Re: Pt IV to Pt II

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From: Jacques Augustowski (py1hy@inx.com.br)
Date: 02/11/03-09:05:20 PM Z


Hi Alberto,
I did it in 1986 and had to find my writings. Now it is cheaper to buy
from Bostick &Sullivan.
I will try to translate what I wrote.
Dissolve 10 gr. of H2PTCL6.6H2O in 100 ml of distilled water, add 3.2
gr. of (potassium chlorate) KCLO3, dissolved in 30 ml of distilled
water and agitate, this will precipitate K2PTCL6.
The resulting mixture will be diluted in in equal volume of etilic
alcohol and left to rest for at least 15 min in an ice bath, filter in a
glass funnel and filter paper. The resulting salt will washed by
decantation by two portions of etilic alcohol at 50% and transferred to
the same filter used before, wash with a little bit of etilic alcohol
the precipitated in the funnel..
With the yellow precipitate on the filter wash it three times with ether
and let it dry until the smell of ether has disappeared. The dry salt
should be put in a Beaker of 100 ml containing 70 ml of distilled water
and should be reduced by an addition of sulfurous gas recently prepared.
The Beaker should be put in a water bath at a temperature between 85 C
and 90 C. during the process agitation must constant and no more of 2 ml
of the sulfurous gas should be added at a time. Between one addition and
the other the odor of sulfur disappears.
the solution should always be kept at a constant volume of 70 ml by the
addition of distilled water. during the reduction the solution will have
a reddish color.
At the end of the agitation a little bit of potassium
hexacloroplai\tinic (II) of potassium (yellow) will be left at the
bottom of this solution., never add in excess the sulfurous gas, it is
best to stop before total reduction, if you don't, complex salts of
sulfides will be formed by the excess of SO2 gas, filter this to take
out the yellow precipitate.. Leave the red solution in a water bath
until crystallization and wash it with equal parts of acetone and ether,
this will result in wet red crystals. Leave it too cool in room temperature.
The crystals should be dissolved in 80 ml of distilled water at room
temperature, the resulting solution should be filtered until no trace of
 of the yellow precipitate is found.
Leave it to dry at room temperature, the resulting color will will be
pinkish, that's the end.

how to make the SO2 gas:
NA2SO3 + H2SO4 ---> NASO4 + SO2 + H2O

Heat the NA2SO3 + H2SO4 and the gas should go through distilled water,
this water is used for the reduction, SO2

I hope this helps you, and don't forged to use a fume hood when making
the SO2 gas.

Jacques Augustowski

Alberto Novo escreveu:

>I have a few grams of chloroplatinic acid (Pt(IV)). Anyone knows how to reduce it to potassium chloroplatinite (Pt II))?
>I have a good laboratory practice, and I know how to safely work.
>
>Alberto
>
>
>
>


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