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Author: Subject: Copper Compound Collection
j_sum1
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[*] posted on 29-11-2014 at 20:48


Quote: Originally posted by blargish  
Quote: Originally posted by nlegaux  
I got some 57% Sodium Dichloroisocyanurate the other day. I guess I will recrystallize it and try making the Copper Complex :D


Here is a cool document with some information about the complex, and the procedure for making it. Apparently, the complex is of the form, Na2[Cu(C3N3O3Cl2)]



zts16 has a lovely picture here. http://www.sciencemadness.org/talk/viewthread.php?tid=45845&...

I feel somewhat inspired. The colour is really pretty. I don't have any sodium dichloroisocyanurate though. I do have some TCCA and if I am not mistaken I can make some by reacting with NaOH.
Thanks for the link although I haven't read much of it yet. There are loads of possibilities. I will also substitute NaOH for KOH and see what the potassium variant looks like. And I can substitute Cu for Pb, Ni, Co and possibly Mn. This could be a fun little project.

By the way, in this post, Nicodem reports a molecular formula different from what you have stated above. Apparently there are 4 dichloroisocyanurate ligands.
Quote: Originally posted by Nicodem  
The reaction of CuSO4 and sodium dichloroisocyanurate in water is described in US3055889 and is claimed to give Na2[CuL4] where L is the dichloroisocyanurate ligand: (C3N3O3Cl2)-. Described are also the preparation of analogous Ca, K, Ba and Li tetrakis(dichloroisocyanuro)cuprates (or whatever they are called). Analogous Cd and Ni coordination compounds are also reported.
US3115493 describes the preparation of a lead dichloroisocyanurate and this is then used in the preparation of Pb[CuL4].
An analogous potassium nickelate dichloroisocyanuric complex is also known (DOI: 10.1016/0022-1902(64)90014-4).

[Edited on 14/3/2014 by Nicodem]
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blargish
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[*] posted on 29-11-2014 at 21:00


Quote: Originally posted by j_sum1  


By the way, in this post, Nicodem reports a molecular formula different from what you have stated above. Apparently there are 4 dichloroisocyanurate ligands.


[Edited on 14/3/2014 by Nicodem][/rquote]


Oops, my bad. There formula given in the document is actually Na2[Cu(C3N3O3Cl2)4], you're right.




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[*] posted on 29-11-2014 at 21:09


blargish, I mispoke in my previous post, what I think I have is copper (II) chromate, which is described in the CRC as reddish brown crystals with the formula of CuCrO4.
nlegaux, the 70% ethanol I used for my recrystallization can be bought cheaply at most pharmacies and works well. Good luck with your isolation.




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[*] posted on 30-11-2014 at 08:18


Trying to recrystallize Ibuprofen with IPA failed... No crystals formed when water was added, even when chilled overnight. I guess I will have to go buy some Ethanol :)

[Edited on 11-30-2014 by nlegaux]
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[*] posted on 14-1-2015 at 04:47


Hi,I am new in this.I want to know how to make copper(||)acetoarsanite (Paris green).this is one of copper compound.
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[*] posted on 14-1-2015 at 09:15


I like making Fehling's solution, although you kinda get a mix of compounds if you crystallize it out, it's still pretty enough to 'collect'.
Try copper(II) ferricyanide and copper(II) ferrocyanide, both different brown-like colors.




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[*] posted on 14-1-2015 at 09:51


Quote: Originally posted by sum  
Hi,I am new in this.I want to know how to make copper(||)acetoarsanite (Paris green).this is one of copper compound.


So why not look up a preparation for it? Simply google searching it seems to indicate one can just add arsenic trioxide to a copper acetate solution. It might be more complicated, so maybe do some research.




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[*] posted on 14-1-2015 at 10:02


Quote: Originally posted by Zyklon-A  
Thanks. Hydrobromic acid and copper (II) hydroxide or carbonate.
HBr (aq) was made from H2SO4 and NaBr I think - not an easy reaction to do, cause it partially oxidizes bromide to bromine.
I ought to find a better way to make such a useful acid.

