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Sir_Gawain
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The temperature is less important than the presence of enough water to start the reaction. There should be a visible reaction and temperature spike.
I’m not the best at the freebasing myself, and I blame my low sodium azide yields on that.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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ManyInterests
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Quote: Originally posted by Sir_Gawain  | | The temperature is less important than the presence of enough water to start the reaction. There should be a visible reaction and temperature spike.
I’m not the best at the freebasing myself, and I blame my low sodium azide yields on that. |
Hmm, that could also be a major problem, since the ingredients were dry and the alcohol was also dry.
So what do you recommend? I will give my previous successful synthesis from 2022:
30.15 grams of hydrazine sulfate
18.43 grams of sodium hydroxide
105ml of 95% ethanol (put 55ml first, then the 30 ml later and finally 25ml)
I took the above from my old notes.
So please tell me what you did to get a good freebase? I have never added water to my freebasing before. All videos I see on the matter all use
alcohol, sodium hydroxide, and hydrazine sulfate and nothing more. Should I add like 15ml of water or something?
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Sir_Gawain
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IIRC, alchemystery uses some water in his potassium azide video. You just add the hydrazine sulfate to the ethanol and slowly add sodium hydroxide
while stirring. If the reaction doesn’t start, you add water a few drops at a time until it does. If you add all the sodium hydroxide at once, then
initiate the reaction with water, it heats up so much it boils. I’ve had this happen once, and it was terrifying.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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ManyInterests
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I will look up that video if I don't already have it (I download any chemistry video I find interesting).
I think this was my mistake in the previous two synthesis. added everything all at once, which was wrong, and then made everything too cold. I will
stand that the coldness is a factor, too.
In all honesty I am not sure how the reaction would look like, or I have seen it but I forgot. I made some hydrazine sulfate that I am still
precipitating out. I moved my setup indoors as it is mostly hydrazine sulfate, but I have my apartment well ventillated (and the beaker is well
covered) in order to allow all the stuff to precipitate at 15C and not allow it to go under 10C. By next weekend I should have everything fully ready
to try again.
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B(a)P
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| Quote: Originally posted by ManyInterests | I will look up that video if I don't already have it (I download any chemistry video I find interesting).
I think this was my mistake in the previous two synthesis. added everything all at once, which was wrong, and then made everything too cold. I will
stand that the coldness is a factor, too.
In all honesty I am not sure how the reaction would look like, or I have seen it but I forgot. I made some hydrazine sulfate that I am still
precipitating out. I moved my setup indoors as it is mostly hydrazine sulfate, but I have my apartment well ventillated (and the beaker is well
covered) in order to allow all the stuff to precipitate at 15C and not allow it to go under 10C. By next weekend I should have everything fully ready
to try again. |
Once you have added the first portion of hydroxide you need to stir until you see the reaction start (some white vapour will be visible and the vessel
will warm), note that it takes a long time to get going. If you have been stirring for 15 minutes with no evidence of a reaction starting, try a
little water (maybe 5% of your ethanol volume), keep stirring until you see the reaction commence. The formation of the sodium sulfate hydrate with
later additions of sodium hydroxide will remove the water.
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ManyInterests
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Thank you for that information. So adding all the ethanol and mixing the hydrazine sulfate first. Then the hydroxide piecemeal. If I don't see what
you are describing, add water dropwise until something reacts.
Yesterday I did the longest hydrazine sulfate synthesis I ever did. Most of the time it was waiting for things to cool down. My.mantle overshot the
temperature again (it peaked at 91C) but I saw plenty of sulfate formation. I let it cool until it was at 23C before it got too late. I brought the
setup inside (with lots of plastic wrap to prevent any gas escape. Overnight it cooled down to 14C and currently I still have it unfiltered at 16C
since I had to go to work. Once I return to it I will put it in a ice bath and cool to just barely over 10C before filtering to prevent much sodium
sulfate formation.
I was extremely patient with this one and I hope for a high yield.
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ManyInterests
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I'm going to get ready for an NHN synthesis and I will do follow your instructions and do everything slowly and steadily. If water is needed I will do
slightly less than 5% of the ethanol. I really want this to succeed. I want to make one final NHN synthesis and get it all done. I want to make more
hydrazine sulfate as it will be useful in the future, but for now I just want to make one final bit of high quality NHN and call it a day for NHN
synthesis.
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Sir_Gawain
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What was your hydrazine sulfate yield?
