PDGN (Propylene Glycol Di-Nitrate)

PDGN is an explosive similar to nitroglycerine. Contrary to popular beleif, nitro really isn't that sensitive, when compared to other explosives that we make and use every day. Anyway, I haven't made PDGN yet, but hopefully will get around to it sometime this weekend. The following is people's comments about PDGN from the explosives and weapon forum:

It really seems that this explosive, propylene glycol dinitrate, should be used more. Propylene
glycol is pretty cheap, it can be had for low cost from the right type of antifreeze with only
a few percentage of impurities like dyes and water that could likely be removed. Anyway, my
experiences of making PGDN were with PG that was from a chem supplier which still was quite
cheap. Also it sounds as if it is easily detonable but still quite safe to handle based on mega's
information. Also, I've noticed no headache from it although it does seem somewhat volatile as
it has a nice sweet smell to it. Anyway onto my experiences with synthing it.

The first time I tried synthesizing it I was using concentrated nitric acid(around 95%) and
98% sulfuric acid. I don't remember the ratios but have them written somewhere. Anyway,
all was going well and the temperature wasn't rising much at all so I decided to increase the
rate of PG addition to the acids, all was going well but as I was adding some PG I gave the
syringe a bit too hard of a squeeze which put in more PG than I had meant to. The runaway
began really rapidly, took only a few seconds for it to start spewing NO2. Worse than that was
that the mixture ignited result in a jet of fire shooting something between 1ft and 2ft out of the
flask. I suppose this might be the result of PGDN rising upwards and staying at the surface
instead of sinking the way NG does.

The next attempt was with an NH4NO3 and H2SO4 mixture:
29g NH4NO3
75g 98% H2SO4
9g propylene glycol
I was more cautious on the addition and kept the temp under 10C until all the PG was added. I
THen removed fro mthe ice bath and allowed the temperature to rise to just over 15C in around
twelve minutes. I then dumped in 500ml of ice cold water, decanted, and then added bicarbonate
solution. Judginf by the volume of PGDN obtained and the density mega gives I got a yield of a bit
over 14g which is around 70% theoretical. I haven't gotten around to testing it though.

USER NAME:pdb
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Quote:
"I suppose this might be the result of PGDN rising upwards and staying at the surface"

You are wrong. NG does stay at the surface of the acides, but of course sinks in water.

That you got an oxydizing reaction with NOx emission by adding too much PG at a time is not surprising. However, that the PGDN ignited is far more amazing. I've never heard of such a thing with NG, which in case of uncontrolled temperature rise would either decompose and/or detonate, but not ignite.

GreenCoat
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Quote:
Originally posted by Bert
"I just read the ingredients on the bottle of generic aspirin in my medicine cabinet... It contains both polyethylene glycol and propylene glycol.

I've read several variations of the "picric acid from aspirin" recipe, I believe there's one on this site somewhere as well. Could anyone comment on the likely outcome of using salicylic acid extracted with alcohol from such a source? The high temperature of the reaction carried out with contaminants such as PG and PEG present would seem a recipe for disaster.

Of course, I have no idea what their percentages in the medication are- Or how soluble in which alcohols they may be. However, most alcohols are not perfectly anhydrous, so it seems likely they would be extracted regardless." I don't think you would have anything to worry about if you washed your acetyl salicylic acid (ASA) with water before going on to the next step. Both PE and PEG are alcohol and water soluble. If I didn't already have access to both phenol and salicylic acid, I would perform an alcohol extraction/filtration to obtain mostly pure ASA, free from fillers and binders. Then obtain sodium acetate and salicylate by boiling a suspension of ASA in NaOH solution. Precipitate salicylic acid with HCl. I know, I know: it's a lot of work. But garbage in, garbage out. This is how it should be done. Any PE or PEG, or other water soluble impurities for that matter, would remain in solution. From reading tablet-forming patents, PE and PEG are added in no more than 2-4% amounts to facilitate blending.

USER NAME: freaky_frank
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I lately made EGDN, normally I make NG, and this stuff yields much better than NG, NG gives me from 20ml glycerine 20ml NG, and EGDN gave me from 20ml EG 27ml EGDN.....
And PGDN gave me from 20ml only a crappy 13ml...

USER NAME: The_Rsert
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Yesterday evening, I made some PGDN (propylene glycol dinitrate).
I used about 50ml (yes, my scale is broken, so I have to estimate) ammonium nitrate (coarse powder), 100ml H2SO4 and 20ml propylene glycol. The nitration takes 20 min. I kept the temperatures easily between 10°C and 15°C with a ice bath. After the addition I waited 30min. I neutralised and washed the final water insoluble liquid (PGDN)
Yield: Approx. 26ml pure dry sweet smelling PGDN with a slightly yellow coloured touch.
I got no headache ,

So, what can I do with this stuff? Any ideas?

EDIT: I've just ignited 20ml in a delved test tube with <1g AP in a drinkiung straw.
The detonation was many times stroner than a 100g ANNM det..
Some little stones shot up to 100m away (I heard the impacts of the stones)
I got a min. 45cm wide/20cm deep crater!
If I can, I will make some pics of the crater tommorow.
PGDN is my new favourite HE!
__________________

USER NAME: simply RED
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A friend of mine made NG, EGDN and PGDN by the following procedure:
60ml H2SO4(96-99%); 40ml HNO3 59-62% and 15 ml the alcohol.
Cooled during nitration of course.
He got about 15 ml yield every time. Then we mix the NG, EGDN and PGDN (45ml) and detonated it. Quite good blast it was for its size.

PGDN/AN works well. Why not PGDN/NH4ClO4?
__________________


USER NAME: stupid939
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When I used EGDN/AN I couldn't get the AN to dissolve very easily. I dreamed I was using it in a shaped charge, and it worked great, but it leaked way too much. Have any of you had this problem?

TNT

Yet another TNT synth, this one from Megalomania.

Trinitrotoluene
melting point
80.1 °C boiling point
ignites at 295 °C trinitrotoluene molecular mass
227.13 g/mol density
1.654 g/mL
table key sensitivity
very low chemical formula
C7H5N3O6 explosive velocity
7028 m/s estimated cost
$?.00/g


2,4,6-trinitrotoluene, or just TNT, is the oft used military and industrial explosive that may be the among the best recognized explosive around. Other names for TNT include: trinitrotoluol; sym-trinitrotoluene; a-trinitrotoluol; 2-methyl-1,3,5-trinitrobenzene; entsufon; 1-methyl-2,4,6-trinitrobenzene; methyltrinitrobenzene; tolite; trilit; s-trinitrotoluene; s-trinitrotoluol; trotyl; sym-trinitrotoluol; alpha-trinitrotoluol; tolite; triton; tritol; trilite; tri; tutol; trinol; füllpulver 1902; Fp02; tritolo; trillit; tolita; tol; and trotil. TNT was first synthesized in 1863 by a scientist named Wilbrand who treated toluene with sulfuric and nitric acid at near boiling temperatures. Although there are several isomers of trinitrotoluene, only the 2,4,6- isomer is of importance. Pure TNT is in the form of small columns or needles and is insoluble in water. It is quite stable, being meltable ,or able to act like a plastic at around 50 °C. TNT can even be boiled although the experiments did this under reduced pressure (50mm Hg) to lower the boiling point to around 245 °C. The normal detonation temperature is 333 °C, the calculated boiling point at normal atmospheric pressure is 345 °C, so don't do it. Some experiments have determined that the presence of foreign material like 1.9% of Fe2O3 will lower the amount of time it takes for TNT to explode once it reaches its critical temperature, or 295 °C, the temperature at which decomposition begins. Also, mixing pure sulfur with TNT will lower the initiation temperature and increase the explosive power. For example, pure TNT explodes at 333 °C, 5% sulfur explodes at 304 °C, 10% sulfur at 294 °C, 20% sulfur at 284 °C, and 30% sulfur at 275 °C. The increase in explosive power is gained through the addition of 5-10% sulfur. Because the stability of TNT is so great, it is harder to detonate it, the sensitivity increases somewhat above 80º C, but is still rather low even when molten. A powerful blasting cap, or booster charge, will be needed to detonate TNT. This lab is carried out in three separate operations, forming mononitrotoluene, then dinitrotoluene, and finally trinitrotoluene.
CHEMICALS APPARATUS
ethyl alcohol 100/500/600-mL beaker
nitric acid Buchner funnel
sodium bisulfite graduated cylinder
sulfuric acid pipet/buret
toluene separatory funnel
water stirrer/stirring rod
thermometer


Prepare a nitrating solution of 160 mL of 95% sulfuric acid and 105 mL of 75% nitric acid in a 500-mL beaker set in a salt-ice bath. Mix the acids very slowly to avoid the generation of too much heat. Allow the mixture to cool to room temperature. The acid mixture is slowly added dropwise, with a pipet or buret, to 115 mL of toluene in a 600-mL beaker while stirring rapidly. Maintain the temperature of the beaker during the addition at 30-40 °C by using either a cold water or salt-ice bath. The addition should require 60-90 minutes. After the addition, continue stirring for 30 minutes without any cooling, then let the mixture stand for 8-12 hours in a separatory funnel. The lower layer will be spent acid and the upper layer should be mononitrotoluene, drain the lower layer and keep the upper layer.

Dissolve one-half of the previously prepared mononitrotoluene and 60 mL of 95% sulfuric acid in a 500-mL beaker set in a cold water bath. Prepare a nitrating solution of 30 mL of 95% sulfuric acid and 36.5 mL of 95% nitric acid in a 100-mL beaker. Preheat the beaker of mononitrotoluene to 50 &Deg;C. Very slowly add the nitrating acid to the beaker of mononitrotoluene, with a pipet or buret, drop by drop while stirring rapidly. Regulate the rate of addition to keep the temperature of the reaction between 90-100 °C. The addition will require about 1 hour. After the addition, continue stirring and maintaining the temperature at 90-100 °C for 2 hours. If the beaker is allowed to stand, a layer of dinitrotoluene will separate, it is not necessary to separate the dinitrotoluene from the acid in this step.

While stirring the beaker of dinitrotoluene, heated to 90 °C, slowly add 80 mL of 100% fuming sulfuric acid, containing about 15% SO3, by pouring from a beaker. Prepare a nitrating solution of 40 mL of 100% sulfuric acid, with 15% SO3, and 50 mL of 99% nitric acid. Very slowly add the nitrating acid to the beaker of dinitrotoluene, with a pipet or buret, drop by drop while stirring rapidly. Regulate the rate of addition to keep the temperature of the reaction between 100-115 °C. It may become necessary to heat the beaker after three-quarters of the acid has been added in order to sustain the 100-115 °C temperature. The addition will require about 90-120 minutes. Maintain the stirring and temperature at 100-115 °C for 2 hours after the addition is complete. Allow the beaker to sit undisturbed for 8-12 hours, it should form a solid mass of trinitrotoluene crystals. Pour the contents of the beaker over a Buchner funnel without any filter paper to collect the bulk of the crystals, save the acidic filtrate as well. Break up the collected crystals and wash them with water to remove any excess acid. Add the collected acid and wash filtrates to a large volume of water, this will cause any remaining trinitrotoluene to precipitate. Decant off as much of the water as possible and combine these crystals with the previous ones on the funnel. Drown the crystals in a large volume of water, filter to collect them, and wash several times with water. Wash the crystals by adding them to a beaker of water, heat the water enough to melt the crystals while stirring rapidly. Repeat the melting and stirring with a fresh batch of water three or four times to wash thoroughly. After the last washing, the trinitrotoluene is granulated by allowing it to cool slowly under hot water while the stirring is continued. Filter to collect the crystals and allow to dry. The TNT can be further purified by recrystallizing from ethyl alcohol, dissolve the crystals in 60 °C and allow the solution to cool slowly. A second method of purification is to digest the TNT in 5 times its weight of 5% sodium bisulfite solution heated to 90 °C while stirring rapidly for 30 minutes. Wash the crystals with hot water until the washings are colorless, then allow the crystals to granulate as before. You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to monitor the temperature.