There is a better way to make CuBr2, without the acid.

NaBr + CaCl2 <--> NaCl + CaBr2

CaBr2 is about 5 times as soluble as NaCl, so it is easily purified by concentration, filtering most of the NaCl, then fractional crystallization.

CaBr2 + CuSO4 --> CuBr2 + CaSO4

Calcium sulfate is 265 times less soluble than CuBr2 (basically insoluble) and can be filtered out, leaving a solution of CuBr2.




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[*] posted on 14-1-2015 at 16:39


Quote: Originally posted by Praxichys  
Quote: Originally posted by Zyklon-A  
Thanks. Hydrobromic acid and copper (II) hydroxide or carbonate.
HBr (aq) was made from H2SO4 and NaBr I think - not an easy reaction to do, cause it partially oxidizes bromide to bromine.
I ought to find a better way to make such a useful acid.

There is a better way to make CuBr2, without the acid.

NaBr + CaCl2 <--> NaCl + CaBr2

CaBr2 is about 5 times as soluble as NaCl, so it is easily purified by concentration, filtering most of the NaCl, then fractional crystallization.

CaBr2 + CuSO4 --> CuBr2 + CaSO4

Calcium sulfate is 265 times less soluble than CuBr2 (basically insoluble) and can be filtered out, leaving a solution of CuBr2.

Yup. Of course, fractional crystallization isn't the easiest, but still.




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[*] posted on 14-1-2015 at 18:30


Here's an idea for displaying your copper compounds. I tried to recreate the peg game that you find at Crackle Barrel with copper compounds and it turned out pretty good.
The compounds are sealed in culture tubes and the triangle is machined acrylic. I have since made a new and improved version, but I don't have a picture handy at the moment.



CopperTriangle.jpg - 141kB
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Zyklon-A
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[*] posted on 14-1-2015 at 18:46


Thanks for that Praxichys, I'll be sure to use that method next time and save what little HBr(aq) I have left.
Beautiful collection Squall181! I know what most of those are, but could you list them?
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[*] posted on 14-1-2015 at 18:57


In my experience copper ferricyanide is a yellow color.



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[*] posted on 14-1-2015 at 19:16


The one's visible in the picture from top right are: Copper Acetate, Copper(II) Chloride, Copper(II) Oxide, Copper, Tetraaminecopper(II) sulfate. The rest are copper nitrate, copper carbonate, copper bromide, copper(I) oxide, copper(I) chloride, copper sulfate, copper sulfide, Copper Cyanurate, and copper aspirinate. I believe that all the ones I have.
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[*] posted on 14-1-2015 at 22:25


Quote: Originally posted by Squall181  
Here's an idea for displaying your copper compounds. I tried to recreate the peg game that you find at Crackle Barrel with copper compounds and it turned out pretty good.
The compounds are sealed in culture tubes and the triangle is machined acrylic. I have since made a new and improved version, but I don't have a picture handy at the moment.





This looks really, nice, I'll have to see what local prices for Plexiglas are. Here is a picture of my collection. Copper benzoate was made after this picture was taken and hence not in it.

copper.jpg - 294kB

From left to right:
Chevreul's salt - Copper I iodide (with water) - Pyridine copper iodide - tetrachlorocopper complex - Copper oxalate - Copper II chloride - Copper stearate - Copper carbonate - Copper acetate - Copper oleate - Copper (durr) - Copper aspirinate - Copper II sulfate - Copper nitrate - Tetraaminecopper II sulfate - Pyridine/Copper nitrate complex - Copper phthalocyanine - Copper sulfate/cyanurate - A mislabeled vial of decomposed copper complex (I have no clue where it came from I found it in a corner of a shelf, but I have no clue what it is.) - Copper bromide - Copper II oxide




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[*] posted on 15-1-2015 at 01:32


Copper (en) perchlorate is fun. Woelen & myself have synthesised this from copper sulphate, ammonium perchlorate and ethylene diamine.

