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Author: Subject: Exotic Primaries - Complex Salts
B(a)P
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[*] posted on 5-11-2020 at 01:45


I have had good success making NHN using hydrazine free based from hydrazine sulfate.
Can you describe your process?
My approach has been as follows:
- make sure everything is as dry as possible to start and stir stir stir stir stir then stir the whole way, also keep everything cold at all times.
- add NaOH in two portions
- after the first portion of NaOH add 1 ml of cold DH2O, if the reaction does not take off add another 1 ml.
- add ethanol once the reaction is proceeding
- at this point the solid portion will be sticky, add the second portion of NaOH, this makes the sodium sulfate go to sodium bisulfate and pull a bunch of water out with it.
- wash twice with ethanol and you have fair concentrated hydrazine in ethanol.
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Laboratory of Liptakov
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[*] posted on 8-11-2020 at 03:07


Interesting process. Two dry powders? A like fine powder? Drying NaOH can be problem. Any ratios between Hydrazine sulfate and NaOH? Basic weight of both compounds? For 1- 2 ml DH2O ? I estimate, vacuum Buchner was used? How much ethanol?
Thanks.




Safety explosive Alfred Nobel 1867. Safety ecologic detonator Dr. Liptakov 2015.
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[*] posted on 15-11-2020 at 16:07


He’s back!!
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[*] posted on 16-11-2020 at 01:08


Quote: Originally posted by Laboratory of Liptakov  
Interesting process. Two dry powders? A like fine powder? Drying NaOH can be problem. Any ratios between Hydrazine sulfate and NaOH? Basic weight of both compounds? For 1- 2 ml DH2O ? I estimate, vacuum Buchner was used? How much ethanol?
Thanks.


Sorry for the slow reply, I missed your message. I just dug out out my lab notes from last time I did this.
10 g of hydrazine sulfate
17 g EtOH start with 10 g then use 7 g for the second rinse
6.15 g NaOH added in two equal portions as described above
1.5 mLs dH2O

I did not use a funnel or filtration I simply decanted the ethanol/hydrazine liquid from the sodium bisulfate once it had settled.

Edit - Yes both solids as fine dry powders stored in a desiccator bag prior to use.

[Edited on 16-11-2020 by B(a)P]
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[*] posted on 19-11-2020 at 03:45


Thanks BP....interest method...:cool:



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