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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ManyInterests
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69.65g. My best yet. Doing it slowly and patiently paid off.
but what didn't pay off was using to make nickel hydrazine nitrate. I really don't understand it, but this time I am confident it is not a failure of
freebasing, I am certain it did freebase. What I did see happening as I was heating the ethanolized hydrazine was that when my mantle switched off
heating at 58C. It went completely nuts and shot up to 75C (AGAIN! Third time!) and I saw some kind of steam coming out of my flask which I thought I
covered up and a lot of bubbling in the flask.
This has to be the reason: My hydrazine got fucked from the heat and simply escaped. When I added some nickel nitrate solution it went straight to
green again and with none of the purple goodness. Meaning all the hydrazine was destroyed in the process.
This is entirely the result of my new mantle. I need to find a work around for this. I simply cannot afford to keep having these failures.
For my hydrazine sulfate synth, I followed the instructions in a video that is no longer on youtube. But here are the reagents:
| Quote: | 355 ml pool bleach (or 500 ml regular bleach selection)
75 ml 50% H2SO4 (add 37.5ml 98% H2SO4 to 37.5ml super cold water)
47.8 g NAoh
34.1 g urea (30ml or 40ml of distilled water to dissolve. use absolute minimum and make sure water is warm.)
0.75 g gelatine (takes 15 ml of warm water to dissolve this)
122 ml HCI |
I did 3 times that amount to great success. It worked quite well the last time as well. I filtered after I cooled everything down to 10C and no more,
so the amount of sodium sulfate left is minimal.
I'm sorry, but I am very upset right now, and I must apologize for the foul language but I am VERY unhappy at this I made NHN successfully many times
and these failures are costing me and frustrating me. I did everything right, but the heating did it in and destroyed my hydrazine. Please tell me I
am correct...
[Edited on 12-4-2024 by ManyInterests]
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Sir_Gawain
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What’s the purity of your nickel nitrate? That’s about the only major variable I can think of.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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ManyInterests
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I bought it from a chemical supplier. It is very pure. I dissolved it in distilled water with 0.04% the weight of the nitrate with dextrin.
It is not the nickel nitrate, I am very confident that it isn't. So far I've done this three times. The first time I did it it worked... but I got a
very poor yield. Only 4g when I was expecting around 15g or so. The second time there was also a big nothing. Then there was this time, and this time
I am very confident that the problem is the heating now, since I am certain that the hydrazine freebased well. There was heat coming out and I saw a
clear change in the hydrazine sulfate to look like the sticky thing I'd expect out of sodium sulfate in that situation.
It is the heating. The first time I tried to heat them I used a cheap hotplate stirrier, but it never went beyond 40C. Probably due to it being very
cold outside. So I transferred it to my mantle to get it to heat to the necessary temperature but I also had a similar runaway. I've had those
runaways in all instant.
I am prepping for another hydrazine sulfate synthesis, the next time I do this, I will use my cheap hot plate stirrer again since the weather is MUCH
warmer than the last time. If I need to heat it up. I will only use my mantle until it reaches 45 or 50C (I set my mantle temp to 51C, but it did not
stop until 58C, then the runaway happened at 60C. This means my thermometer is probably not accurate. I will use a hot water bath to get it to the
appropriate temperature.
It was probably the heat and the destruction of the hydrazine that was the culprit in all cases. NHN can be made at room temperature, but the results
will be chunky and will need additional crushing. When done at a higher temperature it will have the consistency of talcum powder and will need very
little grinding.
At this point I am willing to compromise, I'm sick and tired of all these failures, especially for something that I thought I had accomplished years
ago.
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clearly_not_atara
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Yields aside, there are basic safety reasons not to make energetics with a heating system that malfunctions and overheats. I'd recommend you take a
break until you have some equipment that turns off properly.
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ManyInterests
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| Quote: Originally posted by clearly_not_atara | | Yields aside, there are basic safety reasons not to make energetics with a heating system that malfunctions and overheats. I'd recommend you take a
break until you have some equipment that turns off properly. |
I agree. This needs to be taken care of as it can cause very deadly errors. I intend to make some more picric acid in the future, and part of that
involves several heating steps. It needs to not exceed a certain temperature or else it might go to an explosive runaway. Not something I want or wish
anyone to have.
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Sir_Gawain
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| Quote: Originally posted by ManyInterests |
69.65g. My best yet. Doing it slowly and patiently paid off.
