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A Validated Reverse Phase HPLC Technique for the Determination of TATB Assay

Bhattacharyya S. C., Patil R. S., Santosh M. S. S. N. M., Bhattacharya B., Malik R. K., Mehra A.

Central European Journal of Energetic Materials

2016

Vol. 13, no. 3

641--657

The main hurdle for the estimation of the purity of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) is its insolubility in most of the known organic solvents. In the conventional method, TATB is digested with steam in a modified Kjeldahl digester and the ammonia evolved is estimated quantitatively. To do away with this cumbersome method, a simple, rapid HPLC technique using a reverse phase C-18 column has been established for quantitative determination of the purity of TATB. A sharp and symmetrical peak with a retention time of 2.92 min at 355 nm is obtained for pure TATB when the flow rate is 2.0 mL/min. The linearity of the detector response has been studied with sample concentrations ranging from 10 to 50 mg/L. The method addresses two important issues of sample preparation and the precision of measurement. Unlike the previously reported HPLC techniques which mainly aimed at the detection of TATB, the present work is a validated account of a quantitative estimation of purity. Regular production batch samples have been assayed by this method and the results are compared with those obtained from the conventional analysis. The HPLC method is convenient and reliable for quality control of the product at the plant level.

Studies on the Tailoring of Particle Size and Micromeritic Properties of Reduced Shock Sensitivity RDX (RSS-RDX)

Ramavat V., Sarangapani R., Reddy S. T., Patil R. S., Gore G. M., Sikder A. K.

Central European Journal of Energetic Materials

2013

Vol. 10, no. 4

581--592

The microstructure of explosive particles, as well as formulations, has a significant influence on the shock sensitivity of various energetic formulations. Particle shape and specific size distributions are always important considerations in explosives processing in order to realize better process parameters. The present study aimed to explore crystallization variables required to achieve a specific particle size of Reduced Shock Sensitivity RDX (RSS-RDX). Crystallization process factors such as cooling rate, agitator speed and configuration, etc. have been systematically studied to understand their effect on the particle size. The study also established the crystallization process parameters required to tightly control a specific particle size distribution ranging from 50 to 500 μm by cooling crystallization. Fine particles ranging from 15 to 30 μm were prepared by an ultrasonication technique. Ultrasonic process parameters, including temperature, time and ultrasonic frequency, were studied and the process conditions were optimized. Micromeritic characterization of RSS-RDX revealed the nature of flowability, which in-turn is useful in identifying the ease of processability. Overall, our interest stemmed from an investigation which showed that careful optimization of crystallization variables can lead to a specific particle size distribution.