Sciencemadness Discussion Board

Pretty Pictures (2)

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PHILOU Zrealone - 1-3-2016 at 07:21

I also have a good stones, gemstones and fossiles collection :D
Also some other not yet exposed in my glass shelf...
gem1.JPG - 2.1MB
gem2.JPG - 1.9MB
gem3.JPG - 2MB
gem4.JPG - 2MB
gem5.JPG - 1.9MB

PHILOU Zrealone - 1-3-2016 at 07:36

And a few close up of my bismuth cristals:

bis1.JPG - 1.2MB
bis2.JPG - 1.5MB
bis3.JPG - 1012kB
bis4.JPG - 2MB
bis5.JPG - 1.9MB

crystal grower - 1-3-2016 at 08:07

Wow that's gorgeous.
Do you buy minerals or you dig the them yourself ?
And also what purity bismuth do you use?

Velzee - 1-3-2016 at 12:03

Amazing, all of these.

PHILOU Zrealone - 3-3-2016 at 14:19

Quote: Originally posted by crystal grower  
Wow that's gorgeous.
Do you buy minerals or you dig the them yourself ?
And also what purity bismuth do you use?

I started my collection at the age of 8 (I'm 41 by now), but my personal findings are a minority (less than 0.5% of my collection); most of my collection come from mineral and fossiles fairs...the other part from tiny gifts.

I focus on beautiful gemstones, usually transparent and colored ranging from half-precious to precious, but at a good price and in natural state or just pollished.

The last 5 years I have bought some facetted gemstones, some artifical, thus for a very good price...some are huge.

For the last decade I also bought minerals for the chemical content (Beryls for Berylium, some rare minerals for Ytrium and Selenium, Cinnabar for Mercury, crystaline Silicium, crystaline Bismuth,Stilbine for Antimony, ...)

The Bismuth crystals are probably very pure, I guess they come from the industrial refining process of Copper, Lead and Tin (from cooling chemineys)...they are colourfull and very advertising if you look at them with a magnifier or microscope...you feel like flying into old Maya temples...

[Edited on 3-3-2016 by PHILOU Zrealone]

woelen - 5-3-2016 at 11:34

I made an ampoule with IBr. Very weird crystals are formed in the inside of the ampoule:

This is the ampoule:

IBr.jpg - 238kB

You can see some solid IBr at the bottom of the ampoule, the brown/pink vapor above it, and beautiful crystals at the bottom half of the ampoule.


Here follow some closeups of the crystals:

Crystals on the far side of the ampoule:

IBr_crystals_farside.jpg - 481kB



Crystals on the near side of the ampoule:

IBr_crystals_nearside.jpg - 426kB



Crystals all around the ampoule:

IBr_crystals.jpg - 456kB



One week later, the crystals disappeared at one side of the ampoule, but they are still present on one side:

IBr_crystals_7days.jpg - 196kB

wg48 - 5-3-2016 at 12:00

Fascinating pics woelen. The form of the crystals on the glass sides is reminiscent of the frost patterns on glass. I imagine molecules of the IBr bouncing a round in the tube and only sticking to the crystals with some probability depending which facet of the crystal they hit.

crystal grower - 5-3-2016 at 12:04

Quote: Originally posted by woelen  
I made an ampoule with IBr. Very weird crystals are formed in the inside of the ampoule:

This is the ampoule:



You can see some solid IBr at the bottom of the ampoule, the brown/pink vapor above it, and beautiful crystals at the bottom half of the ampoule.


Here follow some closeups of the crystals:

Crystals on the far side of the ampoule:





Crystals on the near side of the ampoule:





Crystals all around the ampoule:





One week later, the crystals disappeared at one side of the ampoule, but they are still present on one side:


Wow, that's really weirdo :D.
What melting point does it have?

I want to try growing some iodine crystals, too bad that I can't find any iodine for a reasonable price (local eshops offers only big quantities so I can't afford it) and I won't probably get enough from povidone :(.

UC235 - 5-3-2016 at 12:20

If you store bromine in the freezer, it too forms these beautiful feathery crystals on the walls as it sublimates. Mine is stored in the door, and the temperature gradient is sufficient that all of the material migrates to the one side of the upright bottle.

Velzee - 5-3-2016 at 13:34

Quote: Originally posted by crystal grower  
Quote: Originally posted by woelen  
I made an ampoule with IBr. Very weird crystals are formed in the inside of the ampoule:

This is the ampoule:



You can see some solid IBr at the bottom of the ampoule, the brown/pink vapor above it, and beautiful crystals at the bottom half of the ampoule.


Here follow some closeups of the crystals:

Crystals on the far side of the ampoule:





Crystals on the near side of the ampoule:





Crystals all around the ampoule:





One week later, the crystals disappeared at one side of the ampoule, but they are still present on one side:


Wow, that's really weirdo :D.
What melting point does it have?

I want to try growing some iodine crystals, too bad that I can't find any iodine for a reasonable price (local eshops offers only big quantities so I can't afford it) and I won't probably get enough from povidone :(.


http://www.ebay.com/itm/25-grams-0-88oz-pure-elemental-iodin...

Pretty high purity; this is the time in which products from China should be considered. I ordered a smaller amount before, which came out to be legitimate, but I should note that they do tend to lie to the customs(as in my case, they labeled the iodine as "clothing accessories" ).

crystal grower - 5-3-2016 at 23:19

Quote: Originally posted by Velzee  


http://www.ebay.com/itm/25-grams-0-88oz-pure-elemental-iodin...

Pretty high purity; this is the time in which products from China should be considered. I ordered a smaller amount before, which came out to be legitimate, but I should note that they do tend to lie to the customs(as in my case, they labeled the iodine as "clothing accessories" ).

That seems like a good deal but can I trust ebay? (I haven't bought anything from it yet). 5$ isn't very much so I could try it.
Sorry for being off-topic.

j_sum1 - 6-3-2016 at 01:21

I have bought Chinese iodine from eBay a couple of times. Last time was 100g a couple of months ago. Good experiences both times.

NedsHead - 6-3-2016 at 02:00

J_sum1, did you have to contact customs and have it cleared first? I've wanted to buy some iodine/potassium iodide off eBay but wasn't sure if I could legally get it through customs

[Edited on 6-3-2016 by NedsHead]

j_sum1 - 6-3-2016 at 02:14

Nope. I just ordered it and it arrived. I will U2U my eBay seller but it is undoubtedly not the only possible source.

