Sciencemadness Discussion Board

Chemicals for crystal growing

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The Volatile Chemist - 27-2-2016 at 10:15

Quote: Originally posted by Bezaleel  

@Volatile Chemist: I keep wondering about your procedure for crystal growing in silicic acid gel. You say that you combine silicic acid with dilute acetic acid, but silicic acid is a hard substance. Thus it seems like you combined sodium silicate solution (waterglass) with acetic acid and lead acetate solution. But if that is so, then why is there no lead silicate being formed? Or is there, and is metathesis with KI what happens next?

I'm sorry. I didn't actually do the lab in my own lab, but in my AP Chemistry course. yes, it was waterglass we used, and I haven't a clue why the lead silicate isn't formed. Waterglass and silicates in general are rather strange.

crystal grower - 3-3-2016 at 07:42

Have anyone tried growing crystals of tellurium?
If yes could you post the procedure (I assume they are being grown from melt)
and eventually some pics please?
Thanks.

JJay - 4-3-2016 at 07:21

I did some further research on Mrs. Stewart's bluing, and it appears that it contains Pussian blue, oxalic acid, and ammonia. I am going to attempt to produce potassium cyanide from it, but I'll discuss that further elsewhere as to not hijack this thread.

Dmishin - 8-3-2016 at 12:50

Quote: Originally posted by Bezaleel  
That's peculiar as you get a lovely hexagonal bipyramid. Wish I had obtained a seed crystal like that! Did this just form in your solution? I only got tabular crystals from K2SO4.

Yes, I took small seed crystal of such form, and it just grew bigger. I also get tabular and stick crystals sometimes, but bipyramidal are more usual.

Actually, that's an interesting question, how K2SO4 can form a crystal with hexagonal symmetry. Wikipedia says that it has orthorombic crystal system, so order-6 symmetry should not be present. However, I remember reading somewhere that this compound is prone to forming cyclic twins, so probably, my bi-pyramid is not a single crystal, but 3 twinned crystals.

By the way, here is another compound that crystallizes really well: glutamic acid hydrochloride. I measured solubility to be around 50g/100ml. Finally, I have found some application for the sodium glutamate from the Chinese species shop.

DSC01775.JPG - 492kB

Bezaleel - 11-3-2016 at 03:42

Quote: Originally posted by crystal grower  
Have anyone tried growing crystals of tellurium?
If yes could you post the procedure (I assume they are being grown from melt)
and eventually some pics please?
Thanks.

Take care not to breathe the Te vapors. Search on "telllurium breath" for more info. User and moderator Woelen once named tellurium a "socially problematic substance" IIRC.

Quote: Originally posted by Dmishin  
Quote: Originally posted by Bezaleel  
That's peculiar as you get a lovely hexagonal bipyramid. Wish I had obtained a seed crystal like that! Did this just form in your solution? I only got tabular crystals from K2SO4.

Yes, I took small seed crystal of such form, and it just grew bigger. I also get tabular and stick crystals sometimes, but bipyramidal are more usual.
Actually, that's an interesting question, how K2SO4 can form a crystal with hexagonal symmetry. Wikipedia says that it has orthorombic crystal system, so order-6 symmetry should not be present. However, I remember reading somewhere that this compound is prone to forming cyclic twins, so probably, my bi-pyramid is not a single crystal, but 3 twinned crystals.
Peculiar, I only got the tabular ones. I'll try again. Did you cool quickly or slowly for the seed crystals?
Quote: Originally posted by Dmishin  
By the way, here is another compound that crystallizes really well: glutamic acid hydrochloride. I measured solubility to be around 50g/100ml. Finally, I have found some application for the sodium glutamate from the Chinese species shop.
Looks great! How did you separate the sodium chloride from your sodium glutamate? Does it just crystallise out first, leaving the glutamic acid in solution if the pH is low enough?

