Sam Barros’ ChemLabs!

Mission Statement:

ChemLabs’ main purpose is to supply the means of carrying out all of PowerLabs’ chemical procedure needs. It has served for electroplating, metal etching, fuel production / oxidizer production, and others. ChemLabs plays a key role in all of PowerLabs’ rocket research, plasma research, is used to produce fuel for my model planes, and has been in the past used for energetics research.

It should be noted on going through the list of experiments/demonstrations outlined here that most of them involve very serious hazards, either in the form of the chemicals utilized, in the procedures, or in the final products yielded by them. Due to that, these procedures have been written up entirely as illustrations-only, not as a how-to guide. None of the experiments below should be attempted by unqualified individuals working outside of laboratory conditions, and these procedures should not in any circumstances be followed. No claims are made as to the accuracy of these procedures, nor are the safety precautions all-inclusive.

The reason why most of  the experiments are so hazardous is because the intent here has been to show people the practical, interesting side of chemistry. Anyone can watch crystals grow or solutions change color in chemistry class, but the synthesis of energetic materials seems to be expressly forbidden in didactic laboratories and most chemists major without ever having seen it happen. PowerLabs here makes available for educational purposes that which you would otherwise not have access to.

On a more personal note, it is hoped that individuals will satisfy their curiosity by looking at these pages and not go on to try the experiments out by themselves. A quick search for “bombs” or “explosives” or any related word on any major Internet search engine will result in countless pages spreading some of the most stupid, ignorant, and misinformed procedures I have ever laid my eyes upon. This irritates me a great deal because anyone attempting these procedures will be putting themselves and those around them to great danger, and countless accidents have already happened and will continue to happen from people attempting things they see on the Internet. Removing those pages will not solve the problem; new ones will always come to replace them. Having reliable information will not solve the problem either, but it will certainly not aggravate it, and may even be beneficial in that people’s curiosities will be satisfied without the need for them to try it out for themselves. I am not enticing anyone to attempt any of this, I am only showing how it has been made to work safely. As such, the warning remains: PLEASE DO NOT TRY THIS AT HOME!

ChemLabs Demos:

Note: please be aware that the procedures listed here are only a rough draft. Only successful procedures are listed; synthesis that did not work or failed to synthesize the desired chemical are not provided.

  •  Secondary H.E.:

Nitrocellulose synthesis: From varnishes to plastics, rocket fuels and explosives, a full illustrated procedure outlining the different forms of nitration to produce this very useful industrial product. Included are videos of two different forms of NC deflagrating.
Nitro Starch synthesis: A chemical compound similar to Nitrocellulose, and like it capable of deflagration. This compound presented special challenges in purification; the final, successful procedure is outlined and a video showing the deflagration is available.
Nitromannitol synthesis: A nitrated simple sugar, capable of deflagration from flame and detonation from impact.
Nitroglycerine synthesis: One of the first high explosives ever created, it still finds a lot of uses as dynamite in mining and road construction.
Picric Acid synthesis: A chemical very similar to TNT,  found in most laboratories nowadays, useful as a dye, or as a starting base for metal picrates such as those found in the L.E. section. Also capable of detonation. Video of combustion available.
Styphnic Acid synthesis: A PowerLabs exclusive; chemically similar to Picric Acid, but more reactive and prone to initiation, this is the starting chemical for the synthesis of Lead Styphnate, the number one priming compound used nowadays. Includes video of final compound deflagration.
PETN: This compound sports one of the highest detonation velocities of any explosives known and is used in DetCord.

  •  Primary H.E.:

Mercury, Silver and Copper Fulminate synthesis: Some of the earliest explosives ever discovered, fulminates detonate violently on flame, impact, or friction, even unconfined. Videos available, as well as further information on more exotic (gold, platinum, double) fulminates.
Silver and Copper Acetylide synthesis: Acetylide and Carbide salts are notoriously explosive. Capable of DDT in even single crystal amounts. Videos available.
Mercury and Silver Oxalate synthesis: A chemical curiosity. Self decomposes on heating and is said to be explosive. A PowerLabs exclusive with video.
Lead Picrate synthesis: Useful as a priming compound. Detonates from flame; video.
Potassium Picrate synthesis: Chemical curiosity; one of the more powerful/sensitive picrates; Deflagrates from flame.
Lead Styphnate synthesis: PowerLabs exclusive: the number one priming compound used nowadays. Detonates violently from flame, as seen on video.
Potassium Styphnate synthesis: Chemically similar to Lead Styphnate, deflagrates violently to form a spectacular fireball on video.
Explosive Peroxides: Tricyclopropanone Triperoxide, Benzoyl Peroxide and HMTD (Hexametylene Triperoxide Diamine).

