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carbonfeind
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I have never been able to get NaNO3 to dissolve completely even when using fresh sulfuric. I use a 50/50 NH4NO3/NaNO3 mixture.
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quicksilver
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I was going to wash glassware on a day off so I tried a fast experiment.
I re-crystallized several common nitrates, especially NaNO3 & KNO3. The source was stump remover and old bags of fertilizer. I was only doing it
for the pictures (I take quite a few pictures of unique crystalline shapes) but was really surprised at the amount of inerts in the prilled materiel
trapped in the filter paper.
Greenlight brand had certainly 20%+ clay and crap left over.
Grant's stump remover had roughly less about 15% (I wasn't going to dry out several just to be on the money to determine junk in a low grade
material).
Bromide (NaNO3) had about 25% inert as well as being visually obviously filled with inferior and dirty material. Prills come from a drop tower and
it's possible that the shute could be quite dirty and the last of the batch would be sold off at pennies, giving something like stump remover a huge
profit margin.
Bagged prills had about 10-15% of clay and non-caking agents max. except for the ACE house brand Bromide (NaNO3) which was startling in how much
materiel would just NOT go into solution in a rolling boil. In comparison I used very old bottle of NaNO3 and it disappeared in the hot water. As a
very old technical grade I expected SOME insolvable material but the filter held virtually none at all.
The stump remover obviously had material that MAY have been there as just plain garbage from sweepings, etc But realistically with that level of
garbage, the possibility of a poor mixed acid [from such a mix] is high.
The re-crystallized material was so clear, well-defined crystals as to be close to totally transparent. IF the project is worth doing (IMO) it's worth
doing well. Too often I had guessed that prilled nitrates were lower grade than technical; but this was really too much!
Much of the H2SO4 is surplus acid and the blackened material id often too hard to determine. But at 93% (generally) heating it till white wisps of
"smoke" appear will result in a very thin dark layer separated on the bottom of the heated vessel & is very easy to separate, leaving a higher
grade percentage acid and a lack of "junk" that won't add anything positive to an experiment. Two hours and both solids and acid could be cleaned to
nearly reagent grade. That would remove a great deal of problems that appear to have multiple origins.
Incidentally KNO3 can form very strong, thick glass-like needle crystals 3mm wide x 2cm long within a ph of slight alkalinity 7.6-8. Dropping the ph
to 6.8 - 7.2 and the needles thin out to less than a millimeter & very fragile. Not only was this repeatable but no loss in weight could be
recorded from either method. The thick, well formed needles were quite dense, while the thinner materiel was as thin as Nitroguanadine but dense in
growth.
[Edited on 15-12-2009 by quicksilver]
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Zinc
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Today I again tried to make NG.
50 g of ammonium nitrate (contaminated with a few % magnesium nitrate) was added to 95 ml of conc. H2SO4. After adding the ammonium nitrate (I added
it all at once) I put the mix into snow to cool it. After 15 min all of the NH4NO3 was dissolved. The solution was quite clear, only a little milky.
When the mix cooled to 10 C I added 12.5 ml of glycerine in 10 min. The temp. rose only a little. Then I let the mixture to stand at room temperature
for 1 hour. After one hour the mix is opaque and an approx. 1 mm thick clear layer formed on top of the mix. I will leave the mix to stand for some
time more before pouring it in a NaHCO3/NaCl solution.
All reagents are analyical grade, except the ammonium nitrate wich was extracted from fertiliser.
[Edited on 20-12-2009 by Zinc]
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hissingnoise
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Did you swirl the mix as the glycerol was added or did you use a mixing rod?
Anyway, gentle, prolonged swirling before drowning might be a good idea.
The problem I have with NH4NO3 and NaNO3 is that they're more difficult to dry than KNO3 and once dry they start absorbing moisture almost
straightaway.
[Edited on 20-12-2009 by hissingnoise]
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DetaDude
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Saftey is a good blowjob
Please, please, and this has been said before on this thread but bears repeating and take this to the bank from an old salt with the experience of
many years of making NG DO NOT under any conditions stir the nitrating mix with anything but air. Buy a cheap aquarium pump and use glass tubing, an
old pipet heated and bent in an "L" shape works fine.
You may get away with a stir bar or glass rod for awhile but not forever.
