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LC-MS/MS monitoring for explosives residues and OGSR with diverse ionization temperatures in soil & hands : 30 minutes for extraction + elution

Şener Harun, Anilanmert Beril, Mavis Murat Emrah, Gursu Gokce Goksu, Cengiz Salih

Acta Chromatographica

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2022

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Vol. 34, no. 3

304--314

EN

A fast LC-APCI-MS/MS screening/confirmation method was developed and validated for trace analyses of 18 analytes which are explosives and organic gun shot residues including the challenging ones with diverse ionization conditions, in soil and on hands. (+) and (−) ionization modes were used after a single-step, low-volume solvent extraction procedure developed using methanol. Tape-lifting, stub, alcohol wipes, cotton bud were compared for collecting the residues from hands of a shooter. Tape-lifting and stub gave the highest recoveries and tape-lifting was chosen. Gradient elution system using ammonium chloride:methanol was developed. Whole procedure lasted approximately 30 min, was validated in both matrices, applied to real samples as post-blast residues, smokeless powder and the hands of a shooter, after shooting. Most of the recoveries were >80% and since all the precisions were <15%, quantitation was possible for all. Limit of Detection (LOD) and Limit of Quantification (LOQ) values were: 0.2–54.1 and 0.3–190.0 ngg⁻¹ in soil, and 0.2–132.3 and 1.1–355.0 ngg⁻¹ in tape-lift.

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Studies on NTO-, FOX-7- and DNAN-based Melt Cast Formulations

Mishra V. S., Vadali S. R., Bhagat A. L., Garg R. K., Kugaonkar V. M., Raman S., Sinha R. K., Asthana S.

Central European Journal of Energetic Materials

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2017

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Vol. 14, no. 2

403--417

EN

In the present paper, 2,4-dinitroanisole (DNAN) has been evaluated as a melt cast explosive in comparison to the widely used 2,4,6-trinitrotoluene (TNT). The detonation failure diameter of a bare DNAN charge is greater than 100 mm and about 44 mm with 1.5 mm steel confinement. Comparative studies of two sets of formulations were carried out. The first set comprised formulations containing 60% of NTO, FOX-7, HMX or RDX and 40% of DNAN or TNT. The second set comprised formulations containing 30% of NTO, FOX-7, TATB or RDX and 70% of DNAN or TNT. The studies were mainly concentrated on characterization of the formulations, which included determination of the sensitivity parameters and the velocity of detonation (VOD). The study confirmed that DNAN and DNAN-based formulations are relatively insensitive compared to TNT and the analogous TNT-based formulations respectively. The rate of the detonation reaction of DNAN is enhanced in the presence of the high energy ingredients RDX, HMX, FOX-7 and NTO to varying degrees. The VODs of the FOX-7/TNT and RDX/TNT formulations match closely with the proportions of FOX-7 and RDX under study. The VOD and shock sensitivity of the FOX-7/DNAN formulations decrease rapidly compared to the RDX/DNAN formulations, with increases in the proportion of FOX-7 or RDX. The combinations of NTO with TNT, and NTO with DNAN, are more shock insensitive than TNT or DNAN alone. NTO-based compositions are more insensitive than FOX-7-based compositions.

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NTO-based Melt-cast Insensitive Compositions

Trzciński W. A., Lasota J., Chyłek Z., Szala M., Paszula J.

Central European Journal of Energetic Materials

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2016

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Vol. 13, no. 3

592--611

EN

This paper presents research on insensitive melt-cast explosive compositions based on 3-nitro-1,2,4-triazol-5-one (NTO) and containing TNT, wax, Al and RDX. The viscosity of the compositions in the operating temperature range was measured. Thermal analysis was performed as well as thermal stability and sensitivity to mechanical and thermal stimuli were tested. The detonation parameters were also determined. Finally, the acceleration ability (Gurney energy) and the JWL coefficients for the detonation products were established.

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Explosive Properties of 4,4’,5,5’-Tetranitro-2,2’-bi-1H-imidazole Dihydrate

Lewczuk R., Szala M., Rećko J., Cudziło S., Klapötke T. M., Trzciński W. A., Szymańczyk L.

