2011 YÜksek lisans tez özetleri

Simultaneous Spectrophotometric Determination Of Nitramine-Type Energetic Materials

Scope of this thesis is to fulfill the requirements to find a cheap a way of testing the explosive material residuals. For this purpose, the methods in the literature are studied and the deficiencies are designated. From that point on, spectroscopic test methods are developed for the nitramine-type energetic materials, 1,3,5-Trinitroperhydro-1,3,5-triazine (RDX) and Octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) which exist in the field together and difficult to separate. In this study, a new colorimetric test method is developed for the solutions of nitramine-type explosive materials (RXD and HMX) in the acetone-water (1:1 v/v). The developed test method is applied to RDX and HMX mixtures in the varied ratios. Here with this method, mixtures of RDX and HMX both with separately and with TNT are studied. In this method, materials are kept in the alkaline solution (1 M Na₂CO₃ + 0,04 M NaOH) under room conditions and in the hot water bath incubation. At the end of the hydrolysis time, acids are used to adjust the pH and with the use of the Griess reagent, absorbances in the 540nm wavelength are measured. As a result of the waterbath hydrolysis, detected molar absorptivity and the limit of detection (LOD) of RDX are 2.84x10³ L mol^-1cm^-1 and 1.5 μg mL^-1 and molar absorptivity and the limit of detection (LOD) of HMX are 3.55x10³ L mol^-1cm^-1 ve 0.75 μg mL^-1 respectively. As a result of the room temperature hydrolysis of RDX, molar absorptivity and the limit of detection (LOD) are 2.84x10³ L mol^-1cm^-1 ve 1.5 μg mL^-1 respectively. HMX didn’t yield any results in the room condition hydrolysis. This methods is also applied for binary and ternary mixtures of RDX-HMX, RDX-TNT, HMX-TNT, and RDX-HMX-NH₄NO₃. It is observed that absorbances of the mixtures are equal to the sum of the absorbances of the individual materials in the mixture. In this context, sum of the absorbances principle is used to determine the quantity of the each material in the mixture. To minimise the TNT effect in the RDX-TNT mixtures, a different method of sequential extraction process is used. In this method, alkaline hydrolysis and the Griess reagent is used to form the color reaction. This method is also applied to real explosive materials mixtures called as composite B (%60 RDX+%39 TNT+%1 filler material) and octol (%70 HMX+%30 TNT). Quantities of RDX-TNT in the composite B and HMX-TNT in the octol were detected by a standard HPLC method. A study which discriminates between RDX-HMX with spectrophotometric method has not been found in the literature. The developed method is important for the purposes filling this literature gap.

 

  

TEZCAN Canan

Danışman : Doç. Dr. Gül HİSARLI

Anabilim Dalı : Kimya

Programı : Fiziksel Kimya

Mezuniyet Yılı : 2011

Tez Savunma Jürisi : Prof. Dr. Saadet PABUCCUOĞLU

Prof. Dr. Mustafa L. BERKEM

Prof. Dr. Mehmet MAHRAMANLIOĞLU

Doç. Dr. Süheyla PURA ERGİN

Doç. Dr. Gül HİSARLI