| Pages:
1
2
3 |
Oxy
Hazard to Others
Posts: 140
Registered: 1-12-2020
Member Is Offline
|
|
Quote: Originally posted by ManyInterests  |
Yes! I am extremely lucky that the only thing that happened is that my final product was ruined and nothing else. I am not using a hydroxide trap
anymore. |
Why not? Traps are good if they are setup in a correct manner. Just test it before running a reaction.
Have you ever heard of aluminium foil or towels?
|
|
|
ManyInterests
National Hazard
Posts: 942
Registered: 19-5-2019
Member Is Offline
|
|
| Quote: |
Why not? Traps are good if they are setup in a correct manner. Just test it before running a reaction. |
When I start using them. The trap doesn't immediately start sucking up. I don't know when it would do that, I will try a different setup in order to
not have the funnel completely submerged in the solution. That should prevent any accidental suck up.
| Quote: | | Have you ever heard of aluminium foil or towels? |
I've mentioned it before, I did use them. However I would like to observe what is happening.
Edit: I would really like some advice on the temperature with some solid numbers. I've wasted a lot of my precious KNO3 already.
[Edited on 8-11-2021 by ManyInterests]
|
|
|
Oxy
Hazard to Others
Posts: 140
Registered: 1-12-2020
Member Is Offline
|
|
Yes, the whole idea is to submerge the hose output/funnel/whatever in a way that if there will be pressure change and reactor will start to suck then
the process will simply break.
The level of liquid in trap should be of course continuously watched as the volume may increase due to dissolving something or temperature change. So,
even if the trap will look good when starting then after some time it might need some adjustment.
Regarding temperature - the thing you ask is the influence of the temperature on decomposition rate of HNO3. I am not 100% sure but I would say that
water presence will probably not change anything. Keep temperature as low as possible with reasonably fast distillation rate. There are always some
losses but you would need to produce a lot of NO2 to see the effect. In temp of 90 deg C and 1 atmosphere pressure 1 mol of NO2 takes almost 30 liters
of volume. You would need to produce it a lot to see a drastic effect.
Optionally you could submerge your receiver flask in ice cold water (the colder the better and try to condense NO2). But it will not produce clean
HNO3
|
|
|
ManyInterests
National Hazard
Posts: 942
Registered: 19-5-2019
Member Is Offline
|
|
| Quote: | Regarding temperature - the thing you ask is the influence of the temperature on decomposition rate of HNO3. I am not 100% sure but I would say that
water presence will probably not change anything. Keep temperature as low as possible with reasonably fast distillation rate. There are always some
losses but you would need to produce a lot of NO2 to see the effect. In temp of 90 deg C and 1 atmosphere pressure 1 mol of NO2 takes almost 30 liters
of volume. You would need to produce it a lot to see a drastic effect.
Optionally you could submerge your receiver flask in ice cold water (the colder the better and try to condense NO2). But it will not produce clean
HNO3 |
Yes. That was my main question. Every video and synthesis description for WFNA or RFNA always stated the number for the temperature, while
instructions for the 68% were always fairly vague like 'turn it to high' or what Magpie wrote at '70% of max power' If I did what Magpie wrote, it
would meaning having to set my mantle to 210 degrees, which is too high. My mantle can go higher than the 300 degree max (I boiled sulfuric acid
multiple times).
I do need to experiment with my mantel's heat settings. This is because I cannot stick my mantel's thermometer into the distillation joints. I have a
feeling that it is dependent on the reading it gets from the thermometer to know when to stop heating up, otherwise it just keeps on heating up. I
need to make sure that is not the case, otherwise I will end up ruining my end product again. I came so close at my 3rd attempt. 4th one I hope to
make RFNA and dilute it down to 70%. I only need a little WFNA.
I do use an icebath. The NO2 can be cleaned out by bubbling, or doing what Darian Ballard did, by putting the flask in a bowl of sodium carbonate,
putting the whole thing in a freezer bag, and putting it in the freezer for a bit (with the cap not being too tight) which will result in it clearing
up.