Like anything, you might expect a little visit from our friends in blue. (And I don't mean the smurfs.) Be ready for that. I have had one visit and it was painless enough. They said they would record me as legit and I would be unlikely to get another visit for a while.

fluorescence - 6-3-2016 at 06:41

Well....that didn't really work out as expected. So this was supposed to be Hexamminecobalt(III)oxohexacarbonatotetraberyllate but I just recently found the description of how to actually prepare it and I should have had used a Carbonate...so from the fact that even the so called insoliuble Co(III)ammine-Complex didnt really precipitate and that stuff is still full of Ammonia its probably just some Be(OH)2 that has formed.

I just read that even that complex mentioned above is supposed to be white when clean...so no colored Be compound again which is really sad. I'd really like to show you that Be Chemistry can be interesting, too but there is just no good inorganic complex which would be colored. s-Orbitals don't split so there is no transition unfortunately.

I think the only way to make it a bit more colorful would be to bind it to a pi-System that is already colored like in Chlorophyll for Magnesium.

So I will try to prepare the complex mentioned above again in a pure form and hopefully give you a real picture of it. Does anyone know about a good inorganic perhaps colored Be Compound ?

BE.jpg - 69kB

Theoretic - 16-3-2016 at 13:08

A slight break from the preceding, but...
I hope nobody objects to explicit images of naked flames?


56e9b7f1b6651.png - 97kB

Candle in microgravity

Image113.gif - 73kB

Direct photographs of sooting n-C4H10 non-premixed gas-jet flames at 1 µg at Reš42, jet diameter 10 mm, showing evidence of thermophoresis-induced agglomeration at µg.

image005.jpg - 17kB

"CH4/Air premixed flame attached to a carbon-coated brass matrix cooled with water. Fuel rich to fuel lean from left to right and top to bottom by increasing air flow rate and decreasing CH4 flow rate. Small flames dance around and a butterfly appears. When the butterfly flies away, flame is gone."


Last not least:
1.jpg - 35kB

Why you don't extinguish Mg fires with a carbon dioxide extinguisher - even on a space station

Velzee - 17-3-2016 at 10:37

Quote: Originally posted by Theoretic  
A slight break from the preceding, but...
I hope nobody objects to explicit images of naked flames?




Candle in microgravity



Direct photographs of sooting n-C4H10 non-premixed gas-jet flames at 1 µg at Reš42, jet diameter 10 mm, showing evidence of thermophoresis-induced agglomeration at µg.



"CH4/Air premixed flame attached to a carbon-coated brass matrix cooled with water. Fuel rich to fuel lean from left to right and top to bottom by increasing air flow rate and decreasing CH4 flow rate. Small flames dance around and a butterfly appears. When the butterfly flies away, flame is gone."


Last not least:


Why you don't extinguish Mg fires with a carbon dioxide extinguisher - even on a space station


Wow!

The Volatile Chemist - 17-3-2016 at 12:28

Ive brought this up before, but since the last pretty pictures thread topped at 40 pages, and was deemed hard to manage with forum software, shouldn't the same be done here? Or is the software better now?

fluorescence - 22-3-2016 at 08:50

So did another attempt to make a colored Beryllium Compound. This time I used an organic ligand. It took me quite a while and a few tries to get a useful result but it looks quite cool right now.

According to literature there is a Curcumin complex with Beryllium in an alkali solution. Literature suggests using Ammonia but I found that the results are so dark if you use too much indicator that you wont be able to see anything. So I switched to KOH as base.

What you see here are two test tubes filled with the same amount of KOH solution, made from one spatula of KOH in about 30 ml of water.
To one I added a Berylliumsulfate soltuion, made from 2 small spatulas of pure BeSO4 in about 25 ml of water. I took about 3-4 ml of this solution and added it to one of the test tubes and to the other one the same amount of water.

Literature often talks about the precipiate formed (BeOH2) but I did a run with quite much precipitate and it didn't really change that much. The one you see here is only a little cloudy and its really hard to even see the Hydroxide formed. So this can be done in a quite low concentration as well. I then added a few drops of curcumine in Ethanol to both of them.

The one without Beryllium stayed in solution and became brown-orane the other one precipitated and changed to a red color (hard to see on the photo).

In the pictures on the bottom I added a lot of indicator to the left test tube without beryllium and some solid BeSO4 to the other one as you can see as long as they are diluted even higher conc. of indicator and Be althought the both form a red layer where they meet differ in color if you diluted them long enough.

So I know Quinalizarin looks better but that is too expensive for me to buy it so I stay with curcumin but will try something interesting, soo.



BE-Cu III.jpg - 228kB

Copper(II) acetylacetone

Hegi - 22-3-2016 at 14:25

Copper(II) acetylacetonate recrystallized from chloroform... Check out article about preparation - COPPER ACETYLACETONATE PREPARATION

9.png - 595kB 10.png - 775kB

[Edited on 23-3-2016 by Hegi]

Zephyr - 22-3-2016 at 19:02

Those look like amazing crystals! I'm interested in viewing the prep but it seems your link doesn't work?

Sadly my acetylacetone synthesis failed, maybe I'll try again in a few weeks...

DraconicAcid - 22-3-2016 at 20:22

Quote: Originally posted by Zephyr  
Those look like amazing crystals! I'm interested in viewing the prep but it seems your link doesn't work?

Sadly my acetylacetone synthesis failed, maybe I'll try again in a few weeks...

Try this: http://chem.pieceofscience.com/?p=990

Hmmm....there's also this: http://www.magritek.com/wp-content/uploads/2015/03/Lab-Manua...

I wonder if I could make some acac. Or if dimethyl malonate would form similar complexes.

[Edited on 23-3-2016 by DraconicAcid]

Zephyr - 22-3-2016 at 21:11

Wonderful, thanks DraconicAcid. I look forward to more great projects from pieceofscience!

Here's a pic of the drying rack I built for some substance:

IMG_0116.JPG - 4MB

Hegi - 23-3-2016 at 02:26

Quote: Originally posted by Zephyr  
Those look like amazing crystals! I'm interested in viewing the prep but it seems your link doesn't work?

Sadly my acetylacetone synthesis failed, maybe I'll try again in a few weeks...


