Sam Barros' ChemLabs!

 
 
 


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Introduction:

 Chemistry in action!
  ChemLabs is Sam Barros' PowerLabs chemistry division. Whilst PowerLabs mostly deals with electronics, mechanics, physics and engineering on a practical aspect, ChemLabs focuses almost entirely on the practical aspects of chemistry. At some point in time ChemLabs was a fully equipped laboratory with over 150 analytical grade reactants and various pieces of specialized lab glassware and equipment available, suitable for performing almost any conceivable non-industrial chemical procedure or synthesis.
  The laboratory described here was my second chemical lab (the first one was located in Holland and didn't have a fraction of what this one had) and was assembled over a period of approximately one year, during which a couple thousand dollars was invested in every obtainable reagent as well as all the equipment required to handle those reagents, and a couple hundred hours went into using these reagents to synthesize reagents which could not be obtained: This was the case for all the Perchlorates, Nitrates (except NaNO3), Chlorates (except NaClO3), paraformaldehyde, Hexamine, Styphnic and Picric Acid, and others, although the more hazardous chemicals were only synthesized when needed, so as to reduce any danger associated with storing unstable chemicals.
 This page continues to be updated as time permits: several other experiments still need a write-up.
 Please note the following:
 PowerLabs does NOT sell any type of chemicals, or distribute any information about these topics aside from what is made available here.
 

 

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):


  Be sure to click the MSDS link to view safety information for the chemicals described below.

Acids

Bases

Solvents/liquid fuels

Oxidizers

Solid Fuels

Sulfuric (H2SO4) 98% 3000mL

Ammonium Hydroxide (NH4OH) 24% 250mL

Absolute Ethanol (C2H6O) 99.6% 1L

Hydrogen Peroxide (H2O2) 34% 1L

Metallic Sodium (Na) 99.5% 25g

Nitric (HNO3) 65% 3500mL

Potassium Hydroxide (KOH) 85% 250g

Octilic Alcohol 100mL

Benzoyl Peroxide (C14H10O4) 98%, moist! 1000g

Magnesium Powder (Mg) 99% 100g

Hydrofluoric (HF) 70% 1000mL

Sodium Hydroxide (NaOH) 97% 500g

Methanol (CH3OH) 99.5% 500mL

Sodium Peroxide (Na2O2) 96% 50g

Aluminium Powder (Al) 99.5% 25g

Hydrochloric (HCl) 50% 1000mL

Aluminium Hydroxide (Al(OH)3 56% 250g

Isopropyl Alcohol ((CH3)2CH2O) 95% 100mL

Sodium Nitrate (NaNO3) 99% 250g

Magnesium Shavings (Mg) 50g

Perchloric (HClO4) .75N 1000mL

Calcium Hydroxide (Ca(OH)2) 97%

Polyvinyl alcohol ([-C2-H4-O-]x) 95% 500g

Potassium Nitrate (KNO3) 99% 25g

Aluminium shavings (Al) 25g 99%

Picric (C6H3N3O7) saturated water solution 500mL

Sodium Bicarbonate (NaHCO3) 99% 250g

Isobutyl Alcohol (C4H10O) 100mL

Barium Nitrate (Ba(NO3)2) 99% 350g

Iron Powder (Fe) 99.5% 250g

Acetic Glacial
(C2H4O2) 99.5% 100mL

 

Ethylene Glycol (C2H6O2) 99% 500mL

Strontium Nitrate (Sr(NO3)2) 99% 250g

Zinc Powder (Zn) 99% 25g

Phosphoric 85% (H3PO4)

 

Sulphuric Ether (C4H10O) 70% 100mL

Calcium Nitrate (Ca(NO3)2) 25g

Sulphur (S) 99.5% 85g

Oleic (C18H34O2) 99.5% 100mL

 

Petroleum Ether (30 � 60C) 500mL

Silver Nitrate (AgNO3) 99.5% 25g

Sucrose (C12H22O11) 99.5% 25g

Acetylsalicylic (C6H8O4) 99% 250g

 

Ethyl Ether 99.8% (C4H10O) 500mL

Zinc Nitrate Zn(NO3)2.6H2O 98% 25g

Starch, water soluble (C6H10O5)n 99% 50g

Salicylic (C7H6O3) 99% 250g

 

Toluene (C7H8) 100mL

Lead Nitrate (Pb(NO3)2) 99% 25g

Copper shavings (Cu) 99.5% 25g

Citric Anhydrous 99.5% (C6H8O7) 25g

 

Heptane (CH3(CH2)5CH3) 1000mL

Copper Nitrate (Cu(NO3)2.3H2O) 98% 250g

Activated Carbon powder (C) 99% 25g

Boric (BH3O3) 80g

 

Hexane (C6H14) 95% 100mL

Ammonium Nitrate (NH4NO3) 99% 50g

Hexamine (C6H12N4) 98% 200g

Chromic 99% (HCrO3) 100g

 

