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                          Home Workshop Explosives
                              by Uncle Fester
                   Published by Loompanics Unlimited 1990
              Digital transformation by Swedish Infomania 1996

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PREFACE

   To many people, it seems only natural that their Big Brother deems them
unfit or untrustworthy to possess whole classes of substances.  After all,
they are only lowly serfs, and are not intelligent enough or stable enough
to handle explosives or the modem scourge of "killer dope." If this is the
way you think, don't bother to continue reading this book, as it will only
upset you.
   If this stunted mode of thinking is as repugnant to you as it is to me,
the next question to be dealt with is: How, in an unfree, heavily
surveilled country, where the citizens are trained from infancy to be
informers for the state, does one obtain explosiva materials without being
arrested or killed?
   For the vast majority of us who do not have access to the "legitimate"
explosives supply pipeline, there are only two possible routes to take to
obtain explosives.  The first and most obvious possibility is to steal the
explosiva from some outfit that has a large, unguarded legitimately
obtained supply, most likely a quarry.  This is not such a good method for
reasons I will outline.
   First of all, a theft of explosives never fails to catch the attention
of the authorities in a particular area.  There is just something about
explosives that makes such people nervous, especially if there is a chance
they have fallen into the "wrong hands." The intense scrutiny that is
likely to follow such a theft is almost certainly unwelcome, and is bound
to take away most of the pleasure and fun of owning explosives.
   Secondly, the performance of heisted explosives is most probably going
to be disappointing.  This is because the most easily stolen dynamites,
those ripped off from quarries, are in all probability going to be
low-powered rubbish.  This kind of trash works fine for blasting loose
rock, but is next to useless for demolition purposes.
   Finally, ever since the days of the Weathermen bombing campaign of the
early '70's, all dynamites manufactured in the US have been laced with
unique mixtures of trace elements to identify the manufacturer and batch
number of the dynamite, even after it has been exploded. (This is done by
scraping up some of the residue and analyzing it.) As you can imagine, this
identification system makes it much casier to prove whose stick of dynamite
did what, or from whence a particular stick of dynamite came.
   For the above reasons, a second alternativa will be covered in detail in
this book.  That alternativa is the home manufacture of explosiva mixtures
suitable for demolition.
   The emphasis in this book will be to cover the techniques and equipment
suitable for home manufacture of a limited number of very powerful
explosives using as starting materials easily obtained chemicals.  Here,
the long suit is going to be detail of presentation, making the reader
aware of the little things that can go wrong in production of explosives
and how to avoid these little pitfalls.  It is my opinion that this course
of action is much preferable to the presentation given in other so called
"explosives" books, where the authors attempt to cover up their own lack of
detailed knowledge of the field by going through superficial litanies of a
plethora of formulas for making various explosives.  I find such a
treatment of the topic insulting.
   The material in this book is largely the result of numerous experiments
I did in the field in my dorm room back when I was in college.  I know from
experience that these procedures will work for anybody so long as
reasonable care is taken.  You can believe it because I've been there, and
wouldn't tell you so if it were not true.

                        Have fun!
                                        Uncle Fester

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                      THINGS THAT GO BOOM IN THE NIGHT
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  The first step towards gaining an understanding of explosives is to
understand how they work.  From this piece of knowledge, an appreciation
for inany of the finer points of explosive technology will naturally flow.

  An explosive is a substance or a mixture (usually a solid or a jelly in
form) that is unstable.  This unstable substance undergoes a very rapid
chemical reaction after being set off in the proper manner.  The result is
that the originally rather small amount of explosiva is almost instantly
converted into a very large amount of hot gases.  These hot gases are at
first trapped into the amount of space that the explosiva charge originally
occupied, but they expand very rapidly and violently.  The result is the
familiar sight of an explosiva fireball and its accompanying shock wave.

  As we all know, not all explosives are created equal.  Some explode so
flercely that they destroy everything within range, while others are useful
for fireworks, but not much more.  Why the wide variance in power?  The
answer to that lies in the three main factors contributing to an explosives
performance.

   The first and generally the most important factor in determining the
performance of an explosiva is its detonation rate.  To understand what is
meant by the term detonation rate, see the drawing below.

   The drawing shows a charge of explosiva in which a blasting cap has just
gone off, triggering a detonation.  Pay close attention to the detonation
wave spreading outward in all directions from its source at the blasting
cap.  On the outward side of this front, the explosiva is unchanged, but on
the inward side, it has been detonated and converted to hot gases.  The
rate that this detonation wave travels through the explosiva is called the
detonation rate.  This number is usually expressed in the form of meters
travelled per second (m/s).  It is not bard to imagine why a more powerful
explosiva will have the higher detonation rate. The more instantly the mass
of explosiva is converted into hot gases, the less chance these gases will
have to fritter away without doing any damage.  Typical detonation rates
range from over 8000 m/s for cyclonite (RDX) down to a couple thousand for
black powder.

   Just as different explosives have different detonation rates, the same
explosiva under varying conditions will have a range of detonation rates.
For a solid explosiva such as RDX or PETN, this rate depends largely upon
how dense the mass of explosiva is. For example, if the charge consists of
finely crystalline material, its detonation rate will be quite a bit less
than if it has been melted together into one solid rock.  This is because
the finely powdered material is less dense than the rock form.  Those
readers familiar with cocaine will grasp this immediately because cocaine,
like these solid explosives, fluffs up quite a bit in the process of being
powdered up from rock form.

   A liquid explosiva like nitro is always going to have the same density,
so it does not exhibit this effect.  This, however, does not mean that the
liquid explosiva will always have the same detonation rate.  When the pure
liquid explosiva is mixed with binders to make a safer explosiva, its
detonation rate goes down quite a bit.  In the case of nitro, when it is
mixed with binders to make dynamite, its detonation rate can be cut in hall
The solid explosives like PETN or RDX also show this effect when they are
mixed with binders to make plastique.  The general rule is that the pure
substance will be a good deal more powerful (although less safe and
convenient to handle) than the resulting plastique or dynamite.

   The second factor determining the performance of an explosive is how
much hot gas a given amount of explosiva will be converted to when it
detonates.  This factor is just as important as the detonation rate in
determining how violent the resulting explosion will be.  Unlike the
detonation rate, this factor is not influenced by the density of the
explosiva or what binders it may be mixed with.  One gram of black powder
will only produce 270 c.c. of gas (volume of gas adjusted back to room
temperature and normal pressure by use of the ideal gas law) while the same
amount of RDX will make over 1000 c.c. of gas. Since it is this conversion
of the explosiva to gases that makes the blast, the extreme importance of
this factor is easy to understand.

   The final main factor determining how powerful an explosiva is, is how
much heat is produced in the blast (i.e., how hot the resulting gases are).
This is because gases expand when they are heated, so the same amount of
gas when reduced to standard pressure and room temperature can be a good
deal greater when hot.  Black powder produces about 700 calories of heat
per gram, while nitro and PETN make in the neighborhood of 1500 calories
per gram.

   If one takes these three factors together, you can get a good measure of
the relative power of the explosives.  A convenient way to do this is just
to multiply the three factors together to get a number with which to
compare the various explosives.  A list of explosives compiled in this
manner according to power would have RDX, PETN, nitro and a few of its
close cousins crowded at the top, and then a middle group of which TNT is a
typical example, and then a lower group including black powder and mercury
fulminate.

   Most members of this lower group do not detonate like the high
explosives do.  They explode in a different manner called deflagration.
Deflagration can be most closely compared to a rapid burning.  The outer
surfaces of the individual particles catch fire and burn their way into the
centers of the particles. With these explosives, maximum power is obtained
by very finely granulating the material.  This is in contrast to the high
explosives where the greatest power is obtained when the pure material, if
it is a solid, is in the form of a large solid rock.  These lower
explosives find most of their use in blasting caps to provide the initial
shock that sets off the high explosive, and as propellants or primers for
bullets.

   As you probably already know, the high explosives require a fairly
violent blow to set them off.  The forcefulness of the shock needed to
cause detonation varies from explosive to explosive. TNT is very hard to
set off, while on the other extreme, nitro and PETN are pretty easy to
bring to detonation. To meet these varying needs, a range of blasting caps
with increasing power, labelled numbers 1 through 8 are available. With
almost all the explosives detailed in this book, I will note which number
blasting cap is required to set it off. A larger blasting cap than needed
to set the material off is generally not recommended, but may sometimes be
advantageous by causing a condition called "overdriving" in which a more
powerful blast is obtained.
    
    Some of the high explosives covered in this work can also be set off by
exposure to heat or a strong eIectric shock. Where this is applicable, it
will be noted, along with some suggestions for taking advantage of this
property.
    
    Finally, I must warn the reader that only the most powerful of 
explosives are covered in this book. A small amount of them could easily
make the careless experimenter a memory. These materials become most
dangerous when the handler ceases to be afraid of them! For this reason
they are not recommended as an adjunct to drunken revelry or other
tomfoolery. Be warned!
    
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                             THE NITRIC ESTERS
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    Since all of the compounds dealt with in this book, with the exception
of RDX (cyclonite) belong to a class of chemicals called nitric esters,
this discussion will begin by explaining exactly what are nitric esters,
how they are made, what precautions can be followed by the home
experimenter to get maximum yields of product, and some of the pitfalls
likely to ensnare the unwary experimenter during the stages of production,
purification and use of this most powerful class of explosives.
    
    The layman who goes to the library and brings home an armful of good
explosive books is sure to see the term "nitric ester" used repeatedly,
with the predictable response of "Huh?" being the result. Since this class
of explosives is so important, and forms the heart of Home Workshop
Explosives, this term must be explained. An ester is a member of a family
of related chemicals, all of whom can be made by reacting together an
alcohol and an acid (or its derivatives, for those organic chemistry
purists out there). The acid and the alcohol link together by splitting off
a water molecule, and form the new compound, an ester. A nitric ester is an
ester formed when the acid is nitric acid. A very large variety of nitric
esters can be made from nitric acid, just by using a variety of alcohols.
It is likely that all of them are explosive. The simplest nitric ester,
methyl nitrate, is made by reacting together methyl alcohol (wood alcohol
easily found at the local hardware store) and nitric acid. The following
shows how these two react together to form an ester. All nitric esters in
this book are formed by the same mechanism:
    
    CH3OH + HNO3 => CH3ONO2 + H2O
    
    Methyl Alcohol + Nitric Acid => Methyl Nitrate
    
    At the end of this chapter, the details of how to prepare methyl
nitrate will be covered to illustrate the points made in this chapter.
    
    Similarly, ethyl nitrate is made from ethyl alcohol (grain alcohol, the
drinking variety) and nitric acid. The infamous nitroglycerin is the
product of nitric acid and glycerin (glycerol). This same analogy can be
carried throughout the entire class of chemicals called the nitric esters.
    
    For the person interested in producing these chemicals, a main area of
concern is naturally going to be how to get the maximum yield product from
each batch. For the industrial-scale manufacturer, the emphasis may shift
to how to get the cheapest product in the least amount of time. To answer
these questions, the process of forming the nitric esters must be looked at
more closely.
    
    The process of forming a nitric ester belongs to a class of reactions
called equilibrium reactions. What is meant by this is that all of the
starting materials do not automatically and rapidly get converted into
products. A good percentage of the starting materials (in the case of
nitro, glycerin and nitric acid) are likely to iust lav around in the
mixture and refuse to react together.
    
    This frustrating course of events can be avoided for the most part by a
knowledge of what's going on, and using strategy to shape events to our
liking.
    
    Just how much of the starting materials are going to be turned
    into products can be figured out using a little algebra and what
    is called the equilibrium equation. Let's take the case of nitro
    production since nitro is such an effective explosive, and making
    it is required for the creation of gelatin dynamite. This is the
    reaction that forms nitro:
    
    1 Glycerin + 3 Nitric Acid => 1 Nitroglycerin + 3 Water
    
    Here we see that one molecule of glycerin and three molecules of nitric
acid are required to make one molecule of nitroglycerin and three molecules
of water. The equilibrium formula for this reaction looks like this:
    
                   (nitro)*(water)^3
   Constant =  --------------------------
               (glycerin)*(nitric acid)^3
    
    Here the constant is in the neighborhood of 50, but depends upon the
temperature that the reaction is being done at. What this equation means is
that the reaction goes forward making nitro until the concentration of
nitro in the mixture times the concentration of water to the third power,
divided by the concentration of nitric acid times the concentration of
glycerin to the third power reaches the value of the constant.
    
    Now for the point of all this. In order for good yields of product to
be obtained, it is crucial that there be as little water as possible in the
mixture, and that the concentration of nitric acid be as high as possible.
With a little bit of high school level algebra, you can easily prove to
yourself that a little bit of water in the mix, since its concentration is
raised to the third power, will wreak havoc on the amount of nitro allowed
to be produced before the constant number is reached.
    
    There are several methods for keeping the amount of water in the mix to
a minimum. First of all, glycerin used in the reaction should not have any
water in it. This can present a problem because the best source of glycerin
is the local pharmacy, and the bottle it comes in is not likely to say how
much water it contains. I have found a wide variety of quality in drug
store glycerin. Some, like the Gull Pharmacy brand which was my favorite,
was virtually pure glycerin with no added water. Other rubbish brands which
will not be named here had unacceptably high amounts of water in them. How
to deal with this will be covered in more detail in the nitro section, but
let me say right here that the more runny the glycerin is, the more water
it contains.
    
    Another very common method to keep the amount of water in the mix to a
minimum is to add a substance which will soak up water in the reaction
mixture. The most favored chemical for this purpose is concentrated
sulfuric acid. This material has a great thirst for water, and performs its
task admirably. It is usually added to a batch of nitro to the extent of
one part nitric acid, two parts sulfuric acid. Fuming sulfuric acid works
even better, but is expensive. This topic will be covered in more detail in
the sulfuric acid section.
    
    Other chemicals have been used to soak up water in these batches, but
they are not so favored as concentrated sulfuric acid, because they cost
too much. An example of such a substance is phosphorus pentoxide (P2O5)
which reacts with water to make phosphoric acid (H3PO4).
    
    The last easy method to control the amount of water in the reaction
brew is to use as concentrated a sample of nitric acid as possible. This is
because in nitric acid, whatever isn't pure nitric acid is water. For
example, the usual concentrated nitric acid is 70% nitric acid and 30%
water. Nitric acid called fuming nitric acid is 90% nitric acid and 10%
water. The drawback to using the more concentrated forms of nitric acid is
their cost, and their ease of availability. These last two factors are
often enough to rule out their use. More on nitric acid in the nitric acid
section.
    
    The temperature at which the reaction is done is the next vitally
important area of concern for the explosives manufacturer. There is great
danger of not only losing the batch if the temperature of the batch is
allowed to climb too high, but also of a disastrous explosion being the
result.
    
    At first glance, it may seem simple to keep the temperature of the
reacting mix within the proper range. This impression can be of great
danger to the novice experimenter. This is because the reaction producing
the product makes a good deal of heat as it is progressing. If this heat
does not have a chance to escape, regrettable consequences will ensue.
There are some very simple tactics to follow to conquer this difficulty.
    
    The first step in keeping reaction temperatures under control is to
keep the acids used in the reaction in a freezer before use. This will cool
them down well below the temperature required for any explosives
production, and will make for quicker production because it will not be
necessary to sit around and wait for the acids to cool down in an icebath,
because they will already be cold when they go into the icebath. Some heat
will be made by mixing the acids prior to use, especially if fuming
sulfuric acid is used, but the experimenter will still be miles ahead by
keeping his acids in a freezer. He will get the added benefit of helping
his nitric acid to keep better than it would sitting around. Cooling
glycerin and ethylene glycol down in a freezer before use is also good if
nitro or ethylene glycol dinitrate is to be made.
    
    Another important technique used to keep the temperature of the
reaction cool enough is to add the alcohol to the acids slowly in order for
the heat produced in the reaction to be given off gradually. For example,
in the production of nitro, the glycerin is added slowly to the acid,
taking a break between each addition of the glycerin. In this way the heat
produced can be given off to the ice bath surrounding the flask with no
problem. Exactly how fast the alcohol can be added depends on how large the
batch is. I recommend mentally dividing the alcohol up into ten parts and
adding one tenth at a time.
    
    Good stirring is a crucial part of the temperature control strategy.
This is because if there is not stirring while the ingredients are being
added, local areas where the temperature is too hot will develop in the
mix. With stirring, the heat made in the center of the mix will be able to
find its way to the walls of the flask, and from there to the ice
surrounding it. Good stirring has the added benefit of bringing all the
ingredients into contact so they can react. This is crucial to getting good
results.
    
    Choosing a good vessel to make the explosive in is another aspect to
the temperature control problem. The walls of the vessel should not be so
thick that they act as an insulator to the flow of heat from the batch into
the surrounding ice bath. For this reason, many heavy glass measuring cups
are not suitable for use as reaction vessels. This insulation problem
becomes more intense the larger the batch of explosive that is being
cooked, because of the greater amount of heat given off.
    
    On the other hand, measuring cups have a lip on their rims for pouring
that comes in very handy in the production of explosives because the usual
procedure for making nitric esters calls for the batch to be poured into
water or through a filter when the reaction time is up. This little spout
on the rim makes this part of the operation much safer and less messy than
using a mason jar, for example.
    
    An ideal reaction vessel, therefore, would be made of reasonably thin
glass (about as thick as the usual drinking glass) and have a lip on the
rim for good pouring. When making a batch, it should be no more than half
full. This is so that good stirring can be done on the contents, and so
that the top of the batch can be below the level of the surrounding ice
bath. Glasses of this type can be found at fancy bars or in some stores.
    
    Choosing a good thermometer to monitor the temperature of the batches
is an area which cannot be ignored. A laboratory type thermometer, of
course, will work just fne, but many kitchen thermometers will not. Any
portion of the thermometer which comes into contact with the batch must be
completely covered with glass. Metal probes will not do because of the
strong acids used in the production of the nitric esters.
    
    In a pinch, the typical, cheap, outdoors type thermometer can be used.
Here's how: This cheap type of thermometer is just a glass tube f~lled with
mercury attached to a metal backing that has the temperatures printed on
it. Generally, one side has øF and the other side has øC. One just takes
such a thermometer, and with a three sided Sle, nicks the glass thermometer
body at the maximum-temperature allowed for the reaction it is going to be
used in. The glass thermometer body is then removed from its metal backing.
It can be used as a stirrer, so long as care is taken not to bang it around
the inside of the glass reaction vessel when a batch is being made. As long
as the mercury stays below the level of the nick, one knows that the
maximum temperature is not being exceeded.
    
    One last major area of potential trouble for the production of the
nitric esters must be warned about This is nitric acid that has gone bad,
and developed a reddish tint. This is bad news because it means that the
nitric acid has broken down into nitric oxide (NO2) fumes. This acid will
not work well for the production of explosives, and may very well cause a
disaster. In the production of nitro, for example, it makes the reaction
very difficult to control. Bubbling geysers of nitric fumes and detonation
can result. How to prevent this and how to treat the problem in progress
will be covered in the nitric acid section and the nitro chapter.
    
    Once the ingredients have been mixed and the required amount of
reaction time has passed, the most difficult and important part of
explosive production must be tackled. This is the purification of the
reaction mixture into a pure, refined product. The casual observer may be
surprised that the purification of these materials is of such importance.
However, it is an accurate assessment to say that the mixing and reacting
of the chemicals to make the nitric ester explosives is pretty easy. It is
in the purification of the product that the batch is made or broken.
    
    There are two routes to disaster for improperly purified explosives.
Route number one, often taken by improperly purified nitro and its close
relatives is the least dangerous. With nitro, at least in small quantities,
if all the acid used in its manufacture is not removed from the product,
then it begins to break down. Within a day or two, it is no longer
explosive. In all probability, it reverts back to glycerin.
    
    Route number two, taken by nitromannite and nitrocellulose, to name a
couple, is much more dangerous. In these explosives, if all the acid is not
removed from the product, the explosive becomes very sensitive and liable
to explode unprovoked. At higher temperatures, they become wildly
unpredictable.

    For these reasons, great care must be taken in the purification stage
of explosive processing. The directions given in this book will result in
pure, stable substances so long as reasonable care is taken. The point is
to make the reader aware of the great danger involved in cutting corners on
the purification of these materials.
    
    With the major aspects of explosive manufacture discussed in a fairly
general way, it is now time to move on to a specific example to illustrate
the points that have been made. The example that will be used is methyl
nitrate. This choice is not to be construed as an endorsement for methyl
nitrate. On the contrary, methyl nitrate is an inferior explosive. While it
is very powerful and made from very simple materials, it suffers from twin
liabilities that make it unsuitable for most uses. Strike number one is
that it is difficult to purify. It must be distilled to reach a good state
of purity. This is definitely not recommended. In fact, it is a good recipe
for a devastating explosion.
    
    Strike number two is that the stuff evaporates away too easily. This
will ruin any gelatin or plastique that it is incorporated into because
even in the bound up form of gelatin or plastique, the methyl nitrate will
evaporate away, leaving nothing but the binders and fillers. The only way
to stop this is to keep it in a freezer until use (thereby cutting
evaporation to almost nothing because it is too cold to evaporate) or to
seal the explosive in a container that will hold in the vapors against the
pressure they will generate at normal temperature. A good choice for such a
container is a champagne bottle with the cheap plastic stopper.
    