[Edited on 11-3-2016 by Bezaleel]

crystal grower - 11-3-2016 at 05:10

Iodine

P3112756.JPG - 1.2MB

Dmishin - 12-3-2016 at 07:36

Quote: Originally posted by Bezaleel  

How did you separate the sodium chloride from your sodium glutamate? Does it just crystallise out first, leaving the glutamic acid in solution if the pH is low enough?
[Edited on 11-3-2016 by Bezaleel]

Opposite of this. Glutamic acid has relatively low solubility (0.8g/100ml). I precipitated it with stoichiometric amount of sulfuric acid (cheapest acid I have), washed with cold water and then dissolved in HCl. Need to say that precipitate is rather bulky and washing is not easy.
If sulfuric acid is taken in excess, it dissolves glutamic acid again, probably giving its sulfate, which does not crystallize well (very soluble, forms syrup-like solution).

Velzee - 14-3-2016 at 15:31

Quote: Originally posted by crystal grower  
Quote: Originally posted by Velzee  
Chevreul's salt, anyone? xD
By the way; those are some beautiful photos!

[Edited on 1/10/2016 by Velzee]

[Edited on 1/10/2016 by Velzee]

Chevreul's salt is almost top secret :D u cant even find it on wikipedia.
I'd like to growCu3(SO3)2 crystals too but i dont have sodium metabisulfite to prepare chevrls salt.
Do you know where could I buy it ??


Oops! I forgot.
This is where I bought my sodium metabisulfite.

[Edited on 3/14/2016 by Velzee]

[Edited on 3/14/2016 by Velzee]

crystal grower - 19-3-2016 at 02:57

This is my article about growing pottasium dichromate crystals.
It is easy to do and crystal u will get are really nice :).

http://chem.pieceofscience.com/?p=937

The Volatile Chemist - 1-4-2016 at 14:49

Nice. I was just realizing how hard it is to grow nice crystals of most chlorides (non-trans. metal). I had some magnesium chloride and strontium chloride sitting out to crystallize, and although both formed crystals, it seemed impossible to dry them. So I'd rule out them for growing any good crystals.

Cucurbit - 4-4-2016 at 14:07

Great topic, good reason to get out of lurk mode for once - first post!

Here's a good old potassium aluminium alum crystal, the longest side is now 48 mm. Slow evaporation method, this one took > 6 months.
The photo doesn't do it justice!




alum_in_hand1.jpg - 156kB

crystal grower - 4-4-2016 at 20:48

Wow, that's gorgeous, it looks like huge diamond :).
Did you do something to prevent it from dehydration?
If not, do it right now! :) It would really pity to lose this one.

Dr.Bob - 5-4-2016 at 06:14

Cucurbit, that is a really beautiful crystal, like having your own pyramid, without have to travel to Egypt. Great job.

My favorite crystal is a chunk from the end of a silicon boule, about 5" in diameter, that looks like a giant Hershey Kiss. I got it from a place that made silicon wafers and it was supposed to be recylced back in to the melt, but someone there gave it to me as a gift. I have a few 3" wafers as well, never got any intact 5" ones, they were too valuable.

Cucurbit - 5-4-2016 at 08:59

Thanks guys!

Yes, I should put it in a jar when ready to protect it from dehydration, but it will be in its growing bath until it's... hmm, 6 cm mayby. A few days ago and I dropped it - can you believe it :o ... The tip broke off and has to regrow!
But chrome alum is probably more vulnerable to dehydration, the crystal at the right had almost completely degraded to a light purple powder, but I managad to re-grow the remaining core into its original shape. Remarkable how it seems to have a memory!

Also, a picture from some NaCl crystals I'm growing from sea salt. It's a difficult compound to grow into nice crystals but it's possible. I suspect the clumping agent (often ferrocyanide) in ordinary table salt prevents proper growth, it's like a negative catalyst. I hope I can grow these to a few cm, they are like architectural models!



P1014011group.jpg - 108kB NaCl1.jpg - 187kB

The Volatile Chemist - 9-4-2016 at 17:58

Really nice crystals Cucurbit!
I recently decided to try making some sample crystals of the shape of copper sulfate, to demonstrate its crystal habit (for fun mind you). Although I initially had some seed problems, I'm growing from a good sized base seed right now. I've always liked crystals but haven't really tried making any big ones till now. Going to be trying some of these in this thread later, perhaps...

hyfalcon - 9-4-2016 at 20:36

Anyone for NaI(Tl)? I would be curious how one would go about growing one of some size for a scintillation crystal.

100PercentChemistry - 10-4-2016 at 12:51

Tin Ii chloride! When you run a current through it you get tiny crystals of tin.

crystal grower - 10-4-2016 at 22:26

Quote: Originally posted by 100PercentChemistry  
Tin Ii chloride! When you run a current through it you get tiny crystals of tin.

