Pretty Pictures (1)

Some 20 g of copper (II) nitrate hydrate, on a plastic tea strainer. I believe it’s the hexahydrate but have yet to determine its MP. It was obtained by dissolving 10 g conductor copper in 70 % nitric acid, then reducing the obtained solution by about a third, cooling, adding seed crystals, then icing. Most of the solution then crystallised out. The blue is more intense to the naked eye than the photo promises.

Edit: It's been verified to be the hexahydrate: it melts way below 50 C and resolidifies on cooling.

[Edited on 11-10-2011 by blogfast25]

@blogfast- I agree, copper nitrate is much prettier than copper sulfate

macro photography

@blogfast25

Does your camera have macro capability? I find it makes a huge difference when taking pictures of chemicals. The symbol usually looks like a flower:



I'm asking because it looks like the picture is out of focus and it doesn't need to be.

This is not meant to be criticism, just constructive feedback

Hydrated copper(II) nitrate has one of the most beautiful blue crystals seen in labs. It's close to the beauty of tetraamminecopper(II) sulphate or mercury tetrathiocyanatocobaltate(II).

The only problem is that it's very hygroscopic. Later this year I've made some and I've stored them wet in the bottle, but added an ampoule of sodium hydroxide and quartz sand. Over the couple of months, that little sucker managed to suck in both the water and nitric acid residues, and even started eflorescenting the nitrate salt, so I've removed it.
Sometimes when I look at them, I just want to eat them because they look so nice.

Some people dry their crystals in desiccators, but I prefer finishing the job in the bottle. I just take/make an ampoule, put the mixture inside, and stuff some cotton or rough cork (if possible). If the bottle is not tilted, the contents will be super dry in a matter of days. It's a neat way to reduce the consumption of desiccant because the space available for vapors is very small, and if there are any other volatiles, they contaminate the ampoule only.
It's neat for weighing, too.

Copper nitrate is notorious for its will to stay in a solution.

Large, well developed crystals are very hard to obtain. Desiccation would work, but it would require large amounts of desiccant with power of desiccation greater than copper nitrate, and that really narrows it down because Cu-nitrate is one hell of a desiccator itself.
I've just put the desktop lamp under the evaporating dish and cover it with a bent piece of filter paper. Ventilation is neccessary because of excess nitric acid.
I've forgot about it and later found it dehydrated. That happened 3-4 times in a row (I know, I'm lazy), but I've managed to get them, eventually. They're tiny and clumped together.

You just need to remove as much water as you can, and then the whole solution turns solid in a few seconds, as it cools down. Basically, something similar to sodium acetate.
Later, drying with NaOH in a sealed space is neccessary because there's always some water that didn't end up in the crystal lattice.

[Edited on 13-10-2011 by Endimion17]

I had soem very lovely copper nitrate crystals from a solution, dried over a month by windowsill Pics coming soon, I guess.

http://www.sciencemadness.org/talk/viewthread.php?tid=16646#...

http://www.sciencemadness.org/talk/viewthread.php?tid=16220#...

http://www.sciencemadness.org/talk/viewthread.php?tid=15513#...

http://www.sciencemadness.org/talk/viewthread.php?tid=11218#...

Quote: Originally posted by blogfast25

@MrHomeScientist: try seed crystals and what Endimion said. Make seed crystals by dipping a glass rod in your solution, then gently evaporating the water well above a Bunsen or other flame, making sure not to overheat. Sprinkle these into your solution. Bear in mind the fantastic solubility of Cu(NO3)2: at 0 C it’s about 80 g/100 g of water, off the top of my head!

This is a sodium bicarbonate solution I left on a shelf for too long. Nothing special, but pretty nonetheless.



I destroyed the crystals in attempt to improve the lighting and to insert a black background, sadly.

This is what I essentually used for my NOx Generator.





