Sciencemadness Discussion Board - Growing Crystals in Gels

Growing Crystals in Gels

MrHomeScientist - 23-7-2017 at 13:18

I found this really neat demonstration kit from Flinn - Growing Crystals in Gels - Chemical Demonstration Kit. In case the link ever gets broken, here's the text from that page:

Quote:

Grow your own spectacular display of long-lasting crystals in gels—using large-size demonstration bottles! Mix two solutions together to form a gel overnight. Add another solution to the hardened gel and watch amazing crystals begin to form before your eyes! Crystals become more and more beautiful over the next two or three weeks! Introduce your students to the phenomenon of crystal growing with this easy-to-prepare demonstration. Highly visible potassium hydrogen tartrate and lead iodide crystals are grown—making a perfect classroom display. Kit includes a detailed handout with easy-to-follow instructions.

Concepts: Crystal formation, solutions/solubility, ions.
Setup Time Required: 30 minutes total over two class periods
Materials Provided: Acetic acid solution, lead nitrate solution, potassium chloride solution, sodium silicate solution, tartaric acid solution, potassium iodide, and two crystal-growing bottles with caps.

Very cool idea, but it's rather expensive. Based on the materials list, I would surmise the procedure to be something like this:
1) Mix acetic acid and sodium silicate solutions together, and add either lead nitrate or tartaric acid solution.
2) Allow to set up overnight.
3) Add either potassium iodide solution or potassium chloride solution (for lead nitrate and tartaric acid, respectively) on top of the gel, and the crystals grow as the solution seeps down into it.

The problem then is to figure out amounts and concentrations. This would be something very cool to try if you've got the reagents and want to experiment!

j_sum1 - 23-7-2017 at 16:18

It sounds like a more controlled version of the chemical garden demonstration where various salts are dropped into a solution of sodium silicate.

I have not experimented at all with this. But I was at one stage considering electrolytically producing some tin crystals in a gel with the aim of having them more durable than they would otherwise be.

I would be interested in anyone who could give precise recipes for growing crystals in gels.

DraconicAcid - 23-7-2017 at 18:57

I have a book on the subject in my office- I'll get back to you. And it's not like the chemical garden. The silicates are neutralized to form the gel, so you get slow diffusion of cation and anion together to form the precipitate.

j_sum1 - 23-7-2017 at 19:12

Quote: Originally posted by DraconicAcid

I have a book on the subject in my office- I'll get back to you. And it's not like the chemical garden. The silicates are neutralized to form the gel, so you get slow diffusion of cation and anion together to form the precipitate.

I stand corrected.
Looking forward to some wisdom from that book.

pantone159 - 24-7-2017 at 07:11

The following is an excerpt from Chemical Demonstrations, A Handbook for Teachers of Chemistry, Bassam Z. Shakhashiri, Vol 3, 9.47, p372-377.
The source also has demonstrations including mercury crystals, which I did not copy here.

Sodium silicate solution, density c. 1.06 g/mL:
To prepare about 1 L of solution, dilute 160 mL of commercial 38-40% sodium silicate solution to 1.0 L with distilled water and stir the mixture.
Alternatively, dissolve 244 g of Na2SiO3-9H2O in 600 mL of distilled water, then dilute the resulting solution to 1 L.

Procedure A:
Preparation: Pour 15 mL of 1M acetic acid into a 50-mL beaker. Wearing gloves, add 2 mL of 1M lead acetate and stir the mixture.
While stirring the mixture vigorously, slowly pour 15 mL of the sodium silicate solution into the beaker. The mixture must be stirred continuously
while the silicate is added, because if any region of the mixture becomes basic, the lead will precipitate. Pour the mixture into a test tube,
and place in a rack until a gel forms (5-30 minutes).
Presentation: Pour 2 mL of 2M KI solution onto the top of the gel and stopper the tube. Place the tube where it can be observed undisturbed over
a period of several days. Compact yellow crystals of lead iodide will form, growing from the top of the gel toward the bottom.

Procedure B:
Preparation: Pour 15 mL of 1M acetic acid into a 50-mL beaker. Add 2 mL of 2M potassium iodide and stir the mixture.
While stirring the mixture vigorously, slowly pour 15 mL of the sodium silicate solution into the beaker.
Pour the mixture into a test tube, and place in a rack until a gel forms (5-30 minutes).
Presentation: Wearing gloves, pour 2 mL of 1M lead acetate solution onto the top of the gel and stopper the tube.
Place the tube where it can be observed undisturbed over a period of several days.
Yellow fern-like crystals of lead iodide will form in the gel, starting at the top and spreading toward the bottom.

