Common Questions and Answers

 

The only problem I had while making it was that when you dump the finished nitrated liquid into ice water to precipitate the picric acid, a lot of the picric dissolves in the water. Is there any way to get the dissolved picric out of the water? Ensure you have enough ice and add just a little at a time. Keep it cool or it will fail to precipitate properly.

 

 

Safety – Picric Acid:

 

CAUTION! THIS COMPOUND MAY EXPLODE INSTANTLY WHEN TOUCHED WITH METAL

 

Also, don't inhale any of the fumes given off during the nitrate addition to the acid mix. Do all the heating and mixing outdoors or counter by having good ventilation in addition to wearing a gas mask (3M with acidic/vapor/organic filter).

 

It is best handled in a wet 10 percent distilled water form, as picric becomes very unstable when completely dry. This compound should never be put into direct contact with metal, since instantly on contact there is a formation of metal picric, which explodes spontaneously upon formation.

 

Any metal in contact with picric acid should be coated with an acid proof paint or an epoxy coat.

 

Modern safety precautions recommend storing picric acid wet. Dry picric acid is relatively sensitive to shock and friction, so laboratories that use it store it in bottles under a layer of water, rendering it safe. Glass or plastic bottles are required, as picric acid can easily form metal picrate salts that are even more sensitive and hazardous than the acid itself.

 

Safety glasses, adequate ventilation. If working with anything other than a solution or the wet solid full face protection is essential.

 

Maintain at least a 20% water content at all times. Never try to open a bottle of picric acid if crystals are visible at the rim of the bottle, even if the bottle contains water, since the friction when the cap is twisted may be sufficient to detonate the acid.

 

When the substance goes beyond a certain timeframe, it can become dangerous to transport so produce not longer than 2-4 weeks before use.

 

Unstable; may detonate if struck, heated or ground. Highly flammable if dry. May explode if dry - keep wet at all times. Keep water content above 20%. Incompatible with strong oxidizing agents, bases, most common metals, ammonia, strong reducing agents. Avoid shock, friction, heat. Compounds formed by reaction with metals are usually shock-sensitive explosives. The most serious hazard associated with this chemical is the risk of explosion, which is severe if the acid is dry. Nevertheless, it is at least 10-20 times as safe to handle (in regards to shock/friction, in dry form, compared to AP (A. Peroxide).

 

Shells which are to be loaded with these explosives are first plated on the inside with tin or painted with asphaltum varnish or Bakelite.

 

Always keep a bucket full of cold water close to production site in case everything goes wrong. Dump the compound in the bucket if you all else fail.

 

 

Manufacturing method 1 – Picric Acid/Trinitrophenol (from aspirin, Acetylsalicylic Acid)

 

Also called Picric Acid, TNP, Lyddite and Shimose. This explosive is slightly more powerful than TNT, and has a VoD of 7480 m/s at 1.76 g/cm3. Relative briscancy = 1.21

 

It can be used as-is, or to make the following explosives: Ammonium Picrate (Explosive D), DDNP and Lead Picrate.

 

It is relatively storage stable, but will form dangerously sensitive metal Picrates if it comes into contact with certain metals. To store it in absolute safety, make a saturated solution out of it in alcohol and store it in sealed glass containers. It can be stored indefinitely like this.

 

 

You will need:

 

96 aspirin tablets, each containing 300mg of aspirin,

120mL of 95% sulphuric acid,

60g of potassium nitrate,

Acetone,

Distilled water,

Some ice cubes (c. 10),

A pestle and mortar,

A gas or alcohol burner,

A 250mL conical flask,

A 1L container,

Two 250mL beakers,

A 500ml beaker,

A filter funnel,

A thermometer,

Filter papers,

A glass rod.

 

1) Place the aspirins in the pestle and mortar, and crush them. They don't have to be fine, but the finer they are the better.

 

2) Heat 150mL of acetone (methylated spirits will work) in a 250mL beaker until it's nearly boiling. Add the aspirin powder, and stir it with a glass rod until the grains have all disintegrated, leaving a small amount of white powder at the bottom of the alcohol.