I tried this too and got nice crystals of 2-3cm in lenght. Unfortunatelly, they were very delicate and I wasnt able to get them from a solution.

Chemist_Cup_Noodles - 14-4-2016 at 05:50

Quote: Originally posted by Cucurbit  
Great topic, good reason to get out of lurk mode for once - first post!

Here's a good old potassium aluminium alum crystal, the longest side is now 48 mm. Slow evaporation method, this one took > 6 months.
The photo doesn't do it justice!






Jesus that's a whopping crystal. I bet that photo doesn't do it justice! What do you grow crystals of such size in? I'd like to hear more from you about your methodology. I know overall it doesn't change much but still, damn son that's nice.

Cucurbit - 14-4-2016 at 08:48

Tnx! I'm using a tray from soft plastic, intended for heating microwave meals. Hydrophobic plastic is better than glass because there is less chance of crusts creaping up at the walls. I'll soon have to buy a bigger one :cool:

Weekly maintenance consists of filtering the solution and replenishing what was lost due to evaporation. I cover the tray with a 'roof' of paper to protect it from dust and slow down evaporation. It's standing in a small unheated unused room with a rather constant temperature. The rest is just 'neglect tek' :)

I'm glad to see the big one's tip has already grown back in a week!


container1.jpg - 208kBrainbows1.jpg - 777kB

Chemist_Cup_Noodles - 15-4-2016 at 12:16

Quote: Originally posted by Cucurbit  
Tnx! I'm using a tray from soft plastic, intended for heating microwave meals. Hydrophobic plastic is better than glass because there is less chance of crusts creaping up at the walls.


Wow, that's a pretty good idea. Never ever would have thought of using a plastic tray to fix that issue, which has actually been quite a pain in the ass for me recently.

Cucurbit - 15-4-2016 at 14:11

Quote: Originally posted by Chemist_Cup_Noodles  
Quote: Originally posted by Cucurbit  
Tnx! I'm using a tray from soft plastic, intended for heating microwave meals. Hydrophobic plastic is better than glass because there is less chance of crusts creaping up at the walls.


Wow, that's a pretty good idea. Never ever would have thought of using a plastic tray to fix that issue, which has actually been quite a pain in the ass for me recently.



I have to admit it wasn't my idea, I just read it somewhere, applied it and it seems to work!

And it's logical: the more water-repellant the container is, the better.
Glass attracts water, the meniscus is hollow, the solution tends to creep up by capillary suction and evaporation at the crusts's high surface area... a positive feedback loop.

It's no guarantee, without a paper cover I still got crusts, but I hope it helps :D





Dmishin - 18-4-2016 at 01:03

I've found another easy method to avoid crust growth: apply automobile rain repellent to the glassware. I bought a bottle in a nearest automobile accessories shop, and it works really well (btw it works on glass much better than on plastic). According to the label, the rain repellent is made of silicone and isopropanol.

Chemist_Cup_Noodles - 26-4-2016 at 06:23

Quote: Originally posted by Dmishin  
I've found another easy method to avoid crust growth: apply automobile rain repellent to the glassware. I bought a bottle in a nearest automobile accessories shop, and it works really well (btw it works on glass much better than on plastic). According to the label, the rain repellent is made of silicone and isopropanol.


Hm, I think I've seen somewhere about using rain repellent. However, once you get it on, could it easily come off? I'm assuming that if it is silicone and isopropanol, then the isopropanol is probably the main solvent for the silicone and evaporates off. But what if you have a little alcohol in your solution to get it more saturated? Could it dissolve the silicone?

crystal grower - 26-4-2016 at 09:00

Some pretty K2Cr2O7 crystals.