Procedure E:
Preparation: Pour 15 mL of 1.5M tartaric acid into a 50-mL beaker.
While stirring the mixture vigorously, slowly pour 15 mL of the sodium silicate solution into the beaker.
Pour the mixture into a test tube, stopper the tube, and place in a rack until a gel forms (up to several days).
Presentation: Pour 2 mL of 1M CuSO4, 1M KCl, or 1M KNO3 solution onto the top of the gel and stopper the tube.
Place the tube where it can be observed undisturbed over a period of several days.
Crystals of either Cu tartrate or K tartrate will start at the top of the gel and grow downward.

[Edited on 24-7-2017 by pantone159]

tsathoggua1 - 24-7-2017 at 09:41

Mercury crystals? presumably its still a liquid in the gel, or a Hg salt, no?

I'd be interested to see pics if it really is Hg(0) stabilized in solid form in a gel matrix though.

And as for acidifying silicate solutions, its not a bad way to prepare silicon. Adding concentrated sulfuric acid to potassium silicate solution (again concentrated, not sure just how concentrated it is, since its a commercial product bought a long time back) to precipitate very very fine silica, then washing out the potassium sulfate, each time decanting through filter paper after adding much cold H2O, allowing to stand until it settles (its very, very fine) so takes a fair while, and removing the potassium sulfate. Once this is done, using Mg to reduce the precipitated silica in a magnesiothermic or better, aluminothermic reduction. Al is IMO better since then one can test for the presence of Al residues by treatment with strong aqueous NaOH or KOH. Tsath' did this, and he does need to refine the procedure in order to catch any vaporized material, he lost much of it the last time he tried, using Al and carbon crucibles. Need something to direct and catch the vapors. But he did end up with 3 little nuggets of what can only be silicon 'metal', silvery, hard, very very light and does not respond to concentrated sodium hydroxide or caustic potash solution in the slightest. The only other elements that could have been present are hydrogen, oxygen, aluminium, the carbon of the crucibles or sulfur if residual acid or sulfate were present, as well as potassium, and it quite definitely is none of these. Ergo it must be silicon.

MrHomeScientist - 24-7-2017 at 10:48

Thanks for that, pantone159! I'll have to look into trying this when I get back from some work trips.

DraconicAcid - 24-7-2017 at 13:12

Quote: Originally posted by tsathoggua1

Mercury crystals? presumably its still a liquid in the gel, or a Hg salt, no?

Mercury(II) iodide and mercury(II) oxychloride.

pantone159 - 24-7-2017 at 14:18

Quote: Originally posted by DraconicAcid

Quote: Originally posted by tsathoggua1

Mercury crystals? presumably its still a liquid in the gel, or a Hg salt, no?

Mercury(II) iodide and mercury(II) oxychloride.

Yes, these Hg(II) compounds, not Hg metal.

DraconicAcid - 24-7-2017 at 15:13

I just set up a gel with tatrate, and will add some copper(II) sulphate solution to it once it has set, in accordance with the prophesy. I'll let you know how it works.

DraconicAcid - 24-8-2017 at 08:32

Hmmmm...I got some very pale crystals in a blue solution (the gel melted over the summer

ETA: The gel didn't melt, there was just some supernatant over top of the gel. Nice little blue crystals, a lot like copper(II) sulphate. Tough to separate them from the gel, though.

[Edited on 24-8-2017 by DraconicAcid]

DraconicAcid - 25-8-2017 at 10:11

Quote: Originally posted by DraconicAcid

Hmmmm...I got some very pale crystals in a blue solution (the gel melted over the summer

ETA: The gel didn't melt, there was just some supernatant over top of the gel. Nice little blue crystals, a lot like copper(II) sulphate. Tough to separate them from the gel, though.

[Edited on 24-8-2017 by DraconicAcid]

I did get them separated, and put them in the oven at a mere 40 oC to dry. Now they are *very* pale blue- presumably dehydrated. Hmmm. Merck doesn't say anything about copper(II) tartrate forming a hydrate. CRC says it's a trihydrate, but doesn't give a dehydration temp.