    Strike number three, as if any more were needed, is that this explosive
is very sensitive. In many respects, it is more sensitive than nitro,
wit.hout the many redeeming graces of nitro. The one good point about this
material is that the crude stuff before it is distilled (danger!) is very
sensitive to heat, and can be used as a heat detonated explosive.
    
                       PREPARATION OF METHYL NITRATE
    
    This is about the most complicated procedure used in making any of the
nitric esters. If you feel confused when reading this, do not be
discouraged. Many of the better explosives are made much more simply. The
only special piece of chemical glassware that would come in handy for this
preparation is a separatory funnel (unless distillation of the crude
product is attempted ð DANGER!). A good eyedropper can replace the
separatory funnel in this procedure. I'll explain how in the text.
    
    Methyl nitrate is made by reacting methyl alcohol (methanol, available
very cheaply at the local hardware store) with concentrated nitric acid
(70% nitric acid, density or specific gravity 1.42). The water absorbing
chemical in this reaction is concentrated sulfuric acid.
    
                                  H2SO4
                    CH3OH + HNO3 =======> CH3ONO2 + H2O
    
    To begin preparation of methyl nitrate, all three ingredients, methyl
alcohol, sulfuric acid, and nitric acid are cooled down in a freezer. Then
a plastic or styrofoam tub is filled half full of ice. This is the ice bath
which will be used to keep the reaction cold while it is being done. Next a
5 gallon plastic pail is filled 2/3 full of cold water, and placed next to
the tub of ice. This pail is the preliminary disposal site for the used
acids after the reaction is done, and also serves as the emergency safety
dump to toss in runaway reactions before any serious damage is done.
Finally, the ice is wetted with some water to make it work better at
cooling down the reaction vessels.
    
    Now the cold ingredients are measured out. With a glass measuring cup,
measure out 300 c.c. of nitric acid, and 300 c.c. of concentrated sulfuric
acid. (Note: I c.c. = 1 ml. It is also important that the nitric acid not
have a reddish tint to it.) The nitric acid and sulfuric acid are then
mixed together in a measuring cup. The cup filled with the mixed acids is
then placed in the ice bath to keep it cold. In a second measuring cup
nestled well within the ice bath, put 150 ml of methyl alcohol. Then to the
alcohol, add 50 ml of concentrated sulfuric acid. This must be done slowly,
with good stirring so that the temperature of the mix does not go above 10ø
C (50ø F).
    
    Next three glass reaction vessels are put into the ice bath. They
should be about one pint in size (500 ml) have a pouring spout on them and
preferably be tall and thin like a drinking glass. Into each of these glass
reaction vessels is put one third of the nitric acid-sulfuric acid mix.
    
    With all in readiness, the methyl nitrate can be made. The most
conveniently located reaction vessel is picked out, and to it is added 1/3
of the methyl alcohol-sulfuric acid mix. One third amounts to about 60 ml
because of contraction of the solution during mixing. This addition must be
done slowly with good stirring. Care should be taken not to bang the glass
stirring rod against the side of the reaction vessel during stirring. The
temperature of the mix is allowed to go up to 40ø C (104ø F) fairly
quickly, and then kept at this temperature by cooling in the ice bath. The
rate at which the temperature rises can be controlled by how fast the
ingredients are added.
    
    When the full 60 ml has been added, the stirring is continued for
another minute or two, then stopped. The product, methyl nitrate, rises to
the top of the liquid as a clear oil. If one has a separatory funnel, one
can wait for another ten minutes or so for the reaction to finish, then
pour the reaction mixture into the separatory funnel, let it sit for a
minute or two for the methyl nitrate layer to float up again, then drain
off the acids into the 5 gallon pail and pour the methyl nitrate product
into a small glass container that already has 20 ml of cold water and 5
grams of table salt in it. This salt water is the first step in the
purification of the product.
    
    I must warn here against touching methyl nitrate or tasting it, because
it will cause terrible headaches. Too much smelling of the product will
cause the same effect.
    
    If one does not have a separatory funnel, one can improvise. Once the
mixing of the ingredients is done, and the product comes to the top, it can
be sucked up in an eyedropper and squirted into the salt water. This must
be finished before the ten to 15 minute time limit is up, because after
that time great geysers of nitric oxide fumes are gushed up by the acids.
They must be dumped into the pail of water by that time. Once the water
dilutes them, the danger is past.
    
    Nitric oxide is a pretty good poison. Breathing its fumes can easily
lead to a delayed death. It burns the insides of the lungs, which then fill
up with fluids leading to death. Symptoms often do not come on for a day or
two. Whenever a batch starts to bubble up red fumes, it must be drowned in
the pail of water to avoid severe danger!
    
    With the first reaction vessel finished, one can then move on to the
second one, and then the third one. The product layers from the second and
third vessels are put in with the salt water wash that the product from the
first vessel is sitting in. This salt water wash should be swirled around
from time to time as the production is continuing to aid in getting traces
of acid dissolved in the water. Since traces of acid are the enemy here, it
is important that only the methyl nitrate layer be put into the salt water,
not the acid it is floating on. One must take some care in separating the
layers, or in sucking up the product layer with an eyedropper.
    
    The salt water wash bottle has about 175 ml (a little over 200 grams)
of methyl nitrate in it. It should be swirled around some more, then
allowed to sit for a few minutes. If one has a sep funnel, it should be
poured into it, and then the water layer (the bottom one) is drained off.
If an eyedropper is being used, the water layer should be removed with it.
    
    Now. the remaining acid in the crude product must be removed. To do
this, some lye (a volume amounting to about 5 match heads) is dissolved in
about 50 ml of water. This lye water is then mixed in with the crude methyl
nitrate and allowed to react for about 10 minutes with some more swirling.
At the end of this treatment, a drop from the water layer should still be
basic (it should turn red litmus paper blue). Litmus can be obtained at the
local drug store, or at any lab or chemical supply outlet, with no
suspicion.
    
    I cannot overemphasize the importance of removing the acid from the
crude product. Traces of acid left in it will cause it to break down and
become so unstable that it becomes too dangerous to be of any use. If one
has a sep funnel, gentle shaking can be done for a few minutes to make sure
that the methyl nitrate gets into good contact with the lye water. If one
is not at hand, the stirring with the lye water must not be a slipshod job.
Again I must emphasize that at the end of the lye water treatment, the lye
water should still be somewhat basic. If the water is acidic (turns blue
litmus red) a few more match heads worth of lye must be added, and the
treatment continued.
    
    When the lye water treatment is completed, the final purification of
the product is next. The lye water is drained off by use of a sep funnel or
eyedropper, and then 30 ml of ice cold salt water (5 grams of salt) is
mixed in with the methyl nitrate. After a few minutes of gentle shaking in
the sep funnel, or good stirring, the mix is allowed to sit. The salt water
will contain most of the unused lye that happened to find its way into the
methyl nitrate. The salt water layer is separated, and thrown away.
    
    Finally 30 ml of ice cold water is added to the methyl nitrate, and
once again, stirring or shaking is done. The methyl nitrate is now
practically pure, except for some water dissolved in it. The water layer is
separated off of the methyl nitrate, and the product is ready for immediate
use. The small amount of water dissolved in it will cause no real problems
so long as the product is used soon after making it. A more stable product
results if it is distilled, but the great danger in doing this can't be
underestimated, especially for the unskilled. The product distills at 65ø
C. Heating must be gradual, and an oil bath must be used to heat the flask.
The temperature of the oil bath must not get much above 65ø C, or the
contents of the distilling flask will superheat, leading to an explosion.
    
    With the product at hand, storage can be done by pouring it into a
tightly stoppered bottle and placing it in a freezer. This material should
not be stored for more than a few days before use. Methyl nitrate is a
use-it-as-you-make-it explosive. The great friction sensitivity of this
substance means screw type bottles can't be used. All stoppers should be
well greased with vaseline to reduce the danger from this source of
friction.
    
    Methyl nitrate becomes increasingly sensitive as its temperature is
raised. It also does not age well. These facts are especially important for
a product which has not been purified by distillation. One can take
advantage of these facts by using methyl nitrate as a heat and vibration
detonated explosive. For example, a half pint bottle (like a used liquor
bottle) loosely attached with heat resistant tape to the exhaust manifold
of an automobile is very likely to destroy the offending vehicle after a
short warm up period. Similarly, a bottle which finds its way into an
incinerator is very likely to destroy the incinerator.
    
    More certain detonation can be obtained by leading a section of
nichrome wire (toaster heating element) into the liquid. When current flows
through the wire, the red hot heat of it will cause detonation. The variety
of diabolical booby traps which can be constructed.around this principle is
limited only by the imagination.
    
    A more convenient and safer form of methyl nitrate is gelatin. Gelatin
is very easy to make from methyl nikate, and is almost as powerful as the
pure explosive. To make gelatin, a little bit of guncotton (ak.a
nitrocellulose or smokeless powder) is mixed in with the methyl nitrate. A
stiff jelly quickly forms which can be used as a plastic explosive. The
resulting jelly is even more powerful than C-4. The keeping properties of
this gelatin, however, are no better than the pure methyl nitrate. It must
be used soon after production.
    
    Since the production of gelatins by mixing a liquid explosive with
guncotton will be seen repeatedly in this book, something must be said
about guncotton. There are a wide variety of sources one can go to, to get
guncotton. For example, cans of guncotton can be obtained at sporting goods
stores. This material is stocked because some people "reload" their own
ammunition for higher performance or to save money, or just to have fun.
Large drums of guncotton (labelled nitrocellulose, with a second rating
which tells how finely divided it is) can be found at any factory which
makes varnishes. Nitrocellulose is a key ingredient of varnish. This
material works great, but it comes packaged in the drum soaking wet with
isopropyl (rubbing) alcohol because it is safer in this state. The alcohol
must be allowed to evaporate off before it can be used to make gelatin.
Guncotton can also be obtained by taking apart bullets or shotgun shells.
In this source, however, as with the "reloading" supply route, one must
avoid buying what is called "double based" guncotton. Double based
guncotton has a few percent nitroglycerin added to it to give it an added
punch. This material should be avoided unless one is prepared to do the
necessary calculations to compensate for the nitro already in the product.
12 gauge shotgun shells almost always have a double based propellant.
    
    To make the gelatin, one first measures out how much methyl nitrate is
going to be jelled. This can be done by weighing it on a scale, or
measuring its volume in ml and multiplying by 1.2. The result will be its
weight in grams. The methyl nitrate is then poured into a plastic dish.
Then a quantity of guncotton amounting to one tenth the weight of methyl
nitrate is weighed out. For example, with 250 grams of methyl nitrate, one
weighs out 25 grams of guncotton. The guncotton is then added slowly to the
methyl nitrate with gentle stirring with a glass or wooden rod until a
uniform mixture results. Alternative mixing bowl-mixer combinations would
be; stainless steel bowl with plastic or rubber stirrer, or glass bowl with
wooden stirrer. Avoid the plastic bowl-rubber stirrer combination as this
could generate static electricity, and a tiny spark could set the guncotton
off.
    
    The resulting fairly stiff jelly has 9% guncotton, and will be set off
with a number 4 blasting cap when it is fresh. The use of a little bit less
guncotton produces a much more sensitive jell which can be set off with the
weakest of all caps, a number 1. A good firecracker will set off the pure
methyl nitrate.
    
    This gelatin has a severe drawback that the other gelatins do not have.
The methyl nitrate will evaporate out of it on storage. This can be slowed
up by keeping it in a freezer until use. Storage must be very short-term
because of the bad keeping qualities of the methyl nitrate. It should be
noted that frozen gelatin is more sensitive than gelatin at normal
temperatures. Avoid screw type lids. I recommend a zip lock baggie.
    
    Before moving on to the good explosives, some discussion is called for
here on an alternative process for making methyl nitrate, and on the
general topic of distilling methyl nitrate. As you saw repeatedly pointed
out in the above text, one of the big drawbacks of methyl nitrate is that
it does not store well unless it has been distilled. An alternative process
for making methyl nitrate centers around distilling the product directly
out of the reaction mixture (i.e. the methyl alcohol-nitric acid-sulfuric
acid mix), thereby avoiding a lot of the washing hassles that are the main
sticking point of the production method given here.
    
    This method has obvious advantages for industrial-scale production
because it is faster and simpler. For this reason, it was adopted by the
Nazis in the closing days of WW II to make methyl nitrate. Before rushing
off and following their lead, keep in mind that life was cheap in Nazi
Germany, especially the lives of industrial slave laborers. Even in skilled
hands, the distillation of this material is not to be taken lightly.
    
    The foremost precaution which must be taken in distilling methyl
nitrate is to have all traces of nitrous acid removed from the mixture.
This is done by adding urea to it. The fertilizer grade of urea will do for
this purpose, but before rushing off and tossing any nitrogen fertilizer
into the brew, make sure that the nitrogen fertilizer is made of urea, and
not the much more common ammonium nitrate.
    
    The second precaution is to prevent overheating of the mixture while
distilling it. There are a couple of angles to approach this problem from.
Step number one is to heat the distilling flask using an oil or hot water
bath. Direct exposure to the source of heat is a no-no because that will
cause local overheating and result in an explosion. The temperature of the
bath should be just a few degrees higher than the boiling point of the
product. At normal atmospheric pressure, the boiling point is 65ø C.
    
    A more effective method for keeping the temperatures safe during a
distillation is to distill under a vacuum. There is a problem with this
approach because the normal boiling point of methyl nitrate is not very
high to begin with. If it is lowered very much by applying a strong vacuum,
a condenser, or even a collecting flask packed in ice will not suffice to
turn it back into a liquid. With the strong vacuum that an aspirator or
laboratory vacuum pump produces, dry ice would be required to condense the
product. For those not intimately familiar with vacuum distillation, I must
explain that the boiling point of a substance rapidly falls off as the
vacuum becomes stronger.
    
    The vacuum distillation problem can be solved if the source of vacuum
is not very strong. One wants to reduce the pressure inside the flask to
about half normal pressure (a vacuum of 15 inches of Mercury). This will
lower the boiling point of the substance 15 or 20ø C, making it about as
hard to condense as ether.
    
    A good source of such a weak vacuum is a water bed drainage pump. This
T-shaped plastic vacuum source produces just the right vacuum for the job
when cold water is flowing through it. Alternatively, cheap workshop pumps
will do, although one must be wary of the fumes of methyl nitrate they will
exhaust into the air. The water bed pump is far superior for the job.
    
    The condenser must also be effcient. My recommendation is a Graham
condenser which has ice water siphoned through it as a coolant.
    
    The Graham condenser has a spiralled central tube for maximum
efficiency. Again, I must warn that this method is dangerous and should
only be attempted by skilled professionals.
    
--------------------------------------------------------------------------
                         NITRIC AND SULFURIC ACIDS
--------------------------------------------------------------------------
    
    Before moving on into the manufacture of some of the really good
explosives, it would be best to make the reader familiar with the two
ingredients which will be used over and over in the processes described
here. They are nitric and sulfuric acid. A familiarity with these two
substances will take much of the mystery out of explosive manufacture.
    
                                NITRIC ACID
    
    Nitric acid is the key, indispensable ingredient in the manufacture of
the explosives found in this book. The sulfuric acid can often be made do
without, if one is willing to use a greater amount of the most concentrated
nitric acid, and accept a lower yield of product in the process. Not so
with the nitric acid. Only nitric acid in the specified or higher strengths
will give that desired product.
    
    With the premium thereby placed on nitric acid, it is a fortuitous
circumstance that nitric acid is such an important industrial material with
a wide variety of uses ranging from the exotic to the mundane. It can be
found in the pint to quart range in any chemical laboratory (most
abundantly in those labs doing metal analysis) and in the 55 gallon drum
volume in plants involved in the manufacture of explosives(!), fertilizers,
dyes and fabrics. Jewelers and others involved in trading or handling
precious metals often have some on hand, too, because the best test for
determining whether something is made of the "noble metals" (i.e., gold or
platinum) is to apply some nitric acid to the metal and see if there is any
reaction. Only the noble metals stand up to nitric acid. A further test
mixture such as a jeweler is likely to need is aqua regia. This is a
mixture of nitric and hydrochloric acid (mixed on the spot, not purchased
mixed) and is the only liquid which dissolves gold or platinum.

    
    Nitric acid can be obtained in reasonably large amounts, by anyone who
does not look like a refugee from the local insane asylum or drunk tank, at
drug stores or chemical supply outlets. In most cases, a drug store will
have to send out for it, and small chemical suppliers may have to also.
Fuming nitric acid is less likely to be on the shelves than the standard
concentrated nitric acid.
    
    Mail order outfits are another useful source for nitric acid, and for
that matter, sulfuric acid. These two acids, along with hydrochloric acid,
are so widely used that no serious suspicion can be put upon the buyers of
just these materials. There was a scandal a few years back concerning mail
order chemical outfits being set up by the DEA to entrap wanna-be drug
chemists, but to the best of my knowledge, their games did not extend to
the explosives field. A possible exception to this is a chemical supplier I
saw advertise in Soldier of Fortune magazine a few years ago offering
"explosives manufacture chemicals." Such brazen advertising is cause for
suspicion. My judgement on the matter is that since neither nitric nor
sulfuric acid play a central role in "controlled substance" manufacture,
orders for these materials should raise no eyebrows in these dope-crazed
times.

    Nitric acid is a liquid that should be clear if it is the 70% grade,
and yellow colored if it is the 90% grade. The color in the higher strength
acid is caused by the acid breaking down to NO2. This small amount of
breakdown can be tolerated in most instances. The condition that cannot be
tolerated in either strength of acid is when the acid takes on a pink or
reddish brown color, and a cloud of reddish gas can be seen inside the
bottle of acid. In this case, it has broken down so much that it can't be
used for manufacturing explosives. This breakdown process can be largely
stopped by keeping the acid cold and in the dark. A freezer meets these
conditions nicely. Being careful to keep traces of dirt out of the acid
bottle or jug is another big step towards keeping the contents in a usable
condition.
    
    Occasionally, directions will call for what is called "white fuming 
nitric acid." This is the 90% fuming nitric acid which has been treated
with urea to remove the traces of NO2 and the yellow color that comes with
small amounts of it. Urea can also be used to clean up nitric acid that has
a darker color to it, but a point comes where this should be considered
futile. When the red cloud shows up above the surface of the acid, it
should be considered ready for flushing down the toilet. The procedure used
to knock out the NO2 contaminants calls for adding a little bit of urea to
the nitric amd, stirring it in and warming the mixture gently. If the color
persists, dry air is blown through the liquid, and if there is still color,
some more urea is added.
    
    As was hinted at before, the 90% (or higher) strength fuming nitric
acid is not so easy to casually pick up as the standard 70% concentrated
nitric acid. It is also much more expensive to get the fuming acid instead
of the 70% acid ($7 per pint vs. $35 per pint). For these reasons, it is
sometimes advantageous or necessary to make the high strength acid oneself.
    
    The procedure for making high strength nitric acid is pretty simple,
but some chemical glassware is called for to do a good job. Various
pamphleteers have included directions for making high strength nitric acid
in their books, leaving out a crucial aspect of the process. This crucial
aspect is that the nitric acid formed must be distilled under a vacuum.
Without the vacuum, a reddish colored product is made that is not very
suitable for use in making explosives.
    
    To make this good quality high strength acid, the following materials
are needed: concentrated sulfuric acid, sodium nitrate, and dry ice. Also
required is a distilling kit with ground glass joints and a vacuum adapter
so the product can be distilled under a vacuum. The best vacuum source is
an aspirator (cost: $10) because the acid fumes will not harm it, and the
water flow will flush them down the drain.
    
    The distilling kit is a substantial investment at a few hundred 
dollars, so one should not be purchased unless it is going to get enough
work to make the investment worthwhile. Laboratory supply companies will
either carry the equipment or can get it in a few days. Check the Yellow
Pages. The ground glass joints must be greased up with stop-cock grease
before assembling the glassware to keep the joints from getting frozen
together, and to make for a good vacuum seal, free from leaks. No parts may
be made of cork or rubber, because the nitric acid will destroy them, and
become polluted in the process. Only glass or teflon parts are allowed.
    
    Now to begin. Into the 2000 ml distilling flask is put 685 grams (365
ml) of concentrated sulfuric acid. Then 600 grams of sodium nitrate is
mixed in with the sulfuric acid. Simply swirling the flask as the sodium
nitrate is being added will do an acceptable job of mixing. Sodium nitrate
is pretty easily available. I always used to find it on the shelves of my
local Walgreens store, labelled saltpeter (technically this is the wrong
name because saltpeter is potassium nitrate). It sat on the shelf right
next to sublimed sulfur. Very interesting combination.
    
