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Sample records for pentaerythritol tetranitrate petn

  1. Aging of Pentaerythritol Tetranitrate (PETN)

    Energy Technology Data Exchange (ETDEWEB)

    Foltz, M F

    2009-04-22

    Pentaerythritol tetranitrate (PETN) is a relatively sensitive explosive used in many electroexplosive devices as well as in medicine. Of primary interest to LLNL is its use in items such as exploding bridgewire (EBW) detonators and exploding bridge foil initiators (EFI). In these devices the crystalline powder is pressed into a granular, low-density compact that can be initiated by an exploding wire or foil. The long-term stability of this pressed compact is of interest to weapon stockpile lifetime prediction studies. Key points about potential aging mechanisms can be summarized as follows: (1) There are a number of factors that can contribute to PETN instability. These include particle size, polymorphic phase transitions, crystal structure, impurities, moisture, occlusions, chemical incompatibility and biological (microorganism) action. of these factors the most important for long-term aging of high surface area powders used in detonators appears to be that of particle size growth. (2) There is a great deal of literature on the thermal degradation kinetics of PETN, unfortunately much of it with little bearing on ambient temperature aging during long-term storage. PETN is very stable with respect to thermal decomposition. Low-temperature thermal studies have not revealed evidence of chemical degradation products in archived PETN. Data extrapolated to 30 C predicts a half-life of 12 million years. (3) Moisture seems to lower the activation energy for and accelerate the decomposition of PETN. (4) External drivers affecting stability include temperature, moisture, radiation fields, and stress, while internal drivers include residual solvents, and impurities. Temperature affects kinetic processes of crystal growth such as adsorption, desorption, and diffusion rates of molecules on the surface of PETN crystals. A low-level radiation field may induce unexpected changes in the chemical makeup of PETN and its homologue impurities. Stress at high pressure points caused by

  2. Pentaerythritol tetranitrate (PETN) profiling in post-explosion residues to constitute evidence of crime-scene presence

    NARCIS (Netherlands)

    Brust, H.; van Asten, A.; Koeberg, M.; van der Heijden, A.; Kuijpers, C.J.; Schoenmakers, P.

    2013-01-01

    Pentaerythritol tetranitrate (PETN) and its degradation products are analyzed to discriminate between residues originating from PETN explosions and residues obtained under other circumstances, such as natural degradation on textile, or after handling intact PETN. The degradation products observed in

  3. Method development and validation for measuring the particle size distribution of pentaerythritol tetranitrate (PETN) powders.

    Energy Technology Data Exchange (ETDEWEB)

    Young, Sharissa Gay

    2005-09-01

    Currently, the critical particle properties of pentaerythritol tetranitrate (PETN) that influence deflagration-to-detonation time in exploding bridge wire detonators (EBW) are not known in sufficient detail to allow development of a predictive failure model. The specific surface area (SSA) of many PETN powders has been measured using both permeametry and gas absorption methods and has been found to have a critical effect on EBW detonator performance. The permeametry measure of SSA is a function of particle shape, packed bed pore geometry, and particle size distribution (PSD). Yet there is a general lack of agreement in PSD measurements between laboratories, raising concerns regarding collaboration and complicating efforts to understand changes in EBW performance related to powder properties. Benchmarking of data between laboratories that routinely perform detailed PSD characterization of powder samples and the determination of the most appropriate method to measure each PETN powder are necessary to discern correlations between performance and powder properties and to collaborate with partnering laboratories. To this end, a comparison was made of the PSD measured by three laboratories using their own standard procedures for light scattering instruments. Three PETN powder samples with different surface areas and particle morphologies were characterized. Differences in bulk PSD data generated by each laboratory were found to result from variations in sonication of the samples during preparation. The effect of this sonication was found to depend on particle morphology of the PETN samples, being deleterious to some PETN samples and advantageous for others in moderation. Discrepancies in the submicron-sized particle characterization data were related to an instrument-specific artifact particular to one laboratory. The type of carrier fluid used by each laboratory to suspend the PETN particles for the light scattering measurement had no consistent effect on the resulting

  4. First-Principles Studies of Pentaerythritol Tetranitrate (PETN) Single Crystal Unit Cell Volumes and Vibrational Frequencies under Hydrostatic Pressure

    Science.gov (United States)

    Perger, Warren F.; Zhao, Jijun; Winey, J. M.; Gupta, Y. M.