MrHomeScientist - 25-8-2017 at 13:10

Neat! Very interesting results. I don't have any tartaric acid, so I was looking into a way to make it from cream of tartar. This thread has a few options: http://www.sciencemadness.org/talk/viewthread.php?tid=21987

DraconicAcid - 25-8-2017 at 13:44

Apparently, tartaric acid is readily available: https://www.walmart.com/ip/Tartaric-Acid-1lb/190132556 I'm also going to try it with glycinate.

mayko - 2-9-2017 at 20:45

One thing this reminds me of is a series of kits that used to be available; they were each a big glass vial which you'd set a gel in and a chemical reaction would take place. One of them was a typical Liesegang ring pattern that developed; I think it was called Flying Saucer Invasion or something. There were others that had starburst or aurora patterns. I think they were available from Edmund Scientific but I've been unable to track them down.

Here's a few of my earlier experiments with Liesegang rings:
https://www.sciencemadness.org/whisper/viewthread.php?tid=26...

This thread got me motivated to test something that I'd been wondering about, which is what happened if a metal-rich gel was subjected to electrolysis. I made a strong gelatin and copper sulfate solution and let it set; then I cut out a cube and left it on a strip of steel as an anode and a wire as a cathode. I used a wall wart for a power supply.
Start:

IMG_20170826_223643588-electrolysisStart.jpg - 127kB

End:

IMG_20170831_210456347-electroylsisEnd.jpg - 1.5MB

I had some trouble with dehydration, but I was definitely able to get a copper aggregate from the gel, though it seemed to take a lot longer than the control aggregate I grew in ungelled water of the same copper concentration, with the same power supply (days vs. hours for a deposit of comparable size). Another thing that struck me was that the gel-grown aggregate appeared to have a less branched, more cauliflower-like shape than the free-grown aggregate. I don't know if this is because of hindered diffusion, or pressure from the constrictive gel.

Left, Copper aggregate grown in ungelled solution. Right, microscopic closeup

IMG_20170826_222058203-controlDLA.jpg - 608kB

2017-08-27-202210-controlDLA_closeup.jpg - 16kB

Left, Copper aggregate embedded in a gelatin matrix. The ion gradient and an opaque band of solid speckles are also visible. Right, microscopic closeup.

IMG_20170902_201429923-crossSection1.jpg - 365kB

2017-09-02-202631-closeupGelDLA.jpg - 24kB

The gel also develops a distinct gradient of color, where iron cations from the steel anode have migrated into the matrix. More subtle, but also interesting, is the collection of solid speckles in the border between the oxidizing/iron and reducing/copper regions of the gel. These didn't form at all in the leftover gel in the fridge; it's possible that they're the result of dehydration, but their placement is suggestive of some sort of boundary phenomenon.

A thin slice displaying the ionic gradient, as well as speckles:

IMG_20170902_201030403-crossSection2.jpg - 953kB

Gel, chunked by section: oxidizing/iron, boundary/speckles, reducing/copper, left-right.

IMG_20170902_201534928-byRegion.jpg - 458kB

Speckles, microphotograph:

2017-09-02-201948-closeupSpekles.jpg - 15kB

The Volatile Chemist - 3-9-2017 at 15:13

Quote: Originally posted by DraconicAcid

I've done this prep as well. Unfortunately, the same thing happened to my, they dehydrated. I also recall that their crystal structure was rather prismatic (I don't know my crystal structure names well). Also, the prep I used (admittedly an AP Chem prep) stated the product was Copper(II) Hydrogen Tartrate (H₂CuTar₂, which would make more sense considering how copper usually coordinates with the tartrate ion (see wikipedia for Fehling's) but sounds a bit simplified)

DraconicAcid - 3-9-2017 at 15:28

I tried setting up gels for with benzoic acid, aspirin, and oxalic acid, but I thik i may have messed up the pH, as they didn't gel properly.

lab-equip - 4-9-2017 at 03:22

Cool stuff!

mayko - 10-9-2017 at 13:40

Quote: Originally posted by mayko

One thing this reminds me of is a series of kits that used to be available; they were each a big glass vial which you'd set a gel in and a chemical reaction would take place. One of them was a typical Liesegang ring pattern that developed; I think it was called Flying Saucer Invasion or something. There were others that had starburst or aurora patterns. I think they were available from Edmund Scientific but I've been unable to track them down.

