| Pages:
1
2
3
4
5
6 |
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
To report what has been happening in my quest to get some NHN... turns out the reason why I failed is because both my first and second hydrazine
sulfate synthesis were duds. I am not sure where the process failed. But it turned out I didn't get any hydrazine sulfate at all.
That being said. Tonight i decided to make some hydrazine sulfate and I made a full batch. When I added the sulfuric acid, even though it was already
at a 27 or so C, the hydrazine sulfate precipitate immediately began to form. I only let it cool to 18C before beginning filteration. I haven't
weighed my yield yet, but I hope I have enough for a good synthesis or two.
That being said, I need to ask this one question... because to me making hydrazine sulfate has not proven to be dangerous... neutralizing the
byproducts IS. The first time I did it I poured in a calcium hypochlorite solution into the leftover hydrazine in my bathroom and the fumes were
unbearable. It took a long time to clean everything up.
My second time was better, but I wasn't sure if I needed to give it time to fully neutralize, but I did use a lot of bleach mixed with calcium
hypochlorite.
The third time... maybe it was because I was using a full batch... my god I think I nearly died! What happened is that I initially poured water, the
hydrazine leftovers, and bleach into my glass baking pan that I only use for chemistry now... and then I added a bit more bleach and the solution
fizzed. Then I added a good amount of calcium hypochlorite to the thing and mixed it, letting it fizz and fizz and so on.
My pan was too full to add anything else. I figured I would do what I did previously and put it in my bathtub and pour water over it until everything
went down the drain... but instead I went to my kitchen sink.
While carrying the thing I didn't smell anything, but the moment I got to my kitchen sink it's almost like being in a gas attack! My eyes teared up
and I coughed violently. I turned on the faucet and ran away. I let the thing run for a while before returning and the gasses were still there. Just
very isolated. I held my breath before approaching again and made sure the water was pouring away the undissolved calcium hypochlorite. After
everything seemed to wash away I was in a bit of a tizz over the whole thing.
I wasn't short of breath or had any of those symptoms. I decided to leave my kitchen sink on and leave my apartment for a long walk. I had no problem
breathing, albeit I was worried I was feeling some minor sensation when I took a full breath. I started to salivate a little after around 45 minutes
but that stopped after around 20 minutes.
That was one hell of an experience that I hope to never repeat. Someone just told me that the hydrazine byproducts can be flushed down the toilet or
drain and the bacteria in the sewer system will take care of it. Is this true? Because disposing of that stuff is the only thing I ever worry about.
|
|
|
fredsci93
Hazard to Self
Posts: 84
Registered: 29-12-2017
Member Is Offline
Mood: No Mood
|
|
It's safe to flush, what happened to you was the solution was too acidic so upon addition of the bleach chlorine started forming, to avoid this you
can add sodium carbonate/bicarbonate until bubbling stops before you add bleach. Or you could just leave it acidic, so long as you keep it outside
until all the chlorine is liberated.
|
|
|
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
That was still one hell of an experience. I feel a mild bit of lung burn when I breathe deeply though. It'll heal, but between this and nitrogen
dioxide inhalation I really don't want to have any more of these incidents.
I was so fixated on neutralizing the hydrazine I forgot that I put in a lot of acid in it that also needed to be neutralized... because normally
whenever I do anything with acid I always add a lot of carbonate even if it is technically safe to pour down the drain as is.
I am glad that it is more likely chlorine than hydrazine. While that is still pretty nasty stuff I would rather deal with a chlorine gas than a
hydrazine.
|
|
|
MineMan
International Hazard
Posts: 1013
Registered: 29-3-2015
Member Is Offline
Mood: No Mood
|
|
Quote: Originally posted by ManyInterests  | To report what has been happening in my quest to get some NHN... turns out the reason why I failed is because both my first and second hydrazine
sulfate synthesis were duds. I am not sure where the process failed. But it turned out I didn't get any hydrazine sulfate at all.
That being said. Tonight i decided to make some hydrazine sulfate and I made a full batch. When I added the sulfuric acid, even though it was already
at a 27 or so C, the hydrazine sulfate precipitate immediately began to form. I only let it cool to 18C before beginning filteration. I haven't
weighed my yield yet, but I hope I have enough for a good synthesis or two.
That being said, I need to ask this one question... because to me making hydrazine sulfate has not proven to be dangerous... neutralizing the
byproducts IS. The first time I did it I poured in a calcium hypochlorite solution into the leftover hydrazine in my bathroom and the fumes were
unbearable. It took a long time to clean everything up.
My second time was better, but I wasn't sure if I needed to give it time to fully neutralize, but I did use a lot of bleach mixed with calcium
hypochlorite.