    2006-07-01

    The vibrational frequencies of the PETN molecular crystal were calculated using the first-principles CRYSTAL03 program which employs an all-electron LCAO approach and calculates analytic first derivatives of the total energy with respect to atomic displacements. Numerical second derivatives were used to enable calculation of the vibrational frequencies at ambient pressure and under various states of compression. Three different density functionals, B3LYP, PW91, and X3LYP were used to examine the effect of the exchange-correlation functional on the vibrational frequencies. The average deviation with experimental results is shown to be on the order of 2-3%, depending on the functional used. The pressure-induced shift of the vibrational frequencies is presented.

  5. Sublimation Properties of Pentaerythritol Tetranitrate Single Crystals Doped with Its Homologs

    Energy Technology Data Exchange (ETDEWEB)

    Bhattacharia, Sanjoy K.; Maiti, Amitesh; Gee, Richard H.; Weeks, Brandon L.

    2012-07-20

    Pentaerythritol tetranitrate (PETN) is a secondary explosive used extensively in military and commercial applications. Coarsening of PETN during long-term storage changes the physical properties such as surface area and particle morphology which are important factors in initiation and performance. Doping of impurities was proposed to slow the coarsening process since impurities were shown to modify both the kinetic and thermodynamic properties. In this paper, we discuss how doping of PETN with its homologs of dipentaerythritol hexanitrate (diPEHN) and tripentaerytritol octanitrate (triPEON) affect kinetic and thermodynamic parameters. Pure and homolog doped PETN single crystals were prepared by solvent evaporation in acetone at room temperature. Doping concentrations for this study were 1000 ppm, 5000 ppm, and 10000 ppm. Activation energy and vapor pressure of pure and doped PETN single crystals were obtained from thermogravimetric analysis data.

  6. Application of isothermal calorimetry and uv spectroscopy for stability monitoring of pentaerythritol tetranitrate

    International Nuclear Information System (INIS)

    Dosser, L.R.; Pickard, J.M.

    1992-01-01

    Thermal stabilities for a series of pentaerythritol-tetranitrate (PETN) samples with variable surf ace areas were monitored by isothermal calorimetry and UV spectroscopy over the temperature range of 363 to 408 K. Isothermal induction times measured with constant volume calorimetry under an air atmosphere and No evolution rates monitored by UV absorbance at 213 nm under vacuum correlated with the PETN surface area at temperatures equal to or exceeding 383 K. Rate data measured at 383 K are in accord with predictions based on detailed kinetic modeling. Below 383 K, NO evolution data suggested that additional geometric factors may be significant in controlling PETN stability. Mechanisms for influencing surface area upon the rate-determining step are addressed

  7. Atomistic simulation of orientation dependence in shock-induced initiation of pentaerythritol tetranitrate.

    Science.gov (United States)

    Shan, Tzu-Ray; Wixom, Ryan R; Mattsson, Ann E; Thompson, Aidan P

    2013-01-24

    The dependence of the reaction initiation mechanism of pentaerythritol tetranitrate (PETN) on shock orientation and shock strength is investigated with molecular dynamics simulations using a reactive force field and the multiscale shock technique. In the simulations, a single crystal of PETN is shocked along the [110], [001], and [100] orientations with shock velocities in the range 3-10 km/s. Reactions occur with shock velocities of 6 km/s or stronger, and reactions initiate through the dissociation of nitro and nitrate groups from the PETN molecules. The most sensitive orientation is [110], while [100] is the most insensitive. For the [001] orientation, PETN decomposition via nitro group dissociation is the dominant reaction initiation mechanism, while for the [110] and [100] orientations the decomposition is via mixed nitro and nitrate group dissociation. For shock along the [001] orientation, we find that CO-NO(2) bonds initially acquire more kinetic energy, facilitating nitro dissociation. For the other two orientations, C-ONO(2) bonds acquire more kinetic energy, facilitating nitrate group dissociation.