  •  L.E., Deflagrating, Self Sustaining, and Hypergolic reactions:

PowerLabs overview of Deflagrating chemicals, and Potassium Bromate oxidizer demo: A very powerful deflagrating compound is produced with KBrO3 to demonstrate its oxidizing powers. It burns faster than blackpowder when initiated by a drop of sulphuric acid (video).
Sodium Metal in Water: The demo we all saw at school, done in PowerLabs scale 🙂
Chlorate Oxidizers: The readiness with which Potassium and Sodium Chlorate give up their oxygen is demonstrated in two deflagration reactions, one including an M&Ms chocolate, on video!
Potassium Permanganate Hypergol: 3 different versions of a a classic self starting chemical delayed deflagration, with different delays (video!).
Sodium Peroxide Hypergols: Na2O2 is such a powerful oxidizer that on contact with paper or cotton it deflagrates with enough heat to break and melt a Pyrex beaker! (video).
Vesuvian Volcano (Ammonium Dichromate self decomposition): A chemistry lecture classic, on video.
Industrial grade (70%) HydroFluoric acid on glass: 70% HF will eat through a small test tube in under a minute, and generate enough heat to boil in the process! (video).

ChemLabs Supplies:

ChemLabs had the following reactants at its disposal. Notice how no inherently unstable materials are stored; this is vitally important; even in industrial laboratories terrible accidents have happened and continue to happen due to the storage of energetic materials and such accidents are even more common in home laboratories. The only way to ensure that an unstable compound does not explode in storage is to not store it in the first place. With the reactants below it is possible by acid/base neutralization or nucleophilic substitution to produce virtually any fluoride/chloride/phosphate/sulphate/nitrate/acetylide/fulminate/fuel-oxidizer deflagrant mixture, as needed. It is also possible to produce many other chemicals using the ones outlined below as a starting base (in fact several of the chemicals below were produced in such a way).
It is always vital to be thoroughly familiar with a chemical before attempting to utilize it for any synthesis or procedure. For this reason, selected MSDS (Materials Safety Data Sheets) are linked from the name of each chemical below. Never attempt to work with unknown chemicals or chemicals at unknown concentrations before reading about all of its properties and incompatibilities.
(Notice: These chemicals made up part of ChemLabs. They were not for sale nor do I still posses them). DO NOT CONTACT ME ATTEMPTING TO BUY CHEMICALS. I DO NOT SELL CHEMICALS NOR DO I KNOW WHERE TO BUY THEM FROM IN WHATEVER COUNTRY/STATE YOU HAPPEN TO LIVE IN.

To obtain most of the chemicals listed below, be sure to visit our sponsor (and tell them PowerLabs sent you):

ChemLabs Supplies

Acids

Sulfuric (H2SO4)

Nitric (HNO3)

Hydrofluoric (HF)

Hydrochloric (HCl)

Perchloric (HClO4)

Picric (C6H3N3O7)

Acetic Glacial
(C2H4O2)

Phosphoric (H3PO4)

Oleic (C18H34O2)

Acetylsalicylic (C6H8O4)

Salicylic (C7H6O3)

Citric Anhydrous (C6H8O7)

Boric (BH3O3)

Chromic (HCrO3)

Acetic Anhydride (C4H6O3)

Oxalic (C2H2O4.2H2O)

Formic (HCOOH)

Maleic (C4H2O3)

Styphnic (C6H3N3O8)

Solvents/Liquid Fuels

Absolute Ethanol (C2H6O)

Octilic Alcohol 100mL

Methanol (CH3OH)

Isopropyl Alcohol ((CH3)2CH2O)