Chloroform (CHCl3) 99.8% 500mL

Potassium Permanganate (KmnO4) 99% 275g

Naphthalene (C10H8) 99% 50g

Acetic Anhydride (C4H6O3) 99% 450mL

 

Formol (CH2O) 37% 250mL

Sodium Chlorate (NaClO3) 99% 250g

Urea 99% (NH2CONH2) 25g

Oxalic (C2H2O4.2H2O) 99,5% 25g

 

Glycerine (C3H8O3) 99%100mL

Potassium Chlorate (KClO3) 98% 500g

Calcium Carbide (CaC2) (99%) 250g

Formic (HCOOH) 85% 250mL

 

Acetone ((CH3)2CO) 99.5% 450mL

Potassium Perchlorate (KClO4) 98% 100g

Metallic Mercury (Hg) 125g

Maleic (C4H2O3) 99% 25g

 

Xylene (C6H4(CH3)2) 100mL

Ammonium Perchlorate (NH4ClO4) 98% 100g

Menthol (C10H20O)

Styphnic (C6H3N3O8) 99% 25g

 

Distilled water (H2O) 99.98% 3000mL

Ammonium Chromate ((NH4)2CrO4) 25g

Nitrocellulose lacquer 30% 100ml

 

 

Benzene (C6H6) 99% 100mL 

Ammonium Dichromate ((NH4)2Cr2O7) 25g

Phenol (C6H5OH) 99% 75g

 

 

Propylene Glycol (C3H2O8) 99% 1L 

Potassium Dichromate (K2Cr2O7) 100g

Mannitol (C6H14O6) 99,5% 250g

 

 

 

Potassium Bromate (KbrO3) 500g

Resorcinol (C6H6O2) 99% 250g

 

 

 

Copper Sulphate (CuSO4) 99% 25g

MEK (Methyl Ethyl Ketone) (C4H8O) 99% 100mL

 

 

 

Barium Sulphate (BaSO4) 25g

 

 

 

 

Aluminium Sulphate (AlSO4) 50g

 

 

 

 

Copper Oxide (CuO) (II) 99% 250g

 

 

 

 

Iron Oxide (Fe2O3) 250g

 

 

 

 

Mercury Oxide (HgO) both Red and Yellow 50g total

 

 

 

 

Aluminium Oxide (alumina, Al2O3) 100g

 

 

 

 

Lead Monoxide (PbO) 99%  500g

 

 

 

 

Barium Oxide (BaO) 99% 25g

 

 

 

 

Magnesium Oxide (MgO) 98% 25g

 

 

 

 

Manganese Dioxide (MnO2) 95%

 

 

 

 

Chromium Trioxide (Cr2O3) 99% 100g

 

 

 

 

Arsenic Trioxide (As2O3) 50g

 

 

 

 

Potassium Iodate 99% (KIO3) 50g

 

 

 

 

Resublimated Iodine (I) 99% 100g

 

 

 

 

Chromium Trioxide (CrO3) 100g 99%

 

 

 

 

Calcium Hypochlorite (Ca(ClO)2) 99% 500g

 

 

 

 

Sodium Hypochloride 12% 500mL 

 

Others:

Potassium Chloride (KCl) 99.5% 300g
Copper Chloride (CuCl2.2H20) 25g 98%
Potassium Carbonate (K
2CO3) 100g
Mercury Iodide (HgI2) (red) 25g
Mercury Chloride (HgCl2) 25g
Mercuric Acetate ((CH3COO2)2Hg) 97% 25g
Potassium Ferrocyanide (KFe(CN)4) 25g 98.5%
Calcium Carbonate (CaCO3) 50g
Sodium Carbonate (NaCO3) 25g
Sodium Nitrite (NaNO2) 80g
Ammonium Carbonate (NH3CO3) 25g
Potassium Iodide (KI) 99% 50g
Neutral Lead Acetate (C4H6O4 Pb.3H2O) 250g 99%
Calcium Acetate ((Ch3COO2)2CaH2O) 99%
Fluorescein 1% solution 500mL

 

 

 A Small Tour of ChemLabs:

Lab overview 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.

 

 

Some assorted glassware. Some of the glassware includes Beakers (50, 100, 150, 250, 300, 400, 500, 600, 800, 1000mL, two of each), Erlenmyer flasks (2x 50, 2x100, 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 (2x10, 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.

Distillation apparatus and Vacuum Dissicator set up. 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.

Two boxes full of 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. Show to the left 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 9litres of 99.8% analytical grade Sulphuric Acid, 10litres 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.

  Chemical storage shelfs.
 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.

 Questions? Comments? Suggestions? Don't hesitate to e-mail me!

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Last updated 11/02/10

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 Copyright (c) 1999 - 2009 by Sam Barros. All rights reserved.
 Removing any material from this site for display without consent from its author consists in an infringement of international copyright laws and can result in fines up to $50000 per infringement, plus legal costs. So ASK ME before you remove anything from here.