Please stay SAFE. NG is not the boogyman that it's reputation might lead you to believe but it is nothing to get careless with or lose respect for.
Genius creates many a great works............Labor alone finishes them!
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Zinc
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I swirled the mix.
Quote: Originally posted by hissingnoise  |
The problem I have with NH4NO3 and NaNO3 is that they're more difficult to dry than KNO3 and once dry they start absorbing moisture almost
straightaway.
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Yes indeed they are very difficult to dry. To ensure that my NH4NO3 is dry before using it, I remove the mostly dry ammonium nitrate from the jar in
wich it is stored and redry it with a hot air blower just before using it.
After the mixture was left to stand for an another hour and 10 min. the clear layer that separated on the top of the mix has considerably enlarged.
Now it is around 5-6 mm thick. I will leave it stand for some more time, perhaps even more of it forms. It is chrystal clear, I belive that that is
NG.
Should I pour all of the mixture in to the NaCl/NaHCO3 solution or just the NG?
[Edited on 20-12-2009 by Zinc]
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hissingnoise
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I haven't tried the nitrate method, but I'd pour as much as will go in and neutralise the residue in the beaker with a large portion of dilute NaHCO3
to recover all the ngl.
I used to use plain water as first wash, swirling, then decanting most of it before gently adding very dilute NaHCO3.
The drying wash was last!
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Zinc
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I extracted the NG from the top of the mix and poured it in the NaCl/NaHCO3 solution. I will wash it a few times and let it sit over night under the
solution, tommorow I will check if it is stil acidic. If it is more washings will be done. Yield is around 10-15 ml I belive.
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hissingnoise
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There's still a possibility that what separated contains some dinitrate, so you just may end up with slightly less than you expected but even 8-9 ml
would still be respectable.
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Zinc
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Well today I checked the NG. It is still acidic, but the solution under wich it sits is basic. So I dont see the point of removing the solution and
adding a new portion as this one is still basic. Any ideas how to neutralize the NG?
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hissingnoise
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It's important that the ngl is neutralised quickly---when in the basic sol. it should be swirled immediately and for several minutes.
This exposes the interior of the ngl to the basic sol..
Letting it just sit without movement is very dangerous as it will start to decompose and become super sensitive.
If your ngl develops a yellowness it should be discarded straightaway, and carefully. . .
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Zinc
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So a few minutes of swirling is enough to neutralise it?
And is it better to neutralise the NG with an only NaHCO3 solution, or with a NaHCO3/NaCl solution?
I tried to set off some of the undried and partialy nutralized NG with a sparkler, but it didnt go off. The sparkler extinguished before the burning
zone entered the NG (I know a stupid way to ignite dangerous materials). But a few drops when striked with a hammer detonate nicely 
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hissingnoise
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The salt solution removes entrained water; washed, neutral ngl in contact with air will slowly clear without salt solution.
I'd use separate washes for safety---plain water, then neutraliser and saturated salt solution last.
How much did you get, BTW?
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Zinc
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Well I didnt mesure the whole amount but the amount I tried to detonate was 5.5 ml. Around the same amount is still in the jar so I guess I got 10-12
ml.
So after washing the NG with plain water it should be washed with a basic solution. And it should be only swirled in the basic solution for some time,
not let standing under it?
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User
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| Quote: |
And it should be only swirled in the basic solution for some time, not let standing under it?
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Could you be more specific?
The basic solution should be considered a wash to remove acid traces from the NG.
What i do is keep adding carbonate until the solution stops foaming/bubling.
Then leave it standing for a couple of hours.
What a fine day for chemistry this is.
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hissingnoise
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Zinc, you need to stand well clear if you're setting off 5.5 ml!
Small quantities, though, just burn with a bit of popping on ignition. . .
I've had ngl evaporate to dryness sitting in an aluminium bun-case over a burning hexamine tablet.
Ngl-soaked tissue deflagrated quietly when ignited by a Christmas-tree bulb.
Anyway, as soon as ngl is under water, NaHCO3 sol. or salt sol. swirling is pretty mandatory to continually expose fresh ngl to the action of the
solution.
And as I said salt solution can be omitted if your ngl tests neutral and you're in no big rush.
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Zinc
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| Quote: Originally posted by User |
Could you be more specific?
The basic solution should be considered a wash to remove acid traces from the NG.