 

3) Filter this liquid into the other 250mL beaker. Throw away the solid left on the filter paper.

 

4) Gently heat the filtrate to reduce its volume, until crystals begin to appear. Then let it cool and evapourate over night in a warm place.

 

5) Scrape up the crystals, and store them.

 

6) Heat the sulphuric acid to 65*C in a 250ml flask, and while it's heating up gradually stir in the purified aspirin using the thermometer.

 

7) When all of the aspirin has been added, let the solution cool to 50*C.

 

8) Add the potassium nitrate constantly, at a rate of about 1 to 2 grams every minute, while stirring rapidly. The temperature should be kept between about 60*C and 70*C. When I do this, I get very little nitrogen dioxide formed, just nitric acid vapours and CO2, formed by decarboxylation. Others claim to have clouds of nitrogen dioxide formed. This is because they add the potassium nitrate too fast, and it wastes the potassium nitrate.

 

9) When all of the potassium nitrate has been added, let the solution cool to roon temperature, and dump it into 300mL of distilled water, with the ice cubes, in a 1L container. This will precipitate out the Trinitrophenol as light canary yellow crystals.

 

10) Filter the liquid once most of the ice has melted, or remove the ice when the temperature is below 5*C, and discard of the liquid carefully as it is toxic and corrosive. You can concentrate it and extract slightly more Trinitrophenol, but it isn't really worth it..

 

11) Take the crystals formed, and add them to 100mL of boiling water in a 500mL beaker. Stir, and add more water until all the crystals have dissolved.

 

12) Cool the solution in the fridge, and filter out the purified crystals.

 

13) Leave them spread out to dry.

 

 

Manufacturing method 2 – Picric Acid/Trinitrophenol (from aspirin, Acetylsalicylic Acid)

 

How to produce picric acid (2,4,6- trinitrophenol) at home from common ingedients.

 

This method is based on the descriptions in "Improvised Kitchen Plastic Explosives II" by Tim Lewis using acetylsalicylic acid, sulfuric acid and either potassium or sodium nitrate.

 

The ratios given there are 40g acetylsalicylic acid (aspirin), 150ml sulfuric acid and 77g potassium or 58g sodium nitrate = 1: 3,75: 1,9 - acetylsalicylic acid: sulfuric acid: potassium nitrate.

 

First time I attempted to produce PA (picric acid) I used the ratios mentioned in "Kitchen Improvised Blasting Caps" by Tim Lewis and Mega's site. They suggest to use 100 crushed aspirin tablets/ 37,5g (very vague but some people mentioned the acetylsalicylic acid content to be 0,375g per tablet - maybe standard in the US?), 700ml sulfuric acid (!) and 75g of either potassium or sodium nitrate. I think this is too much sulfuric acid: when I poured the nitrated mix in the crushed ice & water it warmed so much all the ice melted and the shit was still warm. The yield was ca. 8g from 30g acetylsalicylic acid:-(acetylsalicylic acid purification

 

1. 120 aspirin tablets each containing 500mg acetylsalicylic acid and 50mg starch & microcristalline cellulose was crushed to powder.

2. This powder was dumped in 600ml of 60 °C ethanol (denaturated brand with 1% butanone) causing the acetylsalicylic acid to dissolve.

3. The hot alcohol/acetylsalicylic acid solution was filtered through two coffee filters.

4. The normally clear liquid (a little brown/yellow coloring resulted from using non-bleached filter paper) was evaporated on a boiling waterbath in a 2l steelbowl. This took about 80 minutes.

5. The result: pure, crystalline acetylsalicylic acid.

6. The acetylsalicylic acid crystals were spread in a glass dish and heated in oven at 70 °C for 30 minutes to evaporate the remaining ethanol. Result: 56g (60g theoretically) nitration

7. Then the 56g acid crystals were put in a 500ml erlenmeyerflask containing 220ml concentrated sulfuric acid 96%.

8. The acid was heated to dissolve the crystals. (Temp. around 70 °C)

9. 220ml sulfuric acid failed to dissolve all 56g acetylsalicylic acid. Small portions sulfuric acid was added until all acetylsalicylic acid was dissolved. Finally a total of 330ml sulfuric acid was used.

