Aminotetrazolate-Pentahydrate Reaction

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All the materials were purchased from Sigma-Aldrich and used as received unless otherwise stated.

Reaction (1)

How to make Sodium Azo-Tetrazolate--Pentahydrate (SAT)

Approximately 2.15 g of Aminotetrazolate monohydrate was added to approximately 62.5 ml of 2 M sodium hydroxide. While being stirred, the solution was heated, increasing its temperature up 10 degrees Celsius, up to 60 degrees Celsius. Over a one hour time period, potassium permanganate (an amount of 2.5 g) was added in increments.
After this, sodium sulfite was added at a slow pace, and powerful stirring destroyed the remaining permanganate. To determine the endpoint of the addition of sulfite, a color change to a yellow
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The solution was heated to 30-35 °C by stirring at a brisk pace until all the material was dissolved. Also, 3.75 g of ammonium chloride was added to this mixture. Immediately after, the formation of a yellow precipitate (Ammonium Azo-Tetrazolate) was observed. The suspension was left in the refrigerator to cool till the temperature was less than 5 °C. The solid was washed in water, filtered and dried. When the solid was weighed, it yielded a weight of 1.532 grams, which gave an expected yield of 74.43%. Reaction (3)

To Make Guanidinium Azo-Tetrazolate (GAT)

5 grams of Sodium Azo-Tetrazolate -Pentahydrate was dissolved with 70 mL of water heated to 80-90 °C. 3.18 grams of Guanidinie Hydrochloride was added to the solution. Immediately after, the formation of a yellow precipitate was observed. The volume of the final solution was reduced to 70 ml, boiled for 2 minutes and allowed to reach room temperature. The suspension left overnight in the refrigerator. The solid was washed in water, filtered and dried. When the solid was weighed, it yielded a weight of 3.89 grams, 82.52 % of the original amount. Reaction (4)

To make Aminoguanidinium Azo-Tetrazolate
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A true decomposition mechanism and true kinetic constants allow for one to correctly predict both the thermal hazard potential and the shelf life of explosive materials for safety purposes. Both the measurements of the kinetics and the Arrhenius parameters corresponding to thermal decompositions are key elements in characterizing energetic compounds. Kinetic constants are also keys to mapping reaction pathways. These constants are not easily obtained. However, techniques such as that of DSC, and TGA under various heating rates, allow for one to obtain both kinetic and thermal decomposition data of energetic materials.
Data obtained from DSC and TGA were utilized to determine the kinetic parameters using the ASTM E 698 standard, which assumes the rate of reaction reaches the maximum value at the maximum peak temperature for the first order reaction. The ASTM E 698 standard uses two different equations, the Ozawa–Flynn–Wall and the Kissinger’s corrected kinetic equation to determine and elucidate the kinetic parameters of solid-state reactions without previous knowledge of the reaction mechanism.

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