Thanks Zephyr! It should work now. What reaction did you try for acetylacetone synthesis?

Zephyr - 23-3-2016 at 20:11

Here is the synthesis I attempted. As you can see moisture leads to issues, and I suspect it was the culprit... A bit of

AcetylAcetone.bmp - 1.8MB

Insight on how it could be done better or issues with this route are appreciated.

HeYBrO - 23-3-2016 at 21:21

how wet was your ethanol? Also, doesn't the equilibrium of hydroxide and ethanol lie heavily to the product side because of the water generated and the pKa's? The org syn procedure uses sodium metal. http://www.orgsyn.org/demo.aspx?prep=CV3P0016 Nurdrage used molecular sieves to make sodium methoxide from methanol and sodium hydroxide, so maybe you could try that if you don't have sodium,

Texium - 24-3-2016 at 15:17

Quote: Originally posted by Hegi  
Quote: Originally posted by zts16  
Nice! I'm actually currently working on an indigo synthesis too, however I'm actually synthesizing my own 2-nitrobenzaldehyde, so it's a more lengthy procedure. I have 2-nitrotoluene now, and I'm currently awaiting the arrival of the solvent that I need for the oxidation step. Then it should be smooth sailing from there. A writeup will be posted once I am finished. :)


Oh man, such a long way. The last step is really smooth sailing besides making your own 2-nitrobenzaldehyde. Did you prepare 2-nitrotoluene?
Yes, I prepared mixed nitrotoluenes by nitration of toluene, and then fractionally crystallized out the p isomer by sticking it in the freezer, waiting for it to freeze out, filtering, and repeating the process again. I actually made use of the p-isomer too, by making an azo compound, 4,4'-dimethylazobenzene, by reaction with zinc and sodium hydroxide in methanol under reflux. I have it as a solution in DCM. It's not as pretty as I'd hoped: looks a bit like unhealthy urine.

PHILOU Zrealone - 25-3-2016 at 06:57

Quote: Originally posted by Zephyr  
Here is the synthesis I attempted. As you can see moisture leads to issues, and I suspect it was the culprit... A bit of



Insight on how it could be done better or issues with this route are appreciated.

I think your scheme is wrong because it looks like you work with an alcoolate of 4-hydroxy-pentan-2-one.

2,4-Pentandione (CH3-CO-CH2-CO-CH3 equal to CH3-C(=O)-CH2-C(=O)-CH3 ) can make a stabler enol because of the resonance between the C=C double link and the C=O double link...such systems are acidic see phenol.

CH3-C(-OH)=CH-C(=O)-CH3 <==> CH3-C(=O)-CH2-C(=O)-CH3 <==> CH3-C(=O)-CH=C(-OH)-CH3

So it looks like you simply have forgotten the C=C double link in your scheme and that the resonance hybrid includes the C atom between the two C=O groups.


AcetylAcetone.jpg - 88kB

[Edited on 25-3-2016 by PHILOU Zrealone]

fluorescence - 30-3-2016 at 05:13

Some Thallium Nitrate on an Iron nail in the flame, a beautiful green although its pretty hard to get on cam, nothing like Barium or Copper would emit.



Thallium.jpg - 97kB

The Volatile Chemist - 1-4-2016 at 14:58

Nice thallium photo! SM Wiki quality...
Zts16, I've been noticing recently that a lot of the solutions within my lab-work end up being urine colored in some way. Yellow is becoming one of my favorite colors, though, along with green, blue and orange...

fluorescence - 2-4-2016 at 05:38

@TheVolatileChemist:

Thanks. Take it if you need it for the wiki. As our Cyanide Chemist I should probably do some pages on transition metal cyanides for our Wiki but I'm too busy doing other stuff and I don't like writing articles :D.

Also if anyone knows a cool colored complex with Thallium I'd be interested. I have an Ebook on Thallium Chemistry but I won't buy special reagents just for that single experiment. So no complicated organic ligands. I found 2 interesting, one with Chromium and Thallium(III)Chloride where Thallium is really in a [TlCl6]-complex so not just a precipitate and one with Cobalt. Problem the fist one requires Hexamminechromium(III)chloride which is either done using cold Sodium Amide or cold temperatures and quite a lot of Ammonia and Cr(II). So nothing I have time for at the moment. And for the Cobalt one...well that was kinda my bad to accientally use Potassium Nitrite instead of Sodium Nitrite and I now have the precipitated Potassium salt -.- . So if anyone has a good suggestion, I don't want to waste it since I'll be needing it soon but for one or two cool compounds I'd gladly sacrifice some of it.



[Edited on 2-4-2016 by fluorescence]

Mabus - 2-4-2016 at 07:59

Nothing fancy, just some urea needle-shaped crystals I made a few days ago. Longest crystals are about 5 cm long.
Too bad they broke when I tried to get them out of the beaker (they are very fragile) :(
mCKH3jE.jpg - 1.9MB

Hegi - 3-4-2016 at 12:20

Quote: Originally posted by Mabus  
Nothing fancy, just some urea needle-shaped crystals I made a few days ago. Longest crystals are about 5 cm long.
Too bad they broke when I tried to get them out of the beaker (they are very fragile) :(


They look really amazing :cool: Nice one Mabus! How fast did they grow?

Mabus - 4-4-2016 at 08:51

Quote: Originally posted by Hegi  
Quote: Originally posted by Mabus  
Nothing fancy, just some urea needle-shaped crystals I made a few days ago. Longest crystals are about 5 cm long.
Too bad they broke when I tried to get them out of the beaker (they are very fragile) :(


They look really amazing :cool: Nice one Mabus! How fast did they grow?

I left them to grow overnight, between 12-18 hours. I think it also helped that the temperature slowly went down from 20 °C in the noon to 5 °C during the night.
I didn't intend to grow such large crystals, I merely wanted to purify some urea I got for free.

Hegi - 4-4-2016 at 12:21

Quote: Originally posted by Mabus  
Quote: Originally posted by Hegi  
Quote: Originally posted by Mabus  
Nothing fancy, just some urea needle-shaped crystals I made a few days ago. Longest crystals are about 5 cm long.
Too bad they broke when I tried to get them out of the beaker (they are very fragile) :(


They look really amazing :cool: Nice one Mabus! How fast did they grow?