Attachment: Copper.mp4 (1.2MB)
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[*] posted on 15-1-2015 at 12:33


Quote: Originally posted by bismuthate  
In my experience copper ferricyanide is a yellow color.

I've been doing a lot of Iron cyanide indicator experimentation recently, it has always had a yellow brown color, with a tint of green, but I just call it brown. It's kinda brown mustard colored for me. I've seen with coloration for others, it has to do with the concentration of the ferricyanide and the concentration of the iron cyanide, which change crystal size.


Nezza, that does look fun!
Numos, your collection is great!




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[*] posted on 15-1-2015 at 23:43


Hey guys try copper tungstate by treating sodium tungstate and copper sulfate or nitrate solutions to obtain dense copper tungstate precipitate.:)
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[*] posted on 15-1-2015 at 23:45


and try potassium bisoxalatocuprate dihydrate


[Edited on 16-1-2015 by sasan]

potassium bisoxalatocuprate dihydrate.jpg - 810kBcopper tungstate.jpg - 692kB
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[*] posted on 15-1-2015 at 23:50


oh I have forgotten copper tetraiodomercurate

[Edited on 16-1-2015 by sasan]

copper tetraiodomercurate.jpg - 727kB
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[*] posted on 16-1-2015 at 00:04


The mention of an orange Cu(II) complex in this paper Copper(II) Complexes With Lignin Model Compound Vanillin got me interested. The synthesis appeared easy so I gave it a go:

[Cu(C8H7O3)2(H2O)2] (2): [Cu2(O2CCH3)4(H2O)2]
(0.160 g) was dissolved at room temperature in 10.0 mL
of acidified water (one drop of glacial acetic acid). The
solution and solid vanillin (0.244 g) were slowly heated
in two separated flasks. When vanillin had melted, the
acetate solution was put over melted vanillin that turned
red and dissolved in ~5 seconds. Orange crystals of 2
were filtered off next day and dried in air for a day.

However both of my attempts following the above failed. There was obviously a reaction because the blue copper acetate solution instantly turned the most beautiful emerald green upon addition to the molten vanillin. Upon cooling a large crop of pale green needle crystals formed which are quite possibly compound 1.

Anyone else care to try this and see if they can achieve the orange compound? I'd really like to know where I went wrong (currently suspecting not high enough temperature at mixing time). I'll need to make some more copper acetate before making another attempt.
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[*] posted on 16-1-2015 at 10:14


Quote: Originally posted by warteo  
The mention of an orange Cu(II) complex in this paper Copper(II) Complexes With Lignin Model Compound Vanillin got me interested. The synthesis appeared easy so I gave it a go:

[Cu(C8H7O3)2(H2O)2] (2): [Cu2(O2CCH3)4(H2O)2]
(0.160 g) was dissolved at room temperature in 10.0 mL
of acidified water (one drop of glacial acetic acid). The
solution and solid vanillin (0.244 g) were slowly heated
in two separated flasks. When vanillin had melted, the
acetate solution was put over melted vanillin that turned
red and dissolved in ~5 seconds. Orange crystals of 2
were filtered off next day and dried in air for a day.

However both of my attempts following the above failed. There was obviously a reaction because the blue copper acetate solution instantly turned the most beautiful emerald green upon addition to the molten vanillin. Upon cooling a large crop of pale green needle crystals formed which are quite possibly compound 1.

Anyone else care to try this and see if they can achieve the orange compound? I'd really like to know where I went wrong (currently suspecting not high enough temperature at mixing time). I'll need to make some more copper acetate before making another attempt.


That's cool- I didn't think vanillinate would make that good of a ligand. I may have to try that. It strikes me as odd, though, that a change in the hydration (without a change in the coordination) would give such a strong change in colour. I suspect that their formulation of compound 2 was incorrect- I wonder if they ever did get a crystal structure?