Central European Journal of Energetic Materials

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2016

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Vol. 13, no. 3

612--626

EN

This paper reports measured explosive properties of 4,4’,5,5’-tetranitro-2,2’-bi-1H-imidazole dihydrate (TNBI•2H2O). Non-isothermal kinetics analysis, calorimetric measurements, detonability tests, small-scale shock reactivity tests (SSRT), detonation velocity measurements and cylinder tests were performed. The results of the cylinder tests were used to determine the acceleration ability of TNBI•2H2O. Some experiments were conducted also with TNT, NTO, FOX-7 and RDX. Our experimental studies have shown that TNBI•2H2O is a thermodynamically stable compound, surpassing TNT with regard to its energetic and detonation parameters. The results of the SSRT indicate that this material has better performance in small charges than RDX, FOX-7 and NTO.

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A Study of the Detonation Properties, Propellant Impulses, Impact Sensitivities and Synthesis of Nitrated ANTA and NTO Derivatives

Jensen T. L., Moxnes J. F., Kjønstad E. F., Unneberg E.

Central European Journal of Energetic Materials

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2016

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Vol. 13, no. 2

445--467

EN

Nitrated derivatives of 5-amino-3-nitro-1,2,4-triazole (ANTA) and 3-nitro-1,2,4-triazol-5-one (NTO) were theoretically characterized with respect to their performance as high explosives and rocket propellants. The detonation velocity and the detonation pressure of the derivatives, calculated with EXPLO5 software, were at the same level or slightly above the performance of 1,3,5-trinitroperhydro-1,3,5-triazine (RDX). The results showed that compositions of 1,3,4-trinitro-1,2,4-triazol-5-one and glycidyl azide polymer (GAP) could give specific impulses just above 2600 m/s in rocket propellants. The sensitivities of the derivatives were evaluated using their heats of detonation, CHNO-ratios, free space in the crystal lattice and N−NO2 bond dissociation energy. The stability and sensitivity of several of the derivatives could be poor due to the low N−NO2 bond dissociation energies. The N−NO2 bond dissociation energies in the derivatives were calculated to be between 41 and 296 kJ/mol when the M06-2X/6-311+G(2d,p) functional was used. Synthetic routes for the most stable derivatives were proposed. In addition, preliminary studies of the chloride-assisted nitrolysis of NTO were performed. The infrared spectrum of the NTO derivative indicated that N−NO2 bonds were formed.

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A Melt-Cast Composition Based on NTO and FOX-7

Belaada A., Trzciński W. A., Chyłek Z., Szala M., Paszula J.

Central European Journal of Energetic Materials

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2016

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Vol. 13, no. 4

882--902

EN

A melt-cast composition containing NTO, FOX-7, TNT, Al and wax was prepared and tested. The viscosity of the melted composition was measured. Its sensitivity to impact, friction, shock wave and jet impact were determined, and its thermal stability and ignition temperature were established. Some detonation properties of the composition were investigated. The heat of detonation was measured using a calorimetric bomb. The detonation pressure and velocity were determined in a plate-dent test. The results of a cylinder test were used for the determination of the Gurney energy, the detonation pressure and energy, and the so-called effective exponent of the expansion isentrope and the JWL equation of state of the detonation products.

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Methods for Preparing Spheroidal Particles of 3-Nitro- 1,2,4-triazol-5-one (NTO)

Lasota J., Chyłek Z., Trzciński W. A.

Central European Journal of Energetic Materials

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2015

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Vol. 12, no. 4

769--783

EN

This paper presents an overview of methods for recrystallizing 3-nitro- 1,2,4-triazol-5-one (NTO), with particular emphasis on methods for obtaining spheroidal particles with low porosity. The effects of selected solvents and surfactants on the recrystallization results was checked. Products in the form of spheroidal particles were obtained for some selected solvent-surfactant systems. The bulk density, surface area, size distribution, and sensitivity to friction and impact were tested for the spherical NTO samples and thermal analysis was also performed.

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3-Nitro-1,2,4-triazol-5-on : otrzymywanie, krystalizacja, właściwości, kompozycje wybuchowe

Lasota J., Trzciński W. A.

Przemysł Chemiczny

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2014

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T. 93, nr 11

1859-1865

PL

Dokonano przeglądu dostępnej literatury na temat metod otrzymywania i krystalizacji 3-nitro-1,2,4-triazol-5-onu (NTO). Podano podstawowe właściwości wybuchowe czystego materiału oraz omówiono skład i właściwości mało wrażliwych kompozycji plastycznych, odlewanych i prasowanych zawierających NTO. Przytoczono przykłady zastosowania kompozycji w amunicji.

