HOMEMADE CYANIDE
Cyanide is the granddaddy of synthetic poisons. Easily made from common chemicals, cyanideis used as is for poisoning bullets and food, and is used in the making of Hydrogen Cyanide,Cyanogen Chloride, Tabun, and numerous other poison gases. A dose as small as 50 milligrams (ingested) can kill an adult man. Of course, the more thebetter.To make cyanide, you must first make ferrocyanide. This can either be made, or preferably,bought.
Ferrocyanide Preparation
Ferrocyanide is obtained by heating 10 parts (by weight) potassium (or sodium) carbonate; 10parts coke. cinders, or coal; and 3 parts iron turnings, all in coarse powder. to a full red heat inan open crucible, stirring occasionally until small jets of purple flame arc no longer seen. Whencool, the soluble matter is dissolved out of it, the solution filtered, evaporated, and crystallized.The crystals obtained are redissolved in hot water and cooled very slowly, forming large yellowcrystals of the ferrocyanide.In order to obtain a pure form, melt dried ferrocyanide in a glass vessel and let cool, dissolvethe fused mass in water, neutralize any excess of alkali with acetic acid (vinegar), andprecipitate the salt by adding strong alcohol to the solution. Wash the precipitate with a littleweak alcohol, redissolve it in water, and crystallize.Sodium Ferrocyanide (Na4Fe(CN)6-10H2O, FW 484.07, mp 82C, CAS# 13601-19-9, AKAYellow Prussiate of Soda) can be ordered quite cheaply from www.sciencealliance.com.Catalog #s and prices are: C7435-100 100g $4.12, C7435-500 500g $8.96. And there's nohazardous shipping fees for it either. Cyanide costs about $47 a pound plus $15 hazardous.
Cyanide Preparation
To convert the ferro to cyanide do this (please note that these instructions were for thepotassium not sodium salt. I'm assuming that the ratios are similar for both); Mix thoroughly 8parts of dry sodium ferrocyanide and 3 parts dry sodium carbonate (pool pH adjuster), heatthem in a steel container (cleaned oil filter can works nicely), with constant stirring (use clotheshanger, straightened out), with a propane torch or other intense heat source till it melts into aclear liquid. Heating is continued until the mix no longer fizzes and the fluid portion is colorless. After a few minutes rest, to allow the contents to settle, the clear portion is poured from theheavy black sediment (iron) at the bottom at the bottom of the crucible and onto to a clean slabor steel bowl. It's then broken up while still warm and stored in airtight bottles. This will be
almost pure cyanide.
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RICIN
Ricin is just about the easiest, and at the same time, most toxic poison that a criminal canmake. Less than a milligram (1/1,000 of a gram) injected or inhaled will kill a person severaltimes over. For individual killings, it has the advantage of being undetectable in toxicologyscans since the poison is a catalyst the starts a chain reaction in the body, and is destroyedbefore the symptoms begin to show.With properly sized and dispersed dry particles, ricin is at least 10x more toxic than the mostpotent nerve gas. A 1% water solution atomized with a small explosive burster has the sameeffectiveness as sarin nerve gas. The only disadvantage ricin has is the time it takes for thevictims to die is about 1 - 2 weeks. So you won't have the quick tactical effect of nerve gas. Butthis can also be good in that, using a covert dissemination, the criminal has time to escapebefore the attack is detected.The information presented below is from a US Patent #3,060,165, assigned to the US Army.
Tips
Here's a few things you need to know to make your production go much easier.The seeds are readily available through wholesale seed suppliers for about $20 for apound of seeds.Castor bean seeds are very tough to crack or peel. Soak them for anhour in a solution of 2 tablespoons lye in 1 cup water. Then use pliers to crack the shell.The shell will peel of the bean easily then.1. Use a 1/2 cup of acetone to every ounce of bean pulp. Blend well. Let sit for several dayswith occasional shaking. Pour off the acetone and add an additional 1/2 cup of acetoneand repeat. This will remove almost all the castor oil from the seeds.2. The patent doesn't mention it, but you can use magnesium sulfate (Epsom salt) instead of sodium sulfate. Epsom salt is easily available in any drug store for just about a dollar apound.3. Use a plastic membrane filter if you can get them. The ricin forms a layer that is difficult toremove from a regular coffee paper filter without scraping off fibers as well.4. Wear a gas mask and gloves. Try to keep the ricin wet at all times to avoid generatingany dust (DEADLY!). And always shower and change clothes after handling.5.
