(517f) Real Time Ir Used in Tagzt Synthesis

The United States Navy is utilizing real-time analytical equipment to manufacture explosives that otherwise may not be manufactured safely. The Navy has adopted the use of real-time acquisition of solution mid-IR to monitor concentrations of explosives in their respective solvents to eliminate having to isolate these materials in large quantities. The use of the real-time analytical instrument has been demonstrated at the laboratory scale and is currently being testing at the pilot plant scale.

The batch reaction synthesis of triaminoguanidinium azotetrazolate (TAGZT) requires the pre-manufacture of the sensitive and dangerous 1.1 explosive, sodium azotetrazolate (NaZT). With the current process yields, three batches of NaZT are needed to make one batch of TAGZT. This process requires the isolation, drying, and storage of the NaZT in preparation for the TAGZT synthesis. Handling the NaZT is neither advisable nor desired, so an alternative process was engineered.

The modified NaZT process eliminated the isolation and handling of the dangerous precursor. In the modified process the NaZT is collected and temporarily stored wet on a Nutsche filter until the TAGZT synthesis is run. The NaZT is less sensitive when wet. The collection of the wet NaZT product is accomplished through a series of crystallizations and filtrations onto the Nutsche filter.

After the desired quantity of wet NaZT is collected on the Nutsche Filter, the NaZT is soluablized in warm water and transferred to a reactor for the TAGZT synthesis. Using real-time analytical methods the concentration of the NaZT (in solution) is determined. The transferred solution is continuously sampled through a flow cell equipped with mid-IR. Laboratory experiments using mid-IR techniques have successfully demonstrated that the concentration of NaZT can be determined, while still in solution with water, with an accuracy within +/- 0.2%. The total weight of NaZT is determined using the known concentration (mol/L) of the NaZT solution via mid-IR techniques along with the total solution volume (radar gauge).