I left them to grow overnight, between 12-18 hours. I think it also helped that the temperature slowly went down from 20 °C in the noon to 5 °C during the night.
I didn't intend to grow such large crystals, I merely wanted to purify some urea I got for free.


This slow decrease in temperature overnight is the goal. Really nice.

A picture of tridymite I found yesterday in a stone pit. The crystals are well shaped and up to 4 mm in lenght.

<img src="http://chem.pieceofscience.com/wp-content/uploads/2016/04/tridymit1.png" alt="Mountain View" style="width:900px;height:600px;">


Sulaiman - 4-4-2016 at 13:27

Quote: Originally posted by Theoretic  
A slight break from the preceding, but...
I hope nobody objects to explicit images of naked flames?



Just wanted to say WOW !

I spent quite a while looking at each, so much going on.
I especially liked the soot generating flame, sort of fills in a mental picture.
more or a pointer to more would be nice.

fluorescence - 9-4-2016 at 05:52

So....I have no idea what I just did.

Some time ago a friend gave me a bag full of natural Arsenic, he purchsed that somewhere, I dunno. Some black chunks, some have impurities some are quite pure. I did some experiments with them like dissolving them, there is a pictrue in this thread. So I decided to try to make some Oxide from it by heating it. I took some small chunks into the test tube and heated them with the burner till the glass became quite soft, dunno where the melting point of my glass is. The chuncks started to smoke producing a dense brown smoke. I stopped and the thing you see on the picture formed. I than took the test tube and turned it upside down. The Arsenic fell out and started smoking brown again. You can see a dark brown trail on the upper part of the test tube where they touched the glass when falling out.

That is not what I expected. I tried this before, back then with a heat gun so it was much slower and back then only white stuff had formed. Ehm...well it looks like an Arsenic mirror, its fully reflective, as you can see there is my reflection in it its silvery on the outside and on the inside it has a quite rough black surface.
It really reminds me of the Arsenic you make using the Marsh test. Also I noticed a familiar smell comiing from the test tube after it cooled down. It reminds me of the smell that Phosphorus has when you burn it. It wil alwys leave behind a white, waxy rest when its burned and that usually smells like the stuff coming from the test tube....

Anny suggestions ? Maybe Sulfide or something that fell apart under the hot temperatures forming elemental Arsenic ?

I read about a suboxide of Arsenic that can form and that smells like phosphorus and is brown as well.

I mean I could have distilled Arsenic as well although I'm not sure if the temperatures really reached 600°C and maybe the fine powdered arsenic when cooled down got coated with this suboxide that appearently smells like garlic. That could be an explanation.

Hard to admit for me as an Inorganic Chemist but I have no idea what this could really be.

As.jpg - 272kB


Edit:

I took one of the small grains and heated it directly with the bunsen burner on a metal surface. It immediately formed the same black stuff behind the metal. So I guess that by heating it wih the burner in the test tube it got the sublimation point of Arsenic faster than Arsenic reacts at these temperatures with the oxygen to form the Oxide. So I guess the black stuff it just Arsenic and some small amounts of Oxides which give the smell.


[Edited on 9-4-2016 by fluorescence]

Boffis - 10-4-2016 at 09:05

Native arsenic is surpringly common, while not widespread, when it does occur it is often abundant. Over my life time in the mining industry I have acquired many incredible specimens some several kgs in weight. However, it is often alloyed with native antimony to form AsSb or stibarsen.

Your last point is almost certainly correct. When strongly heated arsenic sublimes in the absence of air about otherwise it oxidizes to white arsenic As2O3 though in a test tube much may sublime as insufficient air can get in quickly.

If you want to make something out of it: nitric acid is an easier way to oxidize it, it gives arsenic acid (and much brown N2O4)and any antimony impurity is oxidized to sparingly soluble Sb2O3. Arsenic dissolves in alkaline oxidizing solution (ie bleach) as sodium arsenite and in polysulphide solution to give various thioarsenates. Melting with sulphur generates various sulphids depending on ratios and these dissolve in hydroxide, alkaline sulphide and polysulphide solutions to give thioarsenites and thioarsenates. Hydrogen peroxides converts thioarsenates to arsenates.

100PercentChemistry - 10-4-2016 at 12:53

Tin crystals

image.jpeg - 1.1MB

fluorescence - 11-4-2016 at 09:46

@Boffs: Thank you for the ideas. I tried to make Arsenic Acids but I avoid that topic or it gives me headaches otherwise. Problem is that literature isnt very precise on what actiually forms at what moment. And I think you need to really heat the Arsenous Acid to get to the pure Arsenic Acid or something like that. At least its not easy to get a pure form of one of the two and some books just confuse that too much. So I dont even start to untangle that. But there are some interesting As Compounds and I will try to cover them as well. I'm still stuck with Tl at the moment but after that I will try to find some interesting As compounds and hopefully post some good pictures here. Any suggestions are welcome.

[Edited on 11-4-2016 by fluorescence]

Boffis - 11-4-2016 at 17:59

@fluorescence check out; Handbook of Preparative Inorganic Chemistry by Brauer on the forum library.

More information is available in the appropriate volumes of A Textbook of Inorganic Chemistry (try volume VI part 4) and A Comprehensive Treatise on Inorganic and Theoretical Chemistry by Mellor, both of which are also on the forum's library page.

fluorescence - 24-4-2016 at 08:18

Here is some Thallium Chemistry. I wasn't that creative this time simply because I didn't have too much time. Still I like the results. Those are only very small amounts due to the fact that pure Thallium Salts are really expensive and I need them for some other experiments soon and they are not that well soluble as you might expect at least if you dont boil the solution. So I stayed with small samples and still enough compounds formed. Note that all of these compounds are insoluble and seperated pretty fast I just shook them before I took the photos so you could see them better.

I really like how the colors vary with Potassium Ferrocyanide and Chromate both being yellow and many other prec. Ferrocyanides being brownish as well it surprises how the Thallium sample can form a white compound and a yellow one. Usually I check these reactions before I post them here but I didnt have time so if there is any mistake like a side reaction I didnt think of just tell me.
To the Selenide. I suppose this is the Selenide. I tried a new method to make transition metal chalcogenides. There will be a post on it soon i am still drying the Cadmium Sulfide I made for test and then I have to test if its really the Sulfide and not something else. After that I will make a post on how I made this Selenide.