Polyvinyl alcohol ([-C2-H4-O-]x)

Ethylene Glycol (C2H6O2)

Sulphuric Ether (C4H10O)

Petroleum Ether (30 � 60C)

Ethyl Ether (C4H10O)

Toluene (C7H8)

Heptane (CH3(CH2)5CH3)

Hexane (C6H14)

Chloroform (CHCl3)

Formol (CH2O)

Glycerine (C3H8O3)

Acetone ((CH3)2CO)

Xylene (C6H4(CH3)2) 

Distilled water (H2O)

Benzene (C6H6)

Propylene Glycol (C3H2O8)

Oxidizers

Hydrogen Peroxide (H2O2)

Benzoyl Peroxide (C14H10O4)

Sodium Peroxide (Na2O2)

Sodium Nitrate (NaNO3)

Potassium Nitrate (KNO3)

Barium Nitrate (Ba(NO3)2)

Strontium Nitrate (Sr(NO3)2)

Calcium Nitrate (Ca(NO3)2) 25g

Silver Nitrate (AgNO3)

Zinc Nitrate Zn(NO3)2.6H2O

Lead Nitrate (Pb(NO3)2)

Copper Nitrate (Cu(NO3)2.3H2O)

Ammonium Nitrate (NH4NO3)

Potassium Permanganate (KmnO4)

Sodium Chlorate (NaClO3)

Potassium Chlorate (KClO3)

Potassium Perchlorate (KClO4)

Ammonium Perchlorate (NH4ClO4)

Ammonium Chromate ((NH4)2CrO4) 25g

Ammonium Dichromate ((NH4)2Cr2O7)

Potassium Dichromate (K2Cr2O7)

Potassium Bromate (KbrO3)

Copper Sulphate (CuSO4)

Barium Sulphate (BaSO4)

Aluminium Sulphate (AlSO4)

Copper Oxide (CuO) (II)

Iron Oxide (Fe2O3)

Mercury Oxide (HgO) both Red and Yellow

Aluminium Oxide (alumina, Al2O3)

Lead Monoxide (PbO)

Barium Oxide (BaO)

Magnesium Oxide (MgO)

Manganese Dioxide (MnO2) 

Chromium Trioxide (Cr2O3)

Arsenic Trioxide (As2O3)

Potassium Iodate (KIO3)

Resublimated Iodine (I)

Chromium Trioxide (CrO3)

Calcium Hypochlorite (Ca(ClO)2) 

Sodium Hypochloride (ClNaO) 

Solid Fuels

Metallic Sodium (Na+)

Magnesium Powder (Mg)

Aluminum Powder (Al)

Magnesium Shavings (Mg)

Aluminum shavings (Al)

Iron Powder (Fe)

Zinc Powder (Zn)

Sulphur (S)

Sucrose (C12H22O11)

Starch, water soluble (C6H10O5)n

Copper Shavings (Cu)

Activated Carbon Powder (C)

Hexamine (C6H12N4)

Naphthalene (C10H8)

Urea 99% (NH2CONH2)

Calcium Carbide (CaC2)

Metallic Mercury (Hg)

Menthol (C10H20O)

Nitrocellulose Lacquer (C6H12O2)

Phenol (C6H5OH)

Mannitol (C6H14O6)

Resorcinol (C6H6O2)

MEK (Methyl Ethyl Ketone) (C4H8O)

Others:

Potassium Chloride (KCl)
Copper Chloride (CuCl2.2H20)
Potassium Carbonate (K
2CO3)
Mercury Iodide (HgI2) (red)
Mercury Chloride (HgCl2)
Mercuric Acetate ((CH3COO2)2Hg)
Potassium Ferrocyanide (KFe(CN)4)
Calcium Carbonate (CaCO3)
Sodium Carbonate (NaCO3)
Sodium Nitrite (NaNO2)
Ammonium Carbonate (NH3CO3)
Potassium Iodide (KI)
Neutral Lead Acetate (C4H6O4 Pb.3H2O)
Calcium Acetate ((Ch3COO2)2CaH2O)
Fluorescein 

A Small Tour of ChemLabs:
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Hazardous Items

