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ManyInterests
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Quote: Originally posted by DennyDevHE77  | | I don't really understand why everyone is paying attention to this. I've had fuming nitric acid on my skin many times. The result was always in the
form of yellowed skin or small ulcers later, also yellow. But it never caused any painful feelings. The most inconvenient thing was that, for example,
a nail dyed yellow would have to grow back before it returned to its color. |
I have a scar on my left hand that is a reminder of the dangers of that. I am not sure if it was something else in the acid that caused it to burn
through my skin, and this was even after I had immediately plunged my hand in a bicarbonate solution and started to pray it relentless with
bicarbonate spray (before running to the faucet and letting cool water run on my hand for a minute or so.
So I must beg your pardon, but I will need to take caution with all material.
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greenlight
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Just finished the step from nitrourea to DPT on larger scale.
This time, 40 grams of nitrourea was dissolved in 500ml of 37% formaldehyde and heated until dissolution occurred.
Sodium hydroxide solution (5%) was added to the straw yellow clear solution until pH 3 was achieved.
The solution was heated to 65°C and held for just over an hour before cooling in a water bath.
Aqueous ammonia (25%) was added dropwise with stirring until DPT crop precipitated and was vacuum filtered before repeating this base addition two
more times.
The DPT product was very light tan in colour this time which indicates some impurity that may have been formed when the temperature reached 68°C at
one point or the high acid content of the nitrourea used could have caused this.
A recrystallisation is probably the way to go before proceeding further.
Be good, otherwise be good at it 
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greenlight
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Final yield of DPT is 13.00 grams. It is an off-white light brown colour,.
A fresh batch of fuming nitric acid needs to be distilled and any NOx removed before the next step.
I am curious whether an increase in HMX yield can be seen from this method by the presence of phosphorus pentoxide in the nitrolysis reaction?
[Edited on 2-12-2024 by greenlight]
[Edited on 2-12-2024 by greenlight]
Be good, otherwise be good at it
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