For my hydrazine sulfate synth, I followed the instructions in a video that is no longer on youtube. But here are the reagents:
| Quote: | 355 ml pool bleach (or 500 ml regular bleach selection)
75 ml 50% H2SO4 (add 37.5ml 98% H2SO4 to 37.5ml super cold water)
47.8 g NAoh
34.1 g urea (30ml or 40ml of distilled water to dissolve. use absolute minimum and make sure water is warm.)
0.75 g gelatine (takes 15 ml of warm water to dissolve this)
122 ml HCI |
I did 3 times that amount to great success. It worked quite well the last time as well. I filtered after I cooled everything down to 10C and no more,
so the amount of sodium sulfate left is minimal.
[Edited on 12-4-2024 by ManyInterests] |
Using that method, you should be getting twice that amount. The
synthesis is from a writeup by Rosco Bodine. Here it is:https://www.sciencemadness.org/talk/viewthread.php?tid=15091
The single most important thing to get a good yield is to use the exact right amount of hypochlorite. Use concentrated bleach or, even better, liquid
pool chlorinator and test the concentration. Even a little extra hypochlorite and it will destroy the hydrazine. Not quite enough and the excess urea
will also react with hydrazine. I’ll take a picture of my lab notebook where I got 41.5g hydrazine sulfate from 34g urea and post it tomorrow.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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ManyInterests
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That sounds incredible. I will be sure to use it next time.
Right now I just want to make sure that the current yield I made to make another NHN doesn't go to waste.
Edit: I looked over at the thread. It seems identical to the way I normally do it. I wonder what would be different other than giving it an alcohol
wash to drive out the water.
[Edited on 14-4-2024 by ManyInterests]
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Sir_Gawain
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Here it is:
Apologies for the bad handwriting.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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ManyInterests
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Your handwriting is fine. The only thing that got me off was I wasn't aware that carbamide was also another name for urea. It is identical to what I
normally do. In the past I had poor yields due to prematurely filtering out the hydrazine before it sufficiently cooled. I did that because I was
afraid of sodium sulfate formation, but I realize that it actually needs to get a lot colder than I thought and for longer for the sodium sulfate to
start forming.
One other problem is that when I added the sodium hydroxide I didn't sufficiently cool back the solution to 8C again. I did that in my current
synthesis and I never saw that much foaming before. I had a mild overflow but I was able to prevent my heating mantle from being damaged. The only
thing I did differently is that I went to bed while letting it cool down after heating it to 85C. I added the chilled acids the morning after (chilled
in the fridge, not the freezer, but they were ice cold) I used a slight excess of the HCl And H2SO4, but the yield was good enough that I needed to
change filters on my funnel as one was not sufficient to hold all the sulfate.
So with this, I'll split it into two parts after it fully dries since I know that it is going to be plenty.
I will also review the freebasing with it. I now know that I need to start at room temperature, mix the ethanol in the hydrazine sulfate first (it
will not dissolve) and then add the hydroxide piece meal, also adding a little distilled water (less than 5% the ethanol content) anyway to assure a
reaction takes place. One thing I've done to fully contain any would be fumes is to cover up the beaker entirely and instead of using a stir rod or
stirbar I would simply shake and swirl the beaker around to dissolve everything does work.
I did see a video of someone who also put his beaker in the freezer for an hour after shaking it to allow all the stuff to precipitate. I did that
after stirring and seeing a reaction take place when I felt it was getting hotter and I saw the solids start to gel up and the ethanol clearly
separating from everything. I hope I am doing this right. I know it is weird, but it is my autism and anxiety taking over.
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dettoo456
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If the extraction in EtOH presents issues for you, you can always revert to Ca(OH)2 instead of NaOH. Just dissolve up the Hydrazine sulfate, add
req’d (or even excess) Ca(OH)2, heat with vigorous stirring for an hour or two, and then decant/filter while hot.
And if the resulting N2H4 conc% is too low, you can always pull out excess water w/ sieves since they won’t react with any of the hydrazine.
If you need the Hydrazine in Ethanol alone for whatever reason, you can just add EtOH to the N2H5OH, add a shit ton of sieves, and then filter.
[Edited on 15-4-2024 by dettoo456]
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clearly_not_atara
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Carbamide is a popular name for urea when you don't want people to think about urine. Like when it appears in cosmetics or medicine.