    There will be no obvious reaction as the two ingredients are mixed. The
glassware is assembled as shown in the diagram, and the 1000 ml receiving
flask is packed in dry ice (styrofoam tub suggested) and the dry ice is
wetted with rubbing alcohol. Now water is turned on to the aspirator. (See
a college level organic chemistry lab manual for more on aspirators, but
they work just like water bed drain pumps, only better. The threaded end is
the water inlet, the water comes out the opposite end, and the vacuum is
produced at the side arm of this T-shaped device.) The water must be cold
for good results. An automotive type vacuum hose is led from the side arm
to the vacuum nipple on the vacuum adapter, and within seconds a strong
vacuum develops inside the glassware. It should be strong enough that the
glassware can't easily be disassembled. Eye protection is required as
always when dealing with caustic chemicals.
    
    Some bubbling will begin in the 2000 ml flask as nitric acid begins to
boil out of it. Heat should be applied from the hot plate to keep the
process going. A good, but not violent rate of boiling is what the doctor
ordered. In about 20 minutes, close to 300 ml of pure nitric acid will
collect in the dry ice cooled flask. It will freeze shortly after its
arrival there. Since nitric acid contracts on freezing, this poses no
danger of breaking the glass. The heat applied to the distilling flask
should be gentle. There is no need to make everything red hot. When the
bubbling of the distilling flask slows, and the expected amount of product
appears in the receiving flask, the heat is turned off, and the vacuum hose
removed.
    
    As soon as the distilling flask cools off, it is advisable to rinse out
the distilling flask (it contains sodium hydrogen sulfate, a solid often
used as a drain opener) and fill it with a fresh load of sodium nitrate and
sulfuric acid. By repeating the vacuum and heating on this load, another
300 ml of product will come over to the 1000 ml receiving flask. Repeating
the process yet one more time will leave the receiving flask nearly full.
This is a good time to break. A quart of fuming nitric acid is enough to
produce a very useful amount of explosive. Store the product in the freezer
until use.
    
    Before leaving this topic, I should mention one more thing about the
cheap drug store grade of sodium nitrate ("saltpeter"). The product I
always found at Walgreens was nearly soaking wet. In this state; it was
useless for making gunpowder, and not so good for making nitric acid
either. Before using a wet material in this process, spread it out on a
teflon coated cookie sheet or a glass pan and bake it in the sun on a hot
dry day. Do not bake it in the oven because too much raw heat will break it
down into the red poisonous gas, NO2. A microwave oven may be OK for drying
this material. I suggest this for serious experimenters.
    
    One more tip is called for on the nitric acid production process. The
best type of vacuum adapter for use in the distilling set-up shown on page
31 is one that has a drip tip that extends past the ground glass joint.
This will ensure that the nitric acid fumes make it down into the flask and
are condensed and frozen there. Too short a drip tip can lead to the acid
getting condensed in the area of the ground glass joint, and if it freezes
there it could plug up that part of the apparatus. This will choke off the
source of vacuum to the glassware, and may even block the flow of nitric
acid into the receiving flask.
    
                               SULFURIC ACID
    
    Like nitric acid, sulfuric acid is an extremely common chemical, both
in laboratories and in industry. Its wide variety of uses makes obtaining
sulfuric acid a very easy task. For example, any shop doing electroplating
(especially plating chrome) will go through large amounts of sulfuric acid.
Plating shops also use a lot of nitric acid, especially if they are plating
aluminum objects. It is easy then to see how a plating shop can be a
one-stop shopping center for all one's acid needs.
    
    Home hobbyist electroplaters need these acids as well, so this can be a
good and believable cover story for anyone who runs into the embarrassing
situation of being asked what the materials are needed for by a nosey
druggist or other small-time chemical supplier. Mail order outfits may also
be considered safe for ordering sulfuric acid from because of the
commonness of the chemical and because it plays no central role in drug
manufacture.
    
    This is by no means a complete list of all the places that use sulfuric
acid and are likely to have it on hand. Virtually every large-scale
manufacturing process uses sulfuric acid at some point or another. A much
more important question is: Will the material at hand be good enough for
use in explosives manufacture? Here let the reader recall the great
importance of keepin~ the amount of water present in the reaction mixtures
to an absolute minimum, lest the yield of product be reduced to nearly
zero. With this in mind, it should then be obvious that battery electrolyte
sulfuric acid is not acceptable because it is half water. In theory, the
water can be cooked away, but this producŠs dangerous fumes and results in
an inferior product.
    
    Similarly, a lot of industrial sulfuric acid has a strength of around
80%, with the other 20% being water. This grade will not do, either. The
materials that are acceptable are concentrated sulfuric acid, or fuming
sulfuric acid. Fuming sulfuric acid will be clearly labelled as such and
may list what percent by weight SO3 (ak.a oleum) it contains. More on this
later. Concentrated sulfuric acid may only be recognizable as such by a
density (or specific gravity: sp. gr.) reading printed on it. Concentrated
sulfuric acid has a density of 1.85 to 1.91, whether this value is given in
pounds per pint or grams per ml.
    
    Both the fuming and concentrated acids are likely to be kept in glass
bottles, jugs or carbouys because these corrosive acids have bad effects
upon metal. Plastic containers are another possibility.
    
    As was mentioned earlier, there are two useful types or grades of
sulfuric acid. They are concentrated sulfuric acid (H2SO4) and fuming
sulfuric acid (H2SO4 SO3). To get an understanding of the difference
between the two, one should look to how sulfuric acid is made. Huge plants
produce the gas SO3 (sulfur trioxide) by burning sulfur to SO2, and then
inducing it to pick up another oxygen atom by high heat and catalysts to
form SO3. SO3 reacts with one molecule of water to form pure sulfuric acid.
So these plants just mix the SO3 they make with water and turn out pure
concentrated sulfuric acid.
    
    If they leave in a little extra SO3, (i.e., they don't add enough water
to completely turn the SO3 to sulfuric acid), fuming sulfuric acid results.
This fuming sulfuric acid is even better at soaking up water from one's
explosive batches. First it scavenges furiously for enough water to turn
its SO3 to sulfuric acid, and then when this is accomplished, the resulting
concentrated sulfuric acid picks up from there. So fuming sulfuric acid is
a dehydrated sulfuric acid that is even better at soaking up unwanted water
than concentrated sulfuric acid.
    
    Fuming sulfuric acid, like fuming nitric acid, is aptly named. The
stuff actually does fume. These fumes are very dangerous to breathe in
because they form sulfuric acid with the moisture in the lungs and throat,
producing acid burns. For the same reason, rubber gloves must be worn when
handling fuming sulfuric (or nitric acid) acid because the fumes will
likewise burn any skin they come in contact with.
    
    Whenever a fuming acid is to be used in a reaction, it is very important
that good ventilation be provided. The experimenter should be upwind from
the chemicals to ensure safety. This is most important when measuring out
the chemicals, and during the early stages of the reaction. Once the
chemicals have had a chance to react together for a while, and the acid
loses some of its strength, the danger from acid fumes decreases.
    
    There is no really good or practical method for the home experimenter
to make his own sulfuric or fuming sulfuric acid. It would be way more
bother than it is worth, and the product is more than likely going to be of
an unacceptably low grade. Sulfuric acid should either be purchased through
the previously mentioned commercial sources, or obtained from labs or
industries. Good sulfuric acid is clear as water and is almost as thick as
lightweight motor oil. Prices vary with the outlet, but one can expect to
pay in the neighborhood of $15 per gallon for concentrated sulfuric acid,
and $35 per pint for fuming sulfuric acid.
    
    Sulfuric acid keeps really well, so it needn't be treated so gently as
nitric acid. Light and heat have no real effect on it. It is advisable to
cool it down in the freezer before use to cut down on the amount of time
which would otherwise have to be spent cooling the ingredients before they
are mixed to react. The only important storage tip is for the caps to be
kept tightly closed on fuming sulfuric acid so the SO3 fumes do not escape
into the air.

--------------------------------------------------------------------------
                               NITROGLYCERIN
--------------------------------------------------------------------------
    
    If one was for some reason forced to choose a single all-purpose
explosive or if one were to wish away all the explosive substances save
one, nitroglycerin is the chemical to clutch close to one's heart. This
popularly, and for the most part unjustly, maligned explosive is so
powerful, versatile, and easy to make that it is far and away the number
one choice for a Home Workshop Explosive manufacturer.
    
    We've all seen the Hollywood hogwash a million times where the hero
thrusts himself into "mortal danger" with nitro. Small droplets of nitro
oozing from old sticks of dynamite fall to the ground and explode on
landing, like souped up firecrackers. Let me tell you right up front that
this is the purest form of bull. Some of my fondest adventures centered
around nitro, and it is nowhere near that easy to set off. There is no
reason why anyone who takes reasonable care and does not suffer from a
terminal case of the shakes cannot handle nitro safely. I have had occasion
to fall in a drunken stupor on broken sidewalks, and my vial of nitro land
on the sidewalk next to me. No explosion. I have dropped quantities of
nitro from a height of several stories and had it land in a couple inches
of snow with no detonation. It has been my experience that so long as one
works with fairly limited quantities of nitro at a time, and then processes
the product into gelatin or plastique, the dangers one faces are minimal
and manageable.
    
    The need for small batches may at first seem discouraging for those
special applications where a large amount of blasting power is required. It
should not be. This drawback can be conquered by running one's batches
serially. A large part of the nitro manufacturing process is sitting around
waiting while the various cleansing operations work. This dead time can be
profitably filled by starting another batch to feed into the clean-up
section of the operation. It has been my experience that a couple ounces of
product can be routinely run with none of the complications that can arise
from runaway reactions with larger loads. Since only about 45 minutes is
needed to do a batch, a healthy rate of production can be maintained. With
a competent and trustworthy helper at hand, these serial production
techniques are vastly simplified. In the production section of this
chapter, I'll provide my suggestions on how to organize this serial batch
production effort.
    
    Now it is time to delve more deeply into exactly how nitro production
is set up and why one should regard nitro as the explosive of choice.
    
    To answer the last question first, one only has to consider the extreme
simplicity of making and purifying nitro. It was first made in the middle
1800s. This speaks volumes when you consider the crude materials and
equipment available at the time. It has been my experience that anyone who
is not brain damaged or terminally stoned can easily master the process. So
long as attention is paid to following the directions, there is virtually
nothing that can go wrong.
    
    Nitro is a member of the nitric ester family, and is made the same way
as the rest of the family. Nitric acid is reacted with an alcohol (in this
case glycerin) to form the ester nitroglycerin.
    
    Sulfuric acid is added to the mixture to soak up water, and thereby
increase the amount of nitro produced.

                           Sulfuric
 3 Nitric Acid + Glycerin ==========> Nitro + 3 Water
                             Acid

    Both sulfuric and nitric acid have already been covered, so no more
will be said about them other than to say that both concentrated and fuming
nitric acid can be used to make nitro. Same with the sulfuric acid, both
concentrated and the fuming acids will work for making nitro. The
procedures are a little different depending on what strength acids are
being used, but that will be covered in detail in the production section of
this chapter. Let me just say up front that the best yields of product are
to be had when one of the acids used is of the fuming grade. It doesn't
matter which one of the acids is of fuming strength, so cost or ease of
availability is the overriding factor in choosing which acid to get in the
fuming strength. Results are better with the fuming grade because of the
smaller amount of water added to the reaction mixture.
    
    Glycerin is the other ingredient for nitro manufacture. As luck would
have it, it is very easy to find. Look on the shelves of any drug store,
and you will find it. They have it in little bottles for use as an
"emollient" to help dry skin. The problem with just going to the drug store
and picking out a few bottles of whatever is handy is that many brands of
glycerin are cut with water. Since glycerin is a clear liquid, it doesn't
show up just by looking at it.
    
    The first step to bypassing this potential pitfall is to pick up a few
different bottles of the competing brands, and check them for their water
content. The easiest way to do this is to see how runny the glycerin is.
Adding water to glycerin makes it runnier. The difference can be made more
obvious by cooling the bottles down in a refrigerator. Good glycerin will
get thick like honey.
    
    If no brand is clearly superior to the others, one must check to see if
all the brands are garbage, or if they are all good. To do this, the
glycerin is cooked to see how much water will boil out of it. The best way
to go about this is to pour the contents of a bottle of glycerin to be
tested into a glass measuring cup (best if it is made out of pyrex or kimax
so it will withstand the heating) and then place the glass measuring cup
into a small pan or other metal container that is filled with enough
cooking oil to reach about half way up the sides of the measuring cup. This
is placed on a stove and heated. The temperature of the glycerin is
monitored by use of any convenient sized cooking thermometer. The glycerin
should be stirred regularly to make sure that it gets heated evenly. There
is no danger in this process since glycerin is no more unstable than the
cooking oil. When the temperature of the glycerin reaches 100øC (212øF),
boiling may be noted in the glycerin. If it does boil, that means there is
water in it. Glycerin does not boil until a temperature of 290øC is
reached. The heating should be continued until a temperature of around
200øC is reached, and then the heat can be turned off and the contents
allowed to cool.
    
    To interpret the results, simply read on the measuring cup how much of
the glycerin has boiled away. Some small amount of boiling can be expected
because glycerin will soak up water from the air just by being exposed to
humid air. If, however, more than a few percent of the glycerin boils away,
there is too much water in the glycerin for best results. In making these
volume measurements, it is important that the glycerin be at about the same
temperature for both the before and after reading. This is because glycerin
expands quite a bit when it is heated, so taking one reading while the
glycerin is hot will give inaccurate results.
    
    If the glycerin has an unacceptable amount of water in it, one has a
couple of choices. The first and easiest choice is to just keep shopping
until a good grade of glycerin is found. If you do not strike paydirt by
this method, the more difficult route of distilling the glycerin must be
followed.
    
    Industrial manufacturers of nitro almost always distill their glycerin
before using it. This puts their worried little heads to rest on the water
issue. It is pretty safe and easy to do, but the distilling equipment
described in the nitric acid section is needed to do a good job. An
alternative is to follow the procedure described just above for testing the
amount of water in the glycerin. If the temperature of the glycerin is held
in the 150øC range for an hour or so, almost all the water will boil out of
it. It will pick up a yellowish color during the heating process due to the
formation of acrolein compounds, but this does not cause any harm.
Industrial distilling techniques give the same yellow color. It just means
that the nitro will be yellow colored instead of the nice clear product
that could be had with better glycerin. If this clear product is desired, a
vacuum distillation of the glycerin will give it. If the experimenter has
experience doing vacuum distillations, this is the best route to follow. I
must warn that glycerin has a tendency to bump during vacuum distillations.
Adding a healthy amount of glass wool (angel's hair) to the distilling
flask will keep this under control. Boiling chips do not do a good job with
glycerin.
    
    So with the preliminaries taken care of, it is time to move on to the
actual nitro production process. To start with, a 5 gallon plastic pail is
filled about 2/3 full of cold water and placed next to the production area.
It serves the same purpose that it did in the methyl nitrate section. If in
the unlikely event that the batch gets put of control and begins gushing
out the red fumes of poisonous NO2, the batch can be drowned in the water
and the danger averted.
    
    Then on a table next to the water pail is placed a styrofoam tub or
other suitable container about half filled with crushed ice. Into this ice,
a glass vessel is nestled. It should be about a pint in volume and have the
thin glass and pouring lip mentioned earlier when describing the ideal
reaction vessel.
    
    Into this glass vessel, put 100 ml of concentrated nitric acid and 200
ml of concentrated sulfuric acid. These acids should be cold to start with
by being stored in a freezer. They are mixed together by swirling the
container, or mixing with a glass rod or thermometer. This mixing will warm
them up a little bit, but they will quickly cool again in the ice bath.
When the temperature of the acids is under 40øF (4øC), the glycerin can be
added. To do this, about 50 ml of glycerin is measured out. It is then
added to the acid mixture 5 ml at a time. The best way to do this is to let
the glycerin portions run down the side of the glass. This ensures that the
glycerin enters the acid mixture gradually rather than in lump sums.
    
    The mixture must be stirred during the addition to keep the glycerin
from building up in one particular spot. If it should build up in one spot,
a runaway reaction would result. There are several choices for stirring
techniques. My favorite is to tilt the container at about a 45 degree angle
and then rotate the vessel in a manner similar to a cement mixer. This very
gentle technique works well. Another alternative is to swirl the vessel. It
could also be stirred by using the glass thermometer. Doing this, it is
important not to bang it around or to create friction by scraping it on the
walls of the vessel. This is an inferior technique. Nitro factories stir
their batches by blowing a stream of dry air through the mixture. I would
forget about this one too, and just stick to the cement mixer technique or
swirling.
    
    The addition of the glycerin to the acids should take about 25 minutes,
adding ten portions of glycerin of about 5 ml each. The temperature of the
reaction mixture should be w/atched during the addition of glycerin. It
should not be allowed to rise above 50øF. If it gets too close to this
temperature, the additions of glycerin should cease, and the mixing
continued with the vessel nestled in the ice bath until the temperature
drops back down to around 40øF.
    
    Under no conditions should it be contemplated to just add all the
glycerin, nitric and sulfuric acid together all at once "to save time." To
add them all together at once will result in a geyser of red fumes in a
small batch, and possibly an explosion in a large batch. Likewise, it
should not be contemplated to add the acids to the glycerin. This chapter
will cover all the good variations on nitro production.
    
    When all the glycerin has been added, a milky colored solution will
have been formed with little globules of pure nitro dispersed throughout
the mixture. After the glycerin has been added, the mix can be allowed to
warm up a little bit. It can be taken out of the ice bath, and its
temperature allowed to rise into the 50's F. Stirring should be done
occasionally during this period.
    
    About 20 to 25 minutes after the last addition of glycerin, the
reaction can be considered to be finished, and purification and processing
commenced. The first step in processing the nitro is to pour the whole
batch into a little over a quart of cold water. Most of the acid dissolves
in the water, and crude nitro settles out at the bottom of the container as
an oil. It goes to the bottom because it is heavier than water. A small
amount of nitro stays floating on the surface of the water due to surface
tension, but the amount is not that great. Some of the droplets can be sunk
by splashing around on the water surface with some type of stirring rod.
    
    The fact that the nitro sinks to the bottom presents the first obstacle
in the purification of the nitro. It is obviously going to complicate
things getting the nitro off the bottom of the container for further
purification. The best solution is to get a 2000 ml separatory funnel. A
quart or so of cold water can be put in it, and the batches poured into it
when they are done. When the nitro settles to the bottom of the sep funnel,
the stop cock can be opened, and the nitro drained out. The leftover acid
water can then be poured down the drain. It is important here that the
separation between nitro and acid water be as sharp as possible because the
whole idea of the purification process is to remove this acid from the
nitro.
    
    Another possible method of getting the nitro off the bottom of the
container is to tilt it to one side to pool the nitro, and then suck it up
with a plastic turkey baster.
    
    Whichever method is used, the separated nitro is then added to about a
cup of clean, cold water and allowed to sit there for a while. This clean
water will soak up more acid from the nitro. It is good to cause the nitro
to flow around on the bottom of its new container every once in a while, so
that it is not the same old surface exposed to the water all the time. This
water bath should take no more than about an hour.
    
    Next, the nitro must be carefully separated from the water once again,
and added to about a cup of bicarbonate of soda solution. The bicarb
solution is made by adding about 10 grams of Arm & Hammer~ to a cup of
water, and mixing until it is dissolved. The importance of this step cannot
be underestimated. The nitro, even after the water washing it has received
up to this point, still contains some acid. If the acid is not knocked out,
the nitro will not keep. The breakdown of the nitro is fairly rapid. Within
a day of being made, almost all of it will have decayed without this bicarb
treatment to neutralize the excess acid in it. With small batches, this
breakdown is a quiet process, resulting in a non- or poor explosive
mixture. What happens to larger batches is problematic.
    
    When the nitro is added to the bicarb solution, it sinks to the bottom
of the container again because it is heavier than water. It should have a
milky appearance and an oily consistency. It will usually cause the bicarb
solution to start giving off little bubbles, or even some fizzing. This is
the bicarb neutralizing the acid. Acid reacts with bicarb to make CO2 gas.
This is the reason a person belches after drinking some bicarb to treat
heartburn.
    
    The best way to handle this acid-neutralizing process is to rotate the
container so that the nitro rolls around on the bottom of the container,
exposing fresh surfaces to the bicarb solution. Swirling may also be
attempted, as may gentle stirring with a wooden swizzle stick or plastic
straw. A glass stirring rod should not be used because this could result in
grinding friction between the stirrer and the bottom of the container, with
the nitro trapped in between. This could have disastrous consequences.
    
    If one has a sep funnel, it is most convenient to do the neutralizing
process in the sep funnel. This is because, once the nitro has been treated
with the bicarb solution, it must once again be separated from the water.
So if the bicarb treatment is done right in the sep funnel, one avoids the
hassle of transferring the liquids from one container to another, or using
a turkey baster. When using a sep funnel, it is best if the funnel is
tilted at about a 45 degree angle to expose a greater surface area of the
nitro to the bicarb solution.
    
    However one chooses to do the bicarb treatment, one should spend at
least a couple hours on this step. Letting it go overnight does not hurt.
This does not mean that it must, or even should, be constantly attended,
stirred, swirled, or fussed over. An occasional agitaticn IS enough to do
the job well. More agitation and warmer water will get the job done more
quickly, but why be in a hurry when one is having such fun?
    