9Kv 30mA

Large needles of oxalic acid (and that’s only the first crystallisation!) with a weak solution of trioxaloferrate (III) (FeOx₃^3- as supernatant liquid. At low concentrations the trioxaloferrate complex is slightly fluorescent:

Hello everyone, this is uranyl nitrate hexahydrate (fused and cast into the vial so that there's no dust), fluorescing under long-wave UV.
It is a very bad photo because I don't know how to use my camera in low-light conditions, but I think the blur on the image emphasises the glow and actually gives quite a nice effect .

Edit: I'm totally failing at uploading an image. Hang on a minute, I'll remember how to do it soon...

[Edited on 24-11-2011 by Nick F]

[Edited on 24-11-2011 by Nick F]

Quote: Originally posted by Nick F

Hello everyone, this is uranyl nitrate hexahydrate (fused and cast into the vial so that there's no dust), fluorescing under long-wave UV. It is a very bad photo because I don't know how to use my camera in low-light conditions, but I think the blur on the image emphasises the glow and actually gives quite a nice effect . Edit: I'm totally failing at uploading an image. Hang on a minute, I'll remember how to do it soon... [Edited on 24-11-2011 by Nick F] [Edited on 24-11-2011 by Nick F]

Quote: Originally posted by Nick F

[...] It is a very bad photo because I don't know how to use my camera in low-light conditions, but I think the blur on the image emphasises the glow and actually gives quite a nice effect . [...]

What I do in low light conditions is I set my camera down on a pile of books, (or on a tripod) and use the timer option to take a picture.

Here's why. In low light conditions, the camera needs to receive approximately the same amount of light as if it were taking a picture in daylight. The result is a longer exposure length. So if you do so much as twitch during that interval, the picture is ruined.

Setting the camera down on a pile of books and using the timer ensures that the camera won't move when you're taking the picture.

But whatever you do, don't use flash

blogfast25, I have about 29g, the vial is 6.5cm tall.

Bezaleel, the UV source is a common 4W fluorescent tube type, the sort that is used to detect fake money. It looks like this:



I believe they peak at somewhere around 360nm. It is standing up just to the right of the image, its reflection can be seen near the top right of the vial.

White Yeti, I don't even know if my camera has a timer option, it is quite old and was cheap when I bought it!

[Edited on 25-11-2011 by Nick F]

A layer of 6-methylquinoline under water resulting from steam distillation.

Small crystals of rac. N,alpha-dimethyl-beta-phenethylammonium chloride.
(Ok, this should go to the ugly pictures thread, but there is none. )

Thanks to Nick F for the suggested type of UV lamp (found one for under $5 on e-bay). Comparison of uranyl nitrate, erbium acetate, and neodymium carbonate under tungsten incandescent light and UV light.


Images of lead iodide. I dissolved 0.35 grams in 100ml of water, and boiled for about 10 minutes. The substance dissolved slowly, the solution gradually becoming clear.
Cooling down, thin colourless platelets immediately formed on the liquid surface. After cooling down to RT, very many sparkling and deeply yellow platelets had formed.

I enjoy the PbI2 golden rain, good job

Shattered glassy mass of 5-carboxypentyltriphenylphosphonium bromide (I think I named that correctly...) prepared from 6-bromohexanoic acid and triphenylphosphine

The molten material is viscous and can be drawn into threads and so forth, like a proper silica glass, but at a vastly lower temperature.

The crystalline salt was prepared by precipitating the product from chloroform with ethyl acetate.

Quote: Originally posted by plante1999

Wow! This is a realy nice picture! Are you doing a video to show the synthesis on Youtube? [Edited on 24-12-2011 by plante1999]

I was attempting to "blue" some steel over the flame of my modified alcohol burner. I met limited success, as small areas of the piece of metal in question turned to a corrosion resistant iridescent blue. My camera does not pick up the vivid colours of the blued metal, so I have no pictures to display. But as I was washing the piece of metal clean, I found that the soot deposited on the piece of metal made the steel hydrophobic. It's nothing special at all, as the layer of soot wears off very rapidly and does not stand up against abrasion even of the gentlest kind. But it sure does make a nice picture I thought I might share with the community. Without further ado, here is my failure/success, several drops of water on the soot covered bottom of a tin can, the cheapest way you can demonstrate the phenomenon of hydrophobicity.