Thallium Compounds.jpg - 278kB

j_sum1 - 25-4-2016 at 03:23

Interesting work fluorescence. How confident are you in your identification of these substances?
Are you certain that you have no III oxidation state substances there?
I too am suspicious of the selenide. It looks like you might have something else suspended in there.

J.

fluorescence - 25-4-2016 at 13:09

As said I don't know. Some experiments need to be done with Tl(III) which is sometimes made in a Chlorate + HCl boling mixture so this needs a lot power. But I could just check all these structres. As Solid State Chemist I have acess to all the Crystall Structure Data:

So let's check it:

- For the Thallium(I)Selenide, I4/mcm there are some papers on it and none is on Tl(III). I just assume that crystals structures imply that at least someone extracted a pure sample and calculated if the structure can form with the given Atoms and ratio, at least this is what I have to do with my solids.

I checked Reaxys for the preparation, some literature suggests melting the pure Elements together, and some make it from a Selenium Source and a soluble Thallium Salt in solution. And since the SUlfide precipitates as well I assume that it's possible with the Selenide as well. And most sources describe it as black like my stuff is.


- For the Chromate, yeah it appears like Chomate could perhaps oxidize it to Tl(III) somehow. Indeed under acidic conditions Dichromate would be a bit stronger with its redox potential but that would require an acid in there as well.

So lets check the crystal database and the result is there are the following known structures

o Thallium(I) Chromate -> Pmcn/Pnma
o Thallium(I) Dichromate -> P-1

and indeed there is a Thallium (III) Chromate -> Pbcn mentioned.

So let's first check out the paper that is given for the Tl(III):
Too bad I can't find any digital version of it but there is something in the Pigment Compendium. And it seems like the color varies from yellow to red depending if Chromate or Dichromate is used and Tl(I) or Tl(III) is present. Reaxys suggests simple precipitation for the Tl(I) salts and for Tl(III) there is only one descirption where Tl(Iii) Nitrate is reacted with Chromium(VI)Oxide over two days at 40°C.


o Next would be Thallium Thiocyanate:

There is only a Tl(I) known with a room temperature structure of Pbcm (like KSCN) and a high temperatue phase of I4/mcm. I think potassium does the same thing with two different structures. Sodium in contrary has only one structure at least I never found a high temperature NaSCN phase in the literature. So Tl(I) seems to imitate Alkali Metals here and if its insoluble it might be stable as well. According to Reaxys it forms with Thiocyanates and Thallium(I) solutions. And I saw that all solubilities in literature are quite low so I suppose it should precipiate as well.

o For the Ferrocyanide:

I cant find the paper at the moment but I found one earlier. I can only find crystal data on the one with Tl(I) and Fe(II) [P-1]. Interesting thing is the paper said that the crystals are actually yellowish and my stuff is white but they said that it was hard to actually make crytsals and upon touching them they would fall apart to a fine powder. I guess mine is just so small that it scatters light differently and appears white. But I will check the other databases tomorrow and see if I can find more information on the Thiocyanate as well.

But it appears that my ideas where correct. Any suggestions, corrections welcome ! I will check the Gmelin on that if I find some time tomorrow.







[Edited on 25-4-2016 by fluorescence]

fluorescence - 27-4-2016 at 04:15

Addtional:

I found something on the ferrocyanide. According to Alfred Brukl - Elemente der dritten Hauptgruppe Band II,
Thallium(I) can be oxidized to Thallium(III) using either bromine water in acidic conditions or Potassium Ferricyanide so with Fe(III) in there under alkaline conditions. I will try that out when I have more time, seems quite interesting. It says here that Thallium(III)Hydroxide is precipitated and the yellow Fe(II)-Ferrocyanide can be titrated with Permanganate to tell how much Thallium there actually was.
I will try both methods soon, so Tl(I) to Tl(III) with Br2 and with Ferricyanide and I'll try to make some other Tl(III) compounds as well.

[Edited on 27-4-2016 by fluorescence]

arkoma - 28-4-2016 at 06:33

OH YEAH!!! Sassafras Albidum (it IS chemistry related, mua-ha-ha)

sassafras.jpg - 619kB

myristicinaldehyde - 29-4-2016 at 07:28

Arkoma, binomial names have the species part written in all lowercase! :P

JJay - 29-4-2016 at 07:43

That stuff is pretty common. They are most famous for their root bark essential oil, but I am curious about why the leaves smell like lemons.

arkoma - 29-4-2016 at 10:18

The root bark oil is Safrole--Yee-Ha. Just spotted probably another 50 trees on the side of the back road.

Deathunter88 - 29-4-2016 at 19:54

Barium chloride crystallising out of solution!
Largest crystal was about 15cm long, smaller crystals around 3cm ish. It happened by accident as I was evaporating down a solution of barium chloride I had just made with HCl and barium carbonate. I managed to keep most of them intact when getting them out of the dish.

IMG_4091.jpg - 2.9MB

Firmware21 - 30-4-2016 at 03:19

This is why I love copper salts: Easy to make and beautiful.

It's Copper II chloride in excess HCl

DSC_0022.JPG - 2.5MB

fluorescence - 30-4-2016 at 07:46

Wow looks really cool, I like green compounds ^^.
Did you even put some hazard labels on the bottle ?


So here are two other Thallium compounds. As promised I made some Tl(III) Oxide from Ferricyanide(III), KOH and Tl-Nitrate.

And on the right is some Thallium(I)-Iodide. I tried some Tl(III)Iodide as well but it wouldt form. I love how the color changes from the fine powdered orange iodide to the bigger yellow chunks after standing for 5 min. or so.



Thallium II.jpg - 247kB

The Volatile Chemist - 30-4-2016 at 10:28

Nice barium compound 'Deathhunter'! Very reminiscent of strontium chloride, which I'd recently done the same with.

wg48 - 30-4-2016 at 15:55

Patterns in a flame reminiscent of the patterns on the cathode of a low pressure discharge tube.



WP_20160501_00_39_41_Pro.jpg - 1.1MB

WP_20160501_00_39_46_Pro.jpg - 1.1MB

Firmware21 - 4-5-2016 at 12:12

@Fluorescence , Yes, I made them with a label printer. The glue on it is too weak to hold the hazard signs in place, so I had to put some tape...

