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Author: Subject: Hydrazine
Belowzero
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[*] posted on 24-5-2020 at 22:55


Failure


Hello Sciencemadness,
It's been close to 10 years since I was active here and I am glad to see SM is going strong!
Anyway recently I got a new lab up and running and decided to synthesize a small batch of HS which seemed to have failed.

Since I had a hardcopy of this procedure and since it is similar to Rosco's method I gave it a go.
https://www.designer-drug.com/pte/12.162.180.114/dcd/chemist...

I used roughly 1/6th of the amounts used.
Which comes down to:

Urea 22.0g
Bleach 230.0ml 12.5 %
NaOH 32.3g
Pig Gelatine 0.3g
Sulfuric acid 183ml 37%


I didn't confirm the concentration of the bleach however I know this batch is relatively fresh and should be very near to 12.5%
This is 20ml less than the procedure to compensate for its higher concentration.

Now I know the neutralization step is suboptimal compared to the HCl route and took this for granted.
I might just have made very expensive glaubers salt because the procedure did not go as planned.


The dissolving of the NaOH was quite tedious, to buffer the temperature of the bleach I used a large cold water bath.
The temperature never rose above 10 degrees C.

After adding all the reactants a large evolution of gas was witnessed, the temperature rose strongly (no measurements)
almost too hot to touch the flask.
Expecting the foaming as described and seen in my earlier days of making this substance I was surprised hardly any foam was produced at all, only a very small whiteish layer above the liquid. This subsided entirely after a few minutes.

The production of gas stopped entirely after an hour or so and I decided to kick up the heat to just below boiling.
More gas was produced and the heat was turned off again.

I called it quits because no distinct coloration nor foaming was witnessed and dumped the content in a large beaker in a cold water bath. The sulfuric acid was added and left to cool in the same bath, ~10-15 degrees C.

The next day a layer of white precipitate was formed.


No tests have been conducted yet on the product.
I suspect I have made really expensive sodium sulfate.
Now the question is why didnt the reaction foam excessively like it should?


I suspect it is due to metal traces in the reaction , the groundwater contains quite some iron. I use this to wash my glassware.
Of course knowing this I took extra care and flushed it with both NaOH solution and HCl as an attempt to get rid of traces.
Looks like it still was not enough to get rid of it.
Or perhaps I messed something else up like using too much hypochlorite.

Any suggestions ?




[Edited on 25-5-2020 by Belowzero]
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woelen
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[*] posted on 25-5-2020 at 00:50


Did you test the white solid? Does it dissolve in cold water easily? If not, then it might be hydrazinium sulfate (that compound only dissolves with difficulty in cold water). Another test for hydrazinium sulfate is to add this to an acidified solution of KMnO4. This will lead to nearly instantaneous loss of color of the solution. If it is just sodium sulfate, then there will be no loss of color and if it is urea, then there will only be slow disappearance of color.

You could also add some of the solid to a concentrated solution of an acidified chlorate, bromate or iodate. With hydrazinium sulfate you will have a very violent reaction.




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Belowzero
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[*] posted on 26-5-2020 at 08:11


Quote: Originally posted by woelen  
Did you test the white solid? Does it dissolve in cold water easily? If not, then it might be hydrazinium sulfate (that compound only dissolves with difficulty in cold water). Another test for hydrazinium sulfate is to add this to an acidified solution of KMnO4. This will lead to nearly instantaneous loss of color of the solution. If it is just sodium sulfate, then there will be no loss of color and if it is urea, then there will only be slow disappearance of color.

You could also add some of the solid to a concentrated solution of an acidified chlorate, bromate or iodate. With hydrazinium sulfate you will have a very violent reaction.



Thanks Woelen!
I conducted the test with KMnO4 , I dissolved a few crystals in 10 ml of water with a drop of H2SO4.
When I dropped in a few supposed HS crystals the solution went to light pink and then white almost instantly.

Also the material is poorly soluble in cold water, I attempted to dissolve a few wet crystals in 20ml which didnt go into the solution upon stirring.

The wet crystals are now washed ,vacuum filtered and put in a dessicator, I'll conduct more tests to rule out any false positives.

It seems the synthesis did produce HS after all.
I am still clueless as to why the foaming was practically absent, if the yield is good it might be worth investigating since the foaming is the worst part of this procedure and it would be great if this could be prevented.

More results later.


[Edited on 26-5-2020 by Belowzero]
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[*] posted on 26-5-2020 at 15:29


Quote: Originally posted by Belowzero  


It seems the synthesis did produce HS after all.
I am still clueless as to why the foaming was practically absent, if the yield is good it might be worth investigating since the foaming is the worst part of this procedure and it would be great if this could be prevented.

More results later.


[Edited on 26-5-2020 by Belowzero]


The amount of foaming you get is very variable and depends on the additives in the bleach. I switched to pool chlorine for my HS thinking it would not have many additives and it has a high NaClO concentration. However, it foams more than any other NaClO source that I have used before. It does produce a good yield though.
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Belowzero
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[*] posted on 28-5-2020 at 22:23


Quote: Originally posted by B(a)P  
Quote: Originally posted by Belowzero  


It seems the synthesis did produce HS after all.
I am still clueless as to why the foaming was practically absent, if the yield is good it might be worth investigating since the foaming is the worst part of this procedure and it would be great if this could be prevented.

More results later.


[Edited on 26-5-2020 by Belowzero]


The amount of foaming you get is very variable and depends on the additives in the bleach. I switched to pool chlorine for my HS thinking it would not have many additives and it has a high NaClO concentration. However, it foams more than any other NaClO source that I have used before. It does produce a good yield though.


NaClO is actually the only thing it contains according to the label , I'll have another look at what the manufacturer mentions.
The precursors used are all quite pure in fact.
Externally introduced impurities is the only thing I can think of at this point.
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