HMX

HMX
melting point
281 °C

HMX molecular mass
296.16 g/mol

density
1.903 g/mL

sensitivity: very low

chemical formula
C4H8N8O8

explosive velocity
9110 m/s

HMX is a very powerful military explosive with similar properties to RDX, the other great military explosive with which it is often mixed. HMX is technically called octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine, other names include 1,3,5,7-tetranitro-1,3,5,7-tetrazacyclooctane; cyclotetramethylene tetranitramine; and octogen. HMX is itself an acronym for either High velocity Military eXplosive, or Her Majesties eXplosive depending on what country you are in. HMX is very stable, it requires a powerful detonator or booster charge to detonate. It was first developed during WWII in the never ending search for more powerful bombs.
CHEMICALS APPARATUS
acetic acid 500/1000-mL beaker
acetic anhydride 500-mL Florence flask
ammonium nitrate graduated cylinder
methenamine stirrer/stirring rod
nitric acid thermometer
paraformaldehyde
water


Prepare a solution of 748 mL of glacial acetic acid, 12 mL of acetic anhydride, and 17 g of paraformaldehyde, keep this solution at 44 °C while mixing. Prepare a second solution of 217.6 g of ammonium nitrate and 154.6 mL of 99% nitric acid in a 500-mL beaker. Prepare a third solution of 101 g of methenamine, 157 mL of glacial acetic acid, and 296 mL of acetic anhydride in a 1000-mL beaker. Combine the third solution with 112.5 mL of the second solution. Add this combined solution to the first solution over a 15 minute period while stirring rapidly. After the addition, continue stirring for an additional 15 minutes. Next, carefully add 296 mL of acetic anhydride, then carefully add the remainder of the second solution, then add another 148 mL of acetic anhydride, all while stirring. Continue the stirring for 1 hour more. After stirring, add 350 mL of hot water and reflux the whole works for 30 minutes. After this time, cool the liquid down to 20 °C by adding ice. Decant off as much of the liquid from the precipitate as possible and drown the remaining crystals with cold water. Filter to collect the crystals of HMX and wash them with three portions of cold water, allow to dry. The yield is about 95%. You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to monitor the temperature.

Owing to the large volume of reactants in this lab, in excess of 2.5 L, it is necessary to use a 5-L flask, unfortunately this is beyond most laboratories, and especially the home chemist. This reaction can be carried out in a glass gallon jug or similar large capacity glass container. The refluxing step can be done in portions using a round-bottomed 500-mL Florence flask.

CL- 14

CL-14, a code name for 5,7-diamino-4,6-dinitrobenzofuroxan, is an insensitive high explosive compound. Other names for this explosive include 5,7-dinitro-2,1,3-benzoxadiazole-4,6-diamine 3-oxide; 5,7-dinitro-4,6-benzofurazandiamine 3-oxide; and 4,6-dinitro-5,7-diaminobenzofuroxan. CL-14 is classed as an insensitive, thermally stable, high density explosive, a class of explosives the military is very interested in nowadays. CL-14 is more powerful than the usual lineup of explosives including TATB, TNT, RDX, and the like. CL-14 can be used either alone or in admixture with other high explosives.

Prepare a solution of 7.2 g of 4,6-dinitrobenzofuroxan dissolved in 100 mL of water. Add 14.4 g of potassium bicarbonate and 8.3 g of hydroxylamine hydrochloride to the solution and stir for 3.5 hours at 25 C. The reaction mixture is then cooled to 0 C and 100 mL of 4N potassium hydroxide solution cooled to 0 C is added. Stirring is continued for 3.5 hours at 0 C. Filter to collect the yellow potassium salt of CL-14. Place the yellow solid in a beaker with water at room temperature. Add an excess of 1N hydrochloric acid and stir for 1 hour. The yellow solid is filtered to collect it, washed with 50 mL of water, and dried. Synthesis 2: 4.16 g of hydroxylamine hydrochloride is added to a stirred solution of 40.0 g of 85% KOH made up to 300 mL with water at a temperature of 5 C. To this mixture, 5.33g of 7-amino-4,6-dinitrobenzofuroxan (ADNBF) is added, with stirring, at 5 C. Initially, a transient bright-red color appeared then changed to an orange color. Solid particles may be visible in the stirred reaction mixture. Stirring is continued at 5 C for 5 hours. The reaction mixture is poured into 500 mL of ice water and stirred for 15 minutes. The fine yellow solid is filtered to collect it, washed with two 50 mL portions of ice water, and dried to give 4.51 g (69.4% yield) of the potassium salt of CL-14. The potassium salt is stirred with 50 mL of 3N hydrochloric acid for 30 minutes, the yellow solid is filtered to collect it, washed with 50 mL of water, and dried to give 3.69g (65.2% yield) of CL-14.

PLASTIQUE

CHAPTER 1 - AMERICAN PLASTIQUE EXPLOSIVES

Since the first part of WWII, the armed forces of the United States has been searching for the perfect plastique explosives to be used in demolition work. This search led to the development of the C composition plastique explosives. Of this group, C-4 being the latest formulation that has been readily adopted by the armed forces. This formulation was preceded by C-3, C-2, and composition C.

In this chapter we will cover all of these explosives in their chronological progression as they were developed and standardized by the armed forces. All of these explosives are cyclonite or R.D.X. base with various plastisizing agents used to achieve the desired product.

This plastisizer usually composes 7 - 20 % of the total weight of the plastique. The procedure for the manufacture of R.D.X. will be given at the end of this chapter.

All of these explosives are exceedingly powerful and should be used with the utmost care ( detonation velocity from 7700 - 8200M/sec. ). All of these C composition plastique explosives are suitable for and usually the explosives of choice for all demolition work using shaped charges, ribbon charges,and steel cutting charges. All these explosives are relatively easy to detonate with a #6 blasting cap, but as with all explosive charges the highest efficiency is obtained through the use of a booster in conjunction with the blasting cap.

COMPOSITION 'C' - This explosive is just a copy of a British explosive that was adopted early in WWII. This explosive is the 'C' explosive of choice for home manufacture due to its ease of manufacture and the more easily obtained compound. This explosive was available in standard demolition blocks. The explosive was standardized and adopted in the following composition:


R. D. X. 88.3 %
Heavy Mineral Oil 11.1 %
Lecithin 0.6 %


In this composition, the lecithin acts to prevent the formation of large crystals of R.D.X. which would increase the sensitivity of the explosive. This explosive has a good deal of power. It is relatively non - toxic except if ingested and is plastic from 0-40 deg. C.. Above 40 deg., the explosive undergoes extrudation and becomes gummy although its explosive properties go relatively unimpaired. Below 0 deg. C., it becomes brittle and its cap sensitivity is lessened considerably. Weighing all pros and cons, this is the explosive of choice for the kitchen explosives factory due to the simple manufacture of the plastique compound.

Manufacturing this explosive can be done in two ways. The first is to dissolve the 11.1 % plastisizing in unleaded gasoline and mixing with the R. D. X. and then allowing the gasoline to evaporate until the mixture is free of all gasoline. All percentages are by weight.

The second method is the fairly simple kneading of the plasticizing compound into the R.D.X. until a uniform mixture is obtained. This explosive should be stored in a cool dry place. If properly made, the plastique should be very stable in storage, even if stored at elevated temperatures for long periods of time. It should be very cap sensitive as compared to other millitary explosives. With this explosive, as mentioned earlier, a booster will be a good choice, especially if used below 0 deg. C.. The detonation velocity of this explosive should be around 7900 M/sec..

COMPOSITION C-2 - Composition C-2 was developed due to the undesirable aspects of composition 'C'. lt was formerly used by the United States armed forces, but has been replaced by C-3 and C-4. lt's composition is much the same as C-3 and it's manufacture is thc safe also.

I won't go into much detail on this explosive because of its highly undesirable traits. lt is harder to make than C-4 and is toxic to handle. lt also is unstable in storage and is a poor choice for home explosives manufacture. It also has a lower detonation velocity than either C-4 or C-3. But for those of you that are interested, I will give the composition of this explosive anyway. It is manufactured in a steam jacketed (heated) melting kettle using the same procedure used in incorporation of C-3. Its composition is as follows:


R.D.X. 80 %
.
Equal parts of thc following:
.
Mononitrotolulene
Dinitrotolulene
T.N.T. guncotton
Dimethylformide 20 %


COMPOSITION C-3 - This explosive was developed to eliminate the undesirable aspects of C-2. It was standardized and adopted by the military as the following composition:


R. D. X. 77 %
Mononitrotolulene 16 %
Dinitrotolulene 5 %
Tetryl 1 %
Nitrocellose (guncotton) 1 %


C-3 is manufactured by mixing the plastisizing agent in a steam jacketed melting kettle equipped with a mechanical stirring attachment. The kettle is heated to 90-100 deg. C. and the stirrer is activated. Water wet R.D.X. is added to the plasticizing agent and the stirring is continued until a uniform mixture is obtained and all water has been driven off. Remove the heat source but continue to stir the mixture until it has cooled to room temperature. This explosive is as sensitive to impact as is T.N.T.. Storage at 65 deg. C. for four months at a relative humidity of 95% does not impair its explosive properties. C-3 is 133% as good as an explosive as is T.N.T.. The major drawback of C-3 is its volatility which causes it to lose 1.2% of it's weight although the explosive's detonation properties are not affected. Water does not affect the explosive's performance. It therefore is very good for U.D.T. uses and would be a good choice for these applications. When stored at 77 deg. C., considerable extrudation takes place. It will become hard at -29 deg. C. and is hard to detonate at this temperature. While this explosive is not unduly toxic, it should be handled with utmost care as it contains aryl- nitro compounds which are absorbed through the skin. It will reliably take detonation from a #6 blasting cap but the use of a booster is always suggested. This explosive has a great blast effect and was and still is available is standard demolition blocks. It's detonation velocity is approximately 7700 M / sec..