Here's my whole "collection" of componds (including a some elements).
A lot is "homemade".


DSC_0014_1.JPG - 2.2MB

fluorescence - 5-5-2016 at 03:24

Nice,

I like these bottles. Just bought 10 of them last week. But they are crazy expensive here.
So I need to clean them if I dont need them anymore. But yeah really quite useufll.
I see you wrapped some tape around them as well. Although we sometimes stored solvents in them
at the university they seem to let some water through so for many anhydrous compounds I made
without tape around them they werent tight enough.


Chlorine

rasiel - 5-5-2016 at 19:04

Another poster requested I upload a photo of my sample of pressurized chlorine. Just a little ampule cast inside a much larger cube of high quality resin.

Chlorine.JPG - 528kB

I'm setting a goal of photographing each of the elements in case anyone has any requests :-)

Rasiel

rasiel - 5-5-2016 at 19:06

Wooops, I meant for this to show up on the pretty pictures thread. What'i do wrong?? :o

Daffodile - 5-5-2016 at 20:04

That's beautiful and damn amazing dude

XeonTheMGPony - 6-5-2016 at 05:22

What resin did you use? I'm all ways looking for good clear resins like that.

Texium - 6-5-2016 at 06:44

Quote: Originally posted by rasiel  
Wooops, I meant for this to show up on the pretty pictures thread. What'i do wrong?? :o
No problem, merged now.

fluorescence - 6-5-2016 at 09:16

Looks really well done. Some guys I knew tried that as well but after some time they tend to get all brown and cloudy. I hope your resin will stay as it is at the moment. Looks really nice.

UC235 - 6-5-2016 at 10:33

Quote: Originally posted by fluorescence  
Looks really well done. Some guys I knew tried that as well but after some time they tend to get all brown and cloudy. I hope your resin will stay as it is at the moment. Looks really nice.


Sounds like they bought cheap resin without UV protectants.

rasiel - 6-5-2016 at 17:06

PMMA, commercial acrylic... it's the stuff Plexiglass (aka Lucite) is made of. The problem with this resin is that it only cures under heat *and* pressure. If you have an autoclave then give it a shot. It's by far a more presentable option than epoxy which hardens yellow from day one or polyester which is a pain to work with and shows casting seams even when perfectly poured.

However, the resin is not the only consideration. To get those perfectly polished and straight walls with razor sharp edges can only be done by machine. With a lathe or mill you might be able to get a really pro-looking finish but I don't personally have experience in this area.

Anyway, I don't know of a US-based supplier for PMMA but there are a number of places that will sell it to you from China on Alibaba. This is what you're looking for http://goo.gl/L0ycb1

Rasiel

rasiel - 6-5-2016 at 17:17

For those interested in seeing how I'm making the cubes here's a brief but very interesting video that runs through the steps (and you'll see why it's not something easily replicated at home)

https://www.youtube.com/watch?v=hNaOKrE643g

crystal grower - 11-5-2016 at 11:48

Beatiful green-blue crystals of a-modification of NiSO4.6H2O.
Im still growing them, the biggest is about 1cm in diameter :P.

EDIT: I didnt notice that hegi has already posted this picture in another thread, should I delete this post?
file.png - 131kB

[Edited on 11-5-2016 by crystal grower]

rasiel - 11-5-2016 at 12:45

Oh wow, they look like breath mints!

:-)

Rasiel

crystal grower - 11-5-2016 at 12:50

Quote: Originally posted by rasiel  
Oh wow, they look like breath mints!

:-)

Rasiel

Lol, they remind me sapphires :).

wg48 - 11-5-2016 at 13:08

Quote: Originally posted by rasiel  
Another poster requested I upload a photo of my sample of pressurized chlorine. Just a little ampule cast inside a much larger cube of high quality resin.



I'm setting a goal of photographing each of the elements in case anyone has any requests :-)

Rasiel


A potential problem with potting glass in resin is if the resin contracts as it hardens it can crack the glass. This can happen years after the item is potted.

My mother had a hour glass egg timer given to her. It was was potted in a clear block of resin. About a year after she received it it stopped working. The sand would no flow thru the constriction. On close examination there was a crack in the glass thru the constriction. The egg timer was kept as an ornament. Over a few more years many more cracks appeared in the glass and distortion at the surface of the block over the ends of the hour glass could be seen.

I worked on a high voltage power supply that had been potted in a rigid resin. The high failure rate in the field was eliminated when it was potted in silicon rubber.

Of cause in the above cases the wrong resin or incorrect mixing or cutting temperature could have been the cause.

I guess a test block could be made by potting a glass rod in one side of long block to see if it bends.

rasiel - 11-5-2016 at 13:15

Today I took a pic of calcium... the way few people get to see it!



0.jpg - 152kB

fluorescence - 14-5-2016 at 23:17

Some Se82+ cations forming. The first run was too concentrated and appeared almost black this one here is really dilute and still it has a quite strong green color.

For those who actually read my bio ^^, I do a lot of Selenium Chemisry for my Thesis. Certainly not an element I would work with if nobody had asked me to do it. I love toxic compounds but Selenium is just really nasty. And most of my Selenides at work fall apart on air producing some H2Se and it's really terrible to work with that.

I think that Selenium chemistry is something most people have no clues about. If wanted I could do a small article on the forum on actual selenium chemistry and behaviour in comparison to sulfur for example.


Also has anyone made some NaHSe before. I tried yesterday via the Se + NaBH4 in Ethanol method and it didn't really work.