  8. Effects of expiring reimbursability of pentaerythrityl tetranitrate (PETN, pentalong®) on anti-anginal therapy: an observational study.

    Science.gov (United States)

    Grimmsmann, Thomas; Chenot, Jean-François; Angelow, Aniela

    2015-08-01

    Pentaerythrityl tetranitrate (PETN) was the most commonly prescribed long-acting nitrate in Germany. We aimed to assess whether the discontinuation of PETN reimbursability in 2011 resulted in alternative prescriptions of anti-anginal medications or in a discontinuation of anti-anginal therapy. This is an observational study using health claims data from one German federal state analysing all patients discontinuing a PETN treatment. Patients starting a new alternative anti-anginal treatment (long-acting nitrates, molsidome, ivabradine and ranolazine) were compared with patients without a new anti-anginal treatment with respect to use of short-acting nitrates, beta blockers (BBs) and calcium channel blockers (CCBs). Out of 12,909 patients, 12,763 (99%) discontinued PETN until 12/2012. Of these, 52% started an alternative anti-anginal treatment, 43% did not receive any alternative treatment and 5% were excluded from analysis. Before termination of PETN reimbursability, 65% of patients received BBs, 29% CCBs and 10% short-acting nitrates. In patients started on alternative anti-anginal treatment, prescription rates for short-acting nitrates, BBs and CCBs remained constant after discontinuing PETN. In patients without any alternative anti-anginal treatment, prescription rates for BBs and CCBs did not change meaningfully (<3%), and prescription rates for short-acting nitrates decreased from 9% to 6%. Half of the patients discontinued PETN without alternative. This did not lead to increased prescription rates of standard IHD medications or total medication number indicating that there might still be a high percentage of ischaemic heart disease patients treated unnecessarily with long-acting nitrates. The undertreatment with prognostically relevant first-line medications indicates a need for better guideline implementation activities. Copyright © 2015 John Wiley & Sons, Ltd.

  9. Negative Ion Formation of Pentaerythritol Tetranitrate in Atmospheric Pressure Chemical Ionization-Mass Spectrometry and in Corona Discharge Ionization-Ion Mobility Spectrometry

    International Nuclear Information System (INIS)

    Choi, Sung Seen; Kim, Ok Bae; Kim, Yun Ki; An, Seung Geon; Shin, Myung Won; Maeng, Seug Jin; Choi, Gyu Seop

    2011-01-01

    Most organic explosives contain nitro groups and are subdivided into nitro-aromatic compounds, nitrate esters, and nitroamines. 1,3,5-Trinitrobenzene (TNB), 2,4,6-trinitrotoluene (TNT), and 2,4-dinitrotoluene (DNT) belong to the nitroaromatic compounds, pentaerythritol tetranitrate (PETN) is one of the nitrate esters, and the nitroamines include 1,3,5-trinitro-1,3,5-triazacyclohexane (RDX) and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX). Explosives are unstable compounds and their polarities vary from moderate to high due to their nitro groups. These properties impose certain limitations on techniques used for their analysis, since explosives may decompose during analysis or result in poor chromatographic retention. Gas chromatography (GC) is suitable for the analysis of nitroaromatic compounds, but not for nitrate esters and nitroamines, which undergo thermal decomposition under the high temperature conditions of injector and oven. High-performance liquid chromatography (HPLC) would be a better alternative for the more unstable and polar explosives Common analytical