COMPOSITION C-4 C-4 was developed because of the hardening and toxicity that made C-3 unreliable and dangerous due to the dinitrotolulene plastisizer. The following composition is the standardized plastique explosive as adopted by the armed forces:


R. D. X. 91.0 %
Polyisobutylene 2.1 %
Motor Oil 1.6 %
Di-(2-ethylhexy)sebecate 5.3 %


The last three ingredients are dissolved in unleaded gasoline. The R.D.X. explosive base is then added to the gasoline-plasticizer and the resultant mass in allowed to evaporate until the gasoline is completely gone (this can be done quickly and efficiently under a vacuum).

The final product should be dirty white to light brown in color. It should have no odor and have a density of 1.59 gm/cc. It does not harden at -57 deg. C. and does not undergo extrudation at 77 deg. C.. It can be reliably detonated with a #6 blasting cap.

The bristance of this explosive ( ability to do work or fragment ordinance ) is 120 % greater than T.N.T.. C-4 is the best plastique explosive available in the world and probably will remain so for quite some time. This is the #1 demolition explosive in the world and if you've never seen this stuff used it is absolutely amazing. The detonation velocity of C-4 is 8100 M/sec..


CHAPTER 2 - R.D.X. MANUFACTURE

Cyclotrimethylenetrinitramine or cyclonite is manufactured in bulk by nitration of hexamtehylenetetramine (methenamine, hexamine, tec.) with strong red 100 % nitric acid. The hardest part of this reaction is obtaining this red nitric acid. It will most likely have to be made. More on this later. The hexamine or methenamine can usually be bought in bulk quantities or hexamine fuel bars for camp stoves can be used, but they end up being very expensive. To use the fuel bars they need to be powdered before hand. The hexamine can also be made with common ammonia water (5 %) and the commonly available 37% formaldehyde solution. To make this component, place 400 g. of clear ammonia water in a shallow pyrex dish. To this add 54 g. of the formaldehyde solution to the ammonia water. Allow this to evaporate and when the crystals are all that remains in the pan, place the pan in the oven on the lowest heat that the oven has. This should be done only for a moment or so to drive off any remaining water. These crystals are scraped up and plaecd in an airtight jar to store them until they are to be used.

To make the red nitic acid, you will need to buy a retort with a ground glass stopper. In the retort, place 32 grams of sulfuric acid (98-100%) and to this add 68 g. of potassium nitrate or 58 g. of sodium nitrate. Gently heating this retort will generate a red gas called nitrogen trioxide. This gas is highly poisonous and this step as with all other steps should be done with good ventilation. This nitric acid that is formed wiil collect in the neck of the retort and form droplets that will run down the inside of the neck of the retort and should be caught in a beaker cooled by being surrounded by ice watcr. This should be heated until no more collects in the neck of the retort and the nitric acid quits dripping out of the neck into the beaker. This acid should be stored until enough acid is generated to produce the required size batch which is determined by the person producing the explosive. Of course the batch can be bigger or smaller but the same ratios should be maintained.

To make the R.D.X., place 550 g. of the nitric acid produced by the above procedure in a 1000 ml beaker in a salted ice bath. 50 g. of hexamine (methenamine) is added in small portions making sure that the temperature of the acid does not go above 30 deg. C.. This temperature can be monitored by placing a thermometer directly in the acid mixture. During this procedure, a vigorous stirring should be maintained. If the temperature approaches 30 deg. C., immediately stop the addition of the hexamine until the temperature drops to an acceptable level. After the addition is complete, continue the stirring and allow the temperature to drop to 0 dcg. C. and allow it to stay there for 20 minutes continuing the vigorous stirring. After the 20 minutes are up, pour this acid - hexamine mixture into 1000 ml of finely crushed ice and water. Crystals should form and are filtered out of the liquid.

The crystals that are filtered out are R. D. X. and will need to have all traces of the acid removed. To remove the traces of acid, first wash these crystals by putting them in ice water and shaking and refiltering. These crystals are then placed in a little boiling water and filtered. Place them in some warm water and check the acidity for the resultant suspension with litmus paper. You want them to read between 6 and 7 on the Ph scale ( E. Merik makes a very good paper) and it accurate and easy to read. If there is still acid in these crystals, reboil them in fresh water until the acid is removed, checking to see if the litmus paper reads between 6 and 7. Actually the closer to 7 the better. To be safe, these crystals should be stored water wet until ready for use. This explosive is much more powerful than T.N.T.. To use, these will need to be dryed for some manufacture processes in this book. To dry these crystals, place them in a pan and spread them out and allow the water to evaporate off them until they are completely dry.

This explosive will detonate in this dry form when pressed into a mold to a density of 1.55 g./cc at a velocity of 8550 M./sec..


COMPARISON OF DETONATION VELOCITY
M / sec _________________________________
8600|
8500| ***
8400| ***
8300| ***
8200| ***
8100| ***
8000| *** ***
7900| *** *** ***
7800| *** *** *** ***
7700| *** *** *** *** ***
7600| *** *** *** *** ***
7500| *** *** *** *** ***
7400| *** *** *** *** ***
7300| *** *** *** *** ***
7200| *** *** *** *** ***
7100| *** *** *** *** ***
7000| *** *** *** *** *** ***
6900| *** *** *** *** *** ***
|_______________________________________________________________
TNT RDA Comp C Comp C-2 Comp C-3 Comp C-4



CHAPTER 3 - FOREIGN PLASTIQUE EXPLOSIVES

Italian Plastique Explosives - During World War II, the Italian military adopted R.D.X. and P.E.T.N. as their standard explosive. Naturally then their plastique explosive are R.D.X. based. Their explosive suits itself very well to home manufacture. It is mixed together by kneading the components together until a uniform mixture is obtained. This explosive is composed of the following:


R.D.X.(see R.D.X. manufacture) 78.5 %
Nitroglycerin or
Nitroglycol 17.5 %
Petrotroleum Jelly 4.0 %


This is a very powerful explosive composition as are most that contain R.D.X. Its major drawback is toxicity. Since it contains nitroglycerin or glycol, these components can be absorbed through the skin. These are cardiovascular dialators and handling them will give the most intense headaches and are poisonous. Therefore, skin contact should be avoided. This explosive is almost as powerful as C-4 and will work very well. It is equivalent to C-3 in power and can be considered its equivalent in charge computation. It is less toxic than C-3 and a little more plastic. Its detonation velocity is approximately 7800 M/sec.

OSHITSUYAKA JAPANESE PLASTIQUE EXPLOSIVE - An explosive that will lend itself to home manufacture is this explosive that was used by the Japanese in WWII. It is an explosive that was used in ribbon charges and demolition rolls. Of course, the main ingredient is R.D.X. which composes most of the explosives weight. This being a plastique explosive with a wax plastisizer is limited in the tempcrature that can be used. These properties can be improved on somewhat by the substitution of short fiber grease ( wheel bearing grease ) or bees wax for part of the percentage of wax. Their composition is as follows:


R.D.X. (see R.D.X. manufacture) 80 %
Wax (l/2 wax, 1/2 wheel bearing grease) 20 %



CHAPTER 4 - PLASTIQUE EXPLOSIVE FROM BLEACH

This explosive is a potassium chlorate explosive. This explosive and explosives of similar composition were used in World War I as the main explosive filler in grenades, land mines, and mortar rounds used by French, German and some other forces involved in that conflict. These explosives are relatively safe to manufacture. One should strivc to make sure these explosives are free of sulfur, sulfides, and picric acid. The presence of these compounds result in mixtures that are or can become highly sensitive and possibly decompose explosively while in storage. The manufacture of this explosive from bleach is given just as an expediant method. This mcthod of manufacturing potassium chlorate is not economical due to the amount of energy used to boil the solution and cause the 'dissociation' reaction to take place. This procedure does work and yields a relatively pure and a sulfur, sulfide free product. These explosives are very cap sensitive and require only a #3 cap for instigating detonation. To manufacture potassium chlorate from bleach (5.25% sodium hypochlorite solution) obtain a heat source (hot plate, stove etc.) a battery hydrometer, a large pyrex or enameled steel container, (to weigh chemicals), and some potassium chloride (sold as salt substitute). Take one gallon of bleach and place it in the container and begin heating it. While this solution heats, weigh-out 63 G. potassium chloride and add this to the bleach being heated. Bring this solution to a boil and boil until when checked with a hydrometer, the reading is 1.3 (if a battery hydromcter is used it should read full charge).

When the reading is 1.3, take the solution and let it cool in the refrigerator until it is between room temperature and 0 deg. C.. Filter out the crystals that have formed and save them. Boil the solution again until it reads 1.3 on the hydrometcr and again cool the solution. Filter out the crystals that are formed and save them. Boil this solution again and cool as before. Filter and save the crystals. Take these crystals that have been saved and mix them with distilled water in the following proportions: 56 G. per 100 ml. distilled water. Heat this solution until it boils and allow it to cool. Filter the solution and save the crystals that form upon cooling. The proccss of purification is called fractional crystalization. Thesc crystals should be relatively pure potassium chlorate.

Powder these to the consistancy of face powder (400 mesh) and heat gently to drive off all moisture. Melt five parts vaseline and five parts wax. Dissolve this in white gasoline (camp stove gasoline) and pour this liquid on 90 parts potassium chlorate (the crystals from the above operation) in a plastic bowl. Knead this liquid into the potassium chlorate until imtimately mixed. Allow all the gasoline to evaporate. Place this explosive in a cool dry place. Avoid friction and sulfur, sulfides and phosphorous compounds. This explosive is best molded to the desired shape and density (1.3 g./cc) and dipped in wax to water proof. These block type charges guarantee the highest detonation velocity. This explosive is really not suited to use in shaped charge applications due to its relatively low detonation velocity. It is comparable to 40% ammonia dynamite and can be considered the same for the sake of charge computation. If the potassium chlorate is bought and not made, it is put into the manufacture process in the powdering stages preceding the addition of the wax-vaseline mixture. This explosive is bristant and powerful. The addition of 2 - 3 % aluminum powder increases its blast effect. Detonation velocity is 3300 M/sec.


CHAPTER 5 - PLASTIC EXPLOSIVE FROM SWIMMING POOL CLORINATING COMPOUND ( H.T.H. )

This explosive is a chlorate explosive from bleach. This method of production of potassium or sodium chlorate is easier and yields a more pure product than does the plastique explosive from bleach process. In this reaction the H.T. H. ( calcium hypo-chlorate - CaClO ) is mixed with water and heated with either sodim chlorate ( table salt, rock salt ) or potassium chloride (salt substitute). The latter of these salts is the salt of choice due to the easy crystalization of the potassium chlorate. This mixture will need to be boiled to ensure complete reaction of thc ingredients.

Obtain some H.T.H. swimming pool chlorination compound or equivalent (usually 65% calcium hypochlorite). As with the bleach is also a dissociation reaction. In a large pyrex glass or enameled steel container place 1200 g. H.T.H. and 220 G. potassium chloride or 159 g. sodium chloride. Add enough boiling water to dissolve the powder and boil this solution. A chalky substance ( calcium chloride ) will be formed. When the formation of this chalky substance is no longer formed, the solution is filtered while boiling hot. If potassium chloride was used, potassium chlorate will be formed. This potassium chlorate will drop out or crystalize as the clear liquid left after filtering cools.These crystals are filtered out when the solution reaches room temperature. If the sodium chloride salt was used this clear filtrate ( clear liquid after filtration ) will need to have all water evaporated. This will leave crystals which should be saved.

