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Author: Subject: Exotic Primaries - Complex Salts
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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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[*] 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.




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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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[*] posted on 6-2-2021 at 08:49


Sorry for the late answer ;)

Sadly I did not find my old notes, but I used Barium hydroxide back then. But I concluded that it's not working ;)
I will try it again this year.


Quote:

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


Could you somehow judge the yield somehow? How do you know it was
Quote:

fair concentrated

?



[Edited on 6-2-2021 by dangerous amateur]
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[*] posted on 26-9-2021 at 05:43


You can weigh out the sodium sulfate thats left behind and do some maths. calculate the theoretical amount of sodium sulfate which should be synthesised in the procedure. than check it with the one that was left behind. dont forget to add the small amount which is desolved in etoh (solubility of na2so4 is about 0.44g/100g of etoh (100%)). with that you should be able to calculate the mass percentage of the hydrazine in your etoh solution.. correct me if i am wrong.;)
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[*] posted on 28-12-2021 at 22:05


I've seen it mentioned once in this thread, but I made (what I believe to be) tetraamminecopper (ii) picrate. I made this by adding a solution of excess tetraamminecopper (ii) sulfate to a solution of warm ammonium picrate with a bit of ammonia to ensure the complex didn't fall apart. Immediately, a flaky gold-colored precipitate formed. Upon filtering, the filtrate remained the typical color of the tetraamminecopper (ii) ion, indicating that the complex hadn't fallen apart. Drying caused the precipitate to "mat", and I chopped it up while damp with a metal spatula.

20211228_235948.jpg - 239kB

The properties of the product are typical with both a copper salt and a picrate. Upon exposure to flame, a green color is observed, indicating copper is present. The product then melts, followed by vigorous and rapid burning; a noise and flame are both present. To prove the compound I made wasn't just copper (ii) picrate, I made the latter by adding copper (ii) chloride to a concentrated sodium picrate solution. A green precipitate formed, which was filtered. The properties of this precipitate, not only color, are different than the compound I made. Burning is less vigorous, but it burns more readily and doesn't melt beforehand.

Comparison of the supposed tetraamminecupric picrate (left) and cupric picrate (left):
20211229_002933.jpg - 130kB

So, the only conclusion I could come up with was that the product I have is tetraamminecopper(ii) picrate, considering its properties are quite different than both ammonium picrate and copper (ii) picrate, and I don't think that a product could've been made that wasn't this one, given the conditions I performed the reaction in.




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