  10. Photochemistry of the α-Al2O3-PETN Interface

    Directory of Open Access Journals (Sweden)

    Roman V. Tsyshevsky

    2016-02-01

    Full Text Available Optical absorption measurements are combined with electronic structure calculations to explore photochemistry of an α-Al2O3-PETN interface formed by a nitroester (pentaerythritol tetranitrate, PETN, C5H8N4O12 and a wide band gap aluminum oxide (α-Al2O3 substrate. The first principles modeling is used to deconstruct and interpret the α-Al2O3-PETN absorption spectrum that has distinct peaks attributed to surface F0-centers and surface—PETN transitions. We predict the low energy α-Al2O3 F0-center—PETN transition, producing the excited triplet state, and α-Al2O3 F0-center—PETN charge transfer, generating the PETN anion radical. This implies that irradiation by commonly used lasers can easily initiate photodecomposition of both excited and charged PETN at the interface. The feasible mechanism of the photodecomposition is proposed.

  11. PETN Coarsening - Predictions from Accelerated Aging Data

    Energy Technology Data Exchange (ETDEWEB)

    Maiti, Amitesh [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Gee, Richard H. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2011-03-30

    Ensuring good ignition properties over long periods of time necessitates maintaining a good level of porosity in powders of initiator materials and preventing particle coarsening. To simulate porosity changes of such powder materials over long periods of time a common strategy is to perform accelerated aging experiments over shorter time spans at elevated temperatures. In this paper we examine historical accelerated-aging data on powders of Pentaerythritol Tetranitrate (PETN), an important energetic material, and make predictions for long-term aging under ambient conditions. Lastly, we develop an evaporation-condensation- based model to provide some mechanistic understanding of the coarsening process.

  12. Exploring the High-Pressure Behavior of PETN: A Combined Quantum Mechanical and Experimental Study

    Science.gov (United States)

    2006-11-01

    calculations to explore the hypothesized compression-induced polymorphic phase transition [Gruzdkov 2004]. The initial crystal in these Figure 4...Scuseria, G.E., and Chabalowski, C.F. 2004: An ab Initio Study of Solid Nitromethane, HMX , RDX , and CL20: Successes and Failures of DFT. J. Phys. Chem... RDX , HMX , HNIW, and PETN Crystals. J. Phys. Chem. B, 103, 6783. Trotter, J., 1963: Bond lengths and angles in Pentaerythritol Tetranitrate. Acta

  13. Separation and determination of PETN and TNT by HPTLC

    Energy Technology Data Exchange (ETDEWEB)

    Chaloosi, Marzieh; Nejad-Darzi, Seyed Karim Hassani; Ghoulipour, Vanik [Faculty of Chemistry, University of Tarbiat Moallem, Tehran (Iran)

    2009-02-15

    High-performance thin layer chromatography (HPTLC) has been used for the separation and quantification of 2,4,6-trinitrotoluene (TNT) and pentaerythritol tetranitrate (PETN). The compounds were separated on silica gel 60 F{sub 254} with a double development system of trichloroethylene-acetone 4:1 and petroleum ether-acetone 5.7:1. For obtaining chromatograms of these materials, UV detection was performed at 215 and 250 nm for PETN and TNT, respectively. The linear dynamic range was 0.835-83.50 {mu}g per spot for PETN and 0.045-1.44 {mu}g per spot for TNT. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  14. Shock-induced hotspot formation and chemical reaction initiation in PETN containing a spherical void

    International Nuclear Information System (INIS)

    Shan, Tzu-Ray; Thompson, Aidan P

    2014-01-01

    We present results of reactive molecular dynamics simulations of hotspot formation and chemical reaction initiation in shock-induced compression of pentaerythritol tetranitrate (PETN) with the ReaxFF reactive force field. A supported shockwave is driven through a PETN crystal containing a 20 nm spherical void at a sub-threshold impact velocity of 2 km/s. Formation of a hotspot due to shock-induced void collapse is observed. During void collapse, NO 2 is the dominant species ejected from the upstream void surface. Once the ejecta collide with the downstream void surface and the hotspot develops, formation of final products such as N 2 and H 2 O is observed. The simulation provides a detailed picture of how void collapse and hotspot formation leads to initiation at sub-threshold impact velocities.