    At the end of the bicarb treatment, the nitro does not look any
different from when it went into the process. It still has a milky
appearance. This is caused by water trapped inside the nitro, and it should
be removed before the nitro can finally be called pure. If it is left in
the nitro, it could cause problems with detonating the nitro, or with
further processing it into gelatin or dynamite.
    
    The best way to remove the water from the nitro is to let it sit in
contact with a saturated salt solution. This sucks up water from the nitro
in the same way that drinking salt water dehydrates shipwrecked sailors.
Saturated salt solution is water that is holding dissolved in it all the
salt (regular table salt) that it can. The best way to make saturated salt
solution is start with hot water in any container, and add salt to it until
no more will dissolve in it. Good stirring or shaking is essential to
getting the maximum amount of salt to dissolve in the water.
    
    When the water cools down, the clear colored saturated salt solution
(i.e., no crystals of solid salt floating around) is poured off of the
excess salt sitting on the bottom of the container. This is put in a
suitable container and the nitro is separated from the bicarb solution by
use of a sep funnel or turkey baster as described earlier. Then the nitro
is put in contact with the salt solution. There should about two volumes of
salt solution to one volume of nitro. After they sit together in contact
for a few hours, the salt will suck the water out of the nitro, resulting
in a clear product. The product will be yellow if the glycerin was yellow
to start with due to water removal processes. The yield of nitro is about
50 ml, the same volume of nitro as glycerin used in the manufacture. This
process can be shortened if the bicarb solution is also saturated with
salt. This will dehydrate the nitro at the same time it removes the acid
from it.
    
    This yield of nitro can be improved greatly by using the higher grades
of acids. If one of the fuming acids is used, the amount of nitro obtained
from the same sized batch is approximately doubled. This is due to the
lesser amount of water in the mixture, and the higher concentration of
nitric acid. This method using the common concentrated acids was given
first because these acids are the most easily available and cheapest. We
shall now cover the small difference in processing when using the fuming
acids versus the Plain concentrated acids.
    
    Before moving on to production processes using the fuming acids, one
more point should be made. Since the amount of nitro produced corresponds
to the amount of glycerin used, a person may be led to believe that by
using more glycerin in a batch of nitro, more product could be obtained.
This is wrong. It does not work for reasons I shall explain.
    
    Below is the molecular structure of glycerin:

      H
     HC-OH
      |
     HC-OH
      |
     HC-OH
      H

    Notice that it contains three alcohol groups (the OH sections of
    the molecule). Each one of these must react with nitric acid for
    the product to be nitro.

      H
     HC-O-NO2
      |
     HC-O-NO2    Nitro
      |
     HC-O-NO2
      H
    
    If the amount of nitric acid in the reaction mixture becomes
    stretched too thin. as will happen if too much glycerin is added
    to the mix, then by-products will begin to be formed where one
    or more of the alcohol groups of the glycerin has failed to react:
    
     H              H
    HC-O-NO2       HC-OH
     |              |
    HC-OH          HC-O-NO2  mono-nitroglycerins
     |              |
    HC-OH          HC-OH
     H              H

     H              H
    HC-OH          HC-O-NO2
     |              |
    HC-O-NO2       HC-OH     di-nitroglycerins
     |              |
    HC-O-NO2       HC-O-NO2
     H              H

    So the use of more glycerin is self-defeating. These mono and
diglycerins are explosive compounds, but are not so good as nitro itselœ
Some of these compounds will be formed in any nitro process, but the aim
should be to keep their numbers as small as possible.
    
    The natural next question is: How careful do I have to be at measuring
out the ingredients to get good results? The answer is that, one can always
use extra acids and still get good results. It's just that after a certain
point, it gets wasteful. As for the glycerin' so lone as the amount used is
within 10% of the prescribed amount, no problems will be encountered. The
familiar TV and movie image of chemistry requiring to-the-drop accuracy in
measurement is true for doing analysis, but not usually for making
chemicals.
    
    Now let's move on to the variation of nitro production using fuming
nitric acid and concentrated sulfuric acid. This process is no more
difficult than the previous process, but fuming sulfuric acid is more
expensive and more difficult to obtain. As was mentioned earlier, the yield
of nitro is double the amount of glycerin used.
    
    One starts this process with the same set-up as used in the first
method. The tub of ice sits on the table top and the pail of water sits
nearby for dumping out-of-control reactions into. The same type of reaction
vessel (thin walled glass with a pouring lip) is set into the ice bath, and
100 ml of fuming nitric acid is measured out of the bottle or jug of fuming
nitric acid that was previously cooled down in the freezer. To this is
added 50 ml of glycerin. The addition should be slow, covering a period of
about 10 or 15 minutes. It does not need to be as slow as in the first
method because without the sulfuric acid in the mix, the reaction is not so
vigorous. The cement mixer technique of stirring is recommended here again
because of its gentleness. The temperature should be watched carefully, and
kept within the range given in the first method.
    
    After all the glycerin has been added, the mixing should be continued
for a.~few minutes. Then 200 ml of concentrated sulfuric acid (ice cold,
fresh from the freezer) should be measured out. It is then added to the
reaction mixture in small portions over a 10 minute period. The cement
mixer technique of mixing should be continued during the addition of the
sulfuric acid. The temperature of the brew should be watched during the
addition to be sure it does not rise past the allowed limits.
    
    There are two reasons why the temperature of the mixture will tend to
rise during the addition of the concentrated sulfuric acid. First, there
will be some water in the reaction mixture due to the fact that water is
formed as a by-product along with the nitro. Recalling the original
formula, three molecules of water are formed along with each molecule of
nitro made. When concentrated sulfuric acid is diluted with water, a great
deal of heat is given off. One can prove this to oneself by pouring some
concentrated sulfuric acid into some water.
    
    Secondly, when the sulfuric acid soaks up the water in the reaction
mixtures, the reaction will shift into high gear again making more nitro.
This will produce a good amount of heat. The reason why it shifts into high
gear again is because when the water is removed, the equilibrium which was
established between reactants and products is upset. The only way to reach
the equilibrium point again is to form more nitro. See the equilibrium
equation back on page 11 and prove it to yourself with some simple algebra.
    
    When all the sulfuric acid has been added, the mixing should be
continued in the ice bath for a few more minutes, then the reaction vessel
can be taken out of the ice, and allowed to warm up into the 50's F. It
should be held there for about 10 minutes with mixing, then the whole batch
is poured into some water, just like in the first method. From here,
processing into pure nitro is handled exactly as in the first method. The
only difference is that 100 ml of nitro results instead of 50 ml.
    
    Lastly, we come to the final variation on nitro production. This is
when the acids used are concentrated nitric acid (i.e., 70%) and fuming
sulfuric acid. There are a couple complications to this method. First of
all, there are two common grades of fuming sulfuric acid, one contains 20%
SO3 (oleum) and the other contains 40% SO3. So separate directions will
have to be supplied for each grade of fuming sulfuric acid. Secondly,
fuming sulfuric acid reacts pretty vigorously when it comes in contact with
water, so it must be mixed up front with the nitric acid, rather than added
last as in the previous method. If it was added last, the heat it would
produce would send the reaction over the limit. These complications are
easily overcome.
    
    So to start, the same setup is used as in the previous batches. Then
into the reaction vessel nestled into the ice bath is put 100 ml of
concentrated nitric acid (70%). This is ice cold stuff fresh from the
freezer. Then to this is added slowly with good stirring 115 ml of 40% SO3
fuming sulfuric acid, or 200 ml of 20% SO3 fuming sulfuric acid. This
fuming acid will react vigorously when it hits the nitric acid because the
nitric acid is 30% water. It may even splatter, so the opening of the
vessel should point away from the experimenter. It is best if the fuming
acid is allowed to run down the walls of the reaction vessel into the
nitric acid. Stirring is called for during this operation to keep the
reaction dispersed.
    
    When all the fuming acid is added to the nitric acid, they must be
mixed thoroughly, then allowed to cool down in the ice bath until the
temperature of the mixed acids is under 40ø F. Then it is time to add the
glycerin. 50 ml of cold glycerin is measured out and added in 5 ml portions
over a 20 minute period, just as in the first method. The cement mixer
stirring technique is once again king. When all of it has been added,
mixing is continued for a few minutes, then the brew is taken out of the
ice bath and allowed to warm into the 50's F for a while as before. Then it
is poured into water, and purification to pure nitro is done exactly as in
the previous methods. Yield of product is a little over 100 ml if 40% oleum
is used, and about 100 ml if 20% oleum is used.
    
    So, as one can see, making nitro is not an especially difficult
procedure, if one has at hand the required chemicals. Equally easy is
gearing this process up for turning out substantial quantities of nitro.
    
    As was alluded to earlier, larger batches of nitro have dangers
inherent to their production that the smaller batches do not. For instance,
a runaway big batch may blow up rather than just make poisonous gases. So
the aim of the Home Workshop experimenter should be to organize his
production process to take advantage of the dead time in the purification
of the nitro to start new batches, rather than to try to push out monster
batches.
    
    The longest stretch of dead time in the production process is the acid
neutralization with Arm & Hammer bicarb. This several hour long wait would
be a tremendous bottleneck in the production process if one would just sit
around and wait for it to get done. On the other hand, if the waiting time
for the acid to get neutralized is spent starting another batch, no
bottleneck is experienced. All one would have to do is clean up and dry the
reaction vessel, run another batch, and then put it through the
purification process. In this way, one would have several batches running
at once, all at different stages of the production and punfication process.
    
    Another section of the purification method that involves a lot of just
sitting around and waiting is when the nitro is put in contact with
saturated salt solution to remove the water from it. This dead time can be
profitably used in the same manner. It is obvious that a fair number of
containers of crude nitro will be employed in such an operation. They
should all be clearly labelled so that mix ups are avoided. Organization
and logical thinking are indispensable in this situation, but using this
method of organization, production levels in excess of a pint a day of pure
nitro are easily obtainable.
    
    Production can be further increased if there are two people to man the
production line. The most fruitful way to divide labors in such a situation
is for one person to devote himself to running the synthesis reaction
between the glycerin, nitric acid and sulfuric acid, and for the other
person to man the purification operation. With this division of labors,
production can easily exceed a quart per day without resorting to larger
batch sizes.
    
    When the nitro has reached the end of the purification process after
the saturated salt treatment, a perfect place to store the nitro is in the
freezer. The colder the nitro is, the more stable it is. Cold nitro is
pretty difficult to detonate, and frozen nitro is next to impossible to
detonate. A glass container is wonderful for this purpose. As subsequent
batches get finished, the product can simply be poured in with the rest of
the nitro in the freezer until the container is filled.
    
    When the desired amount of product has accumulated, or when the freezer
is full, a decision must be made. That is whether to keep and use the nitro
in its pure liquid form, or to convert it to blasting gelatin, or even to
ruin it by mixing it into a dynamite. In making this decision, the full
range of factors have to be weighed. For instance, one has to consider what
is going to be used as a detonator for the explosive. If one has access to
blasting caps, or can improvise a low-powered cap, gelatin is the
nitro-based explosive of choice. Gelatin, when fresh, retains the full
power of the nitro, and yet is a good deal safer than the pure nitro.
    
    On the other hand, when all one can procure for detonating the
explosive is a strong firecracker, or if the nitro is going to be used for
aerial bombing, then pure liquid nitro may be the way to go. More on this
when detonation systems are discussed later.
    
    If gelatin is the chosen route, one can take heart from the fact that
gelatin is very easy to make from nitro, and that so long as it is fresh,
it packs an amazing punch. What is meant by "fresh" is that the little air
bubbles that get whipped into it in the process of making it are still
visible. Once they disappear, half the power is lost because the detonation
rate goes down.
    
    Now for how gelatin is made. You may be surprised after reading this
and say, "What? There's got to be more!" Really, there is just nothing to
the process. First of all, a suitable mixing bowl and stirrer combination
is rounded up. A really good combination is a stainless steel bowl and a
rubber spatula (small size). Also workable is china with wooden stirrers.
What must be avoided at all costs is a hard bowl with a hard stirrer, like
a glass stirrer on metal or china bowl. The grinding friction during the
mixing could easily set off the gelatin. A combination that generates
static electricity such as plastic on rubber must also be avoided because a
little spark could set the guncotton to burning.
    
    Now into the stirring bowl is put 93 grams (58 ml) of nitro. Then 7 or
8 grams of nitrocellulose (guncotton: see methyl nitrate section for a
discussion of guncotton) is stirred into the nitro. If the nitro is cold,
adding an ml or two of acetone (available off the shelf at the local
hardware store, check in the paint section) to the mix will help a lot in
forming a good even mixture. The use of acetone can be avoided if the nitro
is warmed gently by setting the bowl in warm water before adding the
guncotton.
    
    When the guncotton is all mixed in, a white jelly will result. The more
guncotton that is added, the stiffer the jelly will be, the harder it will
be to detonate, and the weaker it will be. Gelatin with 7% guncotton (i.e.,
7 grams guncotton to 93 grams nitro) when fresh can be set off with a #1
blasting cap (the weakest) and with a #4 when it has set long enough that
the gelatin has turned from white to dear yellow. 9% guncotton in the
gelatin requires a #3 or 4 cap when fresh, and stronger caps when aged.
    
    The gelatin formed in the mixing bowl can be removed using the spatula
and stored in ziplock bags until ready for use. Larger batches of gelatin
can be easily made, so lone as care is taken to ensure that the mixing is
complete and even. A uniform product should result.
    
--------------------------------------------------------------------------
                                NITROGLYCOL
--------------------------------------------------------------------------
    
    Nitroglycol (or ethylene glycol dinitrate) is an excellent alternative
to nitroglycerin. It combines almost all of the good points of nitro with a
few further unique advantages of its own. Its easy manufacture (just like
nitro!) and high power make nitroglycol an attractive choice for any job
requiring shattering explosive power.
    
    One could go on endlessly expounding the points in favor of
recommending nitroglycol, but there is no need to go into such detail. By
knowing the major advantages of nitroglycol, the reader will be able to
make his own informed choices.
    
    The first and foremost advantage of nitroglycol is that it is less
sensitive than nitro. It requires three or four times the force to set it
off. This should be very reassuring to all the timid hearts contemplating
entering the explosives manufacture field. On the serious side, this
difference in sensitivity becomes very important when large amounts of the
pure liquid explosive are being handled.
    
    Another good point about nitroglycol is that it has better storage
qualities than nitro does. Nitroglycol is much better able to withstand a
sloppy purification iob. This is because traces of acid left in the product
will not bring nitroglycol to as rapid a ruin as nitro. This should not be
interpreted as an endorsement of sloppy purification methods. It just means
that with nitroglycol, there is more room for error.
    
    For arctic blasting operations, or just the dead of winter, nitroglycol
has the advantage of being explodable at temperatures which would freeze
nitro into a harmless solid mass. This is because nitroglycol freezes at a
much lower temperature than nitro does. Nitroglycol is also much runnier
than nitro is. This low temperature explodability can also be viewed as a
disadvantage since freezer storage can't be considered as safe as with
nitro.
    
    Finally, nitroglycol is very easy to use. It can be used in all the
ways that nitro can. It forms gelatins with guncotton much more easily than
nitro does. No warming or addition of acetone is required to get a gel to
form.
    
    Nitroglycol is not without its weak points, however. One bad thing
about nitroglycol is that exposure to it brings on headaches much easier
than does nitro. Contact with the skin can bring them on, as can breathing
the vapors. When working with the substance, one should be wearing rubber
gloves. Surgical type gloves are best because they do not interfere with
manual dexterity like the heavier gloves do.
    
    This is a minor drawback. A much more serious difficulty is that the
starting material for making nitroglycol, ethylene glycol, is not available
directly off store shelves. This complication would be very frustrating
were it not for a couple of ways around it.
    
    The first and simplest way around this problem is to order the chemical
from the various chemical supply outlets. Since ethylene glycol has no
major drug production usages, major hassles should not be expected. A
reasonable price is about $30 per gallon. Any orders for this substance
should be placed at a different outlet than the source of the acids.
    
    In many cases, it is the wisest route to avoid chemical purchases when
possible. The paper trail they can leave is unsettling for covert
operations. Luckily for these situations, there is an easy and cheap
alternative source of ethylene glycol: antifreeze.
    
    Other publications have suggested making ethylene glycol by warming
ethanol with sulfuric acid to convert the ethanol to ethylene gas and then
passing this gas through a bed of coke impregnated with phosphoric acid,
and then feeding this product into nitroglycol production. This route is
silly for the Home Workshop Explosives manufacturer. It is much too
involved and subject to failure for workshop use. This method would be much
more at home in a large factory manned by a staff of experienced chemists.
The motto to follow is "keep it simple." Anything that can go wrong is
likely to, over the long haul.
    
    A quick lesson in antifreeze formulations will well serve the
experimenter interested in obtaining usable ethylene glycol from it.
Antifreeze has as its major ingredient ethylene glycol (unless you live in
Russia where vodka is popular). In addition to the ethylene glycol there is
an additive package in the antifreeze. This package varies with the brand
of antifreeze, but the major additive is triethanolamine. This ingredient
is universally used to inhibit rust formation in the radiator. The better
brands will have in addition to triethanolamine, substances intended to
plug small leaks, and other additives as well to extend rust protection to
aluminum radiators and so on. These more complex additive packages are bad
news to the Home Workshop manufacturer, because the lengthening list of
additives make the job of getting pure ethylene glycol from antifreeze very
troublesome.
    
    To avoid these diffculties, the cheapest brand of antifreeze is sought
out. Generic antifreeze is ideal. It is likely to contain only
triethanolamine as an additive. Now the manufacturer is faced with only the
problem of removing the triethanolamine from the mixture. The
triethanolamine must be removed because it will not stand up to the mixed
acids used to convert the ethylene glycol to nitroglycol. Triethanolamine
will break down under those conditions and cause the formation of the
dreaded red gas, NO2, if it is left in the mixture.
    
    To obtain pure ethylene glycol from the cheap antifreeze, distillation
is used. This is the way to go because ethylene glycol boils at 197ø C,
while triethanolamine boils at 335ø C. A very good separation of the two
substances can be obtained by this method without resorting to
fractionating columns.
    
    The best and simplest way to do this distillation is if the Home
Workshop experimenter has invested in the distillation kit described in the
nitric acid section. Such glassware comes in handy again and again for the
serious experimenter. The only bad thing I can say about owning such
equipment is that it is expensive, costing several hundred dollars. Narco
swine surveillance centers on chemicals, not equipment.
    
    Using the chemical glassware, obtaining pure ethylene glycol can
proceed very simply. See the drawing on page 59. The larger distilling
round bottom flask sits directly on the electric hotplate. The so-called
"fifth burner" unit bought at the local hardware store for $20 is perfect
for this job. It should have an infinite control knob to regulate the
amount of heat it gives off. The antifreeze is put in this flask, filling
it about half or 2/3 full. A few pea sized chunks broken off of a Dr.
Scholl's pumice footstone should also be put in this flask to ensure a
smooth boil during the distillation.
    
    The way the distillation is done is as follows: First the flask sitting
upon the heater element is filled about 1/2 or 2/3 full of antifreeze. The
heat is applied from the fifth burner unit until some boiling begins in the
heated flask. These vapors will work their way up through the neck of the
flask, and droplets will begin to appear on the thermometer, and in the
area of the stillhead where it makes the turn to deliver into the
condenser. When these droplets appear, which is soon after boiling begins
in the heated flask, water flow should begin through the condenser. This
will cool off the vapors and turn them back into a liquid. These condensed
vapors will flow down into the other flask where they can be collected when
all the product has arrived. The rate of boiling in the heated flask should
be controlled by varying the amount of heat applied to it so that a slow
trickle of about one drop per second appears in the other flask
    
    Let's now focus in on the stillhead, because it plays such a crucial
role in the distillation.
    
    The thermometer should extend precisely to the position shown in the
drawing. Any other placement will give false temperature readings. Pushed
down lower, it will give false readings on the high side. Placed higher up,
it will read too cold.
    
    The second thing which can be done with the stillhead is that its lower
end can be packed. This will result in a much purer product because a
little bit of packing will act as a fractionating column. To do this, a
glass bottle is smashed on a cement floor, and the resulting pieces are
picked over to find a few small enough to fit in through the top, yet big
enough to keep from falling through the bottom. A few pieces of glass are
enough to do the job.
    
    Alternatively, a little bit of a stainless steel scrub pad can be
pulled into this area.
    
    When distilling the antifreeze, the temperature showing on the
thermometer should be watched closely. Since ethylene glycol boils at 197ø
C, the liquid appearing in the collecting flask should only be saved when
the thermometer indicates that the vapors entering the condenser are close
to that temperature. To clear up any misunderstanding, let's go through a
typical distillation.
    
    When the vapors first reach the thermometer, the temperature shown on
the thermometer will rise quickly. It is unlikely, however, to scoot up
immediately to 197ø C. First the ingredients in the antifreeze with lower
boiling points will distill off. For example, if it is really cheap
antifreeze, some water will boil off at 100ø C. None of this lower boiling
material should be saved. It should be collected in a separate container
and thrown away. Only when the temperature shown on the thermometer gets
into the 190ø C range, should the liquid appearing in the collecting flask
be considered to be ethylene glycol.
    