The third time... maybe it was because I was using a full batch... my god I think I nearly died! What happened is that I initially poured water, the
hydrazine leftovers, and bleach into my glass baking pan that I only use for chemistry now... and then I added a bit more bleach and the solution
fizzed. Then I added a good amount of calcium hypochlorite to the thing and mixed it, letting it fizz and fizz and so on.
My pan was too full to add anything else. I figured I would do what I did previously and put it in my bathtub and pour water over it until everything
went down the drain... but instead I went to my kitchen sink.
While carrying the thing I didn't smell anything, but the moment I got to my kitchen sink it's almost like being in a gas attack! My eyes teared up
and I coughed violently. I turned on the faucet and ran away. I let the thing run for a while before returning and the gasses were still there. Just
very isolated. I held my breath before approaching again and made sure the water was pouring away the undissolved calcium hypochlorite. After
everything seemed to wash away I was in a bit of a tizz over the whole thing.
I wasn't short of breath or had any of those symptoms. I decided to leave my kitchen sink on and leave my apartment for a long walk. I had no problem
breathing, albeit I was worried I was feeling some minor sensation when I took a full breath. I started to salivate a little after around 45 minutes
but that stopped after around 20 minutes.
That was one hell of an experience that I hope to never repeat. Someone just told me that the hydrazine byproducts can be flushed down the toilet or
drain and the bacteria in the sewer system will take care of it. Is this true? Because disposing of that stuff is the only thing I ever worry about.
|
Dude…. Really? You think these chemicals will hurt poop? Be safe. And why don’t you have a gas mask. This is why I suggested CHP! Your trying to
deal with hydrazine inside, without a fume hood and no gas mask. Your thinking is flawed. Yes your making a safer explosive then LA…. But the synth
isn’t safe in your environment. Your trading sensitivity for toxic gases. I urge you to pursue CHP in instead. If you read through the threads you
might find you have everything you need already. You trying to be very safe and critical in the area of explosive sensitivity but a moron with toxic
gases…. It doesn’t fit.
|
|
|
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
I made a mistake. I won't make that mistake again and it never happened like this before... Ever. I doubt I will need to make hydrazine sulfate again
since I do believe I succeeded in making enough.
One day I will make chp. But for now I don't want to since I will need to go around experimenting with ammonia and ammonium perchlorate and other
stuff I have no experience with. I downloaded LoL's videos on the matter for later viewing... Maybe in a year or so.
It was a dramatic mishap, but I never had anything like this ever. It's never the synthesis that is dangerous. It's the disposal.
When I make my NHN I will immediately dump the byproduct in the toilet and not bother any neutralization. Or just pour some normal bleach on it and
call it a day.
|
|
|
Laboratory of Liptakov
International Hazard
Posts: 1407
Registered: 2-9-2014
Location: Technion Haifa
Member Is Offline
Mood: old jew
|
|
God with you at yours "experiments" with chlorine. Chlorine causes pulmonary edema. And with an interval of up to 2 days from inbreathing. Short-term
effect: concentration 0.1% for 10 minute is deadly. (wiki or similar)
I reccommend do Silver acetylide double salt. SADS.
Or go to on perchlorates, where is a large space for research of perchlrates of all species. Their mixtures (or derivates) are one from most
universals (most intersting) energetcs materials. Especially for amateur chemistry. The most famous is probably CHP, which is abbreviation for
Tetramine copper perchlorate subsidized of hexamine, + ammonium perchlorate. Research of organics perchlorates generally:
https://www.sciencedirect.com/science/article/abs/pii/S01661... -----LL
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
|
|
|
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
I was not experimenting with chlorine. I was using bleach to neutralize left over hydrazine.
Also what do you mean by interval 2 days from in breathing you mean I could get pulmonary edema in a day?
[Edited on 14-12-2021 by ManyInterests]
|
|
|
Laboratory of Liptakov
International Hazard
Posts: 1407
Registered: 2-9-2014
Location: Technion Haifa
Member Is Offline
Mood: old jew
|
|
Information about chlorine are free available: Here or anywhere. https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3136961/
You keep all conditions from video Nile Red video?
https://www.youtube.com/watch?v=PCovDr4FVNQ
[Edited on 14-12-2021 by Laboratory of Liptakov]
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
|
|
|
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
Yes I did. The issue didn't happen during synthesis. It happened during my attempts to neutralize the byproduct, which I now know is unnecessary and
it can just be flushed down the toilet... where the bacteria in the sewers will eat it for breakfast.