But it makes me wonder. Could you perhaps achieve the desired rxn with carbamide peroxide and a little catalytic bromide salt? The peroxide converts
the bromide to hypobromite which reacts with the urea to give hydrazine and regenerate bromide, etc.
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ManyInterests
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| Quote: Originally posted by dettoo456 | If the extraction in EtOH presents issues for you, you can always revert to Ca(OH)2 instead of NaOH. Just dissolve up the Hydrazine sulfate, add
req’d (or even excess) Ca(OH)2, heat with vigorous stirring for an hour or two, and then decant/filter while hot.
And if the resulting N2H4 conc% is too low, you can always pull out excess water w/ sieves since they won’t react with any of the hydrazine.
If you need the Hydrazine in Ethanol alone for whatever reason, you can just add EtOH to the N2H5OH, add a shit ton of sieves, and then filter.
[Edited on 15-4-2024 by dettoo456] |
I bought some calcium hydroxide since you mentioned that, if that is a more sure way of freebasing hydrazine, then I will use that method.
I also thank you for all the help you're giving me. I think the reason why it is all happening like this is due to the heating issue. I think my last
time I was too quick in filtering out my hydrazine (I was afraid it would volatilize really fast and I need to hurry as fast as possible) I think like
with making hydrazine sulfate has become more fruitful when I slowed everything down I think I also need to slow down the heating and the whole
process, too.
I made 97.97g from my last synthesis. So things are improving quite well in making hydrazine sulfate. I obviously cannot use all of it once (nor
should I!) but I know I can make a lot of good quality hydrazine sulfate for whatever I need.
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ManyInterests
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Just to drop in an update. I did finally do a successful freebase as I did before. The only thing I needed to do differently was simply add the
hydroxide piecemeal and not let things get TOO cold. It was an incredibly basic process.
| Quote: | | But it makes me wonder. Could you perhaps achieve the desired rxn with carbamide peroxide and a little catalytic bromide salt? The peroxide converts
the bromide to hypobromite which reacts with the urea to give hydrazine and regenerate bromide, etc. |
Possibly. That is something to consider. For now I have a 48g of extra hydrazine sulfate. Given how much I got in terms of practice, I am thinking of
doing one more synthesis to give me over a hundred grams of the stuff to add to it, then I will say I got a good stock.
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Keras
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I tried the hydrazine sulphate classic synthesis (the one you find everywhere on YouTube) with NileRed quantities, except that I replaced gelatine
with 1g of EDTA (which is too much, it doesn’t totally dissolved I had to filter the residue) anddddd… I got 50 g of hydrazine sulfate????
Something went wrong?
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Sir_Gawain
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| Quote: Originally posted by Keras | I tried the hydrazine sulphate classic synthesis (the one you find everywhere on YouTube) with NileRed quantities, except that I replaced gelatine
with 1g of EDTA (which is too much, it doesn’t totally dissolved I had to filter the residue) anddddd… I got 50 g of hydrazine sulfate????
Something went wrong? |
From how much urea? You may have just gotten a good yield. Did you test the purity?
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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ManyInterests
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| Quote: Originally posted by Keras | I tried the hydrazine sulphate classic synthesis (the one you find everywhere on YouTube) with NileRed quantities, except that I replaced gelatine
with 1g of EDTA (which is too much, it doesn’t totally dissolved I had to filter the residue) anddddd… I got 50 g of hydrazine sulfate????
Something went wrong? |
I'm curious as how much of your other reagents you used as well. For me the formula I use (and it is also used by Magpie as linked earlier by Sir
Gawain) is 34.1g. My last synthesis used triple that, 102.3g and I ended up with 96.96g. My best synthesis yet.
I never heard of EDTA before this. Why did you opt to use it in the place of gelatin? unflavored gelatin is ubiquitous and cheap.
I wanted to ask this question and I should have asked it a long time ago: How do you test the purity of hydrazine sulfate? In the past when I was
still inexperienced with hydrazine sulfate synthesis, I was so afraid of sodium sulfate synthesis that I would not allow it to sufficiently cool to
10C and I would filter it at 15C, thus losing a lot of potential yield (and I mean a LOT). Once I allowed it to slowly cool to 11C over the course of
several hours (using the ambient temperature outdoors) my yield improved considerably.
But I am curious as how to test for purity.
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Sir_Gawain
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One way I know is to heat it. Hydrazine sulfate should decompose leaving little residue behind. Another way would be to react with copper sulfate. It
form an insoluble complex that can be weighed to calculate the purity.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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