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Supercritical Water Oxidation of Octol – Containing Wastewater Global NEST Journal, Vol 21, No 2, pp 172-179 Copyright© 2019 Global NEST Printed in Greece. All rights reserved Supercritical water oxidation of octol – containing wastewater Gurbulak E.1,*, Yuksel E.1, Tekbas M.1, Doruk T.2, Eyvaz M.1, Bektas N.1 1Gebze Technical University, Department of Environmental Engineering, 41400, Kocaeli, Turkey 2Ondokuz Mayıs University, Department of Molecular Biology and Genetics, 55105, Samsun, Turkey Received: 23/05/2018, Accepted: 12/02/2019, Available online: 15/02/2019 *to whom all correspondence should be addressed: e-mail: [email protected] https://doi.org/10.30955/gnj.002776 Abstract Considering both the dramatic increase in octol use and the nitro aromatic and heterocyclic nitramine groups in its This study investigated optimum operating conditions of structure, it has become a non-negligible nitro-compound supercritical water oxidation (SCWO) for octol and source of pollution (Chatterjee et al., 2017). This pollution compared the degradation of its components TNT (2,4,6- has harmful effects on the environment and health due to trinitrotoluene) and HMX (octahydro-1,3,5,7-tetranitro- its characteristic of persistent resistance to biological 1,3,5,7-tetrazocine, octogen) under the same conditions. degradation (Snellinx et al., 2002). Jong et al. (2006) Pilot scale experiments were conducted at various determined that HMX had a more recalcitrant structure temperatures, reaction times and oxidant amounts. than other well-known explosives including TNT and RDX. Removal efficiency, by-product analysis and toxicity tests Although 2,4,6 TNT has potential carcinogenic effects, its were selected as the performance criteria for the SCWO. transformation products have adverse effects on the Optimum conditions were determined as a temperature central nervous system of mammals (ATSDR, 1995; Falone of 500 C, 120 s of oxidation time and an oxidant ratio of et al., 2006). Similarly, the US Environmental Protection 150%. Removal of octol was achieved at a rate of 99.99%, Agency (EPA, 1988) has stated that HMX has potential while TNT and HMX were removed individually at a rate of toxic properties which can lead to focal atrophic changes ~85% when they existed in the wastewater. No toxicity in the the liver and kidneys and can also affect the was observed at the end of the octol oxidation, whereas functioning of these organs (ATSDR, 1997). In addition, toxicity was found in the TNT and HMX oxidation due to Panz et al. (2013) stated that compared to individual the formation of TNT isomer and aniline. Higher initial substances, explosive mixtures exhibited more synergetic organic material concentrations promoted the removal toxic effects. It has been determined that TNT and HMX in rates. These results demonstrated that SCWO can be amounts of over 2 µg/L and 400 µg/L, respectively, in effectively used for the degradation of ammunition drinking water have a negative effect on human health wastewater even when concentrations are high. (Chatterjee et al., 2017). Keywords: Supercritical water oxidation, ammunition Several studies have reported on the outcome of such wastewater, octol, TNT, HMX, toxicity. pollutants and on the limitations of their control and 1. Introduction disposal techniques. Physical separation methods such as adsorption and membrane techniques have some For the past 50 years, one of the most important research limitations because of high operation costs and the areas of the defense industry has been the production of secondary pollutants that occur during the treatment lighter and less space-consuming warheads and long- processes (Rodgers and Bunce, 2001; Nehrenheim and range weapons. To this purpose, ammunition with high Odlare, 2008). Advanced oxidation methods focus mainly detonation velocity was produced using explosives such as on photo catalytic and fenton oxidation, which are TNT (2,4,6-trinitrotoluene) and HMX (octahydro-1,3,5,7- relatively uneconomical and concentration dependent tetranitro-1,3,5,7-tetrazocine, octogen) in different methods with lengthy reaction times (Son et al., 2004). combinations. A number of studies in the literature have also Octol is an explosive which has one of the highest investigated the biological degradation of explosives. detonation velocities. It is manufactured by the casting of Moshe et al. (2009) indicated that TNT had a negative water-wet HMX and molten TNT in order to meeting the effect on the biodegradation of HMX. Namely, when there requirements in question. Moreover, the production is TNT in a mixture, the degradation products of TNT process and utilization performance have been well inhibit HMX degradation. Consequently, these treatment known for many years. An additional advantage is that it methods not only fail to meet legal effluent standards, but can be produced in desired shapes and sizes (Hussein also lead to the formation of toxic degradation products et al., 2018). (Chang and Liu, 2007). Gurbulak E., Yuksel E., Tekbas M., Doruk T., Eyvaz M. and Bektas