I contacted someone I know how is a pulmonologist (lung doctor) and they said I'll be fine. Right now I feel quite good. I just need ot remember to
wear a dust mask when doing my future my nitration since I don't want to accidentally inhale any of the very finely ground particles. I have some very
dry HDN (as far as I know. There is no moistness on the paper towels I use. But I don't want any of the fine particles to go into my nose. I never had
a nitro headache.
Let me make it clear again... I breathed no toxic gasses during the synthesis. It was only in the disposal did I make the mistakes.
I also realize you do want me to make CHP. so as I said. I promise you I will make some CHP. But that's for the future. Right now I want to get this
stuff done and move on with my life. I want to be a software dev, not a chemist.
Edit: I tried to get a gasmask off Amazon but they asked for professional cred for it. I did buy a different kind of air purifier, but I didn't use it
because I had no idea this specific reaction was going to happen.
Chemically I understand now why... there was more than just left over hydrazine. There was HCl and H2SO4 in there. Bleach with acid causes problems. I
don't know why it chose to react at the instant I arrived at my sink, but I think it's because I started the faucet that caused the reaction to
commence. Now that I know that, I won't do it again. I won't have to anyway... I do believe I have all the hydrazine sulfate I am going to need for
one or two NHN synthesis. The first of which I will do today.
Edit2: For the RDX/Keto-RDX that I plan on doing, I will need to make sure that I get all temperature controls right. I will probably not be storing
my RDX for long, but I want to see if I can render everything as safe as possible.
BTW, I originally measured my first fuming nitric acid at a specific gravity of 1.518 at 0 C (l kept it in the freezer overnight) but it appears to
have dropped when I took another weight sample at around 1.49 to 1.489. I was around 20-23 C. I hope it is sufficiently strong for an RDX synthesis.
[Edited on 14-12-2021 by ManyInterests]
[Edited on 14-12-2021 by ManyInterests]
|
|
|
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
OK... I freebased some hydrazine... but I think I added far too much ethanol to the mix. I added around 40ml to start (26 grams of hydrazine sulfate)
then around 20 ml. I ended up getting a lot of sodium sulfate in my hydrazine. I panicked and I poured in a lot of ethanol. Not sure how much, but
easily over 60 to 70 ml extra... I hope I didn't mess up my hydrazine freebasing too much with that. At least not enough to mess up my synthesis of
NHN!
|
|
|
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
OMG I DID IT!
I realized that I could have freebased so much more hydrazine! I did it! I did it in the hot method! I haven't filtered it yet, but the solution is so
thick the stirbar is jamming up! I will let it ride for a few more minutes then filter!
I'm so overjoyed!
|
|
|
fredsci93
Hazard to Self
Posts: 84
Registered: 29-12-2017
Member Is Offline
Mood: No Mood
|
|
great stuff, the ethanol has little effect on the yield, btw what color was the NHN filtrate, if an excess of nickel was present in the reaction then
it should be cyan/green if an excess of hydrazine was used it should be white/clear
|
|
|
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
It was as purple as can be! I got me a very large batch of NHN. More than I could ever use in a life time. After testing it out. I'll set aside enough
for a few blasting caps and neutralize the rest.
[Edited on 15-12-2021 by ManyInterests]
|
|
|
fredsci93
Hazard to Self
Posts: 84
Registered: 29-12-2017
Member Is Offline
Mood: No Mood
|
|
nice, looks like a fair bit of NHN
|
|
|
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
The glass pan next to it has all my other filterates. I filtered as much as I could of the stuff before diluting the rest of the filterate with water
and pouring it down the drain. I won't be bothering with any more chlorine or crap.
I did pour bleach on the hydrazine that I didn't extract, but I did it outside and let it fully react before bringing it back to my kitchen sink and
letting the faucet run it clear. There was a smell of something, but nothing weird or awful, so I know I avoided a major problem.
That being said this is the only NHN synthesis I will be doing for a very long time. Like years. It's going to take a few days to dry and I turned my
radiator up to max to give it the temp it needs to draw off all moisture. I can't wait to weigh my yield, but I am sure I got enough for all the
blasting caps I want.
Edit: My hyrazine sulfate appeared to be very pure hydrazine sulfate with little sodium sulfate contamination. I know this because none of the stuff
in it appeared to react like sodium sulfate, and I think I could made another batch just like this one with the amount of hydrazine sulfate I made.
My final yield was around 26 grams. But that's because I immediately began filteration ar 18C and I did not give the sodium sulfate any chance to
form. Hence there was probably very little of it. A 25% yield, but it was plenty for my purposes.