10. The dark red solution (~400ml) was poured in an 1000ml erlenmeyerflask. To prevent spreading clouds of NOx a 100ml erlenmeyerflask was put upside down in the mouth of the 1000ml erlenmeyerflask and only removed for nitrate addition.

11. The addition of 115g dry potassium nitrate (outside) was carried out in small portions using a folded piece of paper. This took 75 minutes. (The color of the solution changes with the addition of the nitrate from very dark red to a yellow/orange tone.)

12. After all potassium nitrate was added the solution was allowed to cool to room temperature. The hot liquid was clear, while cooling many tiny yellow crystals precipated until it was more or less thick slurry. (similar to AP slurry)

 

Precipitation & purification

13. A 1,5l glass standing in a plastic bowl was filled with 750g fine crushed ice (distilled water) and 250ml cold distilled water.

14. The acid was poured slowly into the ice/water mix. Because the acid was poured not slowly enough a *big* foaming started and some of the yellow foam and liquid was lost by overflow. SHIT - i wanted to know the yield of this method! A little red-brown NOx gas was released too, i think it was trapped in the foam.

15. Most of the crystals collected at the bottom of the glass after 20min, ca. 700ml liquid were carefully poured off and replaced by 500ml cold distilled water.

16. After waiting a few minutes for the crystals to settle again, the content was filtered through a coffee filter. The resulting liquid was disposed and the crystals scooped out of the filter. (No metals here, use wood or plastic!) Result: 120g of wet picric acid with unknown water content.

17. Now the 120g picric acid crystals were dissolved in 300ml boiling distilled water and then cooled to 25 °C (perhaps cooling it down to let's say 10 °C would increase the yield a little bit...) Again filtering through a coffee filter the crystals were scooped out of the filter and placed in a pyrex dish.

 

Drying & further processing

18. The pyrex dish with the PA was placed in an oven set to 80 °C, which was checked with a digital thermometer. (most of the time the temp. was around 75 °C) It remained there for 120 minutes.

19. The total amount of dry PA was 44g. What the fuck? There where 76g water in the first filtered crystal portion??? Or are there so much impurities that dissolve in the washing??? I filtered at ca. 25 °C, perhaps cooling it down to let's say 10 °C would increase the yield a little bit...

Optional - Plastic explosive

20. 4,4g white candle wax and 2,2g vaseline (peroleum jelly) were molten in a hot water bath, poured on the dry PA and kneaded in (suggested in KIPE II to produce a plastic explosive). However it didn't get very plastic although it's possible to form little balls that don't crumble. But without a container it will not hold together in larger quantities.

21. The 50g explosive mix were put in a pill box and fired with a 2g AP detonator. Very loud, but not as impressive as I thought. Maybe the wax shit wasn't the best idea, it becomes a little insensitive.

 

 

Manufacturing method 3 – Picric Acid/Trinitrophenol (from aspirin, Acetylsalicylic Acid)

 

From “Preparatory Manual of Explosives – Ledgard.pdf”

 

Picric acid is a pale yellow, odorless solid with a melting point of 123 celsius. It explodes when heated to 300 C. It is relatively insoluble in water, but soluble in alcohol and benzene. Picric acid is toxic and can be absorbed through the skin with effects similar to DNP. Picric acid should be stored wet with 10% water, and kept in a cool place and away from fire. Picric acid will detonate if rapidly heated or on percussion – the percussion is much higher than for most primary explosives.