Edit: I was right. My mantel will continue heating without any input from it's thermometer. No wonder my yields were so low. Even if I didn't have the
hydroxide mishap. The heat would have obliterated much of my precious nitric acid. Thankfully I managed to find a way to fit it into distillation
joint. I hope this will work correctly now.
[Edited on 8-11-2021 by ManyInterests]
[Edited on 8-11-2021 by ManyInterests]
[Edited on 8-11-2021 by ManyInterests]
|
|
|
ManyInterests
National Hazard
Posts: 942
Registered: 19-5-2019
Member Is Offline
|
|
OK this is funny. I don't understand what happened. But it's really weird.
So given the irregularities of the heating. What I did was set my mantel temperature to around 65 to 70 degrees, but the solution did boil and my
thermometer did fluctuate from 85 to 116 degrees and I did get dripping in my receiver flask.
Problem is. The process never took more than an hour or two before it clearly starts to dry up and start to form a hard potassium sulfate cake. This
time there was no such drying. In fact for the past 4 hours (I must have run it for 7 hours or 8 hours at least) there was no drop in how much
solution was in my boiling flask. I raised the temperature but it did not appear to have any discernible effect. I wrapped everything in foil and I
will look at what I got tomorrow.
|
|
|
ManyInterests
National Hazard
Posts: 942
Registered: 19-5-2019
Member Is Offline
|
|
OK I finally did it. Got a density of 1.446. The yield was small, but it is a success. I have some RFNA! Just need to dilute it down to 70% VERY
carefully at room temperature and I can finally go ahead with my experiments!
I turned out that what was left boiling in my flask was just the sulfate. Turning it off caused it to dry rather quickly. At any rate it looks fairly
soft and not hard. So cleaning it should not be a problem.
Feels good man! I feel like I went through another great hurdle!
|
|
|
ManyInterests
National Hazard
Posts: 942
Registered: 19-5-2019
Member Is Offline
|
|
Just putting it that I appear to have gotten a handle on making nitric acid. Today I made two batches. Both appear to be around 70%. One of them have
NO2 contamination while the other is nearly colorless.
My solution was, using magpie's formula, was to add 8 to 9 ml of water (and not more) with very dry powdered KNO3 and a few drops more sulfuric acid
than what he put in. That appears to be doing the trick just fine.
I had to turn my mantel on and off multiple times as I couldn't put my thermometer in it and I needed some way of controlling the temp. either way it
didn't take hours upon hours but was done in less than hour. I hope I can get similar results with the attempts for WFNA.
|
|
|
ManyInterests
National Hazard
Posts: 942
Registered: 19-5-2019
Member Is Offline
|
|
I came back to this thread because while I have already made plenty of good nitric acid (fuming and 70%). But I have one question.
when working with different nitrate salts. Like with NileRed in his video on making nitric acid, he notes that you could use 404 grams of potassium
nitrate or 320 grams of ammonium nitrate.
And going back to Magpie's thread on making nitric acid, he used 225 grams of potassium nitrate. If I was using sodium nitrate, how much should I use?
This is because I will be making a good amount of sodium nitrate and I also want to use that to make nitric acid.
|
|
|
Rainwater
National Hazard
Posts: 939
Registered: 22-12-2021
Member Is Offline
Mood: Break'n glass & kick'n a's
|
|
You should readup on on it
Chapter 4
Stoichiometry of Chemical Reactions .
https://openstax.org/details/books/chemistry-2e
The quantities you stated are likely to be molar equivalents. I didn't run the numbers so lets do that now.
So KNO3 has a molar mass of about 101g/mol
And NH4NO3's molar mass is about 80 g/mol
404 ÷ 101 = 4 mol
320 ÷ 80 = 4 mol
So if you have 4 mols of a nitrate salt, you need 4 mols of H2SO4 to react with it.
H2SO4 has a molar mass around 98 g/mol
98*4 = ~400 ish if your acid is 100% pure
There is a section explaining the math to calculate the amount required when purity is known.
Edit. I cant find the reference
Basicly
X = Weight needed (pure)
Y = purity of your compound ( 100% = 1.00 3% = .03)
Z = weight if your compound equivalent to pure substance
Z = X × ( 1 ÷ Y )
Say you needed 1g of pure acid. And all you have is a 50% solution.