    When the ethylene glycol begins appearing, the heat should be turned
down some on the fifth burner unit to avoid superheating the antifreeze and
giving false high readings on the thermometer. Collection of ethylene
glycol should continue until the temperature shown on the thermometer goes
above 205ø C. About 2/3 of the antifreeze put in the distilling flask will
be collected as pure ethylene glycol in this manner. When the temperature
goes above 205ø C, the heat should f~rst be turned down further on the
fifth burner unit to see if slower distilling will produce more ethylene
glycol. If the temperature persists above 205ø C, then all the ethylene
glycol has been collected. When this point has been reached, the heat
should be turned off, ethylene glycol should be poured into a clean, dry
glass container and the top tightly closed. It must be closed because pure
ethylene glycol will soak up water from the air and dilute itself. The
presence of water in the ethylene glycol will have the bad effects on yield
of product already discussed in the previous sections of this book. The
slop antifreeze material left in the distilling flask should be poured down
a drain when it cools off. Then another run of fresh antifreeze may be
distilled if desired.
    
    It is not necessary to possess chemistry glassware to distill
antifreeze. The stuff is not corrosive, or otherwise particularly dangerous
(so long as it is not drunk, or the hot fumes sniffed!) so a homemade still
can be constructed and used for the process with good results so long as
care is taken in its construction and use.
    
    An antifreeze distillation using this setup will proceed in the same
manner as described for the chemical glassware version, with the difference
that it will not be possible to as closely monitor the process. With some
practice, and using the same brand of antifreeze, it should be possible to
get as good results using this apparatus as with the chemical glassware.
    
    A few words are in order on the construction of this still, as there
are a few trouble spots. First and most important is the cork or rubber
stopper in the metal can. It must fit tightly into the opening in the metal
can so that the vapors are forced up the tubing. Leakage here can result in
fluid running down the side of the can, posing a fire hazard.
    
    The holes in the stopper must be exactly the right size to hold the
tubing and the thermometer. Ragged edges on these holes are not acceptable,
as the resulting leakage could pose the same fire hazards. Cork borers are
available which do a good job of punching clean holes through corks. In
their absence, a very careful job must be done in making these holes. Loose
spaces and ragged edges can be mended by use of silicone bathtub caulk just
prior to inserting the tubing and thermometer.
    
    The coiled portion of the metal tubing can be made by wrapping the
copper tubing around a sturdy round object. Care must be taken to avoid
kinking the tubing shut during this process.
    
    Finally, some support must be provided for the copper tubing so that
its weight does not cause the metal can to tip over, or cause damage to the
cork. Any type of support is OK for this purpose, so long as it does the
job. This requirement for support is not unique to the homemade still, as
the chemical glassware set-ups also need clamping into place or other
measures to hold the pieces together.
    
    Doing a distillation using this homemade still works almost exactly the
same as with chemical glassware. There are only two areas where the method
differs. The first difference is that the thermometer inserted into the top
of the can will measure the temperature of the vapors there, not at the top
of the metal tubing where it begins its descent. This means that
temperature readings on the thermometer are likely to be falsely high. With
some practice and always using the same brand of antifreeze, this can be
corrected for on an empirical basis.
    
    The second, and potentially more troublesome problem has to do with the
design of the coiled condenser portion of the copper tubing. As shown, it
relies solely on air cooling for the vapors to give off their heat and
become liquids once again. This will be sufficient during cold weather in
the workshop, if the rate of distilling is slow enough. Otherwise some
plastic tubing can be wrapped around the coiled portion of the metal
tubing, and a flow of water run through the plastic tubing. The bottle into
which the product drips can also be cooled off by packing it in ice. Under
no conditions is it acceptable for steam to be escaping from the end of the
metal tubing. Enough cold must be applied to the condenser to turn the
vapors back into liquids.
    
                             MAKING NITROGLYCOL
    
    With the ethylene glycol in hand, one is ready to turn it into
nitroglycol. This process is very easy and almost identical to the
procedure used to turn glycerin into nitro. To illustrate just how similar
this process is to the nitro manufacture process, see the formula below:
    
                          Nitric + Sulfuric
           OH-CH2=CH2-OH ===================> NO2-O-CH2=CH2-O-NO2
                               Acids
           Ethylene Glycol                    Nitroglycol

    Compare this to the reaction for making nitro. Here the alcohol is
ethylene glycol. For nitro, the starting alcohol is glycerin. The only
difference in this reaction is that ethylene glycol is one carbon atom
shorter. As far as the practical detail of making the two substances go,
there is very little difference. All three of the variations on the nitro
making process work for making nitroglycol, just by substituting ethylene
glycol for glycerin. The same amounts of all ingredients are used.
    
    There are only two small details where the production of nitroglycol
differs from nitro. The first difference is that nitroglycol is more prone
to form the red gas, NO2 during its manufacture than is nitro. Because of
this tendency, the ethylene glycol should be dripped directly into the
acids rather than allowing the stuff to run down the sides of the glass
into the acids. More attention should also be paid to getting the ethylene
glycol promptly stirred into the acid mixture. It may also prove to be more
fussy about the quality of the nitric acid used in the process than is the
case with nitro.
    
    The second detail in which nitroglycol manufacture differs from nitro
production is the greater ease with which nitroglycol dissolves in water.
As a result of this, less water must be used in washing up the nitroglycol
than was the case for nitro. If the full amount of water was used,
excessive amounts of product would be lost by getting dissolved in the wash
water, and thrown away. To minimize these losses, the final wash with
saturated salt solution should definitely be combined with the bicarb wash.
This is done by the method described in the nitro chapter. The bicarb
solution has salt added to it until it can't dissolve the added salt
anymore. Then this wash water is used on the crude nitroglycol.
    
--------------------------------------------------------------------------
                               NITROMANNITOL
--------------------------------------------------------------------------
    
    Nitromannitol (ak.a nitromannite) is the third most difficult to make
of the good high explosives. Other factors being equal, then nitromannitol
should be the third choice for the Home Workshop Explosive manufacturer
when setting up shop.
    
    The production of nitromannitol is relatively easy because the starting
material for its manufacture, mannitol (mannite), is easily available at a
moderate price from headshops. It is sold wherever fine dealing supplies
are sold because mannitol is a popular cut for cocaine. The person behind
the counter is likely to give you a knowing wink when making the
transaction, but have no idea of its usefulness in explosive manufacture.
If the heat has succeeded in driving all the headshops in your area out of
business, High Times may carry ads for mail-order mannitol. This is not
certain, however, as their snotty "My dope is better than your dope"
attitude may cause them to refuse to carry such ads in the future.
    
    The production of nitromannitol is not without its unique pitfalls,
which combine to make the manufacture of nitromannite about twice as
diffcult as making nitro or nitroglycol. Foremost of these diff~culties is
the sensitivity and poor keeping properties of nitromannite. Under the best
of conditions, it is about as sensitive as nitro, but if it is not
completely freed of all traces of acid during the purification process, it
will rapidly become too dangerous to handle.
    
    Removing these last traces of acid is difficult because nitromannite is
a solid, and so can lock the acid inside its crystals, beyond the reach of
wash water or bicarb. To get at these locked-up acid residues a new
chemical technique must be introduced here. This chemical technique is
called recrystallization. Recrystallization involves dissolving the
nitromannite in a solvent, like alcohol, and then allowing the crystals to
reform from this solvent. This results in the garbage which was formerly
locked up inside the crude crystals being released into the solvent. The
new crystals which form are largely free of their former pollutants. This
may sound complicated but it is surprisingly easy to do. Complete, detailed
instructions will be eiven in the text.
    
    The other new technique which must be mastered to produce nitromannite
is vacuum filtration. This technique is needed because nitromannite is a
solid with very fine fluffy needlelike crystals. It has to be separated
from its reaction mixture or recrystallization liquors by filtration. These
long, fine needle crystals can only be filtered properly by having a vacuum
force the flow of material through the filter. Without this, filtering the
batches could take hours, and the results would be poor. This technique is
very simple and can be improvised using household equipment. It too will be
explained in detail when the time comes.
    
    Making nitromannite proceeds in a remarkably similar manner to the
manufacture of other explosives covered to this point. It is a nitric ester
like the rest, and so is made by reacting an alcohol, in this case mannite,
with nitric acid. See the reaction on next page.
    
    As can be seen from the drawings, mannitol has 6 alcohol groups (OHs)
which react with nitric acid to form nitric ester groups (ONO2s). Other
than the large number of alcohol groups mannite is almost identical to
glycerin or ethylene glycol.

                     OH                            ONO2
                     |                             |
                   H-C-H                         H-C-H
                     |                             |
                  HO-C-H                      NO2O-C-H
                     |                             |
                  HO-C-H                      NO2O-C-H
                     |                             |
                   H-C-OH                        H-C-ONO2
                     |                             |
                   H-C-OH                        H-C-ONO2
                     |                             |
                   H-C-H                         H-C-H
                     |                             |
                     OH                            ONO2

                  Mannitol                     Nitromannitol

    This large number of alcohol groups has an important practical effect
upon what strength acid may be used in its manufacture. Referring back to
the equilibrium equation given in the nitric ester section for
nitroglycerin, the same equation can be written for nitromannite simply by
raising the nitric acid terms and the water terms to the 6th power instead
of the third power. This means that it is crucial in making nitromannite
that the strongest possible nitric acid is used, and as a natural
consequence (since the dilutent for nitric acid is water) that the amount
of water in the mixture be held to an absolute minimum.
    
    For this reason, only fuming nitric acid (at least 90% strength,
density 1.5) can be used to make nitromannite. This fuming nitric acid must
either be obtained through commercial sources, or made according to the
directions in the nitric acid section. The absolute need for the high
strength acid is one of the roadblocks to putting nitromannite into
production in the workshop.
    
    To set up for making nitromannite, one begins with the same equipment
as used earlier. The glass reaction vessel, pail of water and tub filled
with ice are all needed. The important difference is that the temperature
of the reaction must be held to 0øC (32øF) or below, so the ice must be a
good deal colder than usual to keep the reaction at such a cold
temperature. The way this is done is to mix the ice with about half its
volume of table salt. This will drive its temperature down to around -20øC
(0øF) which is cold enough to do the job against the heat given off in the
reaction. An alternative is to pour a bottle of rubbing alcohol onto the
ice and mix it around. This will also lower the temperature of the ice
greatly.
    
    Then into the reaction vessel, nestled deeply into the ice bath, 100
grams of fuming nitric acid (66 ml) is poured into the reaction vessel. Of
course, the nitric acid should come directly from the freezer so that the
ice does not waste itself cooling down the nitric acid. To this nitric
acid, 20 grams of mannitol is added a little bit at a time. Between each
addition of mannitol, the contents of the reaction vessel should be mixed
by swirling. It is best to move the whole tub when swirling the reaction so
that close contact of the reaction vessel with the ice bath is not broken.
A thermometer should be in the reaction at all times, and it should be
watched so that the temperature does not go above 0øC. If it does, the
reddish brown fumes of NO2 are likely to follow. In that event, the batch
gets dumped into the pail of water. So long as the addition of mannitol is
slow, and the temperature is watched, this event is unlikely. The addition
of the mannite should take 20 or 25 minutes.
    
    The mannite should dissolve quickly as it is added to the nitric and
mixed in. To ensure rapid dissolving and quick reaction, the mannitol
should be finely powdered before it is used. Oftentimes, mannite is sold in
head shops in quarter-ounce pressed blocks. These blocks will have to be
mashed with a fork to break them up.
    
    After all the mannitol has been added, and the last of it has dissolved
into the nitric acid, it is time to finish up the reaction. This is done by
adding concentrated sulfuric acid to the reaction mixture. This has the
effect of sucking up whatever water is present in the mixture, thereby
forcing the reaction to completion, and also causing the nitromannitol
which has been produced to come out of solution and form crystals which can
then be filtered out.
    
    To finish off the reaction, 200 grams (110 ml) of concentrated sulfuric
acid is measured out. The sulfuric acid should be ice cold, fresh from the
freezer. It is then added a drop or two at a time with an eyedropper (glass
stem!) to the reaction mixture. Between each drop or two, the acid should
be mixed in by mixing with the eyedropper or the thermometer. The
temperature should be watched closely during the addition of the sulfuric
acid to make sure the temperature does not go above 0ø C. As the
temperature nears 0ø C, the addition of sulfuric acid should be stopped
until the mixture cools off again.
    
    As the sulfuric acid is added, crystals of nitromannite will appear,
slowly at first, and then quite rapidly. By the time half of the acid is
added, the mixture will be getting pretty thick from the large mass of
crystals formed. As the mixture gets thicker, it will be harder to mix in
completely the added acid, so extra effort must be put into ensuring an
even mix as the last of the acid is added. Care must be exercised in using
the thermometer as a mixer here so that it is not banging the sides of the
glass reaction vessel, or grinding the bottom. This grinding could provide
the friction to set the whole batch off.
    
    Finally, when all the acid is added, a mixture with the appearance of a
good heavy slush will be formed. Now the challenging part of the operation
begins. The crystals of nitromannite must be filtered out of the highly
corrosive nitric and sulfuric acid mixture in which they are floating,
quickly enough that they do not rise above the red gas-forming temperature
before they are rinsed with water and thereby rendered more stable. This
operation is complicated by the fact that the nitric and sulfuric acid
mixture in which they are floating will fairly quickly react with filter
paper to form guncotton. This will cause most of the filter paper to
dissolve, and ruin its effectiveness at catching the crystals.
    
    There are a few ways around this problem. The most important part of
the solution is to get the filtering done as quickly as possible. At least
the first part of the filtering must be done very quickly, the filtering
out of the crystals from the acid reaction mixture. Later, when it is
rinsed with water and rendered less corrosive, a more leisurely pace can be
taken. To make this filtration a quick process, there is only one way to
go. That is to have a vacuum pulling from the underside of the filter,
dragging the liquids through as fast as possible. Actually, this would be
the only way to go even if the acids didn't eat filter papers. Packing the
stuff inside a large coffee filter and wringing it out by hand is madness.
Allowing it to sit in a funnel and drip through a filter is silly as well
because the combination of fluffy crystals and viscous acids (concentrated
sulfuric acid is about as thick as light motor oil) will make this take so
long that it is unreasonable, even if one did not have to worry about the
temperature of the mixture rising above 0øC. Genuine chem lab experience is
what separates this book from many pretenders out there, most of which
merely feature reprints from scholarly works which assume the reader has a
high level of chemical skills and can solve these problems for himself
without giving all the details. Place your wild-eyed trust in Uncle Fester.
You won't be disappointed.
    
    Let us first see how this rapid filtration problem would be handled
using chem lab equipment before looking at ways to improvise for the same
effect. To begin with, a source of vacuum would be dose at hand on the lab
bench, such as an aspirator. A water bed pump would serve the same purpose
just as well since a really good vacuum isn't needed. From this vacuum
source, a vacuum hose similar to an automotive vacuum hose would be led to
the glassware set-up.
    
    The filtering flask has a side tube to which a vacuum hose attaches,
producing a vacuum inside the flask. This vacuum serves to rapidly pull
fluids that are poured into the Buchner funnel down into the flask. This
Buchner funnel normally has a flat bottom inside it at about the level
shown by the dotted line in the drawing. The flat bottom is perforated with
many holes, and this is the place where a filter paper is laid, so crystals
are stopped at the filter paper. The fluid proceeds through down into the
filtering flask, and the crystals pile up in the buchner funnel above the
filter paper.
    
    Now using this chem lab equipment, the problem of filtering would
either be handled by piling up several filter papers, soaking them wet and
hoping that the wetness would protect them through a rapid filtering (bad
solution), or by using something other than filter paper to catch the
crystals, something which would stand up to the acids without being eaten
away.
    
    A great alternative to ordinary filter paper for this job is asbestos
paper. This useful material used to be very easy to get at hardware stores,
but has since been outlawed, along with virtually anything else made of
asbestos, in the U.S. It has since been replaced with a woven glass
sheetlike material which works almost as well as asbestos paper. Its only
drawback is that it tends to be thick and stiff, and so is not so easy to
work with. To use this woven glass sheet as a filter, one would only have
to carefully cut a piece out of it with a scissors that exactly fits the
bottom of the Buchner funnel. Once in place, the slushlike nitromannite
could simply be poured through it with the vacuum applied to the filtering
flask, and all the acids would rapidly be pulled through to the filtering
flask and the crystals of nitromannite would pile up in the Buchner funnel.
    
    To modify this process for using common household materials, one should
first look for a replacement for the Buchner funnel. This is easily enough
done by heading to the hardware store and getting a plastic funnel with a
long narrow stem and a plastic screen in the bottom. This funnel very
closely approximates a Buchner funnel. Cost: about $2.
    
    Next, to replace the filtering flask, one can use a Mickey's Big Mouth
malt liquor bottle. This rather sharp-tasting brew is made by the Old Style
Brewery. Cost: nothing, if you like beer.
    
    Finally, to replace the one-hole stopper, a two-hole stopper of the
correct size is needed to fit in the top of a Mickey's Big Mouth bottle. If
easy access is not available to an assortment of different size stoppers so
that you can choose the right one, the Edmund Scientific catalog usually
has quite a variety to choose from with no suspicion involved. This
improvised equipment can be set up as shown on following page.
    
    This is basically the same set-up as with the chem lab glassware except
that the vacuum hose does not attach to the Mickey's Big Mouth bottle since
it has no side tube to put a vacuum hose on. Instead the vacuum hose
attaches to a stiff plastic or wooden tube (no copper allowed! improvise!!)
inserted through one of the holes in the two hole stopper.
    
    This is the source of the vacuum inside the Mickey's Big Mouth bottle.
The stem of the plastic funnel goes through the other hole in the two hole
stopper. Greasing the stem of the funnel with vaseline will greatly ease
its passage through the two hole stopper.
    
    Next a section of the woven glass material mentioned earlier must be
picked up at the hardware store. A section should be carefully cut out of
it so that it exactly covers the plastic screen in the bottom of the
funnel. Good fit is essential here as any loose spots or uncovered areas or
points of buckling of the filter will be places where nitromannite crystals
can escape being caught, and end up going through with the acids. It may
help to wet the filter and push it into place just prior to filtering the
slush.
    
    The procedure to use in filtering the material is this: First of all,
the filtering apparatus is set up as shown in the pictures. Then the filter
is put into place and wetted, then pushed down securely into place, making
sure that the filter lays flat with no buckles or loose edges. Now the
vacuum source is turned on, and the vacuum hose attached to the glassware.
    
    Next, the slushlike nitromannite mixture is poured into the funnel. Not
all of it should be poured in at once, of course, because this is likely to
overflow the funnel unless the funnel is very large. At first, the acids
will quickly rush through the filter, but as a bed of nitromannite builds
up in the funnel, it will slow up, and a greater vacuum will accumulate in
the glassware to pull it through. The first rush of liquid through the
filter should be watched closely to make sure that no significant amount of
nitromannite crystals is coming through. If there is, this indicates that
the filter is poorly cut or placed. It should get better as a bed of
nitromannite builds up above it, but in any case the material which passed
through will have to be refiltered separately at the end of the process.
    
    The filtration will proceed rapidly if a reasonable vacuum is applied
to pull the liquids through. The bed of nitromannite in the funnel (generic
term: filter cake) will rapidly shrink as the acids are filtered out. If
the right size funnel is chosen, all of the batch of nitromannite will fit
in the funnel. As the last of the acids in the slush are filtered out,
cracks will appear in the filter cake. Now it is time to move on to the
next step, rinsing off the crystals.
    
    The aim of all the purification steps in nitromannitol processing is to
remove the residual traces of acids from its manufacture. The first step in
this process is to rinse the crystals with water. To do this, simply pour
cold water into the funnel on top of the nitromannite. It is convenient to
rinse out the crystals clinging to the walls of the reaction vessel at the
same time as the first rinse. This gets them in with the rest of the
product with a minimum of hassles. This first rinse of cold water should be
followed with a couple more, each one amounting to a couple hundred mls of
water. For these last couple of rinses, it is good to turn off the vacuum
(remove vacuum hose first to avoid water backup into acids) and just let
the water move through the crystals slowly. Stir around the bed with a
toothpick to avoid channel formation.
    
    The next rinse for the crystals is a weak bicarb solution. This will
get most of the remaining acids. A few grams of Arm & Hammer in a couple
hundred ml of water will serve the purpose nicely. It is poured through the
filter cake in the same manner as the water rinses were. Finally, another
rinse of cold water is poured through the crystals. When the vacuum pulls
most of the water out of the filter cake, it is time to move on to the
recrystallization of the product.
    
    A glass, china, or plastic plate is a convenient place to dump the
product out of the funnel onto. The best way to do this is to carefully
(after the vacuum is removed) pull the funnel and the stopper out of the
glassware, and then tip the funnel upside down an inch or so above the
surface of the plate. Some gentle tapping with the hand on the side of the
funnel should be enough to make the filter cake fall out of the funnel.
Avoid the temptation to bang the funnel on the surface of the plate to
dislodge the filter cake. When it falls out, a plastic spoon can be used to
scrape out whatever dings to the funnel. The filter should be picked out of
the cake by hand.
    