From what I remember, the Flying Saucer Invasion looked a lot like this one, between copper sulfate and potassium chromate in silica:
https://www.physionet.org/tutorials/epn/html/chp62exp1.htm

I wondered if the products I was thinking of had been pulled for hexavalent chromium toxicity, but it looks like it's included in this kit, (not available to the public at large though):
https://www.flinnsci.com/growing-crystals-in-gels---advanced...

In the course of looking for this I found this book, which turned out to be a pretty interesting, with lots of nice pictures (generally a pretty quick read, though I'm going to have to sit down and look at some of the modelling):
https://www.amazon.com/Crystals-Liesegang-Rings-Heinz-Henisc...

Ch. 1: History & Nature of the Gel Method
Attachment: History_and_nature_of_the_gel_method.pdf (7.6MB)
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One neat thing mentioned here is the growth of crystals from a solution of a complex, diffusing and decomplexing.

Quote:

In the procedures described thus far, the gel is used as the reaction medium, in which the desired material is chemically formed. In a variant of the method (...) for the growth of cuprous chloride crystals, the material is first complexed by means of another reagent (hydrochloric acid), and then allowed to diffuse into a gel free of 'active' reagents. Decomplexing sets in with increasing dilution and leads to the high supersaturations necessary for crystal growth. Cuprous chloride is interesting as a possible laser modulator, in which modulation can be achieved by a transverse electrooptic effect (...) the initial experiments described by Armington and co-workers (1967a, b) were carried out in 2 cm diameter test tubes containing pH 5 hydrochloric acid gels, with 5 ml of supernatant solution of varying acidity, saturated with cuprous chloride. Tetrahedral crystals of 3 mm size grew within about three weeks.

Silver iodide crystal growth is also mentioned, from diffusion of the complex with potassium iodide.

Quote:

There is evidence that the crystals grown in gels can be consider-
ably purer than the reagents used would lead one to expect (...) However general purification rules have not yet been established and, perplexing as it may seem, some enrichment effects are also known (...) Of the crystals doped with the above elements, only those containing Mn were found to be photoluminescent (orange) and cathodoluminescent (red).

Ch. 2: "Gel Structure and Properties"
Attachment: Gel_structure_and_properties.pdf (1.8MB)
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Ch. 3: "Growth Mechanisms"

Quote:

The softness of the gel and, presumably, the uniform nature of the forces which it exerts upon the growing crystal make it possible to overdope specimens until they are metastable as a result of severe internal strain. This can be demonstrated (Dennis, 1967), for instance, by adding a nickel salt to a calcium tartrate growth system. Nickel is accommodated in the crystals, which become green as a result but remain perfectly clear. When the amount of nickel exceeds a certain level, the crystal 'explodes' on contact, audibly if not violently. Nickel contents of the order of 1 % produce this effect

There's also this mention of pressure and solid growth in gel:

Quote:

For the measurement of crystallization pressures, Khaimov-Markov (1958) devised a method of disarming simplicity, as shown by the insert in Fig. 3.2.1. Seed crystals of aluminium potassium alum were placed on the top of a gel, with one of the crystal faces in contact with the gel surface. The gel itself was supersaturated with solute, and as the crystal grew it was lifted up, eventually to a height of several millimetres. By placing weights on the crystal, the lift could be suppressed, as shown by the graph in Fig. 3.2.\{a). In this way, and by monitoring crystal size, the pressure (i.e. the thrust per unit area) could be simply determined. This pressure, in turn, was found to be a simple function of the super- saturation (Fig. 3.2.l(b)).

Ch. 4: "Nucleation"
Attachment: Nucleation.pdf (4.5MB)
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Ch. 5: "Liesegang Rings"
Attachment: Liesegang_Rings.pdf (7.2MB)
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Quote: Originally posted by pantone159

Quote: Originally posted by DraconicAcid

Quote: Originally posted by tsathoggua1

Mercury crystals? presumably its still a liquid in the gel, or a Hg salt, no?

Mercury(II) iodide and mercury(II) oxychloride.

Yes, these Hg(II) compounds, not Hg metal.

Metallic mercury bands are apparently feasible; I wonder what they look like?

Quote:

Among the most exotic structures reported are (...) bands of metallic mercury, made by diffusing mercurous nitrate into an agar gel containing sodium formate (Davies, 1917),

There's also this mention of spiralling patterns; emergent spirals like this occur in other reaction-diffusion systems, like the B-Z reaction, though that might not be what's happening here.

