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Author: Subject: Copper Dichloroisocyanurate Complex Synthesis and Analogs.
Fidelmios
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[*] posted on 7-5-2017 at 13:47
Copper Dichloroisocyanurate Complex Synthesis and Analogs.


Hello Everyone!

Recently I attempted the experiment of mixing Copper Sulfate, and NaDCC. The results were amazing with the pictures linked below. In case you guys are looking for a reference link:

http://www.theamateurchemist.com/synthesis-of-copper-cyanura...

If you wanna stay on SM http://www.sciencemadness.org/talk/viewthread.php?tid=29474

and Woelen's http://woelen.homescience.net/science/chem/exps/raw_material...


So after a successful synthesis I figured a cool thing to do with it was to show Chemiluminscene, and I tried using topical Hydrogen Peroxide. While it seemed to react fast enough, it did NOT produce the red light. I can only assume it is because the concentration was too low.


My additional question is, I tried making the Nickel analog outlined in US3055889 it reads:

"A solution of 0.039 mole of potassium dichlorocyanu

rate in 200 milliliters of water was mixed with 25 milli

liters of water containing 0.0195 moles of nickel chloride.

The precipitate, very close to an Opaline Green color"


I have tried similar, by mixing a saturated solution of both, and I can not seem to get the reaction to go forward! Furthermore, in the paper it specifically points out that the ratios are not important "The reactant ratios are not critical since the complex

will form until the reactant present in lesser stoichiometric

amount is consumed."



Can anyone help with any information of what I should do to move forward?







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j_sum1
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[*] posted on 7-5-2017 at 16:18


This is an incomplete project of mine from two years ago.
I also had a student play with it at one point.

From off the top of my head...
I made a small amount of a copper potassium dichloroiscyanurate complex. This looked almost identical to the sodium variety.
It was evident that complexes were forming with some other cations: I recall Co, Ni. There were others as well. I have read somewhere (a paper posted on this site) that la and Pb also generate complexes.

One of the many tings I would like to get back to.
I found that stoichiometry is useful for getting the best results.
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[*] posted on 7-5-2017 at 16:55


I tried iron once- using a solution of iron(iii). The color intensified, to an impressive red but no precipitate.



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[*] posted on 7-5-2017 at 17:11


US3055889

This paper discusses everything you talked about. The Pb, and Ni salts. If I remember right, the paper also discusses the spectator ions and that they were not important to the reaction.

Quote: Originally posted by j_sum1  
This is an incomplete project of mine from two years ago.
I also had a student play with it at one point.

From off the top of my head...
I made a small amount of a copper potassium dichloroiscyanurate complex. This looked almost identical to the sodium variety.
It was evident that complexes were forming with some other cations: I recall Co, Ni. There were others as well. I have read somewhere (a paper posted on this site) that la and Pb also generate complexes.

One of the many tings I would like to get back to.
I found that stoichiometry is useful for getting the best results.
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DFliyerz
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[*] posted on 7-5-2017 at 17:40


Maybe it's just me, but when I made this compound it smelled awful. Even looking at it makes me think of the smell...
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Fidelmios
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[*] posted on 7-5-2017 at 17:49


Quote: Originally posted by DFliyerz  
Maybe it's just me, but when I made this compound it smelled awful. Even looking at it makes me think of the smell...


Smelled like Pool Tablets to me, like lots and lots of chlorine.
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[*] posted on 8-5-2017 at 14:24


Yeah, and I noticed upon attempting to use it as a watercolor pigment that it will bleach the bristles of a paintbrush upon very short exposure! It's also not lightfast at all- after being painted onto a paper or canvas, the brilliant color fades to a dull grayish purple within the month. Still, it is a very nice compound to look at in bulk form.



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[*] posted on 8-5-2017 at 15:26


I think it may dull in vibrance due to light. It appears since storing, my sample has gotten much, much less purple.

