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 …show more content…
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 …show more content…
The plots for GAT, AGAT and DAGAT were straight lines, and the standard deviations were almost 1 for each, which indicate the independency of the thermal degradation of the energetic materials at various heating rates. However, the standard deviation for AZT was slightly less than that of the others. (27), (33), (40) The slopes of the lines equal for each material -Ea /R (2) through transposing Eq (2) The activation energy was found from the following equation
E = 8.314 * slope (3)
The activation energy values were later used for computing the pre-exponential factors (A) by equation (1). In the meantime, activation energies (Ea) for these energetic compounds were calculated by the Ozawa method. The Ozawa equation according to ASTM E698 is equal to the following
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 …show more content…
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 …show more content…
The plots for GAT, AGAT and DAGAT were straight lines, and the standard deviations were almost 1 for each, which indicate the independency of the thermal degradation of the energetic materials at various heating rates. However, the standard deviation for AZT was slightly less than that of the others. (27), (33), (40) The slopes of the lines equal for each material -Ea /R (2) through transposing Eq (2) The activation energy was found from the following equation
E = 8.314 * slope (3)
The activation energy values were later used for computing the pre-exponential factors (A) by equation (1). In the meantime, activation energies (Ea) for these energetic compounds were calculated by the Ozawa method. The Ozawa equation according to ASTM E698 is equal to the following