N. (2019), Supercritical water oxidation of octol – containing wastewater, Global NEST Journal, 21(2), 172-179. SUPERCRITICAL WATER OXIDATION OF OCTOL – CONTAINING WASTEWATER 173 In the search for ways to uncompromisingly satisfy The main objective of this study was to determine, for the effluent standards and fill the need for sustainable and first time, the optimum operating conditions of SCWO for greener waste treatment technologies, supercritical water the degradation of octol, which is a mixture of nitro oxidation (SCWO) technology has been gaining aromatic and nitro heterocyclic compounds. Moreover, importance because the reaction by-products from its the SCWO removal efficiency for octol was compared with processing are harmless and its short reaction times and the efficiency of the individual treatments of TNT and high treatment efficiency. Thus, SCWO is a promising HMX. Toxicity tests were also carried out for SCWO organic waste treatment technology is carried out above by-products in order to further evaluate the the critical point of water (Tc = 374.3 °C, Pc = 22.1 MPa). environmental impact of the explosive removal technique. Under these conditions, by decreasing the density and 2. Materials and methods dielectric constant of the water, the hydrogen bonds are reduced, which results in water with the high diffusivity 2.1. Chemicals and standards and excellent transfer characteristic of a non-polar Octol (Purity 98%), TNT and HMX explosives used in this medium. In this case, organic matter, oxygen and water at study were obtained from the Mechanical and Chemical all proportions become miscible and form a single Industry Company (MKE) and the Scientific and homogeneous system. Based on these supercritical water Technological Research Council of Turkey (TUBITAK), properties, the reaction takes place almost completely respectively. Hydrogen peroxide (H2O2) (50 wt. % in (>99.9%) and the reaction time is very short, generally aqueous solution) and chromatographic grade methanol from just a few seconds to a few minutes, because there is were purchased from Sigma Aldrich. The TNT and HMX no interphase mass transfer resistance (Jimenez- standards were also obtained from Dr. Ehrenstorfer Espadafor et al., 2011). As a consequence, organic GmbH. materials are oxidized into harmless products and inorganic compounds into a gas or solid phase (Zhang 2.2. Preparation of synthetic wastewater et al., 2017). Since dissolutions of TNT and HMX in water is difficult, the In recent studies, optimum treatment conditions have solutions were first prepared by dissolving the appropriate been clearly determined and degradation mechanisms amount of each explosive in methanol. The HPLC analyses have been defined for many types of industrial hazardous were performed without any interference because the wastes using SCWO (Vadillo et al., 2014; Qian et al., 2016). methanol was used as the carrier solvent. After adding the The SCWO process, therefore, is considered as an prepared methanol mixture to boiling tap water, the alternative to incineration systems in terms of operating methanol was evaporated off in order to obtain the costs, lack of hazardous by-products and disposal desired concentration of synthetic wastewater (Alnaizy (Marulanda and Bola, 2010). Moreover, supported by and Akgerman, 1999). technological developments, the installment of industrial- 2.3. Analytical methods scale SCWO systems has come to the forefront and SCWO 2.3.1. HPLC is being promoted as an emerging treatment technology The composition analyses of the explosive wastewater in European directives (Brinkmann et al., 2016). and effluents were performed using a Thermo Finnigan There are few studies examining the degradation of Surveyor high-pressure liquid chromatograph (HPLC) explosives, as compared to other waste types, using equipped with a variable wavelength UV detector. SCWO. In these studies, the degradation mechanism and The chromatographic column was C18, 25 cm × 4.6 mm, 5 the optimum recovery rate were determined for a single µm. For the mobile phase, the methanol: water ratio was waste type. Chang and Liu (2007) reported that TNT was 50:50, with 1 mL/min of flow rate. For each experiment, degraded with 99.9% efficiency at 550 oC and 240 MPa in 20 µl of the sample was injected into the column at room 120 s with 300% of excess oxygen, whereas Zhao et al. temperature. The detector wavelength was 254 nm. (2008) claimed that the COD removal efficiency of HMX 2.3.2. GC-MS/MS exceeded 99% under conditions of 450-590 °C, 23 MPa By-product analyses were carried out in a TSQ™ 9000 and 300% of excess oxygen in 20 s. Similarly, Buelow et al. Triple Quadrupole GC-MS/MS System. Separations were (2002) reported that TNT and HMX degraded individually performed using a TraceGOLD TG-5MS 30 m x 0.25 mm x o at 600 C in 10 s at half of their water solubility 0.25 µm column. The total GC run time was 32.34 min. concentrations. These various experimental results Helium in a constant flow mode at 1.3 mL/min was used obtained from different studies demonstrated that as the carrier gas.
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