a soapy feeling wash water, but the puck does not fall apart. It does weaken a bit, so I can crack off chunks with finger pressure ( I have strong hands, so YMMV). I’m doing a longer ‘soak test’ for longer term strength when wet.

My opinion of this is that there is significant excess natron / lime in the mix and that is what is washing out in the water, leaving voids and a weaker structure. The bulk of the D.E. has had some degree of ‘binding’ happen, but not enough for high strength. It would be quite reasonable to use silicon containing sands and a lower ratio of lime (perhaps with lye added or instead) and see if an approximation of sandstone could be made.

Clearly in a ‘strong enough’ alkaline environment, silicon dioxide can be made to have some degree of binding that would start one down the path to cements and liquid stones.

In Conclusion

A strong alkali or lye is needed, natron alone is not enough.

Silicon Dioxide and Clay both react to some degree in Lime solutions. Exploring lye, and lime / lye mixes (both quantities and ratios), ought to be fruitful. In particular, using ‘wood ash’ as a lye containing material that would be dumped in quantities near places making clay bricks and / or on silicon bearing sands would be an interesting area to explore.

Clay crumbles tend to remain clay crumbles if only lightly mixed in modest water level slurries. While this is ‘good enough’ to cause someone to notice an effect, it makes for a weak product, and would be a defect in any final method. D.E. is an easy to find silicon dioxide source for experiments, but each shell is a hollow thin thing. LOTS of surface area for surface chemistry to be demonstrated, but not very good for ‘strong bulk’. Using a good grade of sand would be the next step to take.

Excess natron and / or lime solution does not rapidly react away, and may weaken the final product. Exploration of the lower bound and upper bound effects would likely point to where the optimum can be found.

I expect that using Water Glass (Sodium silicate or metasilicate) with sand would work well, and be an easy bypass of the difficulty I’ve had getting lye. From the wiki:

They are used in cements, passive fire protection, textile and lumber processing, refractories, and automobiles. Sodium carbonate and silicon dioxide react when molten to form sodium silicate and carbon dioxide:

[…]

Water Glass[4] was defined in Von Wagner’s Manual of Chemical Technology (1892 translation) as any of the soluble alkaline silicates, first observed by Jean Baptist van Helmont circa 1640 as a fluid substance made by melting sand with excess alkali.[5][6] Glauber made what he termed “liquor silicum” in 1646 from potash and silica.[7] Johann Nepomuk von Fuchs, in 1818, obtained what is now known as water glass by treating silicic acid with an alkali, the result being soluble in water, “but not affected by atmospheric changes”.[8][9] Von Wagner distinguished soda, potash, double (soda and potash), and fixing (i.e., stabilizing) as types of water glass. The fixing type was “a mixture of silica well saturated with potash water glass and a sodium silicate” used to stabilize inorganic water color pigments on cement work for outdoor signs and murals.

So this is a reasonably well traveled path…

http://chemistry.about.com/od/makechemicalsyourself/a/make-sodium-silicate.htm

Prepare Sodium Silicate

Wear proper safety gear, which includes gloves.

Heat 4-8 grams of sodium hydroxide in 10 ml of water.

Once the sodium hydroxide is dissolved, slowly add the 6 grams of crushed silica gel beads. Heat the solution between additions. If the crushed beads won’t dissolve, add a little more water to the solution.

That’s it! You now have sodium silicate or water glass. NurdRage has a YouTube video of this procedure, if you’re interested in seeing how it’s done.

Silica gel being a synthetic form of silicon dioxide that is porous. But this shows that lye reacts with silicon dioxide to make sodium silicate. We can skip a long slow process with lye and sand in a bucket at warm Egyptian temps (but not heated on a burner…) but just mixing ‘water glass’ with sand and evaluating the product for strength and characteristics. If that works well enough, finding a path to that product via other forms of natural silicates and ‘Egyptian Desert Warm’ lye could be followed over a longer time.

It’s pretty clear that using water glass will work:

Concrete and general masonry treatment

Concrete treated with a sodium silicate solution helps to significantly reduce porosity in most masonry products such as concrete, stucco, plasters. A chemical reaction occurs with the excess Ca(OH)2 (portlandite) present in the concrete that permanently binds the silicates with the surface making them far more durable and water repellent. It is generally advised to apply this treatment only after the initial cure has taken place (7 days or so depending on conditions). These coatings are known as silicate mineral paint.
[…]
Refractory use

Water glass is a useful binder of solids, such as vermiculite and perlite. When blended with the aforementioned lightweight aggregates, water glass can be used to make hard, high-temperature insulation boards used for refractories, passive fire protection and high temperature insulations, such as moulded pipe insulation applications. When mixed with finely divided mineral powders, such as vermiculite dust (which is common scrap from the exfoliation process), one can produce high temperature adhesives. The intumescence disappears in the presence of finely divided mineral dust, whereby the waterglass becomes a mere matrix. Waterglass is inexpensive and abundantly available, which makes its use popular in many refractory applications.

which strongly implies that some kind of ‘in situ’ creation of sodium silicate from sand and lye in a mix of minerals ought to be usable for a kind of ‘liquid stone’ pathway.