Quote: Originally posted by mr.crow

Wow!!! At least you can use some of the footage for the next video as a summary. looking forward to it Synthetic capsaicin, sounds spicy

A 7 mm crystal of p-dimethoxybenzene à la PainKilla that grew directly out of the reaction mixture.

Drops of aniline condensing on the upper wall of an RBF while vacuum-distilling aniline. The attachment aniline.background needs to be renamed to a .jpg and is a 1920x1200 image if you'd like to use it as a background. (This gets around the forum's size limits for pictures)

[Edited on 1-1-12 by UnintentionalChaos]

Attachment: aniline.background (730kB)
This file has been downloaded 1132 times

Here is some pictures of a nickelocene, bis(cyclopentadienyl)nickel(II) synthesis I conducted at my home lab over Christmas break.



[Edited on 2-1-2012 by benzylchloride1]



[Edited on 2-1-2012 by benzylchloride1]



[Edited on 2-1-2012 by benzylchloride1]



[Edited on 2-1-2012 by benzylchloride1]

Your selection of glass, chemicals and analytical equipment is unparallelled among amateurs, benzylchloride1. May I ask how you obtain your chemicals? Seeing as you live in the US, most people run into a few problems on that front.

How did you synthesize the nickelocene? I have considered buying some dicyclopentadiene to prepare metallocenes myself. I'm guessing it's the dicyclopentadiene you have in that solvent still?

Btw - I and many others would love if you'd write down something for the prepublication section. You obviously have many interesting, challenging, novel (and legitimate) projects. I for one would love a topic summarizing your carpanone synthesis, as I find total synthesis to be probably the most interesting subject in all of chemistry.

Edit: Oh, and those ampoules are simply lovely

[Edited on 2-1-2012 by Lambda-Eyde]

I obtain many chemicals off of Ebay, and I also know someone that I can buy chemicals through. I am thinking about putting a article together for the prepublication section on the nickelocene synthesis since I really enjoy this prep. I used balloon grade helium as the inert gas in this synthesis. The single piece solvent still was used to distill my THF from sodium benzophenone ketyl prior to use, The pictures do not do justice to the color of the THF still pot. In this post there is a picture of the still that I used for cracking the dicyclopentadiene. I would recommend buying some dicyclopentadiene since it is usually dirt cheap if you have a source for it and it is useful for so many things. I prepared nickel (II) chloride from nickel (II) carbonate purchased on Ebay. From the nickel (II) chloride, I prepared hexaamine nickel(II) chloride using 30% aqueous ammonia, I bought this from High Valley Chemical. The 10% stuff from Ace Hardware can be used, but it requires more acetone for crashing the product out. I would recommend making this coordination complex to anyone interested in amateur chemistry. I produced a solution of sodium cyclopentadienide in THF by adding cyclopentadiene to a stirred suspension of powdered sodium in THF. After the formation of the sodium cyclopentadienide, which is light purplish pink in color, the hexaaminenickel(II) chloride is added and the mixture is slowly heated to reflux, resulting in the generation of a large amount of ammonia gas and a gradual color change to the characteristic bright green color of nickelocene. The mixture was then filtered through pool filter aid under helium, and the solvent removed under vacuum, leaving the crude product, which was then sublimed under dynamic high vacuum from a 80 C oil bath. I would recommend perusing surplus stores of major universities on a regular basis, this seems to be the best way to build a lab very quickly. Interesting that you brought up the carpanone synthesis since I have been working on this lately, I am very close to finishing it, I had to rethink how to synthesize the sesamol. Take a look at the carpanone thread for an update. I am also thinking about writing an article on the preparation of bis(1,2-diphenylphosphino)ethane and other chelating phosphines. I have been interested in these phosphines for making organometallics and coordination complexes. There seems to be no report in the literature for preparing these compounds in solvents other then liquid ammonia. I ended up using a patent for making sodium diphenylphosphide in anhydrous ethylenediamine for my purposes. After adding 1,2-dichloroethane, allowing the mixture to stand overnight and a aqueous work up I got a 60% yield of the product. I tried the reaction twice on two different scales and the yields were within six percent of each other. I am planning on preparing some of the corresponding phosphines from dichloromethane and 1,3-dichloropropane.