Quote:

Liesegang (1939) subjected the Rothmund pictures to more detailed scrutiny, and found that they did not show circles at all, but concentric spirals

Also, light apparently has in impact upon development:

Quote:

Hatschek (1921) discovered the light effect acciden- tally, and reported that the ring spacings in his lead chromate systems were different for formation in darkness and under light. (...)Kiister (1913) worked on silver chromate deposition and obtained no
ring formation in his systems while these were kept in darkness, but prominent rings upon 'rhythmic' (i.e. intermittent, but otherwise unspecified) illumination. Dhar and Chatterji (1934) did obtain rings in darkness, but found their number increased by light, and the spacing between them diminished. Both Roy (1931) and Kisch (1933) reported that their rings were more distinct when formed 'under light' than in darkness.

/etc/

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The B. Vonnegut listed is Bernard, brother of Kurt :cool:

DraconicAcid - 28-9-2017 at 10:58

So I'm getting little crystals of copper(II) benzoate, and the copper-oxalic acid mixture is giving interesting results. I believe I've got light blue powdery bits of copper(II) oxalate, and needle-type crystals of darker blue sodium dioxalatocuprate.

[Edited on 28-9-2017 by DraconicAcid]

CuOxXtalSm.jpg - 21kB

DraconicAcid - 5-10-2017 at 08:48

My second try with copper acetate and aspirin in a gel is giving just a green solution, with no precipitate. Anthranilic acid is giving powdery copper(II) anthranilate, so I may try that again with lower concentrations.

mayko - 23-11-2017 at 22:25

I tried some copper-gelatin with oxalic acid solution but there just quickly formed a lot of powdery blue precipitate at the interface

One cool thing about the copper-gelatin is how reactive it is towards other metals. It will easily chew a hole through aluminum foil, and seems to be limited by dehydration as much as anything.

Here's what it did to a chunk of bulk aluminum:

This reaction creates dendritic copper metal better than any of the electrolysis attempts.

Even a single layer of aluminum foil will embed significant deposits in the gel matrix:

2017-11-16-231844_dendriteSmol.jpg - 19kB

elementcollector1 - 24-11-2017 at 15:12

Well, now you've got me curious. Would there be any benefits to reducing metals in a gel medium as opposed to an aqueous one? I'd imagine diffusion would be much slower, allowing for more solid deposits (an explanation for why those 'trees' are so well-formed, maybe?), but I'm wondering if other metals might be grown similarly, maybe even ones that ordinarily wouldn't grow well in water. I just bought some gelatin, so I'm about to try with copper sulfate and an aluminum alloy plate.

DraconicAcid - 24-11-2017 at 16:52

I think the only benefit is that the mass of crystals is less likely to fall off the cathode.

MrHomeScientist - 27-11-2017 at 07:07

This is awesome work. Glad to see so much experimentation being done!

The copper dendrites in gel are particularly cool. So you made your copper gel (mixing gelatin into concentrated copper sulfate solution?) and just laid it on top of aluminum foil? That's really interesting; I wonder how it eats through the oxide layer? Normally you need chloride ions for that.
Have you tried any other metal solutions? I'd really like to try this with things like nickel, lead, tin, etc. Those dendrites would make a cool element sample.

elementcollector1 - 29-11-2017 at 10:48

Concentrated solution doesn't seem to work for me - the gelatin is refusing to solidify upon being chilled. Not sure if I'm following the right recipe - 50 mL cold liquid, add 1/4 oz. of Knox gelatin, add 50 mL of boiling water and stir until homogenous are the instructions I found.

mayko - 29-11-2017 at 15:49

Quote: Originally posted by elementcollector1

I'd imagine diffusion would be much slower, allowing for more solid deposits (an explanation for why those 'trees' are so well-formed, maybe?)

Quote: Originally posted by DraconicAcid

I think the only benefit is that the mass of crystals is less likely to fall off the cathode.

These are both probably factors, though I can't guess their relative importance. When I've seen copper displace out of low-viscosity solution, it's generally been in bumpy sheets, which would make intuitive sense in a fast-diffusion regime, whereas diffusion-limiting conditions tend to cause branching growths. There's another characteristic parameter, the sticking coefficient, which measures the rate at which new branches sprout; the gel might change that, though it's not obvious how.
https://en.wikipedia.org/wiki/Diffusion-limited_aggregation

Quote: Originally posted by MrHomeScientist

So you made your copper gel (mixing gelatin into concentrated copper sulfate solution?) and just laid it on top of aluminum foil? That's really interesting; I wonder how it eats through the oxide layer? Normally you need chloride ions for that.