    To recrystallize, a heat resistant glass container must be obtained. A
good choice is a one-cup size pyrex measuring cup. The crystals are put
into the cup. Next some alcohol is added to the cup to dissolve the
crystals. The best choice for alcohol is 190 proof grain alcohol. The next
best choice is 91% isopropyl alcohol, available at the corner drug store
right off the shelf. Unsuitable for use are denatured ethyl alcohol
(because acid may have been used to denature it) and 70% isopropyl alcohol
(because of too much water in the alcohol). Methyl alcohol (wood alcohol)
is not a good choice because it dissolves the crystals too well, and so
causes loss of product, and a poorer job of removing the last traces of
acids.
    
    The procedure used to dissolve the crystals is as follows: First, 100
ml of alcohol is added to the crystals. They will not dissolve noticeably
in the alcohol because it is cold. A pan of water is boiled, and when it
boils it is brought over to the table in the workshop and the measuring cup
is put into the pan of hot water. This work should not be done on the stove
because when the alcohol heats up, it will give off fumes which could be
ignited on the stove. The hot water will quickly warm up the alcohol in the
measuring cup, and it will start to dissolve the crystals of nitromannitol.
The alcohol should be stirred to help with the dissolving of the
nitromannitol. A perfect tool for this job is a plastic coffee stirrer from
McDonald's. After a few minutes, the water will have cooled off to the
point where a fresh pan of boiling water should be used for the heating of
the alcohol. Soon after putting the measuring cup in the second pan of hot
water, all the crystals of nitromannitol should be dissolved. If they have
not all gone into solution, then some more alcohol should be added to the
measuring cup to dissolve them. Since the added alcohol is cold, a third
pan of hot water will then also be needed to bring the temperature of the
alcohol up to the required level to dissolve the nitromannite.
    
    When all the crystals have dissolved, the cup should then be removed
from the pan of hot water and allowed to cool. As the alcohol cools,
crystals of nitromannite will reappear. This is because cold alcohol does
not dissolve nitromannite very well, so they are forced to come out of
solution. These recrystallized crystals of nitromannitol are much purer
than the crude material that was started with because the acids that were
formerly locked inside the crude crystals remain in the alcohol.
    
    The colder the alcohol gets, the less nitromannite it will dissolve so
the measuring cup should find its way to a freezer, or be packed in ice.
This will get the largest amount of product out in this step. The
nitromannitol should be white and the crystals should be long and needle
shaped.
    
    Now the pure product can be collected. To do this, the same filtering
setup described earlier is used, except that a regular coffee filter can
now be used, since there are no strong acids left for it to be dissolved
by. All pieces, of course, must be clean and dry to avoid contaminating the
product.
    
    The alcohol which filters through contains some more nitromannite in
it. To get this second crop of crystals out of it, the alcohol is simply
poured back in the measuring cup (or beaker, which could easily be ordered
from the Edmund Scientific catalog) and heating is recommenced. The heating
must be stronger this time. If grain alcohol (190 proof ethyl alcohol) was
used, the mixture should be brought to a boil. This can be done safely for
small batches like this one on an electric stove top by setting the cup in
a pan of hot water and bringing the water to a boil with the overhead fan
running to suck up the alcohol fumes. If isopropyl alcohol was used, no
attempt to bring the alcohol to boiling should be made because isopropyl
alcohol boils at the same temperature that the crystals melt at. This high
temperature will prevent their formation during the crucial water-adding
step to follow. For the isopropyl alcohol, just heat the alcohol up in the
boiling water.
    
    When the grain alcohol starts to boil, or when the isopropyl alcohol
gets hot, water should be dripped into the alcohol. In the case of
isopropyl alcohol, it will also be necessary to stir the water into the
mix. The mixture should be watched closely durine this addition. When the
mixture starts taking on a milky color, stop adding water. This means when
the whole solution gets milky, not just little areas, because local
milkiness in the area where the drops of water land will be seen soon after
starting the water addition. This milkiness is termed "turbidity."
    
    Other publications have erred seriously on this point. They defined
turbidity as a churning, as if it was going to get up and do a dance for
them. It makes one wonder.
    
    When this milkiness is seen, the heat should be removed, and the mix
allowed to cool. Crystals of nitromannite will soon be evident. The
milkiness was caused by small crystals of nitromannite forming in the
solution. They formed because water is an even worse solvent for
nitromannite than is cold alcohol. As the alcohol became progressively more
watery, its ability to dissolve nitromannite went from bad to worse.
    
    When this mix gets cold in the freezer or by packing in ice, the last
of the nitromannitol crystals will have formed. They should be filtered out
like the rest, and the alcohol which filters through should be thrown away.
    
    The combined yield from the two crops of crystals is close to 50 grams.
This packs the explosive punch of a comparable amount of nitro. For long
term storage, the crystals should be soaked with water to absorb any acids
they might generate during storage. It can then be filtered before uce
    
                            USE OF NITROMANNITE
    
    In many respects the use of nitromannite is similar to the use of
nitroglycerin. It requires about the same amount of force to set it off,
and it delivers about the same yield of explosive power when compacted to
rock form. There is a large difference, however, caused by the fact that
nitromannitol is a fluffy solid whereas nitro is a liquid. This flufffiness
means that nitromannite is nowhere near as dense as nitro is. As was
mentioned earlier, to get maximum detonation velocity, and therefore
explosive power, the explosive must be as dense as possible. So the big
problem with nitromannite is to get its density high enough to deliver its
full explosive potential.
    
    The most effective way to compact nitromannite is to melt the substance
by packing it into a glass vessel which will be its ultimate container, and
melt the crystals by setting the glass container in warm to fairly hot
cooking oil. The crystals melt at about 110ø C. When they cool down again,
they will freeze into a solid rock. The same effect can be seen by packing
snow into a container, melting the snow, and refreezing. The ice formed
will take up quite a bit less space than the packed snow, so the substance
is then much more dense.
    
    This method is not to be recommended, because of the great danger
involved. Nitromannitol becomes very sensitive at elevated temperature, so
the heat required to melt large amounts of nitromannite could precipitate
an explosion. The Home Workshop experimenter will have to settle for the
increase in density which can be obtained just by packing the crystals into
place. Care must be taken to avoid friction during the packing process.
    
    The serious experimenter may wish to try packing the crystals into a
vessel, then wetting the crystals down by spraying them with some ether
(starting fluid). This will melt them, and when the ether has evaporated
from the container, they will be rocked and take up less space.
    
    A different approach takes advantage of the properties of nitromannite
to create a self-detonating booby trap device. In the methyl nitrate
section, mention was made of an attack plan featuring a bottle of methyl
nitrate taped with heat resistant tape or other loose yet durable
attachment to the exhaust manifold of a car. Nitromannite is much more
suitable for this usage for several reasons. First of all, it is safer to
make. Secondly, the heat from the exhaust will first melt the crystals,
making them much more dense and more powerful. Finally, nitromannite will
not half boil away before it explodes like methyl nitrate will (boiling
point of methyl nitrate, about 65øC). For these reasons, nitromannite is
much more likely to give satisfactory results in this attack plan.
    
    In a similar vein, attack plans utilizing fuses in contact with exhaust
manifolds leading to detonators, and nitrogen triiodide crystal laid down
to set off the nitromannite from the vibration of the engine cannot be
ignored. A fertile imagination is not only a joy for life, but also the key
to improvised detonation systems. Good results can be obtained by routes
other than the standard blasting cap-explosive charge combo.
    
    A pretty good plastique can be made from nitromannite, just by mixing
it with vaseline. Other, more advanced plastiques can also be made with
nitromannite by preparing silicone polymer gels and so on, but the marginal
advantages of these plastiques (they can be used under water, and in very
hot places) are hardly worth the greater difficulty of preparation they
present. Also, the ingredients used to make these gel matrixes are not the
type of things you go down to the hardware store to get. Unless you work in
the plastics or coatings field, you are unlikely to have easy access to
them in less than 5 gallon pail quantities.
    
    To make the plastique with vaseline, just mix 95 grams of nitromannite
with 12 grams of vaseline in a stainless steel bowl. They can be mixed
together by use of a rubber spatula. When a uniform mixture is made, the
plastique can be wrapped in wax paper until use. A number 5 blasting cap or
equivalent will set it off.
    
--------------------------------------------------------------------------
                                    PETN
--------------------------------------------------------------------------
    
    PETN, or pentaerythritol tetranitrate, is considerably more difficult
to make than the other explosives considered to this point. Its preparation
is not recommended for the casual experimenter, or for those with a clumsy
streak in them. Its power and sensitivity is comparable to the other
explosives in this book. It is also a crystalline solid, so it offers the
same difficulties as nitromannitol in getting it compacted to maximum
density for maximum power. If it were not for an extremely powerful and
versatile plastique which can be made by mixing PETN with nitroglycerin, it
would not be covered in this book.
    
    There are several new difficulties encountered in the manufacture of
PETN which combine to make this process a good deal more difficult than the
preceding ones. First and foremost of these obstacles is the starting
material, pentaerythritol (pentaerythrite). While it may be commercially
available at about $20 per pound, its purchase is definitely not advisable
for the Home Workshop Explosives manufacturer. Its purchase would leave an
all too recognizable paper trail, and could easily lead to suspicion or
investigation either before or after usage. This leaves as the only viable
alternative, making the pentaerythritol from simpler materials which are
not subject to scrutiny, a tactic well known to drug manufacturers. This
necessity to first make pentaerythritol makes this process a two-stage
affair, with all the problems inherent to this approach. The biggest
difficulty, other than all the work involved, is that the pentaerythritol
must be refined to a high degree of purity before it can then be fed into
the final stage of the process for conversion to PETN. The old computer
programming slogan "garbage in, garbage out" holds doubly true in synthetic
chemisky.
    
    Another bad point about the two-stage nature of this process is the
great amount of time which is required to make and purify the 
pentaerythritol. The unavoidable consequence of this is that this part of
the process becomes a bottleneck in the manufacturing operation. The amount
of product which can be made in a given period of time will always be
controlled by how fast the pentaerythritol can be turned out to be fed into
the PETN stage of the process.
    
    Finally, the quality of nitric acid used to make PETN is crucial. This
process is pretty fussy in that white fuming nitric acid must be used. This
means that it can have no trace of the reddish gas NO2 in it. A little bit
of it in the mixture will in short order lead to runaway reactions and the
formation of large clouds of NO2, the dreaded red gas. This ruins the
batch, and poses the danger of poisoning the experimenter, and of possible
explosion.
    
    Now let's look more closely at the frst stage of PETN manufacture,
making pentaerythritol. This adventure in chemistry is custom made for
those who like to handle large volumes of really revolting chemicals and do
endless hours of labor to get a quantity of product measured in fractions
of a pound. Look once again at the materials covered earlier in this book.
    
    Pentaerythritol is made by reacting formaldehyde with acetaldehyde,
condensing them together with the help of calcium hydroxide.

           8 CH2O + 2 CH3CHO + Ca(OH)2 => 2 C(CH2OH)4 + Ca(COOH)2

     Formaldehyde + Acetaldehyde + Calcium Hydroxide => Pentaerythritol
    
    There is not too much which can go wrong with this reaction, so long as
reasonable care is taken to follow the directions. It is, however, very
stinky and potentially unhealthful if the experimenter allows himself to
breathe in the fumes of formaldehyde and acetaldehyde. This reaction is
best done outside with a steady breeze, the "cooker" keeping himself upwind
throughout the process. If the watchful eyes of neighbors preclude this, a
garage with a strong wind flow is acceptable. This may obscure the view of
civic-minded citizens, but their noses are another enemy to be remembered.
This process is best done in a secluded area.
    
    To begin production, a clean plastic 5-gallon pail is filled with 2160
grams (2000 ml) of 37% formaldehyde solution, 210 grams (275 ml) of
acetaldehyde, and 4 quarts of water. These chemicals do not need to be of a
particularly high grade, so if money can be saved by using technical grade
chemicals instead of reagent grade, then do so. Also, the formaldehyde
solution can be replaced by 800 grams of paraformaldehyde. This solid form
of formaldehyde does not have the powerful smell of the formaldehyde
solution, but is much more expensive than regular formaldehyde. The 37%
formaldehyde solution may be sold under the name of formalin, so be aware
of this example of the proliferation of chemical synonyms.
    
    Next, a clean wooden stick must be obtained. A section of broom handle
minus the finish is a good example of what is called for here. This wooden
stick is used to stir the solution. 

    First mix the ingredients already in the pail, then begin adding 
powdered quicklime (CaO, calcium oxide) to the pail in small portions with
vigorous stirring. When the calcium oxide goes into solution, it first
picks up a molecule of water, becoming Ca(OH)2, and then takes part in the
reaction shown above. The CaO should be added at such a rate that the
temperature of the mixture rises to 50ø C (a little over 120ø F) within the
first half hour of adding the CaO. Then the CaO is continued to be added at
such a rate that the temperature of the mixture does not go over 55ø C
(about 130ø F). As can easily be imagined, the fumes of formaldehyde and
acetaldehyde get pretty intense as the solution gets hot. They get less
revolting as the reaction nears completion and the aldehydes get consumed.
The total amount of CaO added is 180 grams.
    
    When all the CaO has been added, the stirring is continued at a more
leisurely pace for another three hours. This long stretch of stirring is
bound to tire even the most dedicated explosive manufacturer so an
alternative which can be used where electricity is available is to suspend
an electric drill or similar motor over the pail, and use a clean paint
stirrer attachment to stir the solution. The fumes are not especially
flammable, so fires are not the hazard they often are when dealing with
more flammable chemicals. Even so, rigging an extra long stem for the
stirrer, so the motor is elevated above the pail rim, is a wise precaution.
    
    When the stirring is done, it is time to filter the now yellowcolored
solution. A large coffee filter fitted inside a plastic funnel will do a
good job of this. The total volume of liquid amounts to about 3 gallons.
Contained in this 3 gallons, is about 3/4 pound of pentaerythritol. Now the
real work begins as the workaholic explosives manufacturer isolates his
product from the mixture.
    
    First, the mixture must be made slightly acid. To do this, hydrochloric
acid (the 28% strength material available from hardware stores is good
enough) is diluted 50-50 with water. Then this diluted HCI is added to the
mixture with stirring until the mixture is acid to litmus (turns blue
litmus paper red). A good way to do this is to add 100 ml of the dilute HCl
right away, and then after stirring and checking for acid reaction, add
smaller amounts of acid until an acid condition is achieved. This will
convert the calcium formate made in the reaction to formic acid and CaCl,
and also knock out left over CaO. In these forms they are more easily
gotten rid of.
    
    Next, the yellow color can be removed by adding 30 grams of activated
charcoal powder (Norite brand is usually used in the lab) and stirring it
around for a few minutes. Then the solution is once again filtered so as to
remove the charcoal, and the filtrate is clear once all the charcoal has
been successfully filtered out. Until then it is black, and the pail is a
holy mess. Get a clean pail. This step can be omitted, but a yellow product
will result which will be more touchy to convert to PETN without the
dreaded red gas being formed. It will also not keep so well.
    
    Now the solution must be reduced in volume so that crystals of 
pentaerythritol can form. To do this the water and other assorted smelly
gunk must be boiled away under a vacuum. Formic acid and the unreacted
aldehydes will be eliminated in this process. The first step in this
adventure is to get a large enough container to hold the reaction mixture
for the boil down. 5-gallon flasks are not commonly available to the
public, but a good substitute is one of those thick glass water jugs often
seen in offices for the water cooler. This is about 5 gallons in volume,
and has a narrow opening which can be plugged with a onehole rubber
stopper, and attached to the vacuum source (either aspirator or water bed
pump).
    
    To get this process going, put the reaction mixture into the glass jug
along with a couple small pieces of a Dr. Scholl's pumice footstone (to
ensure an even boil) and a chunk of paraffin wax the size of a small grape
(to control frothing). The jug should be heated by means of steam, which
can be supplied from a pressure cooker by filling it half full of water,
clamping a section of automotive hose to the outlet on the lid where the
weighted pressure control usually sits, and piping the steam produced from
heating the pressure cooker into a cowling surrounding the jug.
    
    The jug should sit in a large pan and be lifted off the bottom an inch
or so by use of a few wooden blocks. The steam hose is run under the jug so
that the steam rises up around the jug to heat it. The cowling can be as
simple as a plastic garbage bag draped around the jug. A drain hose should
run from the bottom of the pan to a drain or sink to carry away the water
formed from the condensing steam.
    
    When the jug is reasonably warm, vacuum should be applied to it and the
heating continued. The contents of the jug will begin to boil away. This
should be continued until the volume of liquid in the jug is reduced from 3
gallons to one gallon. Then the heating is stopped, and when the boiling
ceases, the vacuum is removed.
    
    Now that the liquid has been concentrated, crystals of pentaerythritol
can form. Just let the jug cool off in the refrigerator overnight. In the
morning, the crystals can be filtered out.
    
    The liquid that filters through contains more product. This can be
obtained by boiling away until the volume of the liquid is halved, i.e.,
reduced to 2 quarts. Upon cooling, a new crop of crystals can be filtered
out. Repeating the process again, and boiling away the liquid down to one
quart gives, upon cooling, another set of crystals. The remaining liquid
can then be flushed down the toilet.
    
    The crude product should be purified before use in PETN production. To
do this, it is weighed, and an equal weight of distilled water is put into
a stainless steel pan, or large pyrex beaker. The volume of water will be
about a pint. The water is heated up on the stove, and the crystals are put
into the water, along with 10 ml of hydrochloric acid. Mix them around
until they dissolve, and boil just a little bit. Upon cooling, a large mass
of crystals will appear. Filter them out. The liquid should then be
concentrated down to about half its starting volume, and then cooled.
Another crop of crystals will appear. By repeating this process a couple
more times, about 350 grams of pure pentaerythritol will be obtained. It
may be somewhat yellowish, but will work for making PETN. This product
should be spread out on wax paper and allowed to dry thoroughly before use.

                             CONVERSION TO PETN
    
    Compared to making pentaerythritol, PETN manufacture is a breeze. The
amount of labor in the process is much less, and the volumes of chemicals
which need to be handled are trivial in comparison.
    
    The reaction here is the standard nitric ester reaction. In this case,
pentaerythritol is the alcohol, and it is nitrated by means of nitric acid
to form the nitric ester pentaerythritol tetranitrate (PETN). Here four
molecules of nitric acid are needed for each molecule of pentaerythritol.
See below:
    
         CH2-OH                         CH2-ONO2
         |                              |
  HO-CH2-C-CH2-OH + 4 HNO3 ==> NO2O-CH2-C-CH2-ONO2
         |                              |
         CH2-OH                         CH2-ONO2

  Pentaerythritol                       PETN
     
    
    Yields are very good, with one gram of pentaerythritol giving 2 grams
of PETN.
    
    To begin manufacture, the nitric acid is first checked. It must be 
fuming nitric acid (90%) and the acid must be completely water white. Any
traces of yellowish or reddish pink color, and the stuff must be purified
according to the directions below. The fuming nitric acid made according to
the directions in the nitric acid section is usually water white,
especially if the vacuum used was strong.
    
    To decolor nitric acid, 800 ml of the fuming nitric acid is poured into
a clean, dry 40 ounce beer bottle, and warmed up by setting the bottle in a
sink of hot water. When it is warm, a gram or so of urea is added to the
bottle and mixed in. Now dry air is blown through the acid. The most
convenient way to do this is to plug the top of the beer bottle with a
2-hole stopper. Through one of the holes, a section of glass tubing is run.
It should be long enough that it extends into the middle of the acid.

    To get air flow, apply a vacuum to the other hole. This will pull air
down through the glass tubing into the acid. Continue the air flow for a
couple minutes and the color will be gone. Watch out for acid splashing up
the tubing when the vacuum is removed.
    
    Once the acid is clean enough to use, making PETN with it is fairly
easy. First the 800 ml of nitric acid is poured into a large reaction
vessel made of glass, with a pouring lip. A beer pitcher is a natural
choice as the reaction vessel. The beer pitcher is nestled into a tub of
ice. The ice should be heavily salted as in the nitromannite process in
order to lower the temperature of the ice. The reaction temperature must be
kept below 5ø C (about 41ø F) so salted ice is required to do this cooling
job. As in the other processes, a pail of cold water should be close by to
dump the batch into if it should go out of control.
    
    Next, 200 grams of pentaerythritol is weighed out. It is then put onto
several clean plates and ground up into a fine powder by crushing the
crystals with the bottom of a drinking glass, or other handy object. Once
they are ground up, the temperature of the acid should be checked to make
sure it is below 5ø C. The temperature of salted ice can get down to 0ø F,
so the acid should cool quickly.
    