  15. Frictional properties of single crystals HMX, RDX and PETN explosives

    International Nuclear Information System (INIS)

    Wu, Y.Q.; Huang, F.L.

    2010-01-01

    The frictional properties of single crystals of cyclotetramethylene tetranitramine (HMX), cyclotrimethylene trinitramine (RDX) and pentaerythritol tetranitrate (PETN) secondary explosives are examined using a sensitive friction machine. The explosive crystals used for the measurements are at least 3.5 mm wide. The friction coefficients between crystals of the same explosive (i.e., HMX on HMX, etc.), crystals of different explosives (i.e., HMX on RDX, etc.), and each explosive and a well-polished gauge steel surface are determined. The frictional surfaces are also studied under an environmental scanning electron microscope (ESEM) to analyze surface microstructural changes under increasing loading forces. The friction coefficients vary considerably with increasing normal loading forces and are particularly sensitive to slider shapes, crystal roughness and the mechanical properties of both the slider and the sample. With increasing loading forces, most friction experiments show surface damage, consisting of grooves, debris, and nano-particles, on both the slider and sample. In some cases, a strong evidence of a localized molten state is found in the central region of the friction track. Possible mechanisms that affect the friction coefficient are discussed based on microscopic observations.

  16. Reactive Burn Model Calibration for PETN Using Ultra-High-Speed Phase Contrast Imaging

    Science.gov (United States)

    Johnson, Carl; Ramos, Kyle; Bolme, Cindy; Sanchez, Nathaniel; Barber, John; Montgomery, David

    2017-06-01

    A 1D reactive burn model (RBM) calibration for a plastic bonded high explosive (HE) requires run-to-detonation data. In PETN (pentaerythritol tetranitrate, 1.65 g/cc) the shock to detonation transition (SDT) is on the order of a few millimeters. This rapid SDT imposes experimental length scales that preclude application of traditional calibration methods such as embedded electromagnetic gauge methods (EEGM) which are very effective when used to study 10 - 20 mm thick HE specimens. In recent work at Argonne National Laboratory's Advanced Photon Source we have obtained run-to-detonation data in PETN using ultra-high-speed dynamic phase contrast imaging (PCI). A reactive burn model calibration valid for 1D shock waves is obtained using density profiles spanning the transition to detonation as opposed to particle velocity profiles from EEGM. Particle swarm optimization (PSO) methods were used to operate the LANL hydrocode FLAG iteratively to refine SURF RBM parameters until a suitable parameter set attained. These methods will be presented along with model validation simulations. The novel method described is generally applicable to `sensitive' energetic materials particularly those with areal densities amenable to radiography.

  17. Time-of-flight mass spectrometry of laser exploding foil initiated PETN samples

    Science.gov (United States)

    Fajardo, Mario E.; Molek, Christopher D.; Fossum, Emily C.