That's an interesting point; I put a few crystals of copper sulfate on a piece of foil with a bit of water and left it until it evaporated to confirm that there was no corrosion. The package lists only gelatin in the ingredients and the nutritional information lists 0 mg sodium, so if there's any salt it's in trace amounts.

Quote:

Have you tried any other metal solutions?

Not yet!

Quote: Originally posted by elementcollector1

Concentrated solution doesn't seem to work for me - the gelatin is refusing to solidify upon being chilled. Not sure if I'm following the right recipe - 50 mL cold liquid, add 1/4 oz. of Knox gelatin, add 50 mL of boiling water and stir until homogenous are the instructions I found.

I used half as much water as the recipe called for; the gel is firmer and easier to manipulate.

NEMO-Chemistry - 7-12-2017 at 20:05

I am looking into Cobalt Iodate using a gel. the paper i am using is this one

Attachment: bjp2014_4_315-320.pdf (504kB)
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gatosgr - 22-12-2017 at 17:26

I have grown large urea crystals in glycerin, the molar ratio was 2:1 urea:glycerol or something.

MrHomeScientist - 28-12-2017 at 17:50

I got around to giving mayko's experiment a try, and I got a very nice copper sulfate gel that's currently sitting on some folded Al foil to try to grow some Cu dendrites.

I pretty much followed the instructions on the gelatin packet: I started with 50mL copper sulfate solution of unknown concentration (it's old; I don't remember!) and added 1 packet of Knox gelatin. To this I mixed in 40mL of boiling water, and stirred to dissolve. After letting it set in the fridge for 3 hours I had a nicely formed beautiful light blue gel.

I extracted this from the beaker and cut the foam off the top to get a disc. I then folded up a piece of Al foil (about 4 layers) and set the gel on top of it, covered with an evaporating dish so it didn't dehydrate.

After letting it sit for a day, there are tiny bits of copper growing up into the gel.

The copper developed pretty quickly in just a few hours, and has stayed the same all day. It has not yet eaten all the way through the foil, though.
Mayko, about how long did it take yours to form those nice, large dendrites?

I'll start up another one this weekend using a large brick of soda can aluminum I melted down a while ago and see if that does any better. Fun stuff!

MrHomeScientist - 1-1-2018 at 19:47

About 5 days on, the copper dendrites are growing nicely! The gel has also darkened and shrank somewhat; possibly due to ion infiltration and dehydration, respectively. Still hasn't penetrated all the way through the foil though!

happyfooddance - 2-1-2018 at 14:30

That is so cool! I can't wait to see how they develop... Pretty impressive for only five days of growth!

elementcollector1 - 2-1-2018 at 21:34

Do you think they're solidly built, or brittle and prone to fracturing easily?

MrHomeScientist - 3-1-2018 at 13:08

I guess we'll find out...
They look decent enough, but they are small and feathery so who knows. My plan was to dissolve the gel in hot water to free the dendrites, to hopefully avoid any mechanical damage.

Bezaleel - 8-1-2018 at 09:46

Quote: Originally posted by NEMO-Chemistry

I am looking into Cobalt Iodate using a gel. the paper i am using is this one

NEMO, did you obtain any results?

I read the paper you attached, but I am quite underwhelmed by their experimental method. Actually, I doubt whether they have made any good use of the gel they created. The crystals they made all grew on top of the gel in their test tubes, where it seems (judging picture 1 in the article) that merely the cobalt diffused into the potassium iodate solution on top of it, instead of the other way around.

It seems to me that the authors did not have any proper nucleation control, as explained of page 370 vv. in this review article. Thus they got many crystals grown together. I think that addition of a layer of neutral 'reaction gel' layer would have much helped them.

Another article of interest can be found here.

MrHomeScientist - 14-1-2018 at 20:17

Here's a picture taken on the 7th, 11 days into the experiment. I used the flash, and you can really see the details on the dendrites.

And here's one from today, 18 days after starting.