And that concludes this round.

In large part just showing that the most likely path (using lye) is not the only path, but that the lime / natron pathways are at best weak, and show a direction, but not a method.

Going forward, trying water glass as a quick path to products, then working backward to ‘in situ’ sodium silicate formation / reaction is likely a good path of investigation.

Finding nice strong lye solutions available without a load of trouble is next on my list of ‘things to do’ on this topic (and thanks to all the folks who have given suggestions of where to find it…) but only just after I order a $20 jug of Water Glass from the hardware store (Lowe’s says they can order it).

Probably in another year ;-)

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About E.M.Smith

A technical managerial sort interested in things from Stonehenge to computer science. My present "hot buttons' are the mythology of Climate Change and ancient metrology; but things change...
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12 Responses to Summary On First Liquid Stone Experiment

  1. omanuel says:

    Thanks fur an intriguing report.

    I an on Orlando, FL. Are you nearby?

  2. Power Grab says:

    I wonder what would happen if you exposed it to microwaves? Some say that the Great Pyramid was an electrical generator, perhaps of microwaves? Is that too goofy?

    I keep thinking of fulgurites. Maybe the equivalent of lightning energy should be applied?

    Sorry if this isn’t helpful! :-P

  3. E.M.Smith says:

    @OManuel:

    For now, I’m in Orlando as well. At least until the end of the month. On the west side near highway 27 and I-4.

    @PowerGrab:

    Well, my first idea was to try to rediscover the path by which the idea of liquid stone might have been discovered / thought up. Second up would be “how to do it with more modern materials” like water glass. I suppose a reasonable 3rd would be “exotic tech” like EM fields applied to inorganic chemistry.. Don’t know how to couple it to quartz sand… but maybe an water solution of lye dampening sand would be a decent microwave sink and get some reactive lift out of it. Could be interesting in a Space Aliens History Channel kind of way ;-)

    Fulgurites? Thermally fused quartz sand via a lightning bolt? Um, I don’t have a lightning generator… maybe a Tesla coil… Tesla coil discharge into silicate with lye? What could possibly go wrong ;-)

    As to the Great Pyramid being a microwave generator: There’s so many things wrong with that… not the least of which is that the size of a radio resonator shrinks with the frequency, and a microwave is mighty small… So very large structures like the pyramids would be more resonant at extra long frequencies. Then there is that whole “made out of insulating rocks” problem… and the lack of a power supply… and…

    I’d be much more inclined to believe in a precursor 10,000 ybp civilization that made them (and the sphinx) reflective of the constellations in the sky, and using unknown construction methods (like, maybe, ‘liquid stone’) and that the early Egyptians just inherited them… Unfortunately for that thesis, we have written records via the Greeks of eye witness accounts of some pyramid being built using “machines” of some sort (likely a crane / lift device).

    Which reminds me, I need to make a posting about Atlantis and the Pillars of Hercules… so maybe we need to hold the ancient wacky ideas comments for that one… where a precursor civilization from long long ago might seem more mainstream ;-)

    But maybe just ONE more idea wouldn’t hurt ;-)

    There are wall markings showing what seems to be a light bulb powered by some kind of apparatus. There’s also an interesting potential for the Lighthouse at Alexandria. For the Lighthouse, the Egyptians did a lot with metals. Perhaps they discovered the ability of laminated different metals to make electricity when heated by a fire. Now the shape of the lighthouse makes sense, with loads of wood being burned in the base to make electricity and even a simple carbon arc lamp would work for the light.

    Back on the bulb… I could easily see a ‘Baghdad Battery’ type of prime energy source with a collection of cells powering a coil, the connections made via copper contactors on a large wooden wheel. Then as the wheel is turned, the coil gets energized, then has a collapse. As a Tesla like coil then makes a big zap through the bulb… With a very reasonable number of contactors on the wheel and a modest rotation rate, it would be very easy to get over a 50 Hz frequency and have little to no perceptible flicker. Only things needed are a wheel, a few ancient batteries of a sort that look to be known in ancient times, the ability to work copper and glass, and a discovery of what coils of wire do when currents start / cut off. At that point, maybe having a simple vacuum pump that can pull a small vacuum in a glass tube and trying various gasses (air, nitrogen via oxygen scavenge of air, CO2, whatever) to find an OK light after finding that air gives some light, if less than ideal. Heck, some of their primitive materials might even be a benefit as the contaminants might make the air mix glow enough to be useful.