These crystals should be heated in a slightly warm oven in a pyrex dish to drive off all traces of water ( 40 - 75 deg.C. ). These crystals are ground to a very fine powder ( 400 mesh ).

If the sodium chloride salt is used in the initial step, the crystallization is much more time consuming. The potassium chloride is the salt to use as the resulting product will crystallize out of solution as it cools. The powdered and completely dry chlorate crystals are kneaded together with vaseline in plastique bowl. ALL CHLORATE BASED EXPLOSIVES ARE SENSITIVE TO FRICTION, AND SHOCK, AND THESE SHOULD BE AVOIDED. If sodium chloride is used in this explosive, it will have a tendancy to cake and has a slightly lower detonation velocity. This explosive is composed of the following:


Potassium or sodium chlorate 90 %
Vaseline 10 %


The detonation velocity can be raised to a slight extent by the addition of 2 - 3 % aluminum powder substituted for 2 - 3 % of the vaseline. The addition of this aluminum will give this explosive a bright flash if set off at night which will ruin night vision for a short while. The detonation velocity of this explosive is approximately 32OO M/sec. for the potassium salt and 290O M/sec. for the sodium salt based explosive.


CHAPTER 6 - PLASTIQUE EXPLOSIVE FROM TABLE SALT

This explosive is perhaps the most easily manufactured of the chlorate based explosives. Sodium chlorate is the product because rock salt is the major starting ingredient. This process would work equally as if potassium chlorate were used instead of the sodium chloride (rock salt). The sodium chlorate is the salt I will cover due to the relatively simple acquisition of the main ingredient. The resulting explosive made from this process would serve as a good cheap blasting explosive and will compare favorably with 30 % straight dynamite in power and blasting efficiency. This explosive can be considered the same as 30 % straight dynamite in all charge computation. These explosives and similar compositions were used to some extent in World War I by European forces engaged in conflict. It was used as a grenade and land mine filler. Its only drawback is its hygroscopic nature ( tendancy to absorb atmospheric moisture ). These explosives also have a relatively critical loading density. These should be used at a loading density of 1.3 g./cc. If the density is not maintained, unreliable or incomplete detonation will take place. These shortcomings are easiiy overcome by coating the finished explosive products with molten wax and loading this explosive to the proper density. This explosive is not good for shaped charge use due to it's low detonation rate (2900 M/sec.). The major part of the manufacture of this explosive from rock salt is the cell rcaction where D.C current changes the sodium chloride to chlorate by adding oxygen by electrolysis of a saturated brine solution. The reaction takes place as follows:


NaCl + 3 H2O --> NaClO3 + 3 H2


In this reaction the sodium chloride (NaCl) takes the water's oxygen and releases its hydrogen as a gas. This explosive gas must be vented a ways as sparks or open flame may very well cause a tremendous explosion. This type of process or reaction is called a 'cell' reaction. The cell should be constructed of concrete or stainless steel. I won't give any definite sizes on the cell's construction because the size is relative to the power source. This cell would have to be large enough to allow the brine to circulate throughout the cell to insure as uniform a temperature as possible.

The speed of the reaction depends on two variables. Current density is a very important factor in the speed of the reaction. The advantages of high current densities are a faster and more efficient reaction. The disadvantages are that cooling is needed to carry away excess heat and the more powerful power sources are very expcnsive. For small operations, a battery charger can be used (automotive). This is the example I will use to explain the cell's setup and operation ( 10 amp / 12 volt). The current density at the anode ( + ) and cathode ( - ) are critical. This density should be 50 amps per square foot at the cathode and 30 amps per square foot at the anode. For a 10 amp battery charger power source, this would figure out to be 5 5/16" by 5 5/16" for the cathode. The anode would be 6 15/16" by 6 5/16". The anode is made of graphite or pressed charcoal and the cathode is made of steel plate (1/4"). These would need to be spaced relatively close together. This spacing is done with some type of non-conducting material such as glass rods. This spacing can be used to control the temperature to some extent. The closer together they are, the higher the temperature. These can be placed either horizontaily or vertically although vertical placement of the anode and cathode would probably be the ideal set up as it would allow the hydrogen to escape more readily. The anode would be placed at the bottom if placed horizontally in the cell so that the chlorine released could readily mix with the sodium hydroxide formed at the cathode above it. As the current passes through, the cell chlorine is released at the anode and mixes with the sodium hydroxide formed at the cathode. Hydrogen is released at the cathode which should bubble out of the brine. This gas is explosive when mixed with air and proper precautions should be taken. PROPER VENTILATION MUST BE USED WITH THIS OPERATION TO AVOID EXPLOSION.

Temperature control is left up to the builder of the cell. The temperature of the cell should be maintaincd at 56 degrees C. during the reaction. This can be done by the circulation of water through the cell in pipes. But the easiest way would be to get an adjustable thermostatic switch adjusted to shut the power source off until the cell cools off. This temperature range could be from 59 degree shut off to a 53 degree start up. An hour meter would be used on the power source to measure the amount of time the current passes through the cell. If the water- cooling coil design appeals to the manufacturer and an easily obtained cheap source of cool or cold water is available, this would be the quickest design to use. Again a thermostatic type arrangement would be used to meter the cold cooling water through the cell. The cooling coils would best be made of stainlcss steel to overcome the corrosiveness of the salts although this is not entirely necessary. A thermostatic valve would be set to open when the brine electrolyte was heated above approximately 58 deg C. and set to close when the temperature fell to approximately 54 deg C.. Again this would be the best and most efficient method and the waste heat could be used relatively easily to heat either a house or perhaps even a barn or shop.

To run the cell, after the cell has been constructed and the concrete has been sealed and has set and cured for several weeks, is very simple. First, to seal the concrete I suggest Cactus Paint's CP 200 series, two componant epoxy paint or an equivalent product. To fill the cell, place 454 g. sodium chloride in thc cell (rock salt is excellent here). Place four liters of distilled water into the cell with the salt. The liquid should cover the anode and the cathode completely with room to spare. Remember that some of the water will be used in the reaction. Thirty three grams of muratic acid, which should be available from a swimming pool supply store is then added to the liquid in the cell. Be careful when handling any acid !!! Then seven grams of sodium dichromate and nine grams of barium chloride is added. The cell is then ready to run if the plates are connected to their respective cables. These cables are best made of stainless steel (the most corrosion resistant available). The power supply is then hooked up and the cell is in operation. The power is best hooked up remotely to lessen the chance of explosion. Any time the cell runs it will be making hydrogen gas. THIS GAS IS EXPLOSIVE WHEN MIXED WITH AIR AND ALL SPARKS, FLAME, AND ANY SOURCE OF IGNITION SHOULD BE KEPT WELL AWAY FROM THE CELL. THIS CELL SHOULD ONLY BE RUN WITH VERY GOOD VENTILATION. The steel plate cathode should be hooked to the negative side of the power source and the anode hooked to the positive side. Again these are hooked to the power supply via stainless steel cables. This cell is then run at the proper temperature until 1800 amp hours pass through (amount per pound of sodium chloride) the electrolyte. The liquid in the cell is then removed and placed in an enameled steel containcr and boiled until crystals form on liquid. It is cooled and filtered, the crystals collected being saved. This is done twice and the remaining liquid saved for the next cell run. The process will become easier as each run is made. It is a good idea to keep records on yields and varying methods to find out exactly the best process and yield. To purify these crystals place 200 grams in 100 ml distilled water. Boil the solution until crystals are seen on the surface. Let cool and filter as before. Save this liquid for thc next cell run. These purified crystals are placed in a pyrex dish and placed in the oven at 50 deg C. for two hours to drive off all remaining water.

The explosive is ready to be made. The crystals of sodium chlorate are ground to a powder of face powder consistancy. Ninety grams of this sodium chlorate are kneaded with 10 grams of vaseline until a uniform mixture is obtained. This explosive is sensitive to shock, friction, and heat. These should be avoided at all cost. This explosive works best at a loading density of 1.3-1.4 g./cc. If this explosive is not used at this density, the detonation velocity will be low and detonation will be incomplete. To load to a known density measure the volume of the container in which the explosive is to be loaded. This can be done by pouring water out of a graduated cylinder until the container is filled. The total number of ml will equal the cc's of the container. Multiply this number times 1.3 and load that much explosive ( in grams of course ) into the container after the container has been dryed of all water. This procedure should be used with all chlorate explosives ( plastique explosive from bleach, plastique explosive from H.T. H.). This explosive is cheap and relatively powerful and is a good explosive.


DETONATION VELOCITY VS. LOADING DENSITY
_______________________________________
|
3300 |
|
3200 | x x x x x x x x x x Incomplete
| x Detonation
3100 | x x x
| x x
3000 | x
| x x x x x
2900 | x
| x
2800 | x
| x
| x
|_____________________________________________________________
. 0.9 1.0 1.1 1.2 1.3 1.4



CHAPTER 7 - PLASTIQUE EXPLOSIVES FROM ASPIRIN

This explosive is a phenol derivative. It is toxic and explosive compounds made from picric acid are poisonous if inhaled, ingested, or handled and absorbed through the skin. The toxicity of this explosive restricts its use due to the fact that over exposure in most cases causes liver and kidney failure and sometimes death if immediate treatment is not obtained.

This explosive is a cousin to T.N.T. but is more powerful than its cousin. It is the first explosive used militarily and was adopted in 1888 as an artillery shell filler. Originally this explosive was derived from coal tar but thanks to modern chemistry, you can make this compound easily in approximately 3 hours from acetylsalicylic acid ( purified aspirin ).

This procedure involves dissolving the acetylsalicylic acid in warm sulfuric acid and adding sodium or potassium nitrate which nitrates the purified aspirin and the whole mixture drowned in water and filtered to obtain the final product. This explosive is called trinitrophenol. Care should be taken to ensure that this explosive is stored in glass containers. Picric acid will form dangerous salts when allowed to contact all metals except tin and aluminum. These salts are primary explosives and are super sensitive. They also will cause the detonation of thc picric acid.

To make picric acid, obtain some aspirin. The cheaper buffered brands should be avoided. Powder these tablets to a fine consistancy. To extract the acetylsalicytic acid from this powder, place this powder in warm methyl alcohol and stir vigorously. Not all of the powder will dissolve. Filter this powder out of the alcohol. Again, wash this powder that was filtered out of the alcohol with more alcohol but with a lesser amount than the first extraction. Again filter the remaining powder out of the alcohol. Combine the now clear alcohol and allow it to evaporate in a shallow pyrex dish. When the alcohol has evaporated, there will be a surprising amount of crystals in the bottom of the pyrex dish.

