NG Synthese

So you want to make nitroglycerine, AGAIN, ...

Okay, let's do
it !!

The stuff needed for making NG:

- 100 ml of >95% H2SO4 (sulfuric acid)
- 70
ml of 65% HNO3 (nitric acid)
- 22 ml of 100%
C3H5(OH)3 (glycerol)
- At least 0.5 kg of
ice for cooling and optional some NH4NO3

From left to right: the 100 ml
H2SO4, the 70 ml HNO3 and the 22 ml
C3H5(OH)3

Sharp observers; I put a bit
more then 23 ml glycerol in the measuring cylinder, because with
a viscous
fluid like this one, alot of product will stick to the sides ...

============RANT============

I can not stress this enough:

Because this synthese involves a pretty sensitive high explosive, you must
NEVER let temperature rise over 20°C !!!!
When temperature gets over a
certain point (rough guess, about 40°C) a runaway reaction will occur, which
itself generates
a lot of heat, and thus is self-sustaining. If, due to some
crazy, totally "out there" reason, runaway does occur,
try to stay as calm
as possible. Pour the entire red fuming and bubbling mix in at least the double
volume of cold water.
The reaction will stop, and you can go extract your
NG, no harm done (if you don't suffer a heart-attack)

BTW: If you do
happen to suffer a hearth attack (wuss) you might want to use the stuff you just
made,
Dip your finger in the NG and put it in your mounth, it will taste
very sweet, and you'll get a head-ache
within a minute, that's because the
nitroglycerine widens your blood vessels in your brain, but I guess it beats
dying.
You don't want more then 0.25 ml in your body, because then you'll
prolly go pretty sick ...

===========END OF RANT==========

Now let's get busy :)

First, pour the
H2SO4 in the beaker in the ice bath, then, slowly add the
HNO3, keeping an eye on the temperature.

Here, the HNO3 is being added to the H2SO4.
Now look what happens next:

With
my pre-chilled acids (straight from the freezer) the temperature shot up from
the sub-zero realm (-5°C for sure,
look at the ice condensing on the bottles
in the first pic) to a nice hot 40-50°C, while evolving HNO3 vapours.

So I suggest doing this step slowly!! Especially when this synth is
performed indoors ...

(HINT from Vulture : adding the
H2SO4 to the HNO3 while stirring will be better
for temperature control)

Meanwhile, I fled the scene getting this from
my lab:

77%
NH4NO3 prills (the other 23 % is a carbonate coating).

They help to keep the temperature down as they dissolve, so I added about
300 grammes of these to my icebath:

Now wait untill the temperature has dropped to around 10°C, and then
slowly start adding glycerine.

After each individual addition, you must stir the mix, so the glycerine
can't form a layer above the acids.

If the temperature gets around 15°C, immediatly stop the addition, and
keep stirring to distribute the heat evenly.

When it has cooled down again, you can resume adding the glycerine in
small portions at a time.

Constantly keep one eye on the mercury, and don't stop stirring.

With this "leet" cooling bath I was able to add the 22 ml of glycerine in
just 15 minutes :)

When all the glycerine is added, allow the reaction to complete for 15
minutes while stirring now and then.

The next step is to water the acid
down, wich will produce quite some heat too.
(allways add acid to water, not
the other way around)
Use the double volume in cold water for this and
you'll be fine, just pour it all in at once.

Now pour off the spent acids, add more fresh water and pour this off
again. Now add a bit more fresh water.

You'll notice some white blobs on the bottom of the reaction vessel.
This is your NG !!
Now measure the pH. I used pH paper with a 1-14 range:

As you can see in the pic below, it still very acidic; pH 1 or less ...

To get "rid" of an acid, you need to add a base, I used Ammonia:

As long as the pH is below 7, add more ammonia (while stirring good)
untill it is a little bit basic.

When using a high concentration of a
strong base, add very small portions between measurements, because too basic is
just as bad as too acidic !

My pH was between 7 and 8, it doesn't show up well on the picture, but
the pH paper is a bit greenish. Good enough :)

Now
suck the NG out of the slightly basic solution, wash with a bit distilled water
to remove
remaining minerals, and transfer it to a measuring cylinder to
check out your yield.

I can't say I'm very thrilled, because from my 22 ml of glycerine, I got
19 ml of NG.
I blame bad yield on the water in the reaction ...

Now
it's time to get the water out of your glycerinetrinitrate. We learned from past
experience that
the saturated NaCl solution is not a good way to go, so just
place it in a shallow container in an improvised dessicator.

Dessicating agent presented here is CaCl2, but
there are lots of other options.
How long it takes untill all the water to
evaporate out of your NG, depends on many factors; surface area of your NG,
temperature, dessicant, ...

You can tell if all the water is out,
because the NG is nice and clear.

2 days later:

It's a bit hard to see, but that is 18.5 ml NG. I'm happy with it, but
still not thrilled ...

I need higer % HNO3 ...

========================From previous
experiments========================

The reaction when it detonates:

4C3H5(NO3)3 (l) -->
12CO2 (g) + 10H2O (g) + 6N2 (g) + O2
(g)

You notice for every 4 molecules of NG that detonate, you get 1
molecule of O2 left over ...
So you may want to add some fuel ...
I guess any fuel will do, as long as it's not acidic.

For example Al
powder, graphite, other explosives with a negative oxygen balance, ...

Testing season is open:

This 20 ml (30 gram) NG was combined with 1.5 gram NC in acetone
solution and 1.5 gram 400 mesh flake Al powder (airfloat, and a mess to work
with) to give ...

This flashy looking slurry :

While the
acetone is evaporating out of it, some ideas on power comparing that are easy to
realise with limited funding ?? => [email-masked]

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