| Pages:
1
..
21
22
23 |
B(a)P
International Hazard
Posts: 903
Registered: 29-9-2019
Member Is Offline
Mood: Confined
|
|
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.
|
|
|
Laboratory of Liptakov
International Hazard
Posts: 1178
Registered: 2-9-2014
Member Is Offline
Mood: cool.gif
|
|
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.
Inventor of primarily - secondary substances CHP (2015) LITHEX (2022)
|
|
|
MineMan
International Hazard
Posts: 902
Registered: 29-3-2015
Member Is Offline
Mood: No Mood
|
|
He’s back!!
|
|
|
B(a)P
International Hazard
Posts: 903
Registered: 29-9-2019
Member Is Offline
Mood: Confined
|
|
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]
|
|
|
Laboratory of Liptakov
International Hazard
Posts: 1178
Registered: 2-9-2014
Member Is Offline
Mood: cool.gif
|
|
Thanks BP....interest method...
Inventor of primarily - secondary substances CHP (2015) LITHEX (2022)
|
|
|
dangerous amateur
Hazard to Others
Posts: 144
Registered: 8-7-2011
Member Is Offline
Mood: No Mood
|
|
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
?
[Edited on 6-2-2021 by dangerous amateur]
|
|
|
Hens2
Harmless
Posts: 1
Registered: 29-7-2019
Member Is Offline
|
|
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.
|
|
|
night429
Harmless
Posts: 35
Registered: 12-11-2019
Member Is Offline
|
|
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.
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):
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.
"The choosing is easy if you don't have a choice"
|
|
|
| Pages:
1
..
21
22
23 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
