VSEPR_VOID
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Trouble Making Hydrazine Sulfate
I am making luminol from phthalic anhydride (I just finished the nitration), and have been having trouble making the hydrazine sulfate required for
the next reaction.
Trial One
Nerd Rage Method
500 mL of 10% ammonia
0.2 g of gelatin
100 mL of MEK
Stir to 10 minutes well adding 186 grams of 10% bleach slowly by hand.
This produced methyl ethyl ketazine, which will take the form of fine droplets
Stir the reaction for 10 minutes
No Yield: No ME-Ketazine layer evaporates after the addition of bleach, even after several days
Trial Two
Nerd Rage Method
750 mL of 10% ammonia
0.2 g of gelatin
100 mL of MEK
Stir well adding 186 grams of 10% bleach slowly by funnel.
This produced methyl ethyl ketazine, which will take the form of fine droplets
Stir the reaction for 10 minutes
Let the layers separate, the top layer is methyl ethyl ketazine
No Yield: No ME-Ketazine layer evaporates after the addition of bleach, even after several days
In addition there was little gas produced well adding the bleach both times.Has anyone else has this problem?
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UC235
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This is a modification of the raschig process. There should be a fair amount of gas produced, which is where much of the yield goes. Is your bleach
fresh and still strongly yellow-green? Do you get cloudiness and a weird fruity smell aside from the MEK scent, or does the reaction mix stay clear?
Perhaps you have too much water in your mixture since you doubled the volume of ammonia. If you're getting cloudiness and the smell of the ketazine,
maybe try saturating with NaCl to break a possible emulsion.
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VSEPR_VOID
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Quote: Originally posted by UC235  | This is a modification of the raschig process. There should be a fair amount of gas produced, which is where much of the yield goes. Is your bleach
fresh and still strongly yellow-green? Do you get cloudiness and a weird fruity smell aside from the MEK scent, or does the reaction mix stay clear?
Perhaps you have too much water in your mixture since you doubled the volume of ammonia. If you're getting cloudiness and the smell of the ketazine,
maybe try saturating with NaCl to break a possible emulsion. |
The bleach is a few months old. It is a yellow-green.
There is no cloudiness and the reaction goes clear.
I tried adding some sulfuric acid to see what would happen and Cl2 was evolved.
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Magpie
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Try this found in Prepublication:
https://www.sciencemadness.org/whisper/viewthread.php?tid=15...
The single most important condition for a successful synthesis is good mixing - Nicodem
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VSEPR_VOID
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I will buy some new bleach and start again.
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UC235
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Chlorine production sounds like lots of breakdown to chlorate or your ammonia is a lot weaker than you think it is and there is still bleach left
over.
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