    2017-01-01

    We report the results of time-of-flight mass spectrometry (TOFMS) measurements of the gaseous products of thin-film pentaerythritol tetranitrate [PETN, C(CH2NO3)4] samples reacting in vacuo. The PETN sample spots are produced by masked physical vapor deposition [A.S. Tappan, et al., AIP Conf. Proc. 1426, 677 (2012)] onto a first-surface aluminum mirror. A pulsed laser beam imaged through the soda lime glass mirror substrate converts the aluminum layer into a high-temperature high-pressure plasma which initiates chemical reactions in the overlying PETN sample. We had previously proposed [E.C. Fossum, et al., AIP Conf. Proc. 1426, 235 (2012)] to exploit differences in gaseous product chemical identities and molecular velocities to provide a chemically-based diagnostic for distinguishing between "detonation-like" and deflagration responses. Briefly: we expect in-vacuum detonations to produce hyperthermal (v˜10 km/s) thermodynamically-stable products such as N2, CO2, and H2O, and for deflagrations to produce mostly reaction intermediates, such as NO and NO2, with much slower molecular velocities - consistent with the expansion-quenched thermal decomposition of PETN. We observe primarily slow reaction intermediates (NO2, CH2NO3) at low laser pulse energies, the appearance of NO at intermediate laser pulse energies, and the appearance of hyperthemal CO/N2 at mass 28 amu at the highest laser pulse energies. However, these results are somewhat ambiguous, as the NO, NO2, and CH2NO3 intermediates persist and all species become hyperthermal at the higher laser pulse energies. Also, the purported CO/N2 signal at 28 amu may be contaminated by silicon ablated from the glass mirror substrate. We plan to mitigate these problems in future experiments by adopting the "Buelow" sample configuration which employs an intermediate foil barrier to shield the energetic material from the laser and the laser driven plasma [S.J. Buelow, et al., AIP Conf. Proc. 706, 1377 (2003)].

  18. Mitochondrial oxidative stress and nitrate tolerance – comparison of nitroglycerin and pentaerithrityl tetranitrate in Mn-SOD+/- mice

    Directory of Open Access Journals (Sweden)

    Stalleicken Dirk

    2006-11-01

    Full Text Available Abstract Background Chronic therapy with nitroglycerin (GTN results in a rapid development of nitrate tolerance which is associated with an increased production of reactive oxygen species (ROS. According to recent studies, mitochondrial ROS formation and oxidative inactivation of the organic nitrate bioactivating enzyme mitochondrial aldehyde dehydrogenase (ALDH-2 play an important role for the development of nitrate and cross-tolerance. Methods Tolerance was induced by infusion of wild type (WT and heterozygous manganese superoxide dismutase mice (Mn-SOD+/- with ethanolic solution of GTN (12.5 μg/min/kg for 4 d. For comparison, the tolerance-free pentaerithrityl tetranitrate (PETN, 17.5 μg/min/kg for 4 d was infused in DMSO. Vascular reactivity was measured by isometric tension studies of isolated aortic rings. ROS formation and aldehyde dehydrogenase (ALDH-2 activity was measured in isolated heart mitochondria. Results Chronic GTN infusion lead to impaired vascular responses to GTN and acetylcholine (ACh, increased the ROS formation in mitochondria and decreased ALDH-2 activity in Mn-SOD+/- mice. In contrast, PETN infusion did not increase mitochondrial ROS formation, did not decrease ALDH-2 activity and accordingly did not lead to tolerance and cross-tolerance in Mn-SOD+/- mice. PETN but not GTN increased heme oxygenase-1 mRNA in EA.hy 926 cells and bilirubin efficiently scavenged GTN-derived ROS. Conclusion Chronic GTN infusion stimulates mitochondrial ROS production which is an important mechanism leading to tolerance and cross-tolerance. The tetranitrate PETN is devoid of mitochondrial oxidative stress induction and according to the present animal study as well as numerous previous clinical studies can be used without limitations due to tolerance and cross-tolerance.