Take forty grams of these purified acetylsalycilic acid crystals and dissolve them in 150 ml of sulfuric acid (98%, specific gravity 1.8) and heat to dissolve all the crystals. This heating can be done in a common electric frying pan with the thermostat set on 150 deg F. and filled with a good cooking oil. When all the crystals have dissolved in the sulfuric acid, take the beaker that you've done this dissolving in (600 ml), out of the oil bath.

This next step will need to be done with a very good ventilation system ( it is a good idea to do any chemistry work such as the whole procedure and any procedure in this book with good ventilation or outside). Slowly start adding 58 g. of sodium nitrate or 77 g. potassium nitrate to the acid mixture in the beaker very slowly in small portions with vigorous stirring. A red gas (nitrogen trioxide) will be formed and this should be avoided. (Caution: This red gas nitrogern trioxide should be avoided. Very small amounts of this gas are highly poisonous. Avoid breathing vapors at all cost!). The mixture is likely to foam up and the addition should be stopped untit the foaming goes down to prevent the overflow of the acid mixture in the beaker.

When the sodium or potassium nitrate has been added, the mixture is allowed to cool somewhat (30-40 deg C.). The solution should then be dumped slowly into twice its volume of crushed ice and water. Brilliant yellow crystals will form in the water. These should be filtered out and placed in 200 ml of boiling distilled water. This water is allowed to cool and the crystals are then filtered out of the water. These crystals are a very, very, pure trinitrophenol. These crystals are then placed in a pyrex dish and placed in an oil bath and heated to 80 deg C. and held there for 2 hours. This temperature is best maintained and checked with a thermometer. The crystals are then powdered in small quantities to a face powder consistancy. These powdered crystals are then mixed with 10 % by weight wax and 5 % vaseline which are heated to melting temperature and poured onto the crystals. The mixing is best done by kneading together with gloved hands. This explosive should have a useful plasticity range of 0-40 deg C.. The detonation velocity should be around 7000 M / sec.. It is toxic to handle but simply made from common ingredients and is suitable for most demolition work requiring a moderately high detonation velocity. It is very suitable for shaped charges and some steel cutting charges. lt is not as good an explosive as is C-4 or other R.D.X. based explosives but it is much easier to make. Again this explosive is very toxic and should be treated with great care. Avoid handling bare handed, breathing dust and fumes and avoid any chance of ignition. After utensils are used for the manufucture of this explosive retire them from the kitchen as the chance of poisoning is not worth the risk. This explosive, if manufactured as above, should be safe in storage but with any homemade explosive storage is not recommended and explosive should be made up as needed. AVOID CONTACT WITH ALL METALS EXCEPT ALUMINUM AND TIN!!


CHAPTER 8 - NITRO-GELATIN PLASTIQUE EXPLOSIVE

This explosive would be a good explosive for home type manufacturer. It is very powerful and is mostly stable. It's power can be compared favorable with the R.D.X. based plastique explosives. The major drawbacks are the problems with headaches in use and its tendancy to become insensitive to a blasting cap with age. It is a nitroglycerin based explosive and therefore the manufacturer would need to be familiar with the handling of nitroglycerin and know the safety procedures associated with its handling. All of the explosive's bad points could be overcome through planning ahead and careful handling of its explosive componants. Gloves should be worn at all times during this explosive's manufacture and use. The nitro headache can be avoided by avoiding skin contact and avoidance of the the gases formed when the explosive would be detonated. This explosive would need to be made up prior to its use to ensure cap reliability and a high detonation rate. Nitroglyccrin is sensitive to shock, flame and impurities. Any of these can and possibly would cause the premature detonation of the nitroglycerin. This is something to remember because the detonation of nitroglycerin is very impressive. Nitroglycerin, discovered in 1846, is still the most powerful explosive available.

This explosive is nitroglycerin made plastic by the addition of 7-9 % nitrocellose. It is possible to make this nitrocellose but much more practical to buy it. It is available as IMR smokeless powder as sold by Dupont. It should be easily obtained at any area sporting goods store.

To make this explosive, take 8% IMR smokeless powder and mix it with a 50/50 ether-ethyl alcohol and mix until a uniform mixture is obtained. This should be a gummy putty like substance which is properly called a collidon. To his collidon is added 92 %, by weight, nitroglycerin. This is very, very carefully mixed by kneading with gloved hands. In chapter 10, nitroglycerin and nitroglycol manufacture is covered. A uniform mixture should be obtained by this kneading. THERE IS DANGER IMVOLVED IN THIS STEP AND THIS SHOULD NOT BE ATTEMPTED UNLESS THE MANUFACTURER IS WILLING TO TAKE THIS RISK. This nitro-gelatin is then ready for use. It is not recommended that this explosive be kept for any length of time. It should be used immediately. If this is impossible the explosive can be stored with a relative degree of safety if the temperature is kept in thc 0-10 deg C. range. This explosive is a good choice if thc R.D.X. based plastique's cannot be made. The plastic nature of this explosive will deteriorate with age but can be made pliable again with the addition of a small percentage of 50/50 % ether-ethyl alcohol. The detonation of velocity of this explosive should be around 7700-7900 M/sec.. This is a good explosive for underwater or U.D.T. type demolition work.


CHAPTER 9 - GELATIN EXPLOSIVES FROM ANTI FREEZE

This explosive is almost the same as the previous formula except it is supple and pliable to -10 deg C.. Antifreeze is easier to obtain than glycerin and is usually cheaper. It needs to be freed of water before the manufacture and this can be done by treating it with calcium chloride to the antifreeze and checking with a hydrometer and continue to add calcium chloride until the proper reading is obtained. The antifreeze is filtered to remove the calcium chloride from the liquid. This explosive is superior to the previous formula in that it is easier to collidon the IMR smokeless powder into the explosive and that the 50/50 ether - ethyl alcohol can be done away with. It is superior in that the formation of the collidon is done very rapidly by the nitroethelene glycol. Its detonation properties are practically the same as the previous formula. Like the previous formula, it is highly flammable and if caught on fire, the chances of are good that the flame will progress to detonation. In this explosive as in the previous formula, the addition of 1 % sodium carbonate is a good idea to reduce the chance of residual acid being present in the final explosives. The following is a slightly different formula than the previous one:


Nitro-glycol 75 %
Guncotton (IMR smokeless) 6 %
Potassium nitrate 14 %
Flour (as used in baking) 5 %


In this process, the 50/50 step is omitted. Mix the potassium nitrate with the nitroglycol. Remember that this nitroglycol is just as sensitive to shock as is nitroglycerin. The next step is to mix in the flour and sodium carbonate. Mix these by kneading with gloved hands until the mixture is uniform. This kneading should be done gently and slowly. The mixture should be uniform when the 1MR smokeless powder is added. Again this is kneaded to uniformity. Use this explosive as soon as possible. If it must be stored, store in a cool dry place (0 - 10 deg C.). This explosive should detonate at 7600-7800 M / sec.. These last two explosives are very powerful and should be sensitive to a #6 blasting cap or equivalent. These explosives are dangerous and should not be made unless the manufacturer has had experience with this type compound. The foolish and ignorant may as well forget these explosives as they won't live to get to use them. Dont get me wrong, these explosives have been manufactured for years with an amazing record of safety. Millions of tons of nitroglycerin have been made and used to manufacture dynamite and explosives of this nature with very few mishaps. Nitroglycerin and nitroglycol will kill and their main victims are the stupid and foolhardy. This explosive compound is not to be taken lightly. If there are any doubts ... DON'T.


CHAPTER 10 - NITROGLYCERIN AND NITROGLYCOL MANUFACTURE

Glycerin and ethylene glycol are related chemically to one another and are grouped as alcohols. Both of these oily substances can be nitrated to form a trinitro group. These trinitro groups are both unstable and will explode with tremendous violence and power. Impurities in this form of the substance will also cause the decomposition of the oil. Glycerin is used for soap manufacture and should be easily bought without question. Ethylene glycol is sold as common antifreeze and should be easily acquired. Ethylene glycol renders a better product and would be the item of choice plus the manufacture of plastique explosives from this oily explosive is much easier than from the glycerin nitro form. If ethylene glycol is used, it is easier to buy the anhydrous form than to dessicate the water from the antifreeze version of this chemical. The glycerin is also best if bought in its anhydrous form. The use of the anhydrous form (water free) prevents the watering down of thc nitration acids and thus gives a much higher yield of the final product.

This nitration is achieved by the action of an acid mixture on the glycerin or glycol. This acid is composed of the following :


Nitric acid (7O %) 30 %
Sulfuric acid (98 %) 70 %
or
Nitric acid (100 %) 38 %
Sulfuric acid (98 %) 62 %


Of course, this is by weight as all the percentages in this book. The first acid mixture won't give as good a yield of nitro compound as the second acid mixture. The first acid strength is the only one that is readily availabie and be bought readily. The 100% nitric acid is however made readily and is really worth the extra trouble because the yield of nitroglycerin or glycol is so much higher. The actual nitration should be carried out in a glass (pyrex) or enameled steel container. The acids are poured into the container. First the sulfuric and then the nitric very slowly. A great deal of heat is generated by this acid mixing. This container should have been previously placed in a salted ice bath. A thermometer is placed in the acid. A stirring apparatus will need to be rigged up. This will be stirred with a fish tank aerator and pump. This compressed air is the only thing that's really safe to stir this mixture as nitration is taking place. As the acid mixture cools, a weight of glycerin or glycol should be measured out. For glycerin, it should equal 1/6 the total weight of the acid mixture. For the glycol, it should also equal 1/6 of the total weight of the acid.

When the temperature of the acid mixture reaches 0-5 deg C., the addition of the glycerin or glycol is begun after the mixed acids have begun being stirred by the air. Again this agitation of the mixcd acids is very important. It will create a gradual rise in temperature and ensures the complete nitration of the glycerin or glycol as it is added. The glycerin-glycol is added in small quantities with a careful eye kept on the temperature of the acids. If at any time, the temperature of the acids rises above 25 deg C., immediately dump the acid-glycol-glycerin into the ice bath. This will prevent the overheating of the nitroglycerin or glycol and its subsequent explosion. If the temperature rises close to the 25 deg C. mark, by all means, stop the addition of the glycerin or glycol. Wait until the temperature starts to fall before continuing the addition.