[Edited on 2-1-2012 by benzylchloride1]

[Edited on 2-1-2012 by benzylchloride1]



[Edited on 2-1-2012 by benzylchloride1]

[Edited on 2-1-2012 by benzylchloride1]

[Edited on 2-1-2012 by benzylchloride1]

Chemiluminescence of 2,4,5-triphenylimidazole!
It's nothing special, but i like this compound!

Running a Sodium Perchlorate cell (Lead Dioxide Anode) with a very high concentration of Perrchlorate and had a power cut. The temperature of the cell fell from 50 to 30 degrees C and I obtained some nice shards of Sodium Perchlorate on the Anode. Most of them seem to come from the MMO just above the Anode proper.



[Edited on 25-1-2012 by dann2]

Just some gray titanium tubing anodized/flamed with a propane torch. I found if you polish the tubing surface with a very fine sandpaper it produces a far more vivid color pattern when the oxide layer forms. I think from memory, the first color to come up is a bronze-gold and then blue the more you heat it. After that it's tricky to get the pinks and greens. If you are not careful and heat it too much, it reverts back to a drab gray with faint colors barely seen. The best color is seen when viewed in indirect sunlight.




[Edited on 26-1-2012 by Morgan]

Recently I did some copper electroplating / brass electroetching. After I was through I let the electrolyte evaporate naturally and this is what I was left with.

- I know CuSO₄ has been done to death but this is all I have lately.

Sodium Chlorate crystals with some Sulphur.

I walked into my lab and was greeted with a pleasant surprise. The urea I extracted from fertiliser crystallised into beautiful large crystals.
Picture:

Those are some nice crystals.
Do you guys ever get into situations where you need the chemical which crystalized with stunning beauty and size, or you need the glassware where it happened in? What do you do? Do you make another sample, buy more glassware or you destroy the crystals?

Quote: Originally posted by Endimion17

Those are some nice crystals. Do you guys ever get into situations where you need the chemical which crystalized with stunning beauty and size, or you need the glassware where it happened in? What do you do? Do you make another sample, buy more glassware or you destroy the crystals?

Quote: Originally posted by UnintentionalChaos

Break those crystals! Take a pic to post in this thread and then pulverize them.

I can't agree more. That's exactly what I did! Apparently, urea crystals are really fragile, I agitated the jar and all the crystals came loose and turned into a slush. I can post a picture, but it isn't pretty

To be honest, I was expecting the water to evaporate and leave a mushy amorphous semisolid of urea mixed with water, I wasn't expecting crystals. The fact I got crystals is quite surprising.
Did anyone else accidentally grow large crystals of urea? The only pictures of urea crystals I found so far were of the microscopic kind.

Quote: Originally posted by plante1999

Nice! How long did it took to dry?

Quote: Originally posted by Endimion17

^^nor they'll ever become. Industrial purity urea is hygroscopic, sometimes even deliquescent (lower quality, moist environment). The more times you try to recristalize it, the less hygroscopic it becomes. Judging by the color of your sample, they aren't pure enough. But I was thinking about really stunning, large crystals or even monocrystals. I'd probably store them for good unless the substance is for some reason too important for my work.