1 × (1 ÷ .50) = 2g of solution will be needed
So to answer your question, you need to know the molar mass of sodium nitrate. Then know how much product you wish to generate.
That will tell you how much acid to add.
[Edited on 27-6-2022 by Rainwater]
"You can't do that" - challenge accepted
|
|
|
ManyInterests
National Hazard
Posts: 942
Registered: 19-5-2019
Member Is Offline
|
|
OK, so I will need to find the molar mass of sodium nitrate to do it then. I did see in a book that 58 grams of sodium nitrate was equal to 68 grams
of potassium. If that is the case I can work with that. But obviously I will need more information.
I am confident about the purity of my stuff. It isn't obviously as pure as store bought stuff, but I am confident I can make all sorts of nitric acids
with them. From fuming to 70%.
edit: I believe this site will help:
https://www.convertunits.com/molarmass/Sodium+Nitrate
https://www.convertunits.com/molarmass/Potassium+Nitrate
https://www.convertunits.com/molarmass/ammonium+Nitrate
This should tell me all I need to know. Goodie! 
[Edited on 27-6-2022 by ManyInterests]
|
|
|
B(a)P
International Hazard
Posts: 1139
Registered: 29-9-2019
Member Is Offline
Mood: Festive
|
|
You can just read it off a periodic table or even easier go to the SM wiki and get the molar mass from the write up of the compound you are interested
in. It might be a good idea to work it out from a periodic table a few times though, this will help you understand what molar mass is all about. It is
a very important foundational knowledge for chemistry. This explains it well.
https://youtu.be/PAqzpZ-nMlg
|
|
|
Fantasma4500
International Hazard
Posts: 1681
Registered: 12-12-2012
Location: Dysrope (aka europe)
Member Is Offline
Mood: dangerously practical
|
|
https://www.webqc.org/balance.php?
this is very helpful and can even give you molar masses if you are a bit creative and the damn thing wont acknowledge the reality of what youre trying
to accomplish, for instance KNO3 = KNO2 + O2 will give you molar mass of all 3
|
|
|
ManyInterests
National Hazard
Posts: 942
Registered: 19-5-2019
Member Is Offline
|
|
Just putting in a report (public lab note). I tried to go for WFNA again but ended up with a product that has a specific gravity of 1.486233 at 15C.
(114.44 grams to 77ml) This would bring it to around 88.5% nitric acid (10 percentage points below where it needs to be). I used 185 grams of sodium
nitrate (dried in the oven overnight) to 120ml of cleaned and purified sulfuric acid (close to 98%) and no added water whatsoever. I did this in a 2
liter boiling flask to give myself more room.
Is it possible that the size of the flask is what caused it to be less concentrated? Because I did see stuff dripping back into the flask as it was
trying to get up to the joints and go over. I used chilled water to go through the jacket to allow for appropriate cooling and placed the receiving
flask in a salt-water ice bath.
Next time I will use a smaller boiling with similar proportions. Either way I need to look up on how to dry nitric acid, I think that'll be an easier
solution. At least there is some good news... I have no problem making good clean nitric acid. Just not the concentration I want.
It is strange. Because the first ever time I went for fuming nitric acid it worked perfectly. I got nearly 100% the first time. I don't know what is
going wrong.
edit: I am not sure if the size of the boiling flask was responsible. But I will try a smaller one anyway. I see that the sulfate cake still looks
moist. It is also possible that my sulfuric acid might need a little more boiling before use? Either way, before I try again, I want to try to dry it
more.
[Edited on 4-8-2022 by ManyInterests]
|
|
|
Tsjerk
International Hazard
Posts: 3032
Registered: 20-4-2005
Location: Netherlands
Member Is Offline
Mood: Mood
|
|
How did you determine the concentration of the sulfuric acid?
|
|
|
CharlieA
National Hazard
Posts: 646
Registered: 11-8-2015
Location: Missouri, USA
Member Is Offline
Mood: No Mood
|
|
"Just putting in a report (public lab note). I tried to go for WFNA again but ended up with a product that has a specific gravity of 1.486233 at 15C.
