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Topic: Precipitating [Co(NH3)5CL)Cl2  (Read 7810 times)

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Offline rmcmillan

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Precipitating [Co(NH3)5CL)Cl2
« on: February 28, 2011, 02:12:09 PM »
I am working with Cobalt Coordination Complexes and after i collect a aqueous solution of [Co(NH3)5Cl]Cl2 and water, I am struggling to collect the complex out of the solution. Heres what I have tried so far:

Evaporation of water using hot plate
-heat turns this coordination complex into cobalt oxide (brown slurry)
Addition of ethanol into solution
-solution turns a foggy pink (solution is originally purplish), I then ran it through Buchner filtration system but only collect about 10% of original mass, even after adding additional ethanol and running through multiple times
Addition of concentrated HCl
-I tried this and I have had mixed results. The original Coordination Complex/H2O solution is pretty diluted. ~.05 grams to 20 mL of water. It appears to precipitate but not that efficiently.

Does anyone have any ideas? I have researched the synthesis of this complex for help and will post the directions.

To avoid any confusion, just imagine dissolving the complex in water, and trying to retrieve it without water. Also, in the time i do this experiment, the [Co(NH3)5Cl]Cl2 Does Not convert into [Co(NH3)5(H2O)]+3Cl-
-Could i just let it settle for a couple days (haven't tried this due to time constraints)
-Is there any reactions with the aqueous solution that will percipitate

Preparation of [Co(NH3)5Cl]Cl2
In the fume hood, completely dissolve 6 g of NH4Cl in ~40 mls of concentrated ammonia in a 400 ml beaker.   With continuous stirring, add 12 g of cobalt(II) chloride-hexahydrate in small portions. With continued stirring of the resulting brown slurry, SLOWLY add 10 mls of 30% H2O2. After the effervescence has stopped, SLOWLY add ~30 mls of concentrated HCl. With continued stirring, heat on a hot plate and maintain 85 o C for 20 minutes.
Cool mixture to room temperature in an ice bath and filter (using a Buchner funnel) the crystals of [Co(NH3)5Cl]Cl2
Wash with 5-6, 5 ml portions of ice water (distilled water cooled in ice) and then 5-6, 5 ml portions of cold 6 M HCl. Note the color of your product.
Dry the product in an oven at 100 o C for several hours. Weigh the product. Calculate the theoretical and experimental percent yield.

Offline enahs

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Re: Precipitating [Co(NH3)5CL)Cl2
« Reply #1 on: March 01, 2011, 10:19:51 AM »
Your procedure said collect the crystals by filtration. Not sure what you are trying to do or get out of the water, since the crystals are not water soluble at low temperature.

Offline rmcmillan

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Re: Precipitating [Co(NH3)5CL)Cl2
« Reply #2 on: March 01, 2011, 11:04:53 PM »
The crystals are soluble in water at cool temperature (room temperature and below). In the lab procedure, the mixture is cooled, which is different from the [Co(NH3)5Cl]Cl2 in just water.

The procedure provided is not what I am trying to accomplish, rather it is a reference to determine how to precipitate it out of water.

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