I know urea is a desiccant, I've actually bought some things that had urea packs to absorb moisture instead of silica gel; sodium hydroxide is not used for obvious reasons

For this first purification, I wasn't aiming for high purity. I bought urea based fertiliser from Lowes and it contains ~30% urea (highest content of all the the fertilisers). The rest of it is "slow release polymer coated sulfur" among other things, most of which are insoluble in water.

Boiling fertiliser in water was the simplest way to extract the urea from all the other junk. I boiled it in a soda lime mason jar, the bottom of which blew off and made a mess. I mopped up all the water solution and put it in another jar to dry, where I forgot it until today. This is why my sample is impure

I'm wondering if I'd get a higher yield by evaporating urine, considering all the trouble I went through for so little urea.

Unknown copper compound crystallized at the bottom of a beaker:





I have larger resolution images that provide a much better view, but I can't find a way around the 800 pixel image width limit.

These were formed from an attempt to neutralize a copper(II) chloride solution with baking soda. Bicarbonate was added to the blue solution until fizzing stopped, but the blue color remained. I had thought to precipitate copper carbonate, for easier disposal. I left the clear solution overnight, and came back to see these beautiful tiny crystals! They look like copper(II) chloride still, strangely. They are sitting on a white layer of unreacted baking soda.

Quote: Originally posted by White Yeti

I know urea is a desiccant, I've actually bought some things that had urea packs to absorb moisture instead of silica gel; sodium hydroxide is not used for obvious reasons For this first purification, I wasn't aiming for high purity. I bought urea based fertiliser from Lowes and it contains ~30% urea (highest content of all the the fertilisers). The rest of it is "slow release polymer coated sulfur" among other things, most of which are insoluble in water. Boiling fertiliser in water was the simplest way to extract the urea from all the other junk. I boiled it in a soda lime mason jar, the bottom of which blew off and made a mess. I mopped up all the water solution and put it in another jar to dry, where I forgot it until today. This is why my sample is impure I'm wondering if I'd get a higher yield by evaporating urine, considering all the trouble I went through for so little urea.

Quote: Originally posted by Endimion17

I'm surprised to hear 30% is the highest content you can buy. I thought technical grade urea is widely available. I can go into a store and buy tons of it every day.

Quote: Originally posted by White Yeti

Quote: Originally posted by Endimion17   I'm surprised to hear 30% is the highest content you can buy. I thought technical grade urea is widely available. I can go into a store and buy tons of it every day. Maybe I'm looking in the wrong store. I hear lots of people go to Home Depot for chemicals, but I live closer to a Lowes instead. I spent half an hour looking through all their fertilisers and the highest I could find was 30%. I also looked for sulfuric acid drain cleaner and copper sulphate, neither of which I could find. I'll make myself a note to check out if Home Depot has a larger selection of chemicals.

Quote: Originally posted by White Yeti

Thanks for the suggestions, but this is not a thread dedicated to buying and finding chemicals. In any case, the recrystallisation worked like a charm, and strangely enough, the solution did not creep up the sides. Does anyone know why? Whenever I do recrystallisations of any kind, I always get "creep" where the solution would go up the sides of the container and sometimes go over the rim.

Quote: Originally posted by zoombafu

I usualy get that creep when i use water as a solvent, so I think it has something to do with the meniscus and the surface tension.

Here's a picture I took of some copper II chloride crystals that I produced.

Quote: Originally posted by White Yeti

Interesting... About CuCl2, I got a colourful equilibrium going between copper acetate and copper chloride once. I dropped some CaCl2 into some copper acetate solution and swirled. Green a copper chloride solution would form around the CaCl2 and then it would turn into blue acetate again after some time. If you swirrled it again, the copper chloride would form again, and disappear just as fast. I'll post a picture if I get the chance. My camera doesn't bring out the colours very well, but it's a fun thing to try out if you're really bored.