Se.JPG - 19kB

j_sum1 - 14-5-2016 at 23:34

I'd love to hear more about selenium chemistry. It will save me actually doing it. :D

fluorescence - 15-5-2016 at 01:57

Yeah avoid ! Such a nasty stuff. I was preparing a sample for the powder diffraction and only used the tip of the of the spatula like the tiny edge and had that on the sample carrier which was no pure Selenide but a mixture of my products and some Sesquiselenide that had formed. I couldt wash it since due to the Selenide it formed a lot of red selenium powder all over the sample as soon as it touched water and so I washed it together with the flux which was RbCl I think ? So the RbCl was really dry and started to suck up water from the air turning my sample into an H2Se Generator xD. The small amout of some tiny grains of Selenide exposed to air was enough to fully cover the complete hallway between my office and the diffractometer room that even as all doors were opened half an hour later when I came back you couldt walk there !!! That stuff is incredibly nasty. And I spent the whole day with the complete sample under the microcope. At one point it just cant get any worse. I always wanted to make H2Te but I think there is no amount tiny enough to actually do it. And that smell is so damn characteristic. H2S doesnt smell like garlic as people say it smells like rotten eggs H2Se smells a lot like garlic it isnt even that unpleasant because I think I know this smell from somewhere but it's usually too concentrated to be in a room with it. Like with chlorine gas, a tiny amount is just enough for your nose.
And also what I found really interesting is that as some might know elemental Selenium actually smells. I always thought this was H2Se and it probably is H2Se but the smell coming from a bottle of Se is a bit different to the smell of real H2Se. Not sure if this is due to concentration but those two have some differences.
Maybe one day I'll do some tellurium chemistry to try this out as well. Who knows.

fluorescence - 18-5-2016 at 06:12

Just discovered while drying my product that Thallium(I)Chromate seems to be thermochromic. Tried it 3 times in a row and it would quickly turn orange-red while heated even slightly and quickly turn yellow again afterwards. Not sure if this is already in the literature I didn't check yet but Tl-Chemistry just surprises me everytime I try it.



Tl Thermo.jpg - 320kB

crystal grower - 18-5-2016 at 06:43

Wow o.O, that's indeed interesting.

Hegi - 18-5-2016 at 23:08

Quote: Originally posted by fluorescence  
Just discovered while drying my product that Thallium(I)Chromate seems to be thermochromic. Tried it 3 times in a row and it would quickly turn orange-red while heated even slightly and quickly turn yellow again afterwards. Not sure if this is already in the literature I didn't check yet but Tl-Chemistry just surprises me everytime I try it.



Wow that is really amazing! :o I had never chance to work with Tl and its compounds. I heard about a few mercury compounds that are thermochromic. If you find more about, please share info. Thanks.

fluorescence - 20-5-2016 at 09:13

There is an interesting book on this topic. Not for solid state compounds but for coordination compounds called Inorganic Chromotropism. The book spends severals pages on thermochromism in for example mercury complexes and why and how it changes. Really interesting to read. Unfortuantely I dont have it I read it once but there is no ebook on it. I might try to get it one day and scan the pages.

The Volatile Chemist - 24-5-2016 at 15:07

Just got a sep funnel! Also, one of those actinic Erlenmeyer flasks and some small volumetric flasks, all of which my AP teacher had decided she didn't need. *Score*

Edit: At least I think it's a pretty picture...it's the most sophisticated piece of glassware in my lab...Also, it was formerly a piece used at OSU, our local university...
image.jpeg - 1.7MB

[Edited on 5-24-2016 by The Volatile Chemist]

fluorescence - 29-5-2016 at 03:22

Nice :D I got mine in a similar way. Went to a pharmacy when they closed and sold all their stuff and bought a lot of glassware. I think the seperating funnel was really cheap or even a gift like yours. Cant' really remember

arkoma - 29-5-2016 at 08:55

TVC-it IS pretty. Both of mine are only 250ml :(

mr.crow - 29-5-2016 at 13:43

Quote: Originally posted by The Volatile Chemist  
Just got a sep funnel! Also, one of those actinic Erlenmeyer flasks and some small volumetric flasks, all of which my AP teacher had decided she didn't need. *Score*

Edit: At least I think it's a pretty picture...it's the most sophisticated piece of glassware in my lab...Also, it was formerly a piece used at OSU, our local university...

[Edited on 5-24-2016 by The Volatile Chemist]


That's a nice sep funnel. Its always nice to save old junk from the university.

The Volatile Chemist - 3-6-2016 at 12:32

Quote: Originally posted by mr.crow  
Quote: Originally posted by The Volatile Chemist  
Just got a sep funnel! Also, one of those actinic Erlenmeyer flasks and some small volumetric flasks, all of which my AP teacher had decided she didn't need. *Score*

Edit: At least I think it's a pretty picture...it's the most sophisticated piece of glassware in my lab...Also, it was formerly a piece used at OSU, our local university...

[Edited on 5-24-2016 by The Volatile Chemist]


That's a nice sep funnel. Its always nice to save old junk from the university.

Thanks, indeed!

Arkoma, it's almost too big. But my teacher didn't offer me the 125mL one she had, it was in her Chemis-tree....

arkoma - 4-6-2016 at 11:54

I'd trade ya in a heartbeat...........................

Brain&Force - 7-6-2016 at 14:53

Holmium acetate isn't hygroscopic. This happened.

<img src=http://i.imgur.com/IlXJllv.jpg width=800>

The Volatile Chemist - 23-6-2016 at 10:54

Still discovering new things about the 'Lanths' I see...looks cool! About how much is in the vial, though?

The Plutonium Bunny - 26-6-2016 at 11:37

Recently, I've been really interested in crystals of pure metals, mostly for my element collection. After being inspired by The Backyard Scientist's video (see his post on page 23 of this thread), I decided to grow some of my own copper crystals. Over a period of six weeks, I used a 40g/L solution of copper sulfate and two copper electrodes with a current of always less than 10mA to grow some truly amazing copper crystal clusters. Unlike nearly all the other experiments I saw online, these crystals are very large and sharply defined - they are not nodules or rounded growths. I think that the extremely low current and the very long growth time contributes to the crystalline nature of this growth.

I made a YouTube video about how I grew this, and I also included a 360° rotation to show the entire crystal. https://www.youtube.com/watch?v=zZniOJ7swic

Also, for those who might like to repeat this experiment (the crystal is truly stunning), I wrote an extensive post on my website with details on the experiment. http://sciencewithscreens.blogspot.com/2016/06/experiment-53-growing-large-copper.html This post also has a link to my experimental data and observations I recorded during the six-week period.

Finally, I also included the less-impressive picture of my first attempt. This used currents of around 20mA over two weeks, and I accidentally broke the crystal. It's still pretty neat, though.

In the future, I will be trying other metals. Does anyone have experience with growing crystals of other metals? Thank you!



crystal - Copy.JPG - 84kB



IMG_1809 - Copy.JPG - 116kB

crystal grower - 26-6-2016 at 12:23

Well, thats... Awesome crystals!