Preparation
Ricin is a protoplasmic poison prepared from castor beans after the extraction of castor oiltherefrom. It is most effective as a poison when injected intravenously or inhaled, the latter requiring extreme commutation and small particle size to be effective, It is believed that thetoxic action is catalytic rather than stoichiometric which probably accounts for the high toxicity
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of the agent.Because of its relative instability ricin must be handled with extreme care. In neutral aqueoussolution it is stable only up to 60"-75" C., and in solid form up to 100"- 110" C., although for short exposures, temperatures up to 130" may be tolerated. It is sensitive to acids, alkalis andhalogens and may also be inactivated by mechanical working such as grinding or pulverizing.These factors are of great importance in developing a satisfactory method for preparing thematerial. Although ricin has been prepared in crystalline condition in the laboratory in small quantities, itbecomes necessary, for purposes of toxicological warfare, to prepare relatively large quantitiesin a high state of purity. This necessitates that as much as possible of the non-toxic materialpresent be removed in the process.In preparing the protein material, the castor beans are first ground and pressed to remove mostof the oil. The pressed cake still retains about 15% oil and this may be removed by means of solvents which will extract an additional 150 pounds of oil per ton of beans and reduce the oilretained in the cake to a little over 1%. In the event that the expressing step is supplemented bysolvent extraction, it is important to prevent detoxification of the protein during the solventremoval step. If residual solvent is removed from the ground beans by blowing with steam,considerable detoxification results. Blowing with nitrogen effectively prevents detoxification butis expensive when carried out on a large scale. After the oil has been removed, the pressed cake or pomace is extracted by agitating withwater at a pH of 3.8+-0.1 at 25" C. which removes substantially all of the toxic protein. Theextraction process is operative within a pH range of about 3 to 4.5 although the preferred rangeis about 3.5 to 4. The optimum operating point is a pH of 3.8+-.1, as indicated above. A carefulpH control is essential in order that as much non-toxic protein as possible may be eliminatedand also that the filtration rate may be held at a satisfactory value. Either HCl or H2SO4 may beused to get the desired pH for the extraction water, but H2SO4 is preferred due to its lower corrosion rate and ease of handling in concentrated form. The acid should be used inreasonably dilute form to prevent undue local concentrations during its addition. A 5%concentration is satisfactory.Following the extraction, the slurry is filtered using either a conventional recessed plate filter or a continuous string discharge vacuum filter. With the latter about 7% of filter aid, based on mealweight, was found necessary for satisfactory filtration.The filtrate from the water extraction step, which contains the ricin, was treated with a 16.7%solution of Na2SO4 to precipitate the protein. This solution is composed of 20 pounds of salt in100 pounds of water and the amount used was such that the salt content equaled 20% of thefiltrate weight. This amount and concentration of salt solution was about optimum consideringthe factors of cost and toxin recovery. Somewhat higher concentrations and larger amounts of solution can be used, however.The precipitation process is not limited to the use of Na2SO4 since a saturated solution of NaClcan be used successfully, but Na2SO4 solution gives better nitrogen fractionation, more rapidprecipitation, and can be operated under wider pH limits. It is desirable to raise the pH to about
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7-8 before precipitation as this gives better recovery and greater non-toxic nitrogen removal.The pH was raised to this value by using NaOH or Na2CO3 the latter being preferred. Thebase used was quite dilute in order to prevent detoxification due to high local concentrations inthe solution. A 5% solution of NaOH was used, whereas with Na2CO3 a 12% solution waspreferred.In general, this higher pH during precipitation gave a greater non-toxic nitrogen fractionationand at the same time maintained the toxin loss at less than 2%. After precipitation, the slurrywas filtered using from 1 to 4% filter aid, based on slurry weight, for satisfactory filtration, theamount of filter aid