(114.44 grams to 77ml)"
I don't mean to be picky, but 114.44/77 = 11.5; only 2, not 7, significant figures. To increase your precision, the easiest way would be to measure
the volume more precisely, perhaps with a graduated pipette or burette.
|
|
|
Texium
|
Thread Moved
5-8-2022 at 06:38 |
ManyInterests
National Hazard
Posts: 942
Registered: 19-5-2019
Member Is Offline
|
|
| Quote: Originally posted by CharlieA | "Just putting in a report (public lab note). I tried to go for WFNA again but ended up with a product that has a specific gravity of 1.486233 at 15C.
(114.44 grams to 77ml)"
I don't mean to be picky, but 114.44/77 = 11.5; only 2, not 7, significant figures. To increase your precision, the easiest way would be to measure
the volume more precisely, perhaps with a graduated pipette or burette. |
I got a glass graduated pipette. i never thought to calculate it that way. I use a graduated cylinder for my calculations. I think I will try again
then.
|
|
|
CharlieA
National Hazard
Posts: 646
Registered: 11-8-2015
Location: Missouri, USA
Member Is Offline
Mood: No Mood
|
|
| Quote: Originally posted by ManyInterests | | Quote: Originally posted by CharlieA | "Just putting in a report (public lab note). I tried to go for WFNA again but ended up with a product that has a specific gravity of 1.486233 at 15C.
(114.44 grams to 77ml)"
I don't mean to be picky, but 114.44/77 = 11.5; only 2, not 7, significant figures. To increase your precision, the easiest way would be to measure
the volume more precisely, perhaps with a graduated pipette or burette. |
I got a glass graduated pipette. i never thought to calculate it that way. I use a graduated cylinder for my calculations. I think I will try again
then. |
CORRECTION: 114.44/77=1.5 (2 significant figues)
I am glad to hear that you have a graduated pipette. If it is graduated in 0.1 ml increments, then you can estimate a volume to 0.01 ml; for a sample
size greater than 10 ml this will allow you to measure the volume to 4 significant figures. With the sample size mass that you used above indicating 5
significant digits, then your calculation will be good to 4 significant figures, or 1.xxx g/ml.
Of course, your estimate of accuracy must take into account the accuracy of your measuring instruments, not just the precision. All in all, I think
that you are heading to achieve good precision in your measurements.
|
|
|
Tsjerk
International Hazard
Posts: 3032
Registered: 20-4-2005
Location: Netherlands
Member Is Offline
Mood: Mood
|
|
Sure 114.44/77 = 1.5, but assuming the graduated cylinder has a better than 1% precision and assuming the liquid was exactly on the 77 ml mark you
could say the volume was in the 76.5 - 77.5 range. That would mean a density between 1.48 and 1.50, which would be 89 - 98% at 20oC.
A density of 1.5 would be something like 80-100%. But either way, a better precision would be nice. If there is a lot of water in there, there is only
one reasonable source which would be the sulfuric acid. The sulfuric acid you could titrate.
|
|
|
Sir_Gawain
Hazard to Others
Posts: 458
Registered: 12-10-2022
Location: [REDACTED]
Member Is Offline
Mood: Stable
|
|
I've done it. I made a batch of nitric acid using ammonium nitrate and the concentration was around 85%. Then I diluted it to 68% with distilled
water. The reaction wasn't very exothermic, but the diluted acid retained a yellow color. I then distilled it again (not fractional) and checked the
concentration.
With ammonium nitrate I haven't been able to get it over 85%. Using the same sulfuric acid, and potassium nitrate, 98% was obtained. I guess for
dilution though, a lower concentration is good because it won't be so exothermic.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
|
|
|
ManyInterests
National Hazard
Posts: 942
Registered: 19-5-2019
Member Is Offline
|
|
OK, so I got something to ask since I got some nifty new equipment.
So previously when distilling, I could not control for temperature because I could not put in the thermoprobe into my flask when distilling, so I had
to device a very peculiar 'on-off' dance where I would observe how the reaction is going in the flask and once I feel it is getting too hot (and the
foam is rising up to the joints... not good!) I would turn it off and let it cool down a little before turning it back on again once it cools off a
little.