P4263602.JPG - 3.7MBP4263607.JPG - 3.2MBP4263608.JPG - 3.1MB

Chemist_Cup_Noodles - 27-4-2016 at 10:23

Oh my god do I love the look of chromates and dichromates. For the life of me I can't find a good source of the anion, or even of chromium itself in order to make some. Maybe I'll just have to buy some and recrystallize it. I do wish that chromates were more soluble though. Anyone know good solvents for them? The mineral crocoite (lead chromate) is beautiful but insoluble in water.
But crystalgrower, if those are your crystals I'd love to hear the details on how you made and grew them. Chromium is seriously one of my favorite transition metals.

crystal grower - 27-4-2016 at 12:06

Quote: Originally posted by Chemist_Cup_Noodles  
Oh my god do I love the look of chromates and dichromates. For the life of me I can't find a good source of the anion, or even of chromium itself in order to make some. Maybe I'll just have to buy some and recrystallize it. I do wish that chromates were more soluble though. Anyone know good solvents for them? The mineral crocoite (lead chromate) is beautiful but insoluble in water.
But crystalgrower, if those are your crystals I'd love to hear the details on how you made and grew them. Chromium is seriously one of my favorite transition metals.

Frankly, these crystals have come from solution which I have forgotten somewhere in mess in my lab and when I found it after few months, there was a pretty surprise waiting for me :P. So time is best recipe IMO.
But if you want to try to grow these crystals a lot faster, you can try this procedure: http://chem.pieceofscience.com/?p=937. And Im sure you can get better results than mine. Although k2cr2o7 has only little water solubilty at room temperatures, the solubilty rises drastically with bigger temperatures, so repeated cooling seems to be very effective for crystal growing.

Chemist_Cup_Noodles - 28-4-2016 at 04:57

Quote: Originally posted by crystal grower  

Frankly, these crystals have come from solution which I have forgotten somewhere in mess in my lab and when I found it after few months, there was a pretty surprise waiting for me :P. So time is best recipe IMO.
But if you want to try to grow these crystals a lot faster, you can try this procedure: http://chem.pieceofscience.com/?p=937. And Im sure you can get better results than mine. Although k2cr2o7 has only little water solubilty at room temperatures, the solubilty rises drastically with bigger temperatures, so repeated cooling seems to be very effective for crystal growing.


Ooh, I'm really liking this website you linked me to. Very very good work. Sleek interface, great content. I see you have quite a wealth of experiments on this page, wow. Where do you source most of your chemicals and glassware? Do you synthesize your own intermediaries or buy them? And it says you're in highschool? Damn son, making me feel bad.
Anyway, being a novice chemist I've always seen the word "alum" thrown around, especially in this thread, but always preceded by potassium and aluminum. I never really understood what exactly it meant. So I never realized that alum was a group of compounds! These are something to behold, truly. I've just cracked open my new bottle of H2SO4 so I'm eager to use it to make some of these now. So by my understanding, an alum is any +3 oxidation state ion and one +1 oxidation state ion with two -2 sulfate ions.

On a side note, spring is being annoying. I've had several solutions that I've left open to air in order to try and let them evaporate faster, but with all this rain it's too damn humid. Also, bugs won't stop flying into them, dying, and in some cases they start to dissolve if it's reactive enough. Little bastards, contaminating my hard work.

Edit: I like these so much I think I'll start a topic for them on the General Chemistry board. I think I'll just call it Alum Crystals Thread.

[Edited on 28-4-2016 by Chemist_Cup_Noodles]

crystal grower - 28-4-2016 at 06:10

Thanks :).
Our sources are various, we buy something o f course, other stuff we synthese ourselves, and also a lot of experiments has hegi done at university lab.
Sometimes we must improvise a little, but we are trying our best to be as profesional as possible. We also accept any donations, though finding a sponsor is very hard of course.
A lot of that great synthesis is Hegi's work so don't think that Im some super chem-kid :D lol.
You're partially right with the alums, you can find a good explanation on wikipwedia: https://en.m.wikipedia.org/wiki/Alum
And to tell something about the "spring problems" you mentioned, just look properly at the third photo of the p. dichromate crystals that i have taken (that small fly in it :P).

Cucurbit - 28-4-2016 at 12:52

Nice bichromate crystals!

And poor insect - unless it's a mosquito, I hate those :mad:

Which reminds me of something... many years ago I used potassium bichromate for gum prints, and got a nice crystal after evaporation of leftovers. I'll see if I can find it and take a picture tomorrow.

And Cup_noodles, I can't wait to see some pics of your alum crystals!