needed being dependent on the type of press used. Washing the filter cakewith Na2SO4 solution removed additional non-toxic nitrogen which is desirable. In this washingstep a 16.7% solution of Na2SO4 was again used. This washing step removed an additional15% of non-toxic nitrogen from the cake. After filtration the filter cake which contains the ricin in combination with the Na2SO4 may bedried and slurried with CCl4 to separate the ricin by flotation. Separation of the ricin after asingle precipitation and washing step is possible, but it is preferred to carry the process throughan additional extraction and precipitation step. This is accomplished by slurrying the filter cakein three times its weight of water and the pH of the slurry is again brought to 3.8+-.1 by meansof 5% H2SO4 The slurry is filtered and a second precipitation is brought about by addingNa2SO4 solution. Although pH control here is not wholly essential it is advantageous to bringthe pH to approximate neutrality by adding 12% Na2CO3. A precipitation time of 45 minutes was necessary to obtain complete removal of the toxin. Infiltering out the precipitate, no filter aid was used and the filter cake was washed with Na2S04solution on the filter whereby an additional amount of non-toxic nitrogen was removed from thecake. This washing was effective only the first time and repeated washings had little effect inremoving further non-toxic nitrogen.The ricin-Na2SO4 precipitate was dried at about 50" to 60" C. on a hot air tray dryer. The driedproduct was ground to pass a 40 mesh screen and agitated with 5 times its weight of CCl4which served the separate the ricin from the Na2SO4 by flotation. After settling. the ricin wasskimmed off the top. This reduced the Na2SO4 content of the mixture from a previous 40 to50% down to 15 to 18%. About 1 to 2% of nitrogen remained in the Na2SO4 salt which couldthen be used for subsequent precipitations.The final precipitation produced a particle size of 1-2 mu. On drying the wet cake, however, thericin cemented together forming larger particles. These could not be broken down to their original size by ordinary grinding methods and since a very line particle size was necessary inorder that the product might be used as a toxic weapon, it was thought desirable to seek somemethod to prevent the agglomeration or cementing process that took place on drying.To attempt lo affect this result, physical conditions prevailing under the precipitation processwere changed. This included changing the temperature of precipitation and the rate of agitation.Other changes included precipitation with only partial saturation of Na2SO4 and the use of wetting and seeding agents. None of these expedients produced any significant improvement inparticle size. Ordinary dry ball and hammer milling of the dried ricin produced considerabledetoxification perhaps due to the generation of excess heat. The use of CCl4 slurry plus the
use of low temperature and low moisture content of the ricin reduced detoxification during ballmilling.Spray drying proved to be an even better method of securing a reasonably small particle size.Best results were achieved by using a solution having about 20% solids, an inlet temperature of 150" C. and an atomizing air pressure of 150 to 180 p.s.i. The particle size secured was 6 to 8mu.The best means of securing a small particle size was by air grinding. This was carried out in anapparatus having a chamber with conical top and bottom. The material to be ground has beenfed into this chamber and is withdrawn from the bottom and forced back into the center of thechamber tangentially through a venturi. Compressed air of about 100 p.s.i. was fed to theventuri to provide the grinding force. The fines are drawn off the top and the large particlessettle to the bottom to be recirculated and reground. This process produced particles having amass median diameter of 2.5 to 3.5 mu.Numerous variations are possible in the several steps of the process commencing with thewater extraction and precipitation which may be a single or multiple step. Although a singleextraction step can be used, as indicated before, some process modifications are necessary for its successful operation on a plant scale. Double extraction proved to be quite efficient butadditional steps beyond the second extraction step were not found necessary. The drawing isself-descriptive and shows the various steps of the process described.
References Cited in this patent:Kabat et al.: J. Biol. Chem., vol. 168, 1947, pages 629-39 .Kunitz et al.: J. Gen. Physiol, vol. 32 (1948), pages 25-31.
