lead styphnate

     Lead styphnate, also called lead 2,4,6-trinitroresorcinate or normal lead styphnate, is an unstable primary explosive that resists shock but will detonate readily from heat or static. It is usually mixed with lead azide to improve its ability to detonate from flame or electric ignition. Other names include bleistyphnat, bleittrinitroresorcinat, or trizinat in German; styphnate de plomb in French; stifnato di piombo in Italian; stifnat or trinitroresortsinat in Russian; and trinitroresorcinato de plomo in Spanish. Lead styphnate was first prepared in 1914 by E. vonHertz from magnesium styphnate. The most frequent application of lead styphnate is in primer caps for bullets, in airbags, and detonators. Due to the toxicity of lead it is being phased out.

CHEMICALS	APPARATUS
----	----
----	----
----	----
----	----
----	----

     A large batch of lead styphnate may be made by using the large batch solution of magnesium styphnate prepared here. Adjust the volume of the solution with water to 110 L and add 330 mL of 70% nitric acid with stirring. Prepare a lead nitrate solution by dissolving 37.4 Kg of lead nitrate in 100 L of water. The solution should be warmed to 50 C and stirred to speed up the dissolving. Allow the solution to cool and adjust the volume with water to 110 L. Place 20 L of magnesium styphnate solution into a stainless steel tank and heat it to 80 C. Add 20 L of lead nitrate solution, with stirring, to the tank over a period of 20 minutes while maintaining the temperature at 80 C. Hold at this temperature for 5 minutes before allowing the solution to cool to 45 C. Decant off as much liquid as possible and pour the lead styphnate precipitate over a filter to collect it. Wash the crystals thoroughly with water and allow to dry. Yield is about 93%. A variant of this reaction is to add 3.8 mL of concentrated hydrochloric acid to 1 L of the magnesium styphnate solution, heat to 80 C, and add, with stirring, 200 mL of a lead nitrate solution (containing 66.2 g of lead nitrate) over a period of 20 minutes. Allow the solution to cool to 45 C and decant, filter, and dry as above. Yield is 92.7%. The yield is slightly less, but you use hydrochloric acid instead of nitric acid. Prepare a solution of 3.74 g of gum arabic and 0.68 g of wet tetrecene in 8 g of water. Place 8.5 g of this solution into a beaker and add 17.3 g of styphnic acid (containing 20% of its weight as water) and stir for 1 minute at room temperature. Add 7.9 g of lead hydroxide (containing 15% of its weight as water) to the solution and stir for 4 minutes. The temperature may rise to around 40 C at this time. Add an additional quantity of 7.9 g of lead hydroxide and continue stirring for 4 minutes. The end result is an intimate mixture of lead styphnate and tetracene bound by gum arabic as a plastic mass. No washing or drying is necessary. It is preferable to keep this mixture moist until it is ready to be used whereupon some of the water may be removed. This material may be combined with a premixed formulation of 9.63 g of barium nitrate and 18.7 g of ground glass. The barium glass mix is blended with the styphnate plastic and used as a primer compound. This composition will not detonate from shock, friction, or even by a blasting cap until it is allowed to dry. Instead of lead hydroxide one can use two 6.52 g batches of dry lead oxide. Add 145 g of lead hydroxide (wet with 16% water) to 267 g of purified styphnic acid in 40 mL of water with rapid stirring. Continue stirring for 4 minutes and then add 145 g of lead hydroxide (wet with 16% water). Stir for an additional 9 minutes. Lead oxide or lead carbonate can be substituted for lead hydroxide in this reaction although the masses will have to be adjusted accordingly. A special cubic form of lead styphnate may be prepared as follows: Suspend 10 g of styphnic acid in 100 mL of water heated to 75 C; only a small amount will dissolve. With rapid stirring add 10 mL of 8N potassium hydroxide, and continue stirring for 5 minutes. Prepare a solution of 20 g of lead nitrate in 50 mL of water and add this solution to the styphnate solution, with stirring, over a period of 15 minutes. This unusual crystal form of lead styphnate is more stable to electric and thermal initiation, but is less stable to shock and friction. Prepare a solution of 11 g of styphnic acid dissolved in a minimum quantity of glycerol. Add enough ammonium hydroxide to the glycerol until the pH is 5. Slowly add, with stirring, 13 g of lead nitrate. A gelatinous precipitate should have formed. Add a small amount of water and stir the mixture until needle-like crystals form. Filter to collect the crystals, wash them thoroughly with water, and dry in the open to obtain lead styphnate. Store the crystals wet for increased safety. Lead acetate can be substituted for lead nitrate if the mass is adjusted accordingly. Heat either the solution of zinc styphnate or manganous styphnate to 65 C and precipitate lead styphnate by adding approximately 300 mL of 30% lead nitrate solution. Collect the lead styphnate by filtering and allow to dry. Store the crystals wet for increased safety.

Home|Explosives|Chemical Weapons|Pharmaceuticals|Pesticides|Precursors
Lab Skills|Lab Equipment|Safety|Rogue Science|Links|What’s New|Contact Me|Disclaimer