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vibbzlab

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Posts: 241
Registered: 6-11-2019
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Mood: Always curious

posted on 9-3-2020 at 23:18

Reinecke's salt Preparation

Hello friends
I decided to try out one of my ever wanted experiment. The synthesis of reineckes salt.
I had looked into too many stuff for its methods of preparation and finally I was able to get a prep method (which was actually the one I found while searching in google in the first place

)
Anyway let's move into prep

Those who directly wanna see the the video can go to the link
https://youtu.be/t2ePnoCM-gk

This is actually a very bad method of synthesis I would say and inspite of knowing that I don't have enough equipment for doing this I tried it out

Reineckes Salt
Preparation :

Ammonium Thiocyanate 8g
Ammonium Dichromate 1.7g

it's a simple procedure of fusing ammonium thiocyanate with dichromate at 150°C

procedure
Take 8g of ammonium thiocyanate in a stainless steel dish and heat till the solid melts( mp is 149°C)
Now add the dichromate which is finely grounded

turn off the heating source when the solid completely melts and then add the ammonium Dichromate because the heat of reaction can maintain the temperature .
Solution would now have attained a purple colour.
continue stirring the compound until it slowly cools and the compound solidify.
Now finely crush the solid and transfer it into 10ml ice cold water
Mix it well so that all the unreacted thiocyanate and dichromate dissolves in the cold water but the reineckes salt do not dissolve in it.
this can be filtered and
recrystallized with water in temperature not more than 60degree Celsius
as the salt immediately hydrolyzes at 65degree C to form hydrogen cyanide which is undesirable.

Now filter the solution while hot and immediately take the clear solution to cool in a refrigerator.
Keep it undisturbed in refrigerator overnight and next day you see the beautiful crimson red colored crystals of reineckes salt which you can filter and dry
The yield was very poor with this method. Around 30%. But yeah I am happy that it at least formed.
You guys cans definitely try seperating
morland salt from the remaining undissolved stuff.

Do watch the full prep video here
https://youtu.be/t2ePnoCM-gk