Metacelsus - 26-6-2016 at 14:55

Quote: Originally posted by The Plutonium Bunny  
In the future, I will be trying other metals. Does anyone have experience with growing crystals of other metals? Thank you!


Bismuth forms nice crystals (see these). You can form them by slow cooling of molten Bi.

[Edited on 6-26-2016 by Metacelsus]

The Volatile Chemist - 26-6-2016 at 19:12

Huh, will have to try the copper crystal thing. I'm bad with the math behind electronics - did you just hook it up to a 9v battery and let it sit, or did you have to use a resistor? Should probably just check your website...

CrystalCage - 27-6-2016 at 17:51

First pic: Te metal, Se metal, copper nanoparticles and a copper acetate solution. Te and Se metal was a souvenir during my internship hahahaha :D. Copper nanoparticles were synthesized from ascorbic acid and copper acetate solution.


Second pic: A potassium ferrioxalate crystal. Around 1.5 inches in size.
Grown around 4 weeks, and grows cleanly and fast as well.
Made from dissolving iron with HCl, forming FeCl2 then precipitated into FeC2O4 using oxalic acid, washed away the chlorides with water, then oxidized into Fe(OH)3 with H2O2 made basic with K2C2O4. The resulting precipitate (Do not decant away the solution!) is then dissolved with oxalic acid again forming apple green solution.

The brown stain is the reacted solution with light, meaning it is light sensitive.
IMG_20160430_204231.jpg - 98kB
IMG_20160628_092447.jpg - 46kB

[Edited on 28-6-2016 by CrystalCage]

Texium - 28-6-2016 at 11:16

Yes, it's quite light sensitive. Make sure to keep your crystal in the dark whenever you aren't taking it out to show somebody, or else you'll find after a while that it will start to turn yellow and crumble... I had a few nice ones that this happened to over the course of a year or so, as I had assumed that they had to be wet to decompose. I was wrong. I have another bag of smaller crystals that were prepared at the same time and kept in a dark drawer, and they are still brilliantly green.

Hegi - 30-6-2016 at 05:19

Quote: Originally posted by The Plutonium Bunny  
Recently, I've been really interested in crystals of pure metals, mostly for my element collection. After being inspired by The Backyard Scientist's video (see his post on page 23 of this thread), I decided to grow some of my own copper crystals. Over a period of six weeks, I used a 40g/L solution of copper sulfate and two copper electrodes with a current of always less than 10mA to grow some truly amazing copper crystal clusters. Unlike nearly all the other experiments I saw online, these crystals are very large and sharply defined - they are not nodules or rounded growths. I think that the extremely low current and the very long growth time contributes to the crystalline nature of this growth.



Hi man,

very nice work! I decided to set up the same experiment and grow my own crystals. I used LM317 as well with 2x120 ohm resistor and potentiometer on adjustement pin of LM317. This resulted in 0.30V between cathode and anode but I could not measure current flowing through the circuit. Display stayed at 0.00 mA. Something must have gone wrong. Would you mind posting your LM317 circuit scheme and how did you measure volatge and current?

Thanks a lot! :)

The Plutonium Bunny - 1-7-2016 at 07:57

Quote: Originally posted by Hegi  


Hi man,

very nice work! I decided to set up the same experiment and grow my own crystals. I used LM317 as well with 2x120 ohm resistor and potentiometer on adjustement pin of LM317. This resulted in 0.30V between cathode and anode but I could not measure current flowing through the circuit. Display stayed at 0.00 mA. Something must have gone wrong. Would you mind posting your LM317 circuit scheme and how did you measure volatge and current?

Thanks a lot! :)


Certainly! Here is a schematic I drew in Paint of my setup. The five 1N4007 diodes drop the output voltage a little bit so that I can get lower output voltages with the LM317. Also, the resistors and potentiometers don't have to be exact- adjustments will still give you a wide range of voltages.

Also, something I learned a while back is that to measure current with a multimeter, the electricity must flow through the multimeter. This is different from measuring voltage, where the multimeter connects to two opposite points. Measuring current requires breaking the circuit and connecting the multimeter to either end of the break. It took me a while to learn this. :)

Good luck, and keep trying! It will be worth it in the end!





copper crystal.png - 25kB

aga - 1-7-2016 at 08:14

It's always a good idea to decouple the ADJ input and have at least a bit of smoothing on the output, thusly :

LM317.gif - 10kB

If not, there is a risk of oscillation which is hard to see on a digital multimeter.

Hegi - 1-7-2016 at 08:48

Thanks guys, my scheme is the same (except i did not use capacitors)... After 24 hours dendritic copper crystals about 0.3-0.4 mm size can be observed. I did measurement of current in the way it is supossed to be measured but NOTHING happened - value stays at 0.00 mA. Voltage is in range 0,27-0,30V and the resistance of the solution is approximately 220 ohm.

Did you observe forming small dendrites at the begining? .. or should I start again? :mad:

The Volatile Chemist - 8-7-2016 at 16:15

I think hackaday did a little article on this prep, was that the result of anyone here? I think it had the first image posted in the article.

alexleyenda - 8-7-2016 at 22:19

Woah, the copper crystals are amazing, I must try that one day.

A colorful reaction to make a new compound and its crystals during my internship.

[Edited on 9-7-2016 by alexleyenda]

rx plus belle lowq.jpg - 533kBbest cristaux low q.jpg - 536kB

wg48 - 14-7-2016 at 09:14

The effect of 8bar water on the seat of my sink water tap.
Its soft water but it may have been caused by inclusions in the poor quality brass or cracks.




100_1092.JPG - 516kB

PHILOU Zrealone - 14-7-2016 at 11:45

Quote: Originally posted by wg48  
The effect of 8bar water on the seat of my sink water tap.
Its soft water but it may have been caused by inclusions in the poor quality brass or cracks.





Soft water is better/gentle for resistance into warming systems but it is also more corrosive to plumbing and piping than hard water.
No pain, no gain :( ;)...no universal curing agent :P

[Edited on 14-7-2016 by PHILOU Zrealone]

Metacelsus - 20-7-2016 at 14:21

This compound I made (at the research lab where I'm working this summer) shows drastically different fluorescence in solution (30 mg/mL in CDCl3) vs. as a solid.

aggregation affecting fluorescence.png - 7.2MB

[Edited on 7-20-2016 by Metacelsus]

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