  19. Non-hemodynamic effects of organic nitrates and the distinctive characteristics of pentaerithrityl tetranitrate.

    Science.gov (United States)

    Gori, Tommaso; Daiber, Andreas

    2009-01-01

    Organic nitrates are among the oldest and yet most commonly employed drugs in the long-term therapy of coronary artery disease and congestive heart failure. While they have long been used in clinical practice, our understanding of their mechanism of action and side effects remains incomplete. For instance, recent findings provide evidence of previously unanticipated, non-hemodynamic properties that include potentially beneficial mechanisms (such as the induction of a protective phenotype that mimics ischemic preconditioning), but also toxic effects (such as endothelial and autonomic dysfunction, rebound angina, tolerance). To date, the most commonly employed organic nitrates are isosorbide mononitrate, isosorbide dinitrate, and nitroglycerin (glyceryl trinitrate). Another organic nitrate, pentaerithrityl tetranitrate (PETN), has long been employed in eastern European countries and is currently being reintroduced in Western countries. In light of their wide use, and of the (re)introduction of PETN in Western markets, the present review focuses on the novel effects of organic nitrates, describing their potential clinical implications and discussing differences among different compounds. We believe that these recent findings have important clinical implications. Since the side effects of organic nitrates such as nitroglycerin and isosorbides appear to be mediated by reactive oxygen species, care should be taken that drugs with antioxidant properties are co-administered. On the other hand, efforts should be made to clinically exploit the preconditioning effects of these drugs.

  20. Technology Challenges in Solid Energetic Materials for Micro Propulsion Applications

    Science.gov (United States)

    2009-11-01

    pressure and low temperature. NAB is used with/without lead rhodanide/ potassium chlorate /nitrocellulose (RK) to aid in the ignition. The impulse thrust...NAB boron/ potassium nitrate PETN Pentaerythritol tetranitrate RK lead rhodanide/ potassium chlorate /nitrocellulose Zr zirconium ZPP zirconium... potassium nitrate (NAB) propellant was selected over HTPB/AP and glycidyle azide polymer (GAP), because of its ignition capability at atmospheric

  1. Integrated Data Analysis (IDCA) Program - PETN Class 4 Standard

    Energy Technology Data Exchange (ETDEWEB)

    Sandstrom, Mary M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Geoffrey W. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Preston, Daniel N. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Pollard, Colin J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Warner, Kirstin F. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Sorensen, Daniel N. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Remmers, Daniel L. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Shelley, Timothy J. [Air Force Research Lab. (AFRL), Tyndall AFB, FL (United States); Reyes, Jose A. [Applied Research Associates, Tyndall AFB, FL (United States); Phillips, Jason J. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Hsu, Peter C. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Reynolds, John G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2012-08-01

    The Integrated Data Collection Analysis (IDCA) program is conducting a proficiency study for Small- Scale Safety and Thermal (SSST) testing of homemade explosives (HMEs). Described here are the results for impact, friction, electrostatic discharge, and differential scanning calorimetry analysis of PETN Class 4. The PETN was found to have: 1) an impact sensitivity (DH50) range of 6 to 12 cm, 2) a BAM friction sensitivity (F50) range 7 to 11 kg, TIL (0/10) of 3.7 to 7.2 kg, 3) a ABL friction sensitivity threshold of 5 or less psig at 8 fps, 4) an ABL ESD sensitivity threshold of 0.031 to 0.326 j/g, and 5) a thermal sensitivity of an endothermic feature with Tmin = ~ 141 °C, and a exothermic feature with a Tmax = ~205°C.

  2. Temperature evolution in silver nanoparticle doped PETN composite

    Science.gov (United States)

    Kameswari, D. P. S. L.; Kiran, P. Prem

    2018-04-01

    Optical absorption and the associated spatio-temporal evolution of temperature silver nanoparticles doped energetic material composite is presented. Silver nanoparticles of radii 10 - 150 nm are doped in Penta Erythrtol Tetra Nitrate (PETN), a secondary energetic material to form the composite materials. Of all the composites the ones doped with 35 nm sized nanoparticles have shown maximum absorption at excitation wavelength of 532 nm. The spatio-temporal evolution of temperature within these composites up on excitation with ns laser pulses of energy density 0.5 J/cm2 is studied. The role of particle sizes on the temperature of composites is studied and a maximum temperature of 2200 K at the nanoparticle interface is observed for 35 nm doped PETN composite.

