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Nitro Glycerin
Nitro Glycerin

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Published by: Michael Andreas Evripiotis on Jun 08, 2010
Copyright:Attribution Non-commercial


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 Nitroglycerin ________________________________________________________________________________  _____ ********************Use information at own risk!!!***********************************--------------------------------------------------------------------------------------------------------------------------------------------------------------------------* Nitric Acid 98-100% 200ml * Water* Sulfuric Acid 98-100% 300ml * Thermometer* Glycerin - 112ml * Glass container + stirring rod* Sodium Chloride - -* Sodium Bicarbonate - - =====================================================================================METHOD:Prepare a mixture of 200 mL of 98-100% nitric acid and 300 mLof 98-100% sulfuric acid by slowly adding one to the other in a1000-mL beaker. Place the beaker into a salt-ice bath duringthe mixing so it may cool, allow the temperature to drop below 10 °Cafter mixing. You can keep the cold acid in the salt-ice bath or youcan transfer the acid mix into a round-bottomed 1000-mL Florence flaskfor better heat dispersion. In either case, prepare a freshsalt-ice bath. Because of the possibility of friction, standard stirringmethods are not advised. Instead, use an aquarium pump to blow airinto the acids as a means to cool and stir them. Regulate the air flowso the acid is being well stirred yet not spattering out. Using aburet suspended above the flask, very slowly add drop by drop 112 mLof glycerol that has been previously cooled to 15 °C. Carefully monitorthe temperature of the reaction at all times, the temperature must staybelow 20 °C, preferably below 15 °C for extra safety. If at any timethe temperature goes near this, stop adding glycerin until it cools.You can use the rate of addition to control the temperature.If the temperature ever rises above 20 °C it is ruined as no morenitro will be made and you are in great danger of the existing nitrodetonating. If the temperature goes above 30 °C, there is a suddenrise in temperature, or a red gas is noticed, DUMP IT INTO COLDWATER IMMEDIATELY!. Keep a bucket of ice water on hand for thistask. After adding all of the glycerin, allow the temperature to dropto 15 °C and sit for 15 minutes. Carefully pour the reaction mix intoa large beaker containing an equal volume of room temperature water.Add this mix to a separatory funnel and allow the nitroglycerin tosettle out, it will form a layer on the bottom of the funnel. Drain offthe nitro layer and keep the acid waste layer for further extraction.Place the nitro back into a clean separatory funnel and add plentyof 38-45 °C water, mix, then separate. Wash the nitro again, then washwith a warm 4% sodium carbonate solution. Wash with warm water threemore times. Give it a final wash of concentratedsodium chloride solution, and let it sit one day before separatingthe layers. Separate and check the nitro for acidity with litmus paper.If it is still acidic keep washing. It must be neutral or it will explode.Keep on washing until it shows that its neutral.

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