EN

A review with 41 refs. Formulations and properties of the title compd.-contg. low sensitive melt-cast, plastic and pressed explosive compns. and their use in munitions were presented.

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Assay of the Insensitive High Explosive 3-Nitro-1,2,4-triazol-5-one (NTO) by Acid-Base Titration

Nandi A. K., Singh S. K., Kunjir G. M., Singh J., Mandal A. K., Pandey R. K.

Central European Journal of Energetic Materials

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2013

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Vol. 10, no. 1

113--122

EN

The insensitive high explosive 3-nitro-1,2,4-triazol-5-one (NTO) is a weak acid (pKa 3.76) due to the labile N–H bond. The weakly acidic character of this compound is exploited for its assay by aqueous acid-base titration. The NTO sample was dissolved in water and the resultant solution was titrated against 0.07 N NaOH solution using phenolphthalein as indicator. Regular batch samples were assayed by this method and the results were compared with those obtained by the HPLC method. The aqueous acid-base titration method was found to be suitable for the quality control of the product.

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Małowrażliwe materiały wybuchowe - 3-nitro-1,2,4-triazol-5-on

Powała D., Orzechowski A., Florczak B., Maranda A., Nowaczewski J.

Przemysł Chemiczny

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2006

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T. 85, nr 3

177-181

PL

Przedstawiono właściwości 3-nitro-1,2,4-triazol5-onu (NTO) oraz wyniki badań nad uzyskaniem jego odpowiedniej postaci krystalicznej. Przeprowadzono badania gęstości nasypowej i nasypowej utrzęsionej uzyskanych kryształów. Zbadano ich charakterystykę granulometryczną a także morfologię ziarna. Uzyskane kryształy wykorzystano do sporządzenia materiałów wybuchowych typu PBX (plastic bonded explosives). Przeprowadzono badania ich wrażliwości na bodźce mechaniczne.

EN

Semicarbazide hydrochloride reacted with aq. 85% HCOOH at 85–90°C to give TO which, with excess acid distd. off and reaction mixt. neutralized with aq.10% Na2CO3, was nitrated to yield NTO m. 267–9°C. This was recrystd. in 12.5 wt. parts of (9:1 v/v) EtOH–H2O, 2 hrs., 1000 rpm, at cooling rates of (i) 20 (ii) 3, and (iii) 10°C/min, to yield (i) spherical 50–150 µm polycrystals, bulk d. 0.77, and tap bulk d. 0.96; (ii) 50–350, 0.92, and 1.05; (iii) 50–300 µm, 0.81, and 1.01 g/ cm3, resp. NTO m.p., 267–8°C. Plastic-bonded explosives (PBX) were prepd., contg. 84 or 90% of 10–150 µm hexogen and NTO as additive, in a butadiene-styrene rubber as binder plastified with 16 or 10% of dioctyl adipate and oil. When added in 20, 20–60, and 80% to either the 84% or the 90% PBX, the NTO additive reduced, leveled off, and still more reduced the sensitivity of the PBX to impact, resp. The EtOH–H2O was superior to ethylene glycol as solvent. The properties of 3-nitro-1,2,4-triazol-5-one and investigations of this material in order to obtain suitable crystalline form were presented. The tests of bulk density and tap bulk density of obtained crystals were carried out. The grain size characteristic and grain morphology were investigated. The resulting crystals were used to prep. of Plastic Bonded Explosives. The tests of the PBX sensitivity to mechanical impacts were made.

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Researches on New Crystalline Form of Some Insensitive High Explosives in PBX

Powała D., Orzechowski A., Maranda A., Nowaczewski J., Lorek A.

Central European Journal of Energetic Materials

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2004

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Vol. 1, nr 1

63-73

EN

In this paper, the results of researches on crystallization of insensitive high explosives were described. 3-Nitro-1,2,4-triazol-5-one (NTO) and nitroguanidine (NQ) were selected. The laboratory methods of preparation were presented. The influence of different solvents and other parameters on crystallization process was investigated. The results of the particle size distribution in the crystals obtained were presented. The suitability of NTO and NQ for their application in plastic bonded explosives (PBX) was checked.