It's interesting how the color of the gel has changed over time, from light blue to green to brown.
Today I decided to stop the experiment, and removed it from the Al foil and cut it into quarters. I placed one of these pieces in a beaker and poured boiling water over top of it, to try to dissolve the gel and keep the copper crystals intact. Unfortunately, they all pretty much crumbled to powder.

A few harder chunks stayed together, but they don't look crystalline at all. I still have the other 3 sections if anyone has any other ideas on how to extract the crystals.

It never made it all the way through the Al foil, but here's what it did to it.

NEMO-Chemistry - 16-1-2018 at 04:13

The only thing I can think off is not what you want, removing any gel will remove support of the crystal and land you a mess, the only method i can think of is to use another gel.

For example alginate, if you make it with a fair amount of starch its pretty firm, then once its formed the crystals you could soak in a chloride solution. That would make a really hard outer, the trick would be to use just enough to cover crystals.

With enough playing you might get close to what you want, but i think the gel will always need to be in place. I have seen a method for water glass crystal gardens, i cant remember a thing about it, except it was a way to remove the water glass solution and keep the garden structure of crystal.

So maybe a little research in that direction might help.

MrHomeScientist - 17-1-2018 at 05:03

This thing is a real pain in the ass to clean up, too. After dissolving the gel in water, I added baking soda to precipitate the copper. The solution clouded up, but NOTHING settled out and it is now unfilterable. Several days of sitting shows a tiny bit settled to the bottom but I don't think it will ever clear up completely. Not quite sure how to dispose of this.

NEMO-Chemistry - 17-1-2018 at 11:19

You got a centrifuge? Or a pillar drill (same thing

), that might settle it into a pellet.

mayko - 17-1-2018 at 11:33

I tried to dissolve away the gel by keeping it submerged and changing the water daily. This seemed to remove the copper but didn't disrupt the gel very much. I wondered if some sort of digestive enzyme (fresh pineapple juice?) could work, but a mold issue set in before I could test it.

DraconicAcid - 8-3-2018 at 13:52

Copper(II) aspirinate doesn't work for me in this method. The copper oxalate that I set up has changed completely to crystals of Na2[Cu(ox)2] (of whatever hydration).

I did set up some tubes with a gel packed with ammonium (di)hydrogen phosphate as a buffer- it gelled within an hour. Layering this with various salts seems to be giving lots of needly crystals of NH4MgPO4 and NH4NiPO4, but the copper and cobalt solutions have just given a solid skin of precipitate between the two layers.

Details- 6 mL of 85% phosphoric acid was diluted with 20 mL of water. 9 mL conc. ammonia was carefully added, and the solution diluted to 60 mL.

5 mL of commercial water glass solution was diluted to 60 mL, then mixed vigorously with the first solution. This was poured into four portions in large test tubes. After the solution had gelled, a layer of ~0.5 mol/L magnesium sulphate/copper(II) acetate/nickel sulphate/cobalt sulphate was carefully layered on top.

DraconicAcid - 20-3-2018 at 15:49

This is the result of diffusing magnesium, nickel, and cobalt into gels of silica/ammonium phosphate.

NH4MgPO4 and NH4NiPO4 seem to give feathery crystals; the cobalt just gives a solid film between the layers.

I'll have to try it again with a much lower concentration of phosphate, or possibly just more acidic (the copper and cobalt may be giving a precipitate of silicate rather than the desired ammonium metal phosphate).
[Edited on 20-3-2018 by DraconicAcid]

[Edited on 21-3-2018 by DraconicAcid]

mayko - 15-11-2018 at 21:25

Lead chemistry has never been interesting enough for me to make the toxicity worthwhile, but that might have just changed:

Quote:

This paper reports on an unusual crystal–crystal transformation phenomenon, which we have called the Morse Code Effect, based on the change in appearance of lead(II) oxalate crystals grown in agarose gels. [...] the needle form crystals extended through the lower gel in an unusual manner, showing apparent discontinuous growth. Needle growth appeared to be interrupted at intervals along the needle axes by small spaces containing one or more poly- hedra which were not, however, joined to the needles. In some cases this gave rise to the ‘‘Morse Code” pattern: the dots are the polyhedra, and the dashes the needles

Lisgarten, J. N., & Marks, J. A. (2018). The Morse code effect: A crystal–crystal transformation observed in gel-grown lead (II) oxalate crystals. Journal of Crystal Growth, 490, 35–40. http://doi.org/10.1016/j.jcrysgro.2018.01.004

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