Quote: Originally posted by zts16  
Yeah, and I noticed upon attempting to use it as a watercolor pigment that it will bleach the bristles of a paintbrush upon very short exposure! It's also not lightfast at all- after being painted onto a paper or canvas, the brilliant color fades to a dull grayish purple within the month. Still, it is a very nice compound to look at in bulk form.
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[*] posted on 8-5-2017 at 23:21


The instability does not surprise me. Even Na-DCCA is not that stable. Open a bottle of that stuff and you smell its pungent odour. This is due to decomposition and production of chlorine and/or chloramine. When kept in a dry tighly sealed container, the Na-DCCA remains good for a very long time, but in contact with air it quickly deteriorates. The copper compound most likely is less stable. When I made it, I dod not keep it around for long. On storage it may produce gaseous compounds, which may lead to pressure buildup and rupture of its container. If you keep it around, be careful with that. I'm not saying that it does no, but it might do so. More research is needed, or someone else needs to jump in who knows already.



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[*] posted on 10-5-2017 at 15:18


Thanks Woelen,


I'll upload some pictures to show a decomposition over time. I doubt much will change if I keep it inside, in a cool area. I still have quite a bit of NaDCC, and I'll try to use it up if I can figure out how to get it to react with other things. I have tried for some time to get it to react with Nickle, and it refuses to.

Quote: Originally posted by woelen  
The instability does not surprise me. Even Na-DCCA is not that stable. Open a bottle of that stuff and you smell its pungent odour. This is due to decomposition and production of chlorine and/or chloramine. When kept in a dry tighly sealed container, the Na-DCCA remains good for a very long time, but in contact with air it quickly deteriorates. The copper compound most likely is less stable. When I made it, I dod not keep it around for long. On storage it may produce gaseous compounds, which may lead to pressure buildup and rupture of its container. If you keep it around, be careful with that. I'm not saying that it does no, but it might do so. More research is needed, or someone else needs to jump in who knows already.
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[*] posted on 12-5-2017 at 12:55


UPDATE: I have re-run the experiment using Iron Sulfate, and while the product is impure, I may be able to isolate the iron analog.


I may have found a flaw in my previous run with the Nickle compound, I used a solution that had been made for crystallization a LONG time ago, doubt that there is any actual change to the compound, but perhaps it made the experiment fail. I will re-preform the experiment tomorrow with updates,
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[*] posted on 21-5-2017 at 18:54


Quote: Originally posted by Fidelmios  
UPDATE: I have re-run the experiment using Iron Sulfate, and while the product is impure, I may be able to isolate the iron analog.


I may have found a flaw in my previous run with the Nickle compound, I used a solution that had been made for crystallization a LONG time ago, doubt that there is any actual change to the compound, but perhaps it made the experiment fail. I will re-preform the experiment tomorrow with updates,

I look forward to the results!




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[*] posted on 22-5-2017 at 20:24


Quote: Originally posted by Velzee  
Quote: Originally posted by Fidelmios  
UPDATE: I have re-run the experiment using Iron Sulfate, and while the product is impure, I may be able to isolate the iron analog.


I may have found a flaw in my previous run with the Nickle compound, I used a solution that had been made for crystallization a LONG time ago, doubt that there is any actual change to the compound, but perhaps it made the experiment fail. I will re-preform the experiment tomorrow with updates,


I look forward to the results!




Update 2: stored some copper cyanurate complex under nickel chloride and some under air in a dram vial. The dram vial seems to be leaking a small amount of chlorine gas under assumed decomposition. The wetted complex, stored under the nickel cimpound has not changed color but a yellow layer has formed at the top of the solution. Will update later.
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[*] posted on 22-5-2017 at 21:13


Hmmm. I must check mine. I put some in an ampoule about 2 years ago. Last time I looked at it it was still purple (ok, periwinkle according to literature), but had lost some of its characteristic brilliance.
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[*] posted on 4-6-2017 at 11:37


Just posted the video https://www.youtube.com/watch?v=vQ5bCVPArPk
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