ETA: They did get a crystal structure, and it is the cis isomer. Z. Naturforsch. 60b, 1273 – 1277 (2005);

Has anyone ever made KCuCl3? It's supposed to form ruby-red crystals, but I've never managed to get it to work.

[Edited on 16-1-2015 by DraconicAcid]




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[*] posted on 16-1-2015 at 10:43


Quote: Originally posted by DraconicAcid  


Has anyone ever made KCuCl3? It's supposed to form ruby-red crystals, but I've never managed to get it to work.


I've never done it personally, but I've come across a prep for it online (the source is attached).

Preparation of Potassium Trichlorocuprate (II)
Dissolve 1.0g of Potassium Chloride (KCl) in 3.7 mL of distilled Water. In a fume hood,
dissolve 5.5g of Cupric Chloride Dihydrate (CuCl2•2H2O) in 50 mL of concentrated HCl in a
250 mL Erlenmeyer flask. Stir the mixture until it is dissolved; this may take several minutes.
Do not heat the mixture as this will drive off the HCl. Essentially dropwise, pour the KCl
solution into the CuCl2 solution slowly and with rapid stirring. Place the Erlenmeyer in an Ice
bath for half an hour. Vacuum filter the red, needle-like crystals in a medium porosity sintered
glass crucible. Spread the damp precipitate onto a watch glass and dry them in an oven that is
not any hotter than 85oC. Once dry, weigh the product and then store the sample in a 3 dram vial
flushed with Nitrogen and sealed with Parafilm wax.


Is this the procedure that you attempted?


[Edited on 16-1-2015 by blargish]

Attachment: Two Interesting Copper Compounds.pdf (299kB)
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[*] posted on 16-1-2015 at 10:51


Quote: Originally posted by blargish  
Quote: Originally posted by DraconicAcid  


Has anyone ever made KCuCl3? It's supposed to form ruby-red crystals, but I've never managed to get it to work.


I've never done it personally, but I've come across a prep for it online (the source is attached).

Preparation of Potassium Trichlorocuprate (II)
Dissolve 1.0g of Potassium Chloride (KCl) in 3.7 mL of distilled Water. In a fume hood,
dissolve 5.5g of Cupric Chloride Dihydrate (CuCl2•2H2O) in 50 mL of concentrated HCl in a
250 mL Erlenmeyer flask. Stir the mixture until it is dissolved; this may take several minutes.
Do not heat the mixture as this will drive off the HCl. Essentially dropwise, pour the KCl
solution into the CuCl2 solution slowly and with rapid stirring. Place the Erlenmeyer in an Ice
bath for half an hour. Vacuum filter the red, needle-like crystals in a medium porosity sintered
glass crucible. Spread the damp precipitate onto a watch glass and dry them in an oven that is
not any hotter than 85oC. Once dry, weigh the product and then store the sample in a 3 dram vial
flushed with Nitrogen and sealed with Parafilm wax.


Is this the procedure that you attempted?


[Edited on 16-1-2015 by blargish]


Yes, from the same source. No red needles or red precipitate of any kind.




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[*] posted on 16-1-2015 at 12:36


I've tried to prepare KCuCl3 by a different method; according to Atherton Seidell's 1919 book on solubilities (p. 268), a mixed solution of KCl and CuCl2 at elevated temperatures (above 72 C or so) will precipitate this double salt as it evaporates, if the compounds are present in roughly equimolar amounts. Had difficulties with the temperature control and set the solution aside, though.

At lower temperatures it appears that a different, blue-green double salt is precipitated from aqueous solution: CuCl2.2KCl.2H2O. I suppose that the use of concentrated HCl in the prep you mention changes things so that this compound isn't the result.




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[*] posted on 17-1-2015 at 07:39


Wow, Those complexes look really nice! If I can get some of the reagents together, I will have to attempt to prepare them.

Where do you buy your Sodium Tungstate? All I have been able to find is a product on amazon (50 grams or so for $100). Since this is the only synthesis for it I would have planned, I am not ready to drop that kind of money on it.

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