The glycol will generate more heat during the nitration than will glycerin. The ice bath may need more ice before the reaction is complete, so add when necessary. After the addition of the glyccrin or glycol is complete, keep the agitation up and wait for the temperature of the glycerin to fall to 0 deg C.. Stop the agitation of the mixed acids and the nitroglycerin. Let the mixture set. Keep a watch on the temperature just in case. A layer of nitroglycerin or nitroglycol should form on top of thc acid mixture. This should be removed with a glass basting syringe. Carefully place this with its own volume of water ( distilled ) in a beaker. To this add small quantities of sodium bicarbonate to neutralize any acid remaining in the nitro compound. In all steps with this nitro oil, keep the oil at ten degrees C. or colder for the glycol. When the addition of the bicarbonate no longer causes a fizzing ( reacting with the excess acid ), check the water-nitro with litmus paper (E. Merik). The reading should be around 7. If it is below 6.5, add more bicarbonate until the reading is seven or close to it. The nitroglycerin or nitro glycol should be settled. It should again be sucked up off the bottom into the clean basting syringe (glass). USE EXTRA CAUTION WHEN HANDLING THIS NITROGLYCERIN OR NITROGLYCOL, BECAUSE THE SLIGHTEST BUMP OR JAR COULD POSSIBLY EXPLODE. WHEN SUCKING THIS OIL OFF THE BOTTOM OF THE WATER, DO NOT BUMP THE BOTTOM WITH THE TIP OF THE BASTING SYRINGE. If neccssary, suck up some of the water and remove it from the nitroglycerin or glycol by forcepts and small pieces of calcium chloride. The calcium chloride is placed in such a way that it only contacts the residual water in the nitroglycerin or nitroglycol. To make this oil safer to handle, add acetone to the nitroglycerin or glycol in the following proportions:


25 % acetone
75 % nitroglycerin or nitroglycol


This will make the oil less sensitive to shock, etc.. This oil when so mixed will still be sensitive to a #8 blasting cap. Remember that the oil contains this acetone when measuring out the oil to be used in other explosives. It may be mixed in the formulas that call for nitroglycerin or nitroglycol and will usually improve the incorporation of these mixtures. To obtain maximum cap sensitivity the acetone should be allowed to evaporate before use of the finished explosive compound.

This oil should not be stored if at all possible. But if completely necessary, store in a cool or cold, dry, place when it is free of acidity. Acidity in this oil can cause the explosive decomposition of this oil in storage.

This oil, if handled or the fumes breathed, will cause tremendous ' headaches and should be avoided at all costs. They are cardiovascular dialators when contacted and extreme care should always be used when handling these explosives.

As stated earlier, these explosive oils have been produced in large quantities and therefore should be reasonably safe. This manufacture process should never be tried by someone that is unfamiliar witb chemistry, chemistry lab procedure, and the explosive compounds produced and their dangers.

Nitroglycerin and nitroglycol detonate at approximately 6700-8500 M/sec. depending on the power of the detonators - the stronger, the higher the velocity.

Sorbitol and Mannitol Hexanitrate!!!

4) Sorbitol Hexanitrate
This is very similar to Mannitol Hexanitrate (see below). Shock sensitive, small quantities burn rapidly if ignited. This procedure will produce a sticky liquid product, which is actually a mixture of nitrates. A solid product can be obtained by dissolving it in ethanol, and adding an equal volume of cold water to precipitate it. This will be pure Sorbitol Hexanitrate.
You will need:
5g of sorbitol,35mL of 70% nitric acid,70mL of 90% sulphuric acid,Distilled water,Sodium bicarbonate,Urea,Two 250mL beakers,A 500mL beaker,A thermometer,A hot water bath,A dropping pipette,An ice bath.
1) Put the sorbitol and nitric acid in a 250mL beaker, and cool it to 5*C in the ice bath.2) Stir it until all the sorbitol has dissolved.3) Slowly add the sulphuric acid, while stirring, making sure that the temperature does not rise above 10*C.4) After all the sulphuric acid has been added, dump the reaction into the 500mL beaker, containing 200mL of distilled water.5) Warm the water/acid/product mixture to 40*C to melt the Sorbitol Hexanitrate. It will settle to the bottom.6) Using the pipette, suck up the prodcut while still warm, and add it to the other 250mL beaker, containing 100mL of water and 10g of sodium bicarbonate.7) Warm it to 40*C, and stir it for 10 minutes.8) Add 5g of urea and stir it for a further 10 minutes.9) Suck up the Sorbitol Hexanitrate with the pipette, and let it dry in a warm place overnight.-=-=-=Mannitol Hexanitrate
"This is a different isomer of Sorbitol Hexanitrate, but this one is more widely used, as a base charge in blasting caps. This procedure produces a white powder, and yields seem to be higher. Lead block expansion for this explosive is a whopping 560 cm3, almost as high as Glyceryl Trinitrate! VoD is 7000 m/s, density is 1.60 g/cm3, relative brisance is 0.96 under these conditions.
To make it, use the procedure for Sorbitol Hexanitrate above, but use mannitol instead of sorbitol (duh...), use a mixture of 6mL of 70% nitric acid, 27g of potassium nitrate and 14mL of 98% sulphuric acid instead of the nitric acid, and use 30mL of 98% sulphuric acid. Omit the step in which the Sorbitol Hexanitrate is melted. Simply filter off the Mannitol Hexanitrate and recrystalise it from ethanol after washing and drying the crude product."------------------------However when 20 grams of mannitol which was ground very fine (beyond any crystalline make-up via ball mill) it was mixed into 130gr (72ml @ 93&) H2SO4 @ 20 C via magnetic stirrer until completely in solution. Material was stirred until transparent. Care was taken to prevent carbonization.The Mannitol-H2SO4 solution was then placed into a refrigerator to maintain temp of 15 C.A solid nitrate (KNO3) was mixed with H2SO4 in a separate beaker: 60gr KNO3 into 182 gr (100ml) H2SO4. This was prepared at 60C and stirred until clear solution was achieved. This solution of mixed acids was then placed in a refrigerator and both solutions brought to 15 C.The mixed acid solution was placed on a magnetic stirring device and into it was introduced the mannitol / H2SO4 solution in small portions (drop wise, 3 drops per second).The temp of 0-15 C was maintained for this addition & was achieved by using an ice and ethylene glycol ("anti-freeze") bath. During the addition the mixture became quite thick. At that juncture 50 ml of 70& HNO3 was added in two portions. The HNO3 being previously chilled to 15 C having been in a refrigerated environment. The solution continued to thicken and was withdrawn from the ice bath and stirring (total time 30 min, stirring) and placed covered in refrigerator. Allowed solution to remain in refrigerator at 15 C. After 2 hours solution solidified and appeared to have no mobility but appeared as a solid.
The nitration is reputed to proceed unevenly and due to the mass created by the forming crystals within the mixed acids this may certainly be true. That is a significant reason to add the liquid HNO3; to maintain the ability to stir the solution as well as add to the nitration level. Overall the nitration is slow but the initial reaction is such that a thick mass (of crystals) is created quite soon after the introduction of the mannitol / H2SO4. There will be both hexanitrate and pentanitrate within the initial nitration. It has been noted that the appearance of needle crystals as opposed to other shapes is indicative of hexanitrate and this should be the target of production after re-crystallization from alcohol. The re-crystallization if carried out a 2nd time will result in a granular formation which is ideal for utility usage and is not a reflection of pentanitrate formation at that time.
Random observations: After addition of mannitol / H2SO4 there appeared to be particulate matter forming in solution and would stick to side of beaker when tipped. At no time did solution appear clear. As soon as mannitol was introduced into mixed acids there appeared to be particulate matter in solution. NOx gas will evolve @100C after one hour. Solubility: Very sol in hot EtOh, MtOh, Acetone. Best is EtOh Acetone exhibits negative vapor pressure. Stability is achieved by addition of Na Salicylates. Also refer to US Patent 1751438 (Sorbitol Hexanitrate) regarding material's need for temp to maintain above a certain level to maintain solidity, etc.

Hybridized Composite Propellants.

I have seen some experimental formulations of modified or hybridized composite propellants enhanced in the performance through the addition of powerful nitramines, namely RDX, HMX and lately the CL-20. But I doubt if they were used actually in big boosters for launching rockets to space.These recipes don’t exactly fit the strictly category of the composite or double based propellants but more of a LOVA gun propellants but with the metal fuel.
One basic formulation range I recently "re discovered" from my files.
AP, 80-100um( oxidizer)
18-22AP 10-15 um ( oxidizer)
18-22RDX/CL-20 1.7-3.0um( oxidizer)
8-10AN( oxidizer)
10-15Polymeric binder
6-65Aluminum fuel
20-24Plasticizer
4-16Cure catalyst 0.03-0.06
Burn Rate Catalyst 0.2-0.5
Bonding Agent 0.06-0.12
Stabilizer 0.3-0.4
Curative 0.9-1,9
Cross Linker 0.3-0.35
A basic nitramine containing LOVA gun propellant look like this.
HMX(2 microns particle size)
75 HTTP( block copolymer)
11.867Of Propylene oxide& Ethylene oxide Trimethylolpropane
3.167Lysine diisocyanate methyl ester
9.9675Titanyl acetyl acetonate 0.025

That's the problem with hearing information second-hand, I suppose. You never know for sure who is right.

Methyl Ethyl Keytone Peroxide!!!!

Methyl Ethyl Ketone Peroxide

I went to the hardware store and, next to the impulse buys, there was some acetone, tolulene, and some methyl ethyl keytone. I already had purchased alot of acetone, so I bought some tolulene and methyl ethyl keytone. I plan on making Tri-Nitro-Tolulene (TNT), and Methyl ethyl keytone peroxide. I already had some sulfuric acid and 35% h202!

I already have a few TNT syths, so I decided to include a recipe for MEKP.
Alot of people are always wondering about this as an explosive. Here is a synthesis I found.

PREPARATION AND PROPERTIES OF METHYL ETHYL KETONE PEROXIDE
The three most common forms of methyl ethyl ketone peroxide are:
MONOMERIC: C4H10(O)4
DIMERIC: C8H18(O)6
ANHYDROUS DIMERIC: C8H16(O)4

The anhydrous dimeric form is the preferable form to create; it is more powerful and less sensitive to shock. Bot hforms are very sensitive to heat. Anhydrous dimeric methyl ethyl ketone peroxide takes many times as sharp of a blow from a hammer to initiate detonation than with trimeric acetone peroxide. This is due to several factors:
(1) It is an oily liquid, not a solid, A solid will not shift shape to fit its container, as will a liquid. Thus, when trimeric acetone peroxide is struck with a hammer, the crystals shatter, causing decomposition; when anhydrous dimeric methyl ethyl ketone peroxide is struck with a hammer, it will shift shape significantly, often avoiding decomposition.
(2) The C-O-O-C group is better shielded in anhydrous dimeric methyl ethyl ketone peroxide than in trimeric acetone peroxide. Thus, random energy surges will be less likely to affect the C-O-O-C group enough to break all of the bonds in the group, which would result in exothermic decomposition, likely starting a chain reaction; this would be perceived as detonation.
(3) There is less stress on the peroxide groups in anhydrous dimeric methyl ethyl ketone peroxide than in trimeric acetone peroxide (bond stress is mostly responsible for monomeric acetone peroxide's incredible instability, and anhydrous dimeric acetone peroxide's relative instability when compared to trimeric acetone peroxide).
(4) The decomposition to an exothermic stage of decomposition of a single molecule of anhydrous dimeric methyl ethyl ketone peroxide requires more energy than with a single molecule of trimeric acetone peroxide. (5) Less energy is liberated from the decomposition of a single anhydrous methyl ethyl ketone peroxide molecule, causing it to be less likely that detonation will occur from the decomposition of just a handful of anhydrous methyl ethyl ketone peroxide molecules. Perhaps the most valuable property of methyl ethyl ketone peroxide is the fact that it can be stored for a long period of time. Chemical decomposition does not proceed beyond the monomeric form, with the obvious exception of deflagration and detonation. Autonomous chemical decomposition is very slow when not in the presence of hydrogen peroxide (which causes the anhydrous dimeric form to begin to decompose slowly into the monomeric form). Because of this, it is wise to prepare anhydrous dimeric methyl ethyl ketone peroxide in an excess of methyl ethyl ketone (this fact has been factored into the below instruction on preparation of methyl ethyl ketone peroxide). Anhydrous dimeric methyl ethyl ketone peroxide is a thick, oily liquid. The anhydrous dimeric form, when pure, possesses a sharp, sour, acidic "burning" odor. The procedure for preparation that will soon be discussed will produce mostly the anhydrous dimeric form.

