Kinetic Spectrophotometric Determination of Propellant Grade Hydrazines using Thiophenes with Active Carbonyl Groups

Selvakumar Subramanian; Somanathan Narayanasastri; Audisesha Reddy Kami Reddy

doi:10.14429/dsj.64.3092

Selvakumar Subramanian Satish Dhawan Space Centre SHAR, Sriharikota
Somanathan Narayanasastri CSIR-Central Leather Research Institute, Chennai
Audisesha Reddy Kami Reddy Satish Dhawan Space Centre SHAR, Sriharikota

DOI: https://doi.org/10.14429/dsj.64.3092

Keywords: Kinetic spectrophotometric method, CF3 enone, thiophene-3-carboxaldehyde, hydrazine, MMH

Abstract

A simple, cost effective, highly sensitive and rapid kinetic spectrophotometric method was developed for hydrazines by using Thiophene-3-carboxaldehyde (3-Thienaldehyde) and 3-Butenone (E)-1,1,1-trifluoro-4-(3-thienyl) (CF3 enone). CF3 enone was prepared by crossed aldol condensation of 3-Thienaldehyde and characterized by UV-Vis, FT-IR and NMR spectra. Reactions of 3-Thienaldehyde (with catalyst) and CF3 enone (in acetonitrile medium without catalyst) with hydrazines were followed spectrophotometrically and compared. Variables such as temperature and concentration were optimized to determine hydrazines in the concentration range of 0.1 mM to 0.1 M for 3-Thienaldehyde and 0.1 mM to 1 mM for CF3 enone. Minimum detectable limits were found to be 0.2 mM (Hydrazine) and 0.1 mM (MMH ) for 3-Thienaldehyde. For CF3 enone, Minimum detectable limits were found to be 0.007 mM (Hydrazine) and 0.01 mM (MMH). Rate of the CF3 enone reaction was studied as there is gradual decrease in absorbance for the peak at 320 nm for the interaction of hydrazines. Initial rate and fixed time methods were adopted for kinetic study. CF3 enone based kinetic spectrophotometric method is rapid and sensitive with no catalyst requirement for interaction of hydrazines when compared with the classical CHO functional group based method.

Defence Science Journal, Vol. 64, No. 1, January 2014, DOI:10.14429/dsj.64.3092

Author Biographies

Selvakumar Subramanian, Satish Dhawan Space Centre SHAR, Sriharikota

Mr S. Selvakumar is presently working as a scientist at chemical testing lab, Solid Propellant Base Booster Plant/SDSC- SHAR centre / ISRO. He received his MSc from Bharathidasan university, Tiruchirapalli. He is having more than twelve years experience in synthesis and characterization by spectroscopy and chromatographic techniques in solid propellant processing. His main area of scientific interest is development of analytical techniques for solid propellant ingredients and liquid propellants. His main research interest is development of sensing techniques based on conjugated polymers and metallophthalocyanines for isocyanate vapors and liquid propellant vapors.

Somanathan Narayanasastri, CSIR-Central Leather Research Institute, Chennai

Dr N. Somanathan is Senior Principal scientist and head of Polymer lab at CSIR-CLRI. He received his PhD from University of Madras, Chennai. His research activity mainly focuses on functional/specialty polymers for flexible electronic applications, solar energy harvesting, intelligent materials, biosensors and chemo sensors. He had been visiting scientist for many European universities. He has more than 70 papers in peer reviewed journals and contributed a chapter in the Hand Book of Advanced Materials testing, Marcel Dekker. He is reviewer for many journals of International repute.

Audisesha Reddy Kami Reddy, Satish Dhawan Space Centre SHAR, Sriharikota

Dr K. Audisesha Reddy had been a meritorious student from his school and college days. He was an academic rank holder in MSc Organic chemistry from S.V.University, Tirupati. He received his PhD in Polymer Chemistry from IIT, Chennai. He is presently working as a Dr Brahmprakash Professor, Solid Propellant Base Booster Plant. He has vast experience in composite solid propellant processing and manufacturing. He was also President of SHAR-Chennai chapter of High Energy Materials Society of India (HEMSI) and organized National and International conferences.