This system worked. It isn't super efficient or scientific, but it worked. But now I have a knew glass thermometer adapter that can accommodate my
thermoprobe easily, so I can have more control over the temperature.
When using it, my thermometer can go half-way into my 1 liter flask, and around a quarter in to my 2 liter flask. Would this pose a problem? I also
need some confirmation as to what temperature range I should be looking for when making WFNA. Is it around 85 to 90C?
I did learn that... yes, diluting the acid down is not an issue and it can be done quite easily, just control for the exothermic reaction and it isn't
going to be an issue.
Right now I just want to make sure I am going to get good WFNA consistently. I also wanting to explore how the temperature control can be used to
further purify nitric to WFNA by distilling it a 2nd time with sulfuric acid and keeping the temperature range only at 85 to 90C?
|
|
|
Rainwater
National Hazard
Posts: 939
Registered: 22-12-2021
Member Is Offline
Mood: Break'n glass & kick'n a's
|
|
Using an excess of sulfuric acid will help remove any water in the appratus.
I did not see that mentioned before
Using an insulated fractional column of some kind, place the thermowell just above your solution, set your temperature to 86c (if i remimber
correctly) and compare the head temp.
Anhydrous acid will come over first, when the lower thermowell reads a different temperature than the head, your starting to get water in your acid.
NO2 contamination can be removed with a gentle vacuum and reflux of you want a nice clear acid. But if your diluting later, their isnt much
point as the addition of water will clear up the acid aswell.
"You can't do that" - challenge accepted
|
|
|
Alkoholvergiftung
Hazard to Others
Posts: 190
Registered: 12-7-2018
Member Is Offline
|
|
I wouldnt destill ammoniumnitrate. I ve read that they used ammoniumsulfate to purificate Sulfuric acid the ammoniumsulfate reactes with HNO3 to form
N2O gas. I think the same oculd happen when you destill ammoniumnitrate. (Ive read it again it only happens when you have an exceed of H2SO4.)
[Edited on 23-5-2023 by Alkoholvergiftung]
|
|
|
Lionel Spanner
Hazard to Others
Posts: 168
Registered: 14-12-2021
Location: near Barnsley, UK
Member Is Offline
|
|
For what it's worth, I've successfully distilled azeotropic nitric acid using concentrated sulphuric acid with hydrated magnesium nitrate (fertiliser
grade). The mixture stops evolving nitrogen dioxide and the azeotrope comes over as a clear pale yellow liquid.
|
|
|
ManyInterests
National Hazard
Posts: 942
Registered: 19-5-2019
Member Is Offline
|
|
| Quote: Originally posted by Rainwater |
Using an excess of sulfuric acid will help remove any water in the appratus.
I did not see that mentioned before
Using an insulated fractional column of some kind, place the thermowell just above your solution, set your temperature to 86c (if i remimber
correctly) and compare the head temp.
Anhydrous acid will come over first, when the lower thermowell reads a different temperature than the head, your starting to get water in your acid.
NO2 contamination can be removed with a gentle vacuum and reflux of you want a nice clear acid. But if your diluting later, their isnt much
point as the addition of water will clear up the acid aswell. |
That would work if I had a 2 necked flask, but I don't. I only have a 1 neck. I wish I could put in two thermometers to get one reading at the bottom
and the other at the top. Unless I am misunderstanding you?
I am OK with a little discoloration. I do, however, wants to consistently get WFNA to use for some RDX synths. For everything else I can dilute it
down or just make it an azeotrope from the get-go since from what I've seen, the only thing that really needs pure WFNA is RDX. Most everything else
from nitroglycerin or EGDN and other stuff can be done with a simple azeotrope, which hasn't been a problem for me for a long time.
|
|
|
Raid
Hazard to Everyone
Posts: 203
Registered: 14-11-2022
Location: N/A
Member Is Offline
|
|
you could use dilution calculation to dilute the HNO3
|
|
|
| Pages:
1
2
3 |
![[*]](images/xpblue/default_icon.gif){kind=icon}