PREPARATION OF ANHYDROUS DIMERIC METHYL ETHYL KETONE PEROXIDE
CHEMICALS NEEDED: -40mL 27.5% H2O2 solution (other concentrations may be used; the volume of hydrogen peroxide solution will need to be adjusted accordingly; the quantity of sulfuric acid used will also need to be adjusted) -25mL Methyl Ethyl Ketone CH3COCH2CH3 (sold as a solvent at hardware stores; keep in mind that it will dissolve most plastics) -5mL 98% sulfuric acid (other concentrations may be used, the volume of sulfuric acid will need to be adjusted accordingly) -200mL NaHCO3 solution

1) Place 25mL of methyl ethyl ketone in a 100mL beaker. Place this beaker in an ice bath at temperatures ranging preferrably from -10 to 5 degrees Celcius; the lower end of the described recommended temperature range is preferrable.
2) Place 40mL of 27.5% H2O2 solution in a 100mL beaker. Place this beaker in an ice bath at temperatures ranging preferrably from -10 to 5 degrees Celcius; the lower end of the described recommended temperature range is preferrable.
3) Wait fro the temperature of both the methyl ethyl ketone and the temperature of the 27.5% H2O2 solution to fall into the recommended temperature range. Then, pour the beaker of methyl ethyl ketone into the beaker of hydrogen peroxide solution. Stir this solution for thirty seconds.
4) Add 5mL of 98% sulfuric acid slowly, drop by drop, taking care to keep temperatures within the recommended temperature range, into the beaker containing the monomeric methyl ethyl ketone peroxide. If the temperature rises above 5 degrees Celcius, stop adding the sulfuric acid immediately.
5) After all of the sulfuric acid is added, wait 24 hours. It is highly recommended to attempt to keep the temperatures within the recommended temperature range during the entirety of every step of the prepataion (this is a very common mistake made when attempting to make trimeric acetone peroxide; most will not bother to keep the temperatures around zero degrees Celcius while waiting 24 hours or so for the reaction to complete; the result of that is far less stable acetone peroxide due to lower yields of the trimeric form and higher yields of the dimeric form).
6) The beaker should now have two layers; a thick oily layer on the top, and a translucent white, relatively thin liquid on the bottom. The thick oily layer on top is the anhydrous dimeric methyl ethyl ketone peroxide. All traces of acid must now be removed. Pour this beaker into a 300mL beaker. Then slowly add 200mL of NaHCO3 solution. Stir vigorously for five minutes; try to keep the size of the pockets of the oily liquid (the anhydrous dimeric methyl ethyl ketone peroxide) as small as possible when stirring.
7) Most of the anhydrous dimeric methyl ethyl ketone peroxide will now begin to sink to the bottom of the beaker. Extract it with a syringe. Some will also remain on the surface; extract this also with a syringe (it is possible to isolate the anhydrous dimeric methyl ethyl ketone peroxide by decantation, but this process can be very time consuming, frusturating, and will not be able to harvest nearly as much of the anhydrous dimeric methyl ethyl ketone peroxide as the syringe extraction method). If you wish to further deacidify the anhydrous dimeric methyl ethyl ketone peroxide, place it in an airtight aluminum container, in an ice bath (extremely important!). Leave the methyl ethyl ketone peroxide in the airtight aluminum container until bubbles no longer form. A safer alternative to this process is to add noon-crumpled pieces of aluminum foil to the anhdrous dimeric methyl ethyl ketone peroxide (also in an ice bath); however this will often make it difficult to recollect all of the anhdrous dimeric methyl ethyl ketone peroxide, due to it sticking to the pieces of aluminum foil; it can be very difficult to remove from that surface.
9) Now pour the deacidified anhydrous dimeric methyl ethyl ketone peroxide into an open glass, or plastic (not made of a polyhydrocarbon plastic!). Let it stay in the open at temperatures around 15 degrees Celcius to allow most of the water to evaporate off.
10) Now that the anhydrous dimeric methyl ethyl ketone peroxide is dehydrated, it is ready for use.

STORAGE: Pour the anhydrous dimeric methyl ethyl ketone peroxide into a sealed plastic container (not made of a polyhydrocarbon plastic!) for storage. The reason for sealing it is to prevent loss of anhydrous dimeric methyl ethyl ketone peroxide due to evaporation. The lower the temperatures are during storage, the better, with the exception of temperatures so low that it freezes the anhydrous dimeric methyl ethyl ketone peroxide. Density of MEKP = 1.0g/cm3 Freezing point = approximately -5 to -10 degrees Celcius Dimeric 2-peroxybutane explodes upon contact with concentrated sulfuric acid. It seems that dimeric 2-peroxybutane (MEKP) is more stable than previously thought. It does not explode unless severely shocked. I have tried to explode as much as 4mL using only fuse, and that resulted in nothing but a tall pillar of flame. It does explode with a sharp crack when hit *hard* with a hammer. I suggest using aqueous ammonia instead of sodium hydrogen carbonate for neutralizing acid. A dimeric 2-peroxybutane / ammonium nitrate dynamite: 11mL (or grams) of dimeric 2-peroxybutane mixed with 100g of ammonium nitrate.

Sulfates, Barium Sulfate.

Most sulfates are not water soluble, are geologically stableand can be easily and cheaply obtained by mining, ratherthan having to be produced through complicated and expensivechemical processing. Therefore sulfates pass the first testfor possible inclusion in any pyro formula; they areinexpensive. Indeed native sulfates such as barite (BaSO4)and celestite (SrSO4) are the starting materials for otherbarium and strontium compounds used in fireworks.Sulfates certainly appear attractive because their oxygencontent compares favorably with that of metal chlorates,perchlorates and nitrates, as Table 1 illustrates. Also acomparison of the heat evolved from reaction of aluminum andvarious oxidizing agents again shows that sulfates comparefavorably with more familiar pyrotechnic oxidizers. (SeeTable 2.)

Table 1
Percent oxygen contained (percent by weight) for variouspyrotechnic oxidizers and sulfates, for the anhydrouscompound.
Nitrate Chlorate Perchlorate Sulfate
Ammonium 0.60 0.47 0.54 0.48
Barium 0.37 0.32 0.38 0.27
Calcium 0.58 0.46 0.41 0.47
Copper 0.51 0.42 0.49 0.40
Gadolinium 0.42 0.35 0.42 0.32
Lithium 0.69 0.53 0.60 0.58
Magnesium 0.65 0.50 0.57 0.53
Potassium 0.47 0.39 0.46 0.37
Sodium 0.56 0.45 0.52 0.45S
trontium 0.45 0.38 0.45 0.47

Table 2Heat produced (cal/g) from a mixture of an oxidizer orsulfate with aluminum. Values from AMCP 706-185(1967) and/orVasilev (1973) (*).
Sodium perchlorate 2,600
Lead nitrate 1,500
Sodium chlorate 2,500
Barium nitrate 1,400
Potassium perchlorate 2,400
Cu sulfate 1,400/1,560*
Potassium chlorate 2,200Ca sulfate 1,300/1,470*
Sodium nitrate 1,800Na sulfate 1,200/1,360*
Potassium nitrate 1,800K sulfate 1,200/1,180*
Lithium sulfate 1,620*Barium sulfate 900/910*
Magnesium sulfate 1,610*
Lead sulfate 800
Ammonium nitrate 1,600

However, low cost is not the only criteria for selectingoxidizers for use in fireworks compositions. A quick checkof Table 1 reveals several oxidizers with high oxygencontent, for instance, calcium, sodium, and ammoniumnitrates, sodium chlorate, and magnesium perchlorate.However, of these only sodium nitrate has found use, albeitlimited primarily to military pyrotechnics. All of thesecompounds are hygroscopic and therefore unusable in the realworld. In fact, magnesium perchlorate is used as a dryingagent under the trade name of "Anhydrone".There can be no doubt that the largest problem concerningthe use of sulfates as oxidizing agents is their waters ofhydration, for example:Na2SO4-10H2O and CuSO4-5H2O. Although the ten extra oxygenatoms in sodium sulfate raise its total oxygen content from45% to 70%, this extra oxygen contained in the waters ofhydration is not available for productive work. In truth itonly gets in the way, since a large amount of heat isrequired to first remove the water of hydration from acomposition's outer surface before the ignition temperaturecan be reached. Then once the reaction becomes selfsustaining, even more heat, produced by a burning star forinstance, will be removed from the reaction in the form ofvaporized water. (It should be noted that the latent heat ofvaporization for water is 540 calories per gram of water at100° C. This value represents heat that must be supplied bythe pyrotechnic reaction to change water at 100° C intosteam at 100° C.) There is also the possibility, inmagnesium containing compounds, of the water vapor reactingwith the magnesium forming hydrogen and magnesium oxide,effectively removing a large amount of fuel, with littlegain in heat. In the case of sodium sulfate decahydrate,where 56% of each molecule is water, 31,920 calories of heatwould have to be supplied simply to remove all the water ofhydration in the form of steam from each 100 grams ofsulfate. For example, in a composition using potassiumperchlorate as the oxidizer and aluminum as the fuel, 13.3grams of aluminum and potassium perchlorate would be neededjust to remove the water from each 100 grams of sodiumsulfate decahydrate, before any useful work (heat and/orlight) would be produced!As a further complication, the temperature at which watersof hydration are liberated varies from sulfate to sulfate,e.g., sodium sulfate decahydrate loses all its water at 100°C while manganese sulfate monohydrate does not lose all itswater until the temperature reaches 400-450° C! And toreally complicate things, manganese(II)sulfate can exist aseither mono, tri-, tetra, penta, hexa, or heptahydrate!Although the tetrahydrate is the most common form.However, US Patent 2,885,277 claims to make use of thewaters of hydration in magnesium sulfate heptahydrate,MgSO4-7H2O (Epsom salts), to produce hydrogen gas when thesulfate is reacted with magnesium. It is further claimedthat this combination will function as either a torch or asalute. It would be well to note that Ellern (1968, p. 272)expresses doubt concerning the safety and utility of suchmixtures.The use of sulfates as oxidizers suffers from yet anotherproblem. As Dr. Conkling (in press) has pointed out "Inpyrotechnics, the solid liquid transition appears to be ofconsiderable importance in initiating a self propagatingreaction. The oxidizing agent is frequently the keycomponent in such mixtures, and a ranking of commonoxidizers by increasing melting point bears a strikingresemblance to the reactivity sequence for these materials."Unfortunately the melting point of most sulfates is muchhigher than either chlorates, perchlorates or nitrates. Onlyfour sulfates (manganese, copper, zirconium and iron) havemelting points below that of barium nitrate, and these fourare well hydrated (tetra or penta). Melting points aresummarized in Table 3.