    https://www.physicsforums.com/threads/the-color-of-plasma.461404/

    CF4: blue
    SF6: white blue
    SiF4: light blue
    SiCl4: light blue
    Cl2: whitish green
    CCl4: whitish green
    H2: pink
    O2: pale yellow
    N2: red to yellow
    Br2: reddish
    He: red to violet
    Ne: brick red
    Ar: dark red

    So even air ought to give a yellowish bit of red light… If they used salt in the tube, they could get a bright yellow from the sodium salt fairly easily. ( I used to paint my Jacob’s Ladder – coat hanger wire and a 15 kV neon sign transformer – with salt solution to make a very nice yellow arc of several inches in length, so the idea of making light via high volts in air is not all that far fetched. Pull a partial vacuum with pumps of tech no harder than available to ancients ( Greek Fire was pumped with wood / leather valve pumps ) and run a discharge through a glass tube with the walls ‘contaminated’ with salt water bits. Likely to make a light, IMHO, with out much trouble.

    Just need the HV… that can be made with the above wheel ‘chopper’ and a flyback winding.

    Just saying… nothing really all that hard about making such a device…

    (Even a tiny bit further on the far side… they might have used Mercury in the lamps… they had it: http://nature.berkeley.edu/classes/eps2/wisc/hg.html “Mercury was among the first metals known, and its compounds have been used throughout history. Archaeologists found mercury in an Egyptian tomb dating from 1500 BC.” so not that far fetched to think they might have used a bit of amalgamated metal for the electrode and found it started easier.)

    but that’s for another day and not really part of “Liquid Stone”…

  4. p.g.sharrow says:

    Wimshurst machine will generate plenty of juice for a discharge tube and well within the abilities of the Egyptians.
    http://en.wikipedia.org/wiki/Wimshurst_machine
    Hell! even you or I could make this work! ;-) pg

  5. Jason Calley says:

    Two comments: First, regarding the Egyptian synthetic stone, Michel Barsoum, a Professor of material Science, has done electronmicroscopy on pyramid samples and found that they incorporated DE. https://www.youtube.com/watch?v=EDHtQCYn7ZU Well worth watching his video. Somewhere around 45:00 he starts into some more detailed analysis, but I enjoyed his entire talk.

    Second, concerning the lighting system of the Pharos: A buddy of mine was reading a translation of a book written during (I think) the15th century by a German man who had been taken as a slave by the Islamic Caliphate. During part of his time in slavery he was in Cairo, and related a story he heard there concerning the Pharos. There was, many years previously, a large concave mirror at the top of the tower with a fire built in front of it. The mirror could reflect the light to sea in a powerful beam. More importantly, during the day, a man could stand at the focus of the mirror and see ships far at sea. That way, the rulers of Cairo were always warned in advance of any fleets approaching their city. The Christian nations of Europe wished to capture Cairo but were unable to do so unless the mirror was destroyed. The Pope gave special permission to a priest to publicly renounce Christianity and to move to Cairo and take up Islam. After many years the now-Islamic priest worked his way up in rank to become the Imam in charge of the Pharos. Christian Europe made ready to invade Cairo, and at the proper time, the priest destroyed the mirror, allowing the fleet to attack and capture the city with no prior warning.

    I do not remember the details about by whom or exactly when the book was written, but I can ask my friend if you want to know.

  6. omanuel says:

    E.M. Smith,

    Sorry I missed your reply. We left Orlando Wednesday morning, spent last night in Atlanta, GA (T = 14 F on Thursday morning) and am now back in Cape Girardeau where last night’s T = -17 F.

    When passing through TN today, I asked several times but everyone said they had not seen Al Gore.

    Sorry I missed the chance for a face-to-face meeting with you.

  7. E.M.Smith says:

    @OManuel:

    There will be other days…

    @All:

    Looking over the D.E. sample that was fairly solid, now that it has dried, it reminds me of a porous chalk. Looks like an easy way to make a silicious chalk, if desired. Likely also would be a fine filter medium, given that unreacted D.E. is, and this is a bit more dense.

  8. omanuel says:

    @ E.M. Smith

    Yes, Big Brother is going down hard (would be “biting the dust” but it’s covered with snow and ice). Perhaps a godsend to keep the champagne cold for the celebration!

  9. omanuel says:

    PS – One of the anti-nuclear energy sites posted this news about charges of corruption in a firm making Thoroum-based nuclear reactors:

    http://m.theglobeandmail.com/report-on-business/snc-lavalin-faces-rare-corporate-fraud-and-bribery-charges/article23108284/?service=mobile

  10. Gary says:

    I get my Lye and Potassium Hydroxide from Dudadiesel.com.
    They sell biodiesel supplies.
    Were the only ones that had a reasonable price, and delivery is quick.

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