The more hazardous items are kept in a cupboard for added safety. The acids and bases come in large bottles; the brown ones are for light sensitive chemicals such as hydrogen peroxide and nitric acid, and the large heat resistant 1L graduated Schott Duran for Sulphuric. The smaller bottles (250, 100, and 50mL) contain chemicals that are not used frequently, are very expensive, or are too hazardous for mass storage (examples include mercury metal, sodium peroxide, phosphoric acid, arsenic, etc). Oxidizers and solids in general come in plastic bottles ranging from 25g to 1kilogram. The Hydrofluoric and Perchloric acid, and the distilled water all come in Teflon bottles. These feel like they are constantly covered in oil or butter, due to the extremely low coefficient of friction of PTFE.

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Glassware & More

Some of the glassware includes Beakers (50, 100, 150, 250, 300, 400, 500, 600, 800, 1000mL, two of each), Erlenmyer flasks (2x 50, 2×100, 250, 1000mL), Filtration flasks (250 and 150mL), Test tubes (200x20mm and 15x10mm, 8 of each, all with accompanying rubber corks), glass balloons (100, 250mL), flat bottom flasks (50, 100, 150mL), buchner funnel, decanting flasks, glass funnels, hourglasses of assorted sizes (10), alumina ceramic mortar and pestle (250 and 600cc), glass pipettes (2×10, 25, 50 and 100mL), pipette pumps, titration pipette, thermometers (-10 to 250C mercury and 2 alcohol ones from -30 to 150C), pincers (3), scalpels (3), glass stirrers, boiling beads, metal spoons and spatulas, and many others. All this glassware was manufactured in Germany, and is “Duran”, by Schott. This is the highest quality glassware I have ever seen, as it is even more heat resistant than Pyrex. I only managed to break one piece of glassware by thermal shock so far (the Sodium Peroxide experiment above shows how it happened). It also withstands impact better than regular glass, though I have always been extremely careful not to drop them because of their price (several times that of ordinary glassware).
For the hydrofluoric acid experiments a 1L polyethylene beaker was obtained. It held up O.K. but became permanently stained; unfortunately Teflon beakers could not be obtained for the purpose of those experiments, even though they would be more appropriate.

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Advanced Equipment

Some of the more “advanced” equipment includes a 0 – 360C thermostat controlled hotplate (300W), a 50cm long serpentine glass condenser (both seen on the picture to the left, which show a distillation apparatus set up for the distillation of Nitric Acid. Not show in the apparatus is the venturi pump and vacuum line, which was necessary for reduced pressure distillation). The picture to the right shows a vacuum dissector. It consists in a 10L glass vessel weighting over 15kilograms, containing 2 kilos of Silica Gel in the bottom, and attached to a vacuum pump. A substance to be dried is placed inside the dissector and a vacuum is pulled inside it with the attached pump (in this picture a refrigerator pump is being used. This worked reasonably well and could dry most things within a couple of hours). As the water evaporates from the material it becomes trapped in the silica gel. Once the silica has become saturated (evidenced by it change of color from blue to pink, thanks to a cobalt indicator added to it) it needs to be heated at 150C for a couple of hours so it can once again perform its duty. This dissector greatly increased the speed of the procedures in the lab, making procedures that require multiple crystallizations take hours, as opposed to days. It was found that Silica can absorb most solvents almost as well as water, though it deteriorates quicker in doing so.

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More Chemicals

I was fortunate enough to find someone to buy my chemicals once I moved out of Sao Paulo and could not take them along with me to USA. Shown above are two of the six boxes in which they were put. The box to the right contains fluorescein, and miscellaneous fuels. The box to the right contains mostly acids, from which I can identify 9 litres of 99.8% analytical grade Sulphuric Acid, 10 litres of 68% analytical grade Nitric Acid, and a half kilogram bottle of  Benzoyl Peroxide (stabilized by the addition of 20% water). There are also some oxidizers in the box.

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Safety Equipment

Not shown also are all the safety equipment required for working with some of the hazardous chemicals above. These include an organic vapor-rated activated carbon filter gas mask, polycarbonate goggles, face shield, nitrile gloves, fume cupboard, fire extinguisher, earmuffs, and others.