    When the temperature of the acid is low enough (stir the acid to get an
even temperature throughout the pitcher) pentaerythritol can be added to
the acid in small portions with good stirring. The temperature must be
closely watched during the addition to make sure it does not go above 5ø C.
Using the thermometer as the stirrer takes care of both problems at once.
The reaction gives off heat, so the pentaerythritol must be added fairly
slowly, especially if the acid was not very far below the 5ø C upper limit
to begin with. When the upper limit is neared during addition of
pentaerythritol, stop adding it, and continue stirring until the
temperature falls enough to allow putting more pentaerythritol into the
batch. 
    
    When all of the pentaerythritol (200 grams) has been added to the acid,
continue stirring it in the ice bath for another 15 or 20 minutes.
Acceptable colors for the reaction mixture are clear, white, and yellow. If
its color is red or pink, be careful as an eruption of the dreaded red gas
may be about to ensue. Be watchful for fumes bubbling from the batch.
    
    At the end of the 15 to 20 minute stir period, it is time to end the 
reaction and begin to collect the product. To do so, the first step is to
dump the batch into about a gallon and a half of ice water. Ice cubes
should be floating around in the water because when the batch is dumped
into the water, a good amount of heat will be given off. This is the heat
of dilution of the nitric acid. A plastic pail with a pour spout is a good
choice because after the batch is dumped into the ice water, it must be
filtered, a job requiring it to then be poured out of the pail into a
funnel.
    
    So the batch is dumped into a gallon and a half of ice water. It is a
good idea to stir the ice water as the batch is poured in to get the acid
dispersed throughout the water. As the batch is dumped into the water,
crystals of PETN will form. They will be white to yellow in color. They
should be allowed to sit until the ice cubes melt in the pail.
    
    Now it is time to filter out the crude crystals of PETN. A large coffee
filter (cafeteria coffee maker size) put into a large plastic funnel will
work well. Pour the batch into the funnel at whatever rate it can handle.
The acid water that filters through can be thrown away. The crystals in the
filter are rinsed by pouring cold water over them while still in the
funnel. About a quart of cold water, slowly poured, trying to reach all
crystals will do the job.
    
    Some crystals will still be clinging to the sides of the pail into 
which the batch was dumped, so a good idea is to flush them out of the pail
with some portions of water and add them to their brothers in the funnel.
The best time to do this is just before the one quart cold water rinse.
    
    Now the coffee filter is bundled into a ball and the water is squeezed
out of it. After the water is squeezed from the crude crystals the traces
of acid on the crystals are eliminated. To do this, a couple quarts of
distilled water are mixed with 20 grams of Arm & Hammer~ bicarb and then
the bicarb water is heated almost to boiling. This is poured into a clean
beer pitcher, and the crude PETN crystals are mixed in. They are kept in
contact with the bicarb water with some stirring for about an hour. It is
not required that there be constant stirring. Just enough to keep the
crystals floating around (once every 5 minutes or so will give good
results) is all that is needed. Then the crystals are filtered again,
rinsed over with some more distilled water (about a cup or two), and then
squeezed out. These crystals are then spread out on some wax paper and
allowed to dry before moving on to the final stage in the purification
scheme, recrystallization.
    
    Recrystallization must be done because of the traces of acid locked
inside the crystals from when they were originally formed when the batch
was dumped into the gallon and a half of ice water. All of the rinses have
not been able to get at the insides of the individual crystals. Also, the
yellowish crud which was tainting the pentaerythritol will be removed
during the same process, resulting in a fairly white PETN. The purer PETN
keeps better and stores more safely.
    
    The solvent used to recrystallize PETN from is acetone. A good quality
acetone can be purchased by the gallon at the local hardware store. Look in
the paint section. PETN's very soluble in acetone, so it is not the ideal
recrystallization solvent, but it is common and cheap. Besides, the
suggested method found in the scientific books can be modified to give
better results.
    
    To start the recrystallization, the crude crystals of PETN, amounting
to around a pound of product, are put into a glass container of about a
quart capacity. An equal weight (about 600 ml) of acetone is added to the
crystals of PETN, and they are mixed with a glass or wooden rod. Do not use
plastic as the acetone dissolves most plastics. A great deal of the PETN
will quickly dissolve into the acetone.
    
    Next, the acetone must be heated to dissolve the rest of the PETN.
Since acetone is very flammable, great care must be used during the heating
to avoid a fire. This operation should be done in a garage or other
structure that is open to wind blowing through it. Good ventilation is a
must! Smoking is an invitation to disaster! Direct heat must also not be
used to warm up the acetone. For example, setting the container holding the
acetone/PETN mixture on a hotplate is a no-no because the fumes of acetone
will come into contact with the burner and ignite Likewise, a double boiler
set-up is not going to work.
    
    The acetone can be heated by boiling a large pan of water in another
room, and carrying the boiling water to the garage and placing the
container into the hot water. As an alternative, a pressure cooker
half-filled with water can be set onto a hotplate upwind from the acetone,
and steam from the pressure cooker can be carried via hose to the acetone
solution, just as was shown in the drawing in the pentaerythritol section
of this chapter.
    
    When the acetone gets hot, the remainder of the PETN should dissolve
with some stirring. If it fails to all dissolve, add some more acetone. The
acetone should be heated to boiling (56ø C) for maximum dissolving power.
    
    Once all the PETN dissolves into the acetone, the frst crop of pure
PETN can be obtained. To get this first crop of crystals, just let the
acetone solution cool down, first by removing it from the heat, then by
packing the container in ice, and fnally by putting it in the freezer. As
the acetone gets colder, its ability to dissolve PETN decreases, and
crystals of PETN form.
    
    These crystals of PETN are filtered out either by using a vacuum system
as shown in the nitromannite section (best) or by pouring them through a
coffee filter and wringing them out. Plastic funnels must be avoided, of
course.
    
    The acetone which filters through still contains a very large amount of
PETN. It is returned to the quart-size glass container and half the acetone
is boiled off. This is best done by means of steam directed at the bottom
of the glass container, via a hose from a pressure cooker. Acetone boils
away quickly and easily.
    
    When half of the acetone has boiled away, the heat is removed, and once
again the acetone solution is cooled down. This results in a second crop of
crystals. They are filtered out, and the acetone which filters through is
returned to the glass container.
    
    This acetone which remains still contains a lot of PETN. The best way
to get the PETN out of the acetone which remains is to drip 190 proof grain
alcohol (vodka) or 91% isopropyl alcohol into the acetone with stirring. As
alcohol is added to acetone, its ability to dissolve PETN decreases. This
is because PETN doesn't dissolve well in alcohol, so adding it to the
acetone makes the solution lousy at dissolving PETN. This method is much
better than boiling away more acetone because that method leads to a final
crop of crystals that are dirty. When the solution is about half alcohol,
all the PETN should be out of solution in the form of crystals. This is
filtered out, and the acetone-alcohol mix is then tested to see if all the
PETN is out of it by adding some more alcohol to see if more crystals form.
If they do, alcohol is added until no more crystals form.
    
    If the PETN is coming out of solution in the form of an oil that sinks
to the bottom of the container, this indicates that it is pretty impure,
and that the alcohol was added too fast without enough stirring. All that
can be done in these cases is to put it in the freezer, and wait for it to
solidify into crystals.
    
    The PETN crystals are transferred to a large sheet of waxed paper,
spread out and allowed to dry. When the solvents have evaporated from them,
the PETN can be processed into plastique. My favorite PETN plastique is
made by mixing PETN with nitroglycerin. I like it because it is extremely
powerful (more powerful than C-4), easily detonated, and made from readily
available materials. Its lone drawback is that the ease of detonation also
means that rough handling could set it off. It must be treated with
respect.
    
    To make this plastique, 80 grams of PETN are put into a stainless steel
bowl, and then 20 grams (12ml) of nitroglycerin is poured over the
crystals. This mass is mixed with a rubber spatula until an even, uniform
plastic mass resembling PlayDough is made. This substance can be wrapped in
wax paper until used. A large f~recracker or cherry bomb will set it off.
Nitroglycol can be used in place of nitroglycerin to give a material which
works at low temperatures and which is somewhat harder to detonate.
    
    Another plastique can be made from PETN by mixing 98 grams of PETN with
12 grams of vaseline in the same manner as with the previous plastique.
This forms a plastique which is almost as powerful as C-4 and is able to
withstand rough treatment like C-4. A number 6 blasting cap is required to
set this plastique off. Of course, a sufficiently large piece of nitrogen
triiodide will also work. This plastique has the disadvantages of not
tolerating high temperatures well (the vaseline starts to melt and run
away) and also not being usable underwater since the plastique will
disperse into moving water
    
    Other plastiques can also be made from PETN, and they can be made to
very closely resemble C-4, but their manufacture requires the use of
materials which are not readily available to the typical consumer. Since
ordering these materials would leave a paper trail leading to the workshop,
it is not recommended to try to duplicate C-4. The very minimal advantages
are far outweighed by these other, more pressing considerations.

--------------------------------------------------------------------------
                                    RDX
--------------------------------------------------------------------------
    
    RDX, also called cyclonite or cyclotrimethylenetrinitramine, is the
last of our fine family of easily prepared, high power explosives.
    
    In many ways RDX bears a striking resemblance to PETN. It is about as
sensitive and powerful as PETN, and both are crystalline solids which can
be made into plastiques. Beyond this, the manufacturing processes for these
materials are quite similar as well. In both instances, a two-stage
manufacturing process is called for because the starting material for
making RDX may be difficult to obtain without causing suspicion.
    
    The starting material for making RDX is a substance called 
hexamethylenetetramine. It may also be sold under such names as methenamine
or urotropine. If it can be quickly purchased on a cash basis, a price of
about $15 per pound is reasonable. If, on the other hand, this substance
can't be so easily obtained, then once again, the route to follow is to
make the starting material from simpler, non-suspicion-arousing materials.
Luckily, hexamethylenetetramine is much quicker and easier to make than
pentaerythritol.
    
    There is another completely different method for making RDX, and it
does not make use of hexamethylenetetramine as the starting material.
However, that process requires acetic anhydride as a key ingredient. Acetic
anhydride is central to the manufacture of several drugs, for example
heroin and phenylacetone (the starting material for methamphetamine). For
this reason, acetic anhydride purchases, and that whole other method of RDX
production are to be avoided.
    
    One could conceivably produce the acetic anhydride from simpler
materials and then feed that material into RDX manufacture, but that is not
such a good idea. The reason for this is because acetic anhydride
manufacture centers around first making a substance called ketene (not
ketane as was written in a pretender publication). This ketene stuff is god
awfully nasty fearfully poisonous, and to make things worse, is a gas. Its
preparation is something which should only be attempted by a real pro with
proper equipment. Its preparation is nowhere near so simple as would be
inferred from reading those pretender publications. To get an idea of what
is really called for in ketene production, check Organic Syntheses,
collective volume 1, pages 330 to 334. Also, using the ketene to make
acetic anhydride is not so simple because an extremely effective
fractionating column, almost a yard long, is required to get a clean
product.
    
    The method given here is much better because it uses simple and cheap
ingredients that are easy to obtain. They are also pretty safe as far as
chemicals go, with the exception of the fuming nitric acid. Also, these
reactions are fairly easy, and result in mixtures that are pretty easily
purified.
    
    A well-ventilated garage is a good site for making the 
hexamethylenetetramine. The neighbors should not pay this process so much
attention as the pentaerythritol process because the odor here is less
intense and much shorter-lived. No special equipment is needed for this
reaction either. All that is required is an electric hotplate with variable
heat control, and a large enamelled dish to do the reaction in.
    
    This large enamelled dish should be at least a gallon or so in 
capacity, and built to be able to withstand some heating and rough
treatment. A very good choice is one of those roasting pans built to hold
turkeys or hams. Look for one that is square or rectangular in shape so
that the liquid may be poured out of the pan at the corner. The enamel can
be substituted for with teflon coating.
    
    To make hexamethylenetetramine, 2000 grams (1850 ml) of 37%
formaldehyde solution is poured into the enamelled dish. Then to this is
added 1100 grams (1200 ml) of ammonium hydroxide solution. As was mentioned
before, this material is just ammonia dissolved in water, and may be sold
under such monikers as strong ammonia solution 27%, or 58% NH4OH or ammonia
water 26 degree balme. The ammonia solution should either be cooled down in
the freezer before use, or have 250 grams of ice added to it.
    
    The ammonia is added slowly to the formaldehyde with good stirring. A
fair amount of heat is given off in the reaction, and the reek of
formaldehyde and ammonia will get intense for a while until all the ammonia
has been added. Then all the formaldehyde will be tied up, and only a weak
smell of ammonia will remain. Stir some more to be certain that an even
solution has been obtained.
    
    The solution in the pan or dish contains about a pound and a quarter of
product dissolved in a bunch of water. The task now is to obtain the
hexamethylenetetramine, which is a crystalline solid, from the water. To do
this, first the dish is placed on the hotplate, then heat is applied to it
to bring it to a slow boil. As the water boils away, portions of about 15
ml of the ammonia solution are added to it every ten minutes or so. This is
to ensure that enough ammonia is present to keep any formaldehyde which may
be floating around unreacted, tied up.
    
    When about half of the solution is boiled away, the heat should be
removed from the pan and the solution is allowed to cool down to the point
where it is about as hot as hot tap water. Then it is filtered through a
coffee filter placed inside a plastic funnel. This is to remove any gummy
material which may have been formed from the formaldehyde. This gummy stuff
will quickly plug the filter, so be prepared to change the filter several
times.
    
    The liquid which filters through still contains the product. It is 
returned to the pan. Its volume should be a little over 2000 ml. It is once
again boiled away until its volume is around 800 ml (1/3 or so of the
previous volume). Now the first crop of product can be obtained. Remove the
pan from the heat and allow it to cool, then cool it further either by
packing the pan in ice or putting it in the freezer. As it cools, a large
mass of crystals will appear.
    
    These crystals are then filtered out by filtering them through the 
vacuum filtering apparatus shown in the nitromannite chapter. Feel free to
pack them down a little with a spoon to help squeeze the liquid out of
them. Then the crystals are dumped out onto wax paper. The liquid should go
into a separate jug for temporary storage until all the crystals are
cleaned out of the pan. A rubber spatula will be very handy for scraping
the cling-one off the walls of the pan.
    
    When the first crop has been collected, the liquid is returned to the
pan. Then the crystals of product are rinsed off. To do this, they are
packed back into the filtering funnel, and rinsed off with 190 proof grain
alcohol. A few rinses should remove the smell of ammonia from them. Then
they should be spread out on fresh wax paper until they are dry. They
should have no smell. They should also be clear or white in color.
    
    The liquid which has been returned to the pan still contains a lot of
product. To get it, first pour the liquid into a glass beer pitcher or
similar container. Then about 10 grams of powdered activated charcoal is
added to the liquid. If the lab brand of charcoal called Norite is
available, this is best. Otherwise, the various other types of activated
charcoal will work so long as they are powdered up before use.
    
    This activated charcoal will take up the yellowish color from the 
solution. First stir it in for a few minutes. Then set up the vacuum
filtration system again, with double layers of filter paper. Pour the
solution through it. A clear solution should result. If it is still black,
all the charcoal isn't out of it. Wash up the system, change the filters,
and filter some more. If it is still yellowish, add some more activated
charcoal and continue.
    
    The clear solution can now be returned to the original dish, and heat
reapplied to it. The goal here is to evaporate the liquid to dryness and
collect the crystals which are left when the water is gone. Heat it
reasonably strongly at first, then steadily back off on the heat as the
volume of liquid goes down. One does not want to burn the crystals.
Finally, end up with just a warm setting, and drive off the last of the
water. Then scrape out the crystals of product from the pan. The total
yield of hexamethylenetetramine should add up to around 560 grams.
    
    All the hexamethylenetetramine should be spread out onto wax paper
sheets and allowed to dry. When it is thoroughly dry, it is ready to be
turned into RDX. Very humid weather may cause the crystals to soak up water
from the air and melt, so beware of spreading them out to melt instead of
dry.
    
                             PREPARATION OF RDX
    
    Once the hexamethylenetetramine is dry, one is ready to proceed to turn
it into RDX. This reaction is a good deal more touchy than the ones covered
in the earlier sections of this book. If directions are not followed
concerning acid strengths, temperatures, and reaction times and conditions,
the dreaded red gas is likely to appear, or at least the yield of product
will be ruined. Have no fear, however; all the little things which are
likely to go wrong will be covered, along with the several right ways to do
this reaction. So long as one stays on the right path, and off the road
leading to disaster, all will be well.
    
    RDX, unlike the other explosives covered in this book, is not a nitric
ester. This means that the equilibrium equation presented back in the early
part of the book can be ignored for this explosive. Instead, the factors
most influencing yields in this reaction are kinetic. This means that there
are several side reactions which occur at the same time as the desired
reaction, and getting a good yield depends upon suppressing these side
reactions, and encouraging the desired reaction.
    
    One encourages and suppresses reactions by carefully controlling the
time of reaction, the temperature(s) at which it is run, and the
concentration of the ingredients, among other ways. Just how this strategy
works for RDX production must now be explained.
    
    First, we have the desired reaction, producing RDX from 
hexamethylenetetramine and nitric acid:
    
    A very important competing reaction is the breakdown of the 
hexamethylenetetramine by water into its hydrolysis products, formaldehyde
and ammonia:
    
                             Acid
           C6H12N4 + 6 H2O ==========> 6 Formaldehyde + 4 Ammonia
                            Catalyst

    The water finds its way into the mixture because water is the diluent
for nitric acid, and even the 90% fuming acid obtained commercially is
going to have 10% water as the dilutent. The nitric acid made as directed
in the nitric acid section will have next to no water in it, so long as the
saltpeter was dry, and the glassware was dry. This is anhydrous nitric
acid, and so avoids this side reaction, so long as the
hexamethylenetetramine is dry, and the glassware is dry.
    
    This side reaction is also greatly slowed down if the batch is made at
a low temperature. The cold temperature slows down the unwanted reaction
quite a bit more than the desired reaction producing RDX. By doing the
reaction at -20ø C (0ø F), an additional one sixth of product is obtained.
This side reaction is further curtailed if the batch is not allowed to sit
around any longer than is absolutely necessary before pouring it into water
and ending the reaction. The best waiting period after the end of adding
the hexamethylenetetramine to nitric acid, before dumping the batch into
water, is about 15 minutes. This is about the length of time required for
the last of the hexamethylenetetramine to dissolve into the nitric acid,
with slow stirring.
    
    Another side reaction involves nitric acid adding to the 
hexamethylenetetramine to form a salt. This side reaction is not so easily
controlled as the preceding hydrolysis reaction. It just has to be lived
with, and is the reason that the best yield one can get is around 75% of
the theoretical yield.
    
    With a good grounding in the ins and outs of this reaction, let's go on
to see how these principles are put into practice Using the commercially
available fuming nitric acid of 90% strength (density 1.51), the same
set-up is used as for the previous reactions. A beer pitcher makes a good
reaction vessel, and it should be nestled in a tub of ice, with a 5 gallon
pail of water nearby to dump the batch into in case it goes out of control
and begins spouting red gas. One must be especially on guard when doing
this reaction, because the onset of the dreaded red gas can be the result
    
    Then into the pitcher, 770 ml of the fuming nitric acid is placed. This
acid should be cooled down beforehand by storing the acid in the freezer.
Then 100 grams of hexamethylenetetramine is weighed out, and it is added to
the acid slowly, in small portions, with slow stirring. A good tool to do
this stirring is a section of glass rod, bent at a right angle about an
inch before its end. This stirrer will look like an overly long hockey
stick, and works like an agitator when slowly twirled between the fingers.
Overly fast stirring is to be avoided, because this contributes to an
overly fast reaction which may get out of control and start to fume. The
temperature of the mixture should under no circumstances be allowed to go
above 20ø C, and it would be best if it were held well below that
temperature. Since one is starting with acid from the freezer, where its
temperature should be around -20ø C, this should be no hard task The amount
of time required to add all the hexamethylenetetramine to the acid is going
to be about half an hour.
    
    Then the slow stirring is continued, while a close watch is kept on the
crystals of hexamethylenetetramine in the acid. When the last of them has
dissolved, wait 5 minutes, then pour the whole batch into a gallon of cold
water. The length of time between the end of adding the
hexamethylenetetramine, and the point when it has all dissolved, is around
15 minutes. As was stated earlier, it is bad idea to let the batch sit
around any longer than the recommended period. Once it has all dissolved,
wait a few minutes, then pour it into the gallon of water.
    
    When the batch is poured into water, crude crystals of RDX will form.
They must next be filtered out, so for this reason, it is wise to choose a
water container which will easily pour into a funnel for the filtering
process. Three beer pitchers, each holding an equal volume of cold water
ready to accept 1/3 of the batch, is a good arrangement.
    
    Next the crude crystals of RDX are filtered out of the water by using
the vacuum filtration set-up described in the nitromannite chapter. The
best filter to place in the funnel is a piece of glass wool. This material
can be found at any place selling aquarium supplies. It is called angel's
hair. A piece of it is pushed down into place over the filter holes, and
then wetted into place with water before beginning the filtration. This can
be used for the nitromannite filtration as well.
    