Salicylic Acid Needles

[Edited on 1-3-2012 by Vlassis]



[Edited on 1-3-2012 by Vlassis]

Oxalic Acid from Ethylene Glycol/Nitric Acid

copper acetate

A mix of copper acetate and copper metal in Hdpe dish.

I love the needle crystal pics lately. I'll try to keep the theme going with one of my own.

Testosterone barbs/needles forming and settling out:


Tank

There we go centered.

It's surprisingly beautiful, and now we can see the copper metal. If only I had the brains to take pictures of these things when they happen.

Phthalic acid





Phthalic anhydride boiling/condensing/freezing


[Edited on 3-2-2012 by AirCowPeaCock]

Quote: Originally posted by AirCowPeaCock

It's surprisingly beautiful, and now we can see the copper metal. If only I had the brains to take pictures of these things when they happen. Phthalic acid Phthalic anhydride boiling/condensing/freezing [Edited on 3-2-2012 by AirCowPeaCock]

Nice phtalic acid! Did you synth it yourself and if so, how?

Quote: Originally posted by m1tanker78

I love the needle crystal pics lately. I'll try to keep the theme going with one of my own.

Sure puts the 'tossed' in testosterone ─ a 'testament' to all things testicular . . .()

Quote: Originally posted by AirCowPeaCock

That phthalic acid was synthesized using the same process nurd rage uses--which I dislike. Its not as much as it looks, its mostly air--based on my phthalic anhydride yield (4.3 g) [...] [Edited on 3-2-2012 by AirCowPeaCock]

Quote: Originally posted by AirCowPeaCock

yeah, its not too expensive--atleast not if you just want a few gram. I don't know how he got 13g of Phthalic anhydride from 50g of gloves. I could only get half that will 200g of gloves! -- my gloves must suck!

Hope I am not repramanded for (bad speelling too pehaps) putting ugly pictures in the pretty pictures thread.
Here we have a bar of pure Copper that has had the top portion melted into a ball. Copper has a high melting temperature and I have been able to achieve this melting feat using a lit match! The flame of a lit match can easily melt Copper as the picture shows.
There is some oxide on the ball. I should have perhaps cleaned up the Copper with an acid dip or somesuch.

The bar of Copper (I should mention) is 48swg Copper wire.
Dann2

Quote: Originally posted by blogfast25

Quote: Originally posted by AirCowPeaCock   yeah, its not too expensive--atleast not if you just want a few gram. I don't know how he got 13g of Phthalic anhydride from 50g of gloves. I could only get half that will 200g of gloves! -- my gloves must suck! Even 13 g of PAA from 100 g of gloves would sound improbably high to me. DOP content of gloves: max 30 %, something like that? Also: try an old shower curtain, cheaper than virgin gloves! [Edited on 3-3-2012 by blogfast25]

Quote: Originally posted by UnintentionalChaos

I found shower curtain to have much lower DOP content than the gloves. The shower curtain I tried to extract contained 10% DOP based on mass lost after several hours of soxhlet extraction. The gloves I used were a solid 36% DOP and I scraped 73.6g of fairly clean phthalic acid from 570g of gloves following a recrystallization (85% yield)

Recrystallization of Piperine

Got to love the needles. Here is piperine (&chavicine?) that was extracted from black pepper with IPA being recrystallized from 10ml of etOH/IPA mix. Slowly cooled overnight. One of my favorite things is watching a recrystallization come to fruit. Ever so satisfying...

Quote: Originally posted by AirCowPeaCock

I think the way to go is xylene oxidation, I've found a few references to oxidation in the liquid phase. Even with 5% efficiency (I imagine) it would be much cheaper than any PVC source.

Quote: Originally posted by White Yeti

@Bot0nist Nice crystals! Those rival the beauty of those on the wikipedia page.

Quote: Originally posted by Bot0nist

25grams fresh ground aromatic pepper. Followed the same workup I used <a href="http://www.sciencemadness.org/talk/viewthread.php?tid=10676&page=2#pid222835">here</a> .