[Edited on 15-12-2021 by ManyInterests]
|
|
|
Laboratory of Liptakov
International Hazard
Posts: 1407
Registered: 2-9-2014
Location: Technion Haifa
Member Is Offline
Mood: old jew
|
|
Finally done. We already thought you wouldn't survive the synthesis....
But you have advantage. Covid will die before, than he gets to your sink.
[Edited on 15-12-2021 by Laboratory of Liptakov]
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
|
|
|
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
Yes. I threw everything at this including my kitchen sink. Now I need to dry this stuff near the radiator without it blowing up!
On disposing of my remaining nickel nitrate? Just dilute the liquid and throw it away in a bag or flush it down the toilet? Is nickel nitrate also bad
for poop?
After my wonderful chlorine gas incident, I think I will experiment with Phosgene AND Phosphine! OK OK I am kidding.
|
|
|
Laboratory of Liptakov
International Hazard
Posts: 1407
Registered: 2-9-2014
Location: Technion Haifa
Member Is Offline
Mood: old jew
|
|
You can try drying only small part of NHN. For example cca 3g for first attempts of behavior. And other leave in wet consistency.
All you can flush, is good flush....
Development of primarily - secondary substances CHP (2015) Lithex (2022) Brightelite (2023) Nitrocelite and KC primer (2024)
|
|
|
ManyInterests
National Hazard
Posts: 937
Registered: 19-5-2019
Member Is Offline
|
|
That is good. Because the only danger I ever subjected myself to was disposing of dangerous chemicals. Never making them. Except maybe one time with
nitric acid, but that was very minor compared to my chlorine issue. Making hydrazine was nowhere near as dangerous as I thought it would be.
Freebasing it was a joke once I got the actual product and not sodium sulfate!
|
|
|
Raid
Hazard to Everyone
Posts: 203
Registered: 14-11-2022
Location: N/A
Member Is Offline
|
|
could i use starch instead of dextrin to make NHN?
or should I just convert the starch into dextrin.
i think that the starch could work because of the similar chemical structure.
but I'm not sure. i guess I could test.
|
|
|
Hey Buddy
Hazard to Others
Posts: 441
Registered: 3-11-2020
Location: Bushwhacker Country
Member Is Offline
|
|
Dextrin is a process of starch like you said, so possibly. Capping agents and crystal modifiers are all kind of interchangeable as long as they don't
react. PVP, glycols, dextrin, CMC, gelatine all modify crystal shapes.
--I attempted to reproduce NHN procedure #2 from: "Synthesis and Characterisation of Metal Hydrazine, Nitrate, Azide and Perchlorate Complexes" Patil
2013
Briefly, they claim NH4NO3 can be dissolved with hydrazine and Ni metal reacted at room temperature to form NHN.
Ive tried this four times with alcoholic hydrazine at both room temp and elevated temperatures and using both Ni metal as well as Ni2O3. I can get a
partial reaction with nickel metal if left at elevated temp over night but it does not complete to form NHN. I have found this paper to be
unreproducible in terms of Nitrates. I have not attempted perchlorates or azides by their methods.
|
|
|
Raid
Hazard to Everyone
Posts: 203
Registered: 14-11-2022
Location: N/A
Member Is Offline
|
|
ok thanks, i'll try making it with starch and report my findings. and then ill convert the starch to dextrin and try that.
|
|
|
Raid
Hazard to Everyone
Posts: 203
Registered: 14-11-2022
Location: N/A
Member Is Offline
|
|
so i tried making NHN for first time, and when i add the nickel nitrate to the hydrazine freebase a green precipitate forms. i know its supposed to be
a purple color and this is not purple. how do i fix this. BTW i was not using the hexahydrate i was using the raw nickel nitrate from making it, im
guessing this is the problem but im not sure. also the green precipitate does NOT redisolve into solution. it just kinda sits there. one more note is
that i used H2O2 in the nickel nitrate synthesis and maybe converting the "NHN" to some sort of other nickel salt.
|
|
|
Raid
Hazard to Everyone
Posts: 203
Registered: 14-11-2022
Location: N/A
Member Is Offline
|
|
ok i tried it again with the hexahydrate and still the same outcome
|
|
|
B(a)P
International Hazard
Posts: 1139
Registered: 29-9-2019
Member Is Offline
Mood: Festive
|
|
| Quote: Originally posted by PINKBOII | | BTW i was not using the hexahydrate i was using the raw nickel nitrate from making it, im guessing this is the problem but im not sure.
|
What do you mean by 'raw'? It is very difficult to get anything other than the nickel nitrate hydrate. Did you purchase or make the hydrazine?
|
|
|
| Pages:
1
2
3
4
5
6 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