    Unlike the earlier explosives, the crude RDX can be kept and used as
is, once it has been well washed down with water while in the funnel. Some
litmus paper comes in handy to tell when the last of the acid is being
rinsed from the RDX. If a drop or two of the rinse water doesn't turn blue
litmus paper red, then the acid is rinsed off the crystals. If this crude
RDX is stored for any length of time, it should be stored underwater.
    
    This crude RDX can be purified very well by recrystallizing it from
acetone. For every gram of RDX, 10 grams of acetone should be used. Ten
grams of acetone is 12.7 ml. The recrystallization is done like the
previous recrystallization from acetone. The acetone-RDX mixture is heated
by setting the container in hot water, and the mixture is stirred until the
RDX dissolves. Then the solution is cooled down by packing the container in
ice. A large amount of really nice looking RDX crystals form. They are
filtered out, and the acetone solution is then boiled down to half its
previous volume. Upon cooling, another crop of crystals form. Finally,
water is added to the acetone solution to get the last of the RDX to
precipitate out. This RDX has no acid in it, and stores really well.
    
    The yield of RDX by this method is about 60%, which translates to about
95 grams of RDX per batch. The yield can be increased by a few grams if
double the stated amount of nitric acid is used, but this is bad strategy
considering the cost of fuming nitric acid. A much better strategy for
increasing yields is to use the anhydrous fuming nitric acid that can be
made according to the directions given in the nitric acid section Use of
this material gives a yield of around 110 grams per batch.
    
    To use the anhydrous nitric acid, one sets out pretty much as in the
previous example, except that the ice must be heavily salted. This is
because the reaction must be done at a much lower temperature. A
temperature of around -20ø C (0ø F) is needed to use the anhydrous nitric
acid. If the temperature of the batch goes much above this, the familiar
penalty of the dreaded red gas is promptly dished out. Dry ice soaked down
with rubbing alcohol or acetone would do a great job of keeping the batch
cold, if the dry ice is easily available in your workshop. Naturally, the
nitric acid is taken straight from the freezer, and not allowed to warm up.
    
    The same quantities of ingredients are used in this method as in the
previous one. A big difference, however, comes in the length of time
required to add the hexamethylenetetramine to the acid. This time period
should be roughly tripled to 90 minutes, so that the heat given off from
the reaction doesn't get too intense. Then the stirring is continued slowly
until all of the crystals are dissolved. After waiting a further 5 minutes,
the batch is dumped into water as before and the previous instructions can
be followed the rest of the way.
    
    When contemplating RDX production, one may be tempted to try to use the
cheaper 70% strength nitric acid (density 1.42) instead of fuming nitric
acid. This just does not work. At the usual temperatures, no reaction
results, and at higher temperatures, red gas is made. There is an
alternative method starting with 70% nitric acid, which is then watered
down further, and hexamethylenetetramine is added to this. The resulting
product is the nitrate salt which was briefly mentioned earlier as an
unavoidable side reaction. This salt can then be isolated and added to
fuming nitric acid to give RDX.
    
    This route is not so good as the ones given above because more steps
are involved, and the process is wasteful of hexamethylenetetramine. Also,
the total yields are lower. Its only good point is that it uses roughly
half as much fuming nitric acid. Since high strength nitric acid is easier
to make than hexamethylenetetramine, the scales tip heavily towards the
processes given here.
    
    A very nice plastique can be made from RDX by mixing it with vaseline
in the same proportions as for PETN. It is a little more diffcult to
detonate than the PETN plastique. A number 8 blasting cap is called for in
this case.
    
    If the material is being used straight, it can be set off with a 
firecracker which has had some nitro soaked into the wrapping paper. To get
maximum firepower out of the charge, it must be compacted to a higher
density than the fluffy crystalline state. The only common solvent which
works really well for melting the crystals into a rock is benzene. Good
luck in finding that one at the hardware store! Acetone may do an
acceptable job. Be sure to let the rerocked RDX set around until it no
longer smells like acetone. The warmer the acetone, the better it will work
for this purpose. 
    
--------------------------------------------------------------------------
                             DETONATION SYSTEMS
--------------------------------------------------------------------------
    
    Without a means of detonating an explosive, the products described in
this book are nothing more than dangerous curiosity pieces. This often
overlooked facet of explosive use generally is the point that trips up
newcomers to the field. To procure or make explosive substances is a pretty
straightforward operation. Rigging a detonation system, on the other hand,
can seem mysterious by comparison. For this reason, conventional and
~mprov~sed detonators must be covered. Since all explosives in this book
are detonatable by these methods, reference to this section can be made
throughout the book.

    All explosives can be set off by either a sufficiently strong 
electrical shock, or by being struck a hard enough blow. The exact amount
of power required by either of these methods depends upon the explosive in
question. For instance, static electricity from walking across a carpet can
be enough to set off guncotton, while TNT is notoriously hard to set off
with a shock. The other explosives fall somewhere in between these two
extremes. Similarly, TNT requires a heavy whack with a sledge hammer to set
off, while nitro or gunpowder can be set off with a moderate blow from a
hammer or similar metal object.

    With this superficial intro to the topic behind us, let's move on to 
applying these prin†ples to the practical task of detonating a Home
Workshop Explosive. The simplest, safest and most reliable route to follow
is if one has access to blasting caps. These little wonders are made
specifically to do the job in question, and their performance is hard to
top. So long as one uses the required size or larger, no problems will be
encountered. The body of the blasting cap should be inserted into the
explosive. With a large pile, a spot near the bottom is preferred.
    
    If, on the other hand, one does not have blasting caps, then 
improvisation can lead to good results. For example, a good firecracker is
suffficient to set off pure nitro. Delay mechanisms can be rigged by pla†ng
the firecracker fuse near the filter end of a cigarette, and then allowing
the cigarette to burn down to the fuse. This will give a few minutes delay.
Since many firecrackers are duds, it would be wise to rig several backups.
    
    A #1 blasting cap equivalent can be improvised by putting into use the
detonation train principle. This prin†ple is often used to set off
difficultly exploded substances like ammonium nitrate. Here it will be put
into practice simply by dipping a good sized firecracker into nitro. The
paper wrapping will absorb the nitro, and then the nitro will go off with
the explosion of the firecracker, adding its punch to the blast. These
nitro crackers are great fun by themselves. If you are bored by
commercially available fireworks, they are highly recommended. The only
pitfall in their manufacture is if the firecracker is wrapped in a sheet of
waxy or glossy paper. Then this should be removed so that the nitro can
soak into the coarser paper beneath.
    
    Larger blasting caps can be improvised along the same lines by allowing
the firecracker to set off a larger amount of nitro, or by packing a
nitro-soaked firecracker into some gelatin, and allowing the ensuing
detonation train to do its work.
    
    Alternatively, a couple of good books list directions for making 
improvised blasting caps that more closely resemble the commercial product.
The best of the lot are The Poor Man's James Bond and Kitchen Improvised
Blasting Caps. Have fun!
    
    The electric shock method of detonation is one that is often ignored,
but one that can prove very useful for bagging elusive game. One of my
favorite electric detonators is a spark plug. The newer cars with the
electronic ignition send a lot more juice to the spark plugs than the older
models. This spark, particularly from the hotter spark plugs, will suffice
to set off nitro and usually nitroglycol. The possibilities for this method
are bounded only by the imagination.
    
    In putting this detonation method into practice, a clean spark plug
should be used so that the explosive is not going to be fouled up with
carbon deposits. To test out the method, a couple drops can be deposited on
the electrode of the spark plug, and after attaching the plug to the
distributor, the engine can be cranked.
    
    Gelatin is a tricky substance to detonate by this method. Too weak a
shock will just set it on fire with no explosion likely to result.
Experimentation is the only way to tell if the particular model in question
produces enough shock to bring on detonation.
    
    Other sources of electric shock provide intriguing possibilities along
similar lines. Working out the details are bound to provide hours of pure
enjoyment for the serious experimenter.
    
    A final method of detonation that is supremely simple and suitable for
rigging booby traps makes use of a curious substance called nitrogen
triiodide. This very easily made substance has the strange property of
being pretty stable when wet, and yet wildly explosive when dried down to
the crystal form. The smallest touch will set it off in this dry state. It
explodes powerfully enough to set off nitro, all gelatins, and if used
liberally, even dynamite.
    
    Nitrogen triiodide is often made by high school chemistry teachers as a
class demonstration to impress the students. Considering the sorry state of
secondary education in this country, you can get an idea of just how easy
this stuff is to make. If you are not brain damaged, you will have no
problems.
    
    To make nitrogen triiodide (NI3) one first gets iodine crystals. These
can be ordered without suspicion from any of the mail order supply outfits,
or ordered from a pharmacy. If one is forced to deal with a pharmacy, these
terminally snoopy people may inquire what they are needed for. Good answers
to such nosey questions are that one is experimenting with treatments for
fishtank infections, or that you are stocking up on it so iodine tincture
can be made in your bunker after they drop the big ones.
    
    Iodine crystals (I2) are black and heavy. A quarter pound should cost
around $20. If much more than this is charged, you are being ripped off.
The crystals should be spread out on a plate, and ground finely using the
bottom of a small glass. It is very important that a fine grind is
obtained, or the product is likely to go off by itself during the drying
process.
    
    The other required ingredient is ammonium hydroxide. This is just a
strong solution of ammonia in water, and it can also be obtained with ease
from mail order suppliers, or a pharmacy. The product one needs here is
called ammonium hydroxide (NH4OH). The strength level should be about 58%
NH4OH or 28% NH3 or 26 degrees balme. All these mean the same thing; just
one of the ways that chemists have to confuse the general public. Cost: no
more than $10 per pint.
    
    A product that will just not do is the ammonia which can be picked up
in the grocery store. This stuff is just 3% ammonia, and is loaded with
soap to boot. It can't be made to work, either, by distilling the ammonia
out of it. The soap in it begins foaming like crazy as it is heated up,
making this operation futile.
    
    With the supplies on hand and ready, NI3 is made just by mixing one
volume of iodine crystals with about ten volumes of NH4OH. A glass
measuring cup is perfect for this reaction. They should be allowed to react
for ten or 15 minutes with occasional stirring. Beware of breathing in
ammonia fumes from the ammonium hydroxide during this process. Good
ventilation is a must.
    
    Then a drip type coffee filter is placed in a funnel or other suitable
holder. The funnel is then placed in the mouth of a beer pitcher, or other
suitable container to catch the ammonia water which will filter through.
    
    Then the batch is stirred up well to suspend all the crystals in the 
liquid, and quickly poured into the filter. Any crystals sticking to the
cup can be rinsed out with some more ammonium hydroxide, or scraped out
with a rubber spatula.
    
    The crystals of NI3, which are black, should be lightly squeezed in the
filter to free them from excess solvent. Then the paste-like product should
be loaded, while still wet and stinking hke ammonia, into the corner of a
zip lock baggie. Here they may be stored for a while in the refrigerator to
await further experimentation.
    
    To get the feel of this substance, a few lumps should be taken out of
the baggie and spread out to dry on a tabletop or cement floor. When it ~s
dry, the smallest touch with any stick or similar probe will set it off.
The blast which results can be really surprising. Another good line of
experimentation is to stretch the stuff out in a long thin line and see how
thin it can be spread and still get the whole line to blow off when any
part of it is touched. Also, you should practice to see how long it takes
to dry out larger lumps of the material.
    
    With this experimentation successfully finished, one can move on to the
nitty gritty of rigging a booby trap surprise. A lump of NI3 a tattle
bigger than a pea will set off nitro with ease. A lump about twice that
size placed against the outside of a bottle containing nitro will be sure
of setting it off counting the shielding effect of the glass. A somewhat
larger lump will detonate gelatin, and a little more will do the job with
more difficultly exploded substances.
    
    Since the explosive container is likely to arouse suspicion, it may
often be good practice to run a thin line of the NI3 from an area that the
target will step on to the explosive stash. So long as the blast occurs
close enough to the target, all will be well.
    
    On the other hand, in many cases it is better to rely on the curiousity
of the mark, and just set the lump against the bottle or baggie of
explosive. When he comes to examine it, the small nudge will set off the
NI3 and result in detonation. Here ingenious disguises of the explosive
booby trap can pay handsome dividends.
    
    As should be obvious from the preceding sections, the NI3 must be put
into place while still wet, and have time to dry in place before it becomes
activated for use. This is the reason why attention must be paid to drying
times for various size lumps of NI3. The time will vary with temperature
and humidity because water is the main ingredient to evaporate off from the
NI3. NI3 can be carried around safely in a baggie so long as it is still
wet from being made. Once it dries, it is set to explode!
    
    WARNING! The filter used in this process will itself become explosive
when it dries because of the small pieces of NI3 caught in it It should
either be flushed down the toilet immediately, or saved and treated like
the dangerous explosive it is. 
    
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                             APPENDIX 1: SAFETY
--------------------------------------------------------------------------
    
    The acids used in the manufacture of these explosive compounds are
dangerous and caustic materials, so a small bit of preaching is called for
here to help prevent needless accidents from befalling careless
experimenters. We all like to imagine that nothing bad can happen to us,
but all it takes is a moment of inattention to result in a lifetime of
misery.
    
    The most crucial area of the body to protect when working with
chemicals is the eyes. In comparison to the eyes, damage done to other
parts of the body is minor and short-lived. For this reason, the sensible
experimenter will wear clear plastic goggles. The best goggles are sold in
college bookstores for use by chemistry students in their lab courses.
These are cheap, easily bought and perfect for the job. An OK alternative
is the large plastic eyeglasses with side shielding often used with
chainsaws.
    
    Eye protection should be worn whenever acids are being measured out,
and while batches are being made. Not until the acids are washed away by
flushing the product with water can the goggles be removed.
    
    Some of the reactions in this book call for the use of chemicals like
formaldehyde or acetaldehyde or ammonia. The same rules must be followed
for these materials. They will cause damage if splashed into the eyes.
Beyond that, their fumes can cause similar damage. Good ventilation must be
provided for their use.
    
    The acids used to make explosives can also cause serious skin burns if
they are allowed to sit on the skin for more than a minute or so. Vigilance
is the best protection against this hazard, along with a willingness to
rinse one's hands regularly when working with the acids. Rubber gloves can
also be worn to protect the skin. Surgical gloves are the best because they
leave the experimenter with a degree of nimbleness in the fingers. Next
best are the "living gloves" popular with dishwashers fearful of "dishpan
hands."
    
    When fuming acids are being used, gloves are a must. This is because
the acid fumes will settle on exposed skin and begin to burn. The arms
should be similarly protected in these cases by wearing long-sleeved
shirts. The importance of good ventilation, and of keeping upwind of the
air flow is obvious here.
    
    If the unthinkable should happen, and large volumes of acids are
splashed upon your body, time is of the essence. You must run directly to
the shower, jump in with all your clothes on, and flood the affected area
with cool or lukewarm water while peeling your clothes off. A good rinsing
for 10 minutes or so is called for, and can be followed with a rinse of
bicarb solution.
    
    At the end of a day's work, or just while on break, you can bet there
are droplets of acid on your skin you didn't notice. These can be wiped out
with a leisurely shower. The clothes should go directly to the wash, or
they are going to have holes eaten in them.
    
    Glassware coated with residues of acids or explosives are a very real,
but often overlooked, source of danger. All utensils used in these
processes should be thoroughly rinsed with water as soon as possible after
use. When the items in question have been in contact with substances that
don't dissolve in water, they should be further rinsed down with rubbing
alcohol or acetone until clean. When explosives are in solution, they are
usually very hard to detonate. We can then consider these rinse materials
safe to flush away. They may reprecipitate in the lines but a good follow
up with bleach should destroy most of them.
    
    Major spills of explosives should never happen to the careful and
conscientious manufacturer. Minor spills can be dealt with by following
some general guidelines. If it was batch material before drowmng in water,
dilute it with some water, then soak it up in a bunch of Kleenex. Follow
this with some alcohol or acetone, depending upon what solvent the
explosive dissolves in, and mop it up with some more Kleenex.
    
    If it is more refined material, dilution with alcohol or acetone and
mopping up with Kleenex is the first step. Then for the solid explosives,
rub in some vaseline on the area, and continue wiping it up. If you don't
get it all, at least it will be made more shock resistant. In all cases,
the dilution and mop up should be continued until it looks like all of the
explosive is gone The Kleenexes can then either be flushed away, or
carefully bumed outside. An explosion may result from this latter course,
so be prepared for the fireworks.
    
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                APPENDIX II: ASPIRATORS AND WATER BED PUMPS
--------------------------------------------------------------------------
    
    The use of vacuum to filter liquids and to distill materials at more
reasonable temperatures is central to many of the processes in this book.
With the great importance assumed by a reliable source of vacuum for these
operations, it would well serve any explosive manufacturer to become
familiar with convenient sources of vacuum, and the hidden problems they
pose.
    
    The best source of vacuum for the lab operations described in this book
is the aspirator, also called the water pump. Its bastard cousin, the water
bed drain pump works the same way, but produces a weaker vacuum due to
inferior engineering and construction. Let's take a quick look at these two
devices to see how their performance can be optimized.
    
    These devices work by running a cold stream of water through them. The
rush of water down the body of the aspirator produces a vacuum in the side
arm portion of the device. An automotive vacuum hose of the appropriate
size can be attached to the side arm and led to the glassware needing
vacuum. This hose should not be more than 3 feet long for highest strength
vacuum.
    
    Most aspirators and water bed pumps have a threaded section at their
top to allow them to be screwed onto the end of matching threaded faucets.
If this is not convenient or possible, then a section of hose or plastic
tubing can be fitted to connect the aspirator and faucet. A couple of hose
clamps to keep everything together are called for when doing this. The
water exit of the aspirator must also have hose connected to it to lead to
the drain. This cuts down on splashing from the stream of water, and also
results in a better vacuum. The flow of water out of the aspirator should
be unimpeded, and the exit hose should be of larger diameter than the input
feed line.
    
    Water for the aspirator should be as cold as possible for best results.
This is because the vapor pressure of water at the particular temperature
of water being used is the best possible vacuum from an aspirator. Since
cold water has a lower vapor pressure, the best vacuum will come with cold
water.
    
    A most annoying habit that these type of vacuum devices have is their
propensity to puke water back into their vacuum lines. The root cause of
this behavior is usually traced back to variations in water pressure or
flow rate. Things like a toilet flushing or a well pump kicking on and off
are typical culprits.
    
    The way this back puking works is that a pretty good vacuum will get
built up in a piece of glassware, just about equal to the maximum the
aspirator can deliver. Then the water flow slows down and the amount of
vacuum being produced by the aspirator goes down. The next thing that
happens is that the stronger vacuum in the glassware proceeds to pull water
down the vacuum line from the aspirator to the glassware. When the product
one wants is anhydrous nitric acid or glycerin or ethylene glycol, this is
a disaster. Good aspirators have valves to make this a less routine
occurrence.
    
    There are a few steps one can take to make this puking a very rare
happening. First of all, city water supplies tend to have the pressure
variations ironed out of them. No well pumps kicking on and off. This is
the ideal water system for aspirators. Just turn the water on strong at the
start and leave it there.
    
    Secondly, the aspirator should be at a lower level than the glassware
it serves. Six inches to a foot is a convenient level. This positioning of
the aspirator forces any water that pukes back into the line to crawl
uphill to get to the glassware. The delay won here is often enough to get
the situation to straighten itself out.
    
    Finally, watchfulness can catch a problem before it develops into a
disaster. Be aware of the problem' and it cannot catch you by surprise.
    
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        BOILING POINTS UNDER VACUUM FOR ETHYLENE GLYCOL AND GLYCERIN
--------------------------------------------------------------------------
    
    Since the best way to get a great quality ethylene glycol or glycerin
from crude commercial mixtures is to vacuum distill the mixture to get the
pure product, a table of boiling points for these two substances at various
strengths of vacuum will be given to make it simpler to spot the product
fraction. A fair amount of practice at vacuum distillation is generally
needed before one becomes a pro at it. See a college level organic
chemistry lab text for a detailed discussion of vacuum distillation. Both
ethylene glycol and glycerin are good substances to practice with because
they are pretty safe materials.
    
Perfect vacuum = 0 mmHg Normal Pressure = 760 mmHg

-------------------------------------------------
    mmHg
(boiling points)   Ethylene Glycol      Glycerin
-------------------------------------------------
      1             53ø C               125ø C
     10             92ø C               167ø C
     40            120ø C               198ø C
    100            141ø C               220ø C
    400            178ø C               263ø C
    760            197ø C               290ø C
-------------------------------------------------

    A well working aspirator running on cold water will give a vacuum of
from 10 to 25 mmHg. Of course, the temperature at which the product will
boil in any particular experiment depends upon the strength of the vacuum
being produced by the aspirator on the given occasion. This can typically
vary by about 10 mmHg. Very bad vacuums should be dealt with by looking for
leaks at the ground glass joints (always use stopcock grease on these
joints!). Other culprits can be collapsed vacuum hoses or ill-fitting
rubber, glass or teflon stoppers. Corks can never be used because they
always leak. Sometimes, the aspirator will be installed upside down. The
threaded end should always be up. 
    
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