Table 3Melting point for various anhydrous oxidizers and sulfates.Values are from the CRC Handbook. d decomposes, sd slightdecomposition.

Copper perchlorate 82
Ag perchlorate 486
Iron perchlorate >100d
Thorium nitrate 500
Strontium chlorate 120
dTh perchlorate 501
Lithium chlorate 128
Ba perchlorate 505
Scandium nitrate 150
Sr nitrate 570
Manganese(III) sulfate 160
dBa nitrate 592
dAmericium nitrate 170
Zn sulfate 600
Copper sulfate 200
sd 650
dTh(I) sulfate 632
Silver chlorate 230
Silver sulfate 652
Lead chlorate 230
Mn(II) sulfate 700
Lithium perchlorate 236
Lithium sulfate 845
Sodium chlorate 248
Nickel sulfate 848
Magnesium perchlorate 251d
Sodium sulfate 884
Lithium nitrate 264
Ytterbium(III) sulfate 900
Calcium perchlorate 270
Yttrium sulfate 1000
Sodium nitrate 307
Cesium sulfate 1010d
Rubidium nitrate 310
Rubidium sulfate 1060d
Potassium nitrate 334d
Potassium sulfate 1069
Calcium chlorate 340
Samarium sulfate (basic) 1100
Potassium chlorate 356
Magnesium sulfate 1124d
Potassium perchlorate 400d
Lanthanum sulfate 1150
Zirconium sulfate 410
dsulfate 1170d
Cesium nitrate 414
Calcium sulfate 1450
Barium chlorate 414
Barium sulfate 1480
Iron sulfate 480d
Sr sulfate 1605d
Sodium perchlorate 482

It is evident that getting compositions based on sulfates asoxidizers to ignite while not impossible ... is not going tobe easy. There can be no doubt that it is going to take anextremely hot ignition source!Copper sulfate with its low melting point looks like a primecandidate but again, the water of hydration is a problem.Exposed to moist air, CuSO4 becomes CuSO4-H2O, and whenwetted, CuSO4-5H2O. Also, because copper sulfate is watersoluble, it is seldom found in native form (chalcanthite).Therefore it is manufactured from copper metal and sulfuricacid, and as a result fails the first test, it is not cheap.It is also not safe with chlorates.Although certainly attracting because of their low costoxygen content, sulfates have for the most part, not beenemployed as oxidizing agents. However, them have found theirniche in strobe formulas.Vander Horck (1974) reported on several formulas usingcalcium and copper sulfates demonstrated to him by BobWinokur who later (Winokur, 1974) made additional commentsabout them. Further Dr. Shimizu (1981) presents severalstrobe ("twinkler") formulas using sulfates, i.e.,strontium, barium, sodium and calcium. Advantage is taken ofthe great difficulty of igniting and then sustainingignition in sulfate based compositions. Therefore flashes oflight are produced each time the sulfate reaches its meltingpoint or decomposition temperature, burning commences andshortly thereafter extinguishes only to repeat, producingthe strobe light effect.Sulfates have long been used in color flame compositionsmore for their metal than oxygen content. However, for themost part, the color produced by sulfate based compositionsnot containing metal fuels such as aluminum or magnesium,will be found to be less than satisfactory, since only metalfuels are capable of producing the high temperaturesnecessary to melt or decompose most sulfates. The use ofvarious sulfates is detailed below:Copper sulfate: In older literature, e.g. Kentish (1878)compositions for blue flames can be found using coppersulfate and potassium chlorate, where the copper ion is usedto produce the blue color. THIS COMBINATION IS DANGEROUS.Safer and more effective blue formulations are available.Barium sulfate: Troy Fish (1981) recommends the use ofbarium sulfate in parlon bound green stars. He notes that asa result of barium sulfate's extreme insolubility (0.000413grams per 100 ml of boiling water!), it is one of the fewnontoxic barium compounds. I have been able to locate onlyseven formulas using barium sulfate, and all seven useeither magnesium, aluminum or magnalium.Calcium sulfate: Despite the many obstacles noted above,calcium sulfate hemihydrate (plaster of Paris) [CaSO4-1/2H2O] has been used as an oxidizer in fireworks andpyrotechnics: In combination with sodium and barium nitratein white light compositions (Ellern, 1968, formulas 36, 37and 38), as an incendiary when combined with aluminum (USPatent 2,424,937, Vol. 3 of the "Black Book", 1982), oraluminum and magnesium sulfate (US Patent 4,381,207), andwhen compounded with aluminum, Teflon, and sulfur (US Patent4,349,396) as a metal cutting torch.Calcium sulfate combined with either aluminum or magnesiumhas been suggested as a "flash report" mixture! (Sanford,1974)This sulfate is found in pink tableau fire or starcompositions using potassium perchlorate as the oxidizingagent. Weingart (1947) has the only modern formula I have been able to locate that uses calcium sulfatewithout either aluminum, magnesium or magnalium.Potassium sulfate: The Technico Chemical Receipt Book 1896long ago recommended the use of potassium sulfate in bluecompositions. There is only one modern formula usingpotassium sulfate, Dr. Shimizu's white "twinkler" usingmagnalium as the metal fuel.Strontium sulfate: This sulfate had long ago been used inthe production of red or purple flames. However, there areno formulas using strontium sulfate in Lancaster, Ellern orWeingart. There are however, three "twinkler" formulas inShimizu using strontium sulfate. All three containmagnalium.Sodium sulfate: I have been able to locate only fourformulas using sodium sulfate, all by Dr. Shimizu, who usessodium sulfate in combination with magnalium for yellowstrobe stars.Manganese sulfate: Perhaps the most interesting use ofsulfate is the addition of manganese sulfate (MnSO4 H2O) toaluminum sodium nitrate flare compositions. Farnell etal.(1972) discovered that this compound alters "thedecomposition of sodium nitrate to form oxides of nitrogenrather than its normal decomposition products of nitrogenand oxygen." This change results in a 55% decrease inburning rate, a 155% increase in luminous output, and a 466%increase in luminous efficiency!Although not a mainstays of the fireworks trade, sulfateshave found employment along with the proverbial kitchensink, used frying pans, oil of spike and philosopher's wool!!!

Literature cited
AMCP 706185, 1967, Engineering Design Handbook, MilitaryPyrotechnics SeriesPart 1; Theory and Application. NTIS AD 817071.Black Book, 1982, Improvised Munitions Black Book, Vol. 3.Desert Publications.Conkling, J., (in press), The Chemistry of Pyrotechnics andExplosives: Basic Principles and Theory. Marcel Dekker, NewYork.CRC Handbook of Chemistry and Physics, 1981, 62nd edition.Ellern, H., 1968, Military and Civilian Pyrotechnics.Chemical Publishing Inc., NY.Fish, T., 1981, Green and other colored flame metal fuelcompositions using parlor. Pyrotechnica Vll, pp. 2537.Farnell, Westerdahl and Taylor, 1972, The Influence ofTransition Metal Compounds on the AluminumSodium Nitrate Reaction. Third International PyrotechnicsSeminar.Kentish, T., 1887, The Pyrotechnists Treasury, The CompleteArt of FireMaking. Chatto and Windus, London.Sanford, R., 1974, Plaster of Paris flash powders, AmericanPyrotechnist Fireworks News, p. 527.The Technico Chemical Receipt Book 1896.Merck Index, 1983, The Merck Index: An Encyclopedia ofChemicals, Drugs, and Biologicals. Merck and Co., 10thedition.Shimizu, T., 1981, Fireworks: The Art, Science, andTechnique. Maruzen Publishing Co.US Patent 2,424,937, July 1947, Incendiary Composition.US Patent 2,885,277, May 1959, Hydrogen Gas GeneratingPropellant Compositions.US Patent 4,349,396, September 1982, MetalCutting Pyrotechnic Composition.US Patent 4,381,207, April 1983, Pyrotechnic Composition.Valsilev, A.A., et al., 1973, Combustion of mixtures ofmetal sulfates with magnesium or aluminum. Translated fromRussian. NTIS AD 785988, 5 pp.Vander Horck, M.P., 1974, Unconventional star compositionsdemonstrated. American Pyrotechnist Fireworks News, 7(4),issue no. 76, p. 506.Weingart, G. W., 1947, Pyrotechnics. Chemical PublishingCo., NY, pages 61 and 134.Winokur, R., 1974, More on unconventional stars. AmericanPyrotechnist Fireworks News, 7(5), issue no. 77, p. 516.

PICRIC ACID: a powerful and easy to make explosive. Step by step instructions with pictures!

TNPEN

TNPEN

molecular mass
318.16 g/mol d
ensity
1.25 g/mL
(O2N)3C6H2OCH2CH2(ONO2)
explosive velocity
appx 6000 m/s

TNPEN is an acronym for ß-(2,4,6-trinitrophenoxy) ethanol nitrate, also called 2,4,6-trinitrophenoxyethyl nitrate; or glycoltrinitrophenylether nitrate. TNPEN was first prepared by H.A. Lewis back in 1925, others have since revised the method, with this particular preparation developed by R.C. Elderfield in 1943. TNPEN will ignite when heated in the open and will detonate if struck as if by a hammer, so its stability is not that low, compared to TNT it is as stable and has 122% the explosive power. There is some conflicting data that indicates the stability may be lower. The recommended uses of this explosive are in detonators or boosters, and as an ingredient in propellents. The detonation velocity ranges from 5500 m/s to 6600 m/s depending on the density which can range from 1.15 g/mL to 1.6 g/mL
CHEMICALS APPARATUS
acetone beaker
ß-(2,4-dinitrophenoxy) ethanol 250-mL Florence flask
ethyl alcohol graduated cylinder
nitric acid filter paper
sulfuric acid stirrer/stirring rod
water thermometer


Prepare a solution of 10 g of ß-(2,4-dinitrophenoxy) ethanol in 55 mL of 94% sulfuric acid in a small beaker. Prepare a second solution of 21.5 mL of sulfuric acid, 13.2 mL of nitric acid, and 15.7 mL of water in a round bottomed 250-mL Florence flask, chill this solution to between 0-10 °C with a salt-ice bath. It does not matter what concentration of acids are mixed so long as the total water content comes out to 15.7 mL. While stirring, slowly add the ß-(2,4-dinitrophenoxy) ethanol solution to the cold acid mix. When the addition is complete, the temperature is raised in 30 minute intervals to 20 °C, 30 °C, 40 °C, 60 °C, and in a 15 minute interval to 70 °C. After chilling, the cream-colored crystals are filtered using glass filter paper, washed free of acid, and recrystallized by dissolving in acetone and adding ethyl alcohol. You will need a graduated cylinder for measuring liquids, a stirring rod or magnetic stirrer for mixing, and a thermometer to monitor the temperature.