What i do is keep adding carbonate until the solution stops foaming/bubling.
Then leave it standing for a couple of hours.
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That is what I did, pour the NG in a basic solution, when the solution wasnt basic any more I added more of the basic solution and let the NG stand
under it over night (now it has been under the solution for almost 24 h). I also swirled it quite a bit today. Now the solution is basic, but the NG
is still acidic. Perhaps more swirling is in order  I will leave it again over
night and check it tommorow.
[Edited on 21-12-2009 by Zinc]
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User
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Somehow NG and other esters of this kind are very good at trapping acid.
I once had the idea of adding acetone to take the NG in solution for more reaction surface with the base.
The downside is that it might get difficult to regain the product back from the solution.
Also stirring with a wooden rod or ice stick reduces friction.
Some time ago I placed the freshly made NG in a plastic container and added a stirbar and the base.
I let this stir for a couple of hours for better neutralisation.
The downside to this is that the NG is dissolved in the water which makes the yield suffer.
Another thing that i often noticed is that this material behaves very strange in water enviorment.
It somehow forms a film on the water and tiny droplets float to the surface that dont like to sink, maybe this is somekind of supension formation or
that there is air trapped.
the longer it is stirred the more of this layer is formed.
[Edited on 21-12-2009 by User]
What a fine day for chemistry this is.
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hissingnoise
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Sometimes the droplets will sink but it's frustrating as there's always some ngl that refuses to drown.
The quantity, though, is smaller than it looks and doesn't represent any significant loss of product. . .
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Picric-A
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Add a couple of drops of washing liquid solution to the NG drops, should cause them to drop.
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hissingnoise
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Yes Picric-A, it could be a surface-tension thing---have you tried it?
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User
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Lol adding a bit of dishwash soap breaks surface tension.
Some times I got the drops down by letting a pippet suck and spit quickly just below the surface.
What a fine day for chemistry this is.
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quicksilver
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This should be carved in stone in the labs of most hobbyists.
(IMO) people should stop ignoring "Plant-Level" methods of working with various materials. NG is left for at least a day or two in a completely
saturated solution of anti acid and salt back when DuPont had to move his works due to a very tragic explosion. After they lost human life they
learned that the solutions should be saturated and that the longer the better. The problem (like the liquor industry) is that people need the item
NOW, not later. But a full 24 hours is not over-doing it. The salt and (baking soda) carbonate, etc- would be placed in a blender to totally saturate
the water until not a molecule's room is left. Then the NG should be introduced (outside the blender of course) and will sink with "some" milky
translucence. When it's totally clear, the water's out, but a ph should wait, lest you get a false reading from the solution. Safety takes time.
The surface tension issue has viability but I believe that a totally saturated solution may not have that issue unless there is a reasonable amount of
dust or other floating particulate. Repeated success appears to balance on saturated solution of anti-acid and salt. Just an opinion.
[Edited on 24-12-2009 by quicksilver]
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mfilip62
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I got some idea about NG that may be crazy
or great and simple...
What about toluene!?
Is it good idea to mix NG with toluene and will it dissolve NG!?
Pro is that they both don't mix with water.
NG/water emulsion will disappear instantly and you would get NG/toluene mix waiting to be evaporated.
And con is that NG is oxidizer and toluene is fuel, so I don't know will it
be dangerous to mix them!?
If so,that would be the best method to extract NG from water/acid mix.
I prepared my NG with 30g of 65%HNO3 /35g of 96% H2SO4 and 9g of glycerin.
Temperature never risen more than 30°C and I was stirring it for 30 min.Stupidly,I decided to neutralize whole acid/NG mix with baking soda...
It buns with nice bluish flame only when strongly heated with open flame,that leads me to the conclusion that it was only partially nitrated
or that acid leftover decomposed it during the night.
At least in theory,toluene wuld "crap out" ionic product(salts,acid remains...) and everything that has H-bounds(glycerine,H20...),
dissolwing only pure NG.
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User
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I also thought of this a couple of years ago.
It could be a yield improving method but there are some problems with it.
first of all .. is yield that important?
Secondly how are you planning to extract the NG from from the toluene when it is dissolved ?
And if it increases the purity by great extend it would have been used in the industry.
No i don't really think it practical but still I like the idea.
What a fine day for chemistry this is.
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