The Volatile Chemist - 30-4-2016 at 09:48

Ammonium Chloride surprisingly makes needle-like crystals, something at least I hadn't seen before.

image.jpeg - 1.8MB

crystal grower - 30-4-2016 at 11:08

@the volatile chemist
Once i grew nh4cl crystals with needle like shape too, and they had hashtag reminding layout ### :D.

The Volatile Chemist - 30-4-2016 at 14:34

Quote: Originally posted by crystal grower  
@the volatile chemist
Once i grew NH4Cl crystals with needle like shape too, and they had hashtag reminding layout ### :D.

:) Yeah, they were kinda unique, It might've had to do with excess ammonia or HCl, to be honest I forget which I used. What other shape grew for you besides needle-like? I just got a crust with beads, and then the needle-shaped ones.

crystal grower - 1-5-2016 at 02:30

these are crystals of nh4cl that I´ve grown few years ago (I didnt care much about the procedure in that time, I just dissolved some sal ammoniac in the water and waited what it will do :)).
It´s interesting that it crystallized into "three forms". At the very buttom a crust was formed, above a # like needles crzstallized and at the top were something like prisms and another crystastals crzstallized on them (reminding me sceptre quartz)
Sal ammoniac is really interesting stuff and I´ll maybe write an article about it in near future :).

this.JPG - 3.1MB upr.JPG - 3.4MB

[Edited on 1-5-2016 by crystal grower]

Cucurbit - 2-5-2016 at 13:36

Very nice ammonium chloride crystals!

Here's this potassium bichromate crystal. Old, impure and damaged... in my memory it was much nicer but hey, I promised to post a picture!



bichromaat1.jpg - 198kB

The Volatile Chemist - 17-5-2016 at 14:11

Yes, it is quite interesting stuff. Unfortunately, I only just recently realized that the crap on the sides of the crystallizing dish was soap from my ammonia supply. So the stuff I collected is garbage...

Velzee - 16-8-2016 at 21:38

Potassium ferrioxalate crystals, contaminated with potassium oxalate and chloride:


image.jpeg - 404kBimage.jpeg - 1.1MB

Praseodymium sulphate octahydrate

Bezaleel - 9-2-2017 at 15:28

On pg 3 of this thread, Nezza posted a beam-shaped crystal of Pr2(SO4)3.8H2O.
Mine appear to have a somewhat different form. Here are 4 pictures of the same crystal. I needed to stop growing it further, because I ran out of solution.
The long side is less than 1 cm long.
Overzichtsfoto Pr2(SO4)3.JPG - 246kB


[Edited on 9-2-2017 by Bezaleel]

crystal grower - 10-2-2017 at 02:21

Quote: Originally posted by Bezaleel  
On pg 3 of this thread, Nezza posted a beam-shaped crystal of Pr2(SO4)3.8H2O.
Mine appear to have a somewhat different form. Here are 4 pictures of the same crystal. I needed to stop growing it further, because I ran out of solution.
The long side is less than 1 cm long.



[Edited on 9-2-2017 by Bezaleel]

Oh my god, this one is just beautiful. Awesome clean crystal faces

woelen - 10-2-2017 at 02:55

These look very good. How long did it take to grow these crystals?

Bezaleel - 10-2-2017 at 05:16

I took a seed crystal from the solution, about 1mm in thickness, which was just big enough to tie a thread around. It was suspended in the solution from which it had formed for almost 1 week (6 days, if I remember well - I started somewhere last week). The solution evaporated in the boiler room with a larger beaker over it to keep out most of the home dust in the air. The air in the boiler room is relatively dry and the temperature is quite constant (between 19 and 22C). Evaporation speed was about 30ml from the 100ml when the crystal was first suspended from the monofilament thread.

Maybe it's interesting to know that a plastic beaker is preferred over a glass one, because in an earlier experiment with a solution of the very same Pr-sulphate, the solution crept upwards along the walls of that glass beaker (more than 8 cm up!). It forms ugly crusts on glass beaker walls. I also think that a plastic (PE) beaker makes it easier for the crystals to nucleate. In glass beakers, my rare earth solutions super saturate almost without exception.

The pH of the solution is 6.

Also of interest may be the dissolution behaviour. In order to get all of the Pr2(SO4)3.8H2O dissolved, about 20% more solution was needed than the volume from which the first tiny seed crystals appeared. I am tempted to conclude that the dissolution-crystallisation cycle has some hysteresis.

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