 

VOD: 7400

Sensitivity: Low

Stability: Good

Flammability: Burns with smoky flame but may flash on strong ignition

Toxicity: Above moderate

Classification: Secondary explosive

Overall value (as secondary explosive): High

 

Materials:

50 g of aspirin

350 ml of 95% ethyl alcohol

350 g of 98% sulfuric acid

115 g of potassium nitrate or 95 g of sodium nitrate

 

Summary: In this procedure, picric acid is prepared by the reaction of common aspirin with potassium or sodium nitrate in the presence of excess concentrated sulfuric acid. After the reaction, the entire mixture is then drowned into an excessive amount of ice water, whereby the picric acid precipitates, and is then collected by filtration, washed and then dried.

 

Hazards: Use caution when handling 98% sulfuric acid, which is highly corrosive and chars many substances. Extinguish all flames before using 95% ethyl alcohol, which is flammable.

 

Procedure: Place 50 g of aspirin into a beaker, and then add 350 ml of 95% ethyl alcohol (note: about 50 g of aspirin can be obtained by crushing up 100, 500 mg tablets of store bought aspirin tablets – these crushed up tablets can be added directly to the 350 ml of 95% ethyl alcohol). Thereafter, stir the mixture to fully dissolve the aspirin, and then filter off any insoluble impurities – such as starch, and other fillers (if using medical aspirin tablets), and then recrystallize the aspirin from the 95% ethyl alcohol solution. Thereafter, vacuum dry or air-dry the collected aspirin crystals. Now, into a clean flask equipped with thermometer, motorized stirrer and powder funnel, place 350 g of 98% sulfuric acid, and then place this flask into an ice bath, and chill to 0 celsius. Thereafter, slowly add in small portions, 115 g of potassium nitrate or 95 g of sodium nitrate to the sulfuric acid over a period of about 1 hour, while rapidly stirring the sulfuric acid, and maintaining its temperature below 5 celsius. After the addition of the sodium or potassium nitrate, slowly add the dry recrystallized aspirin, in small portions, over a period of about 1 hour while rapidly stirring the sulfuric acid/nitrate mixture, and keeping it temperate below 5 celsius. After the addition of the aspirin, replace the powder funnel with a condenser, and reflux the mixture for 2 hours at 60 celsius while rapid stirring. After 2 hours, remove the heat source and allow the reaction mixture to cool to room temperature. Then gradually add the reaction mixture to 1500 ml of ice water, and then allow the entire mixture to stand for 3 hours. Thereafter, filter off the precipitated picric acid, wash excessively with 10, 250 ml portions of ice cold water. Note: washing with base to remove traces of acid should be avoided as formation of the corresponding picrate salts may develop. After the washing process, vacuum dry or air dry the solid product.

 

Note, equipment used: a condenser and a hot plate stirrer is a bonus but not required.

 

 

Manufacturing method 4 – Picric Acid/Trinitrophenol (from aspirin, Acetylsalicylic Acid)

 

 

1. Crush 20, 5 grain aspirin tablets and add 1 tsp. of water to it to make a paste.

 

2. 2. Stir in 1/2 cup of ethyl alcohol to the aspirin paste and then filter the solution to remove any solid particles.

 

3. Evaporate the alcohol and recover the crystals that are left.

 

4. Pour 1/3 cup of concentrated sulfuric acid into a large jar and add the crystals from the alcohol solution.

 

5. Heat the acid in a simmering hot water bath for 15 mins. The acid should turn a reddish color.

 

6. Now add 15 gms. of potassium nitrate to the acid 5 gms. at a time while stirring.

 

7. Let the acid cool to room temperature then pour the acid slowly into 1 1/2 cups of water and let it cool down again.

 

8. Filter off the particles of picric acid and wash them with 1 cup of ice water. Dry these crystals before using them.

 

Picric acid is a very strong dye. Contact with it will stain just about anything. Picric acid also reacts with metal to form picrate salts that are a hazard.

 

 

Alternative booster:

 

Bullseye gunpowder + NM

 

A high explosive can be composed out of bullseye gunpowder. Nitromethane is added to a quarter kilo of bullseye until it is the consistency of thick gel. Then one eighth of a kilo of pure ammonium nitrate (from cold packs) is added to it and kneaded. This is placed in a plastic bag and detonated in a metal pipe with #8 detonator. This has twice the power of C4.