  3. Laser-Induced Breakdown Spectroscopy: A Review of Applied Explosive Detection

    Science.gov (United States)

    2013-09-01

    ammonium nitrate (AN)), and explosive primers and propellants ( potassium chlorate and ammonium perchlorate...trinitrotoulene, DNT = 2,4-dinitrotoluene, PETN = pentaerythritol tetranitrate, TATP = triacetone triperoxide, AN = ammonium nitrate, KClO3 = potassium chlorate ...Sucrose C12H22O11 Precursor Material Chlorate KClO3, NH4ClO4 Primer, Propellant Note: EGDM = ethylene glycol dinitrate, TNT = 2,4,6

  4. The construction and evaluation of a high pressure manifold and vessels for a Calvet type microcalorimeter

    International Nuclear Information System (INIS)

    Jones, D.E.G.; Turcotte, A.-M.; Fouchard, R.C.

    2003-01-01

    A Setaram C-80 calorimeter has been modified in order to measure the heat flow of energetic materials at pressures up to 69 MPa. A manifold and sample cells capable of operating at high pressure were designed, constructed and evaluated. This paper will describe, in detail, the high pressure manifold construction, safety assessment and calibration. As well, the results for initial trials with ammonium nitrate (AN), and pentaerythritol tetranitrate (PETN) at various pressures and heating rates will be discussed

  5. Direct Analysis in Real Time Mass Spectrometry of Potential By-Products from Homemade Nitrate Ester Explosive Synthesis

    OpenAIRE

    Sisco, Edward; Forbes, Thomas P.

    2015-01-01

    This work demonstrates the coupling of direct analysis in real time (DART) ionization with time-of-flight mass spectrometry (MS) in an off-axis configuration for the trace detection and analysis of potential partially nitrated and dimerized by-products of homemade nitrate ester explosive synthesis. Five compounds relating to the synthesis of nitroglycerin (NG) and pentaerythritol tetranitrate (PETN) were examined. Deprotonated ions and adducts with molecular oxygen, nitrite, and nitrate were ...

  6. Biodegradación del explosivo tetranitrato de pentaeritritol (PETN por bacterias aisladas de ambientes mineros

    Directory of Open Access Journals (Sweden)

    Yerson Durán

    2013-12-01

    Full Text Available El tetranitrato de pentaeritritol (PETN es el detonante más energético y recalcitrante empleado en la actividad minera ya que posee cuatro grupos nitro unidos mediante enlaces éster; además es un contaminante orgánico persistente según el Convenio de Estocolmo. En el presente trabajo es evaluada la eficiencia de degradación del PETN por bacterias aisladas de ambientes mineros. En primer lugar se seleccionó las cepas con mayor crecimiento durante tres subcultivos en medio mínimo con PETN como única fuente de nitrógeno. Luego, se identificó mediante análisis del gen RNAr 16S las cepas Bacillus sp. J8A2 y Enterobacter sp. M1B. Las velocidades específicas de crecimiento fueron de 0.057 h -1 para J8A2 y 0.042 h -1 para M1B, y las velocidades específicas de degradación de 0.72 y 1.16 mmol de PETN/g de proteína.h, respectivamente. Además, el extracto crudo de la cepa J8A2 mostró una actividad específica (U de 1.03 mmol de PETN/h y una actividad específica por proteína (U/g de 138.6 mmol de PETN/g.h.

  7. Implementation of a PETN failure model using ARIA's general chemistry framework

    Energy Technology Data Exchange (ETDEWEB)

    Hobbs, Michael L. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2017-01-01

    We previously developed a PETN thermal decomposition model that accurately predicts thermal ignition and detonator failure [1]. This model was originally developed for CALORE [2] and required several complex user subroutines. Recently, a simplified version of the PETN decomposition model was implemented into ARIA [3] using a general chemistry framework without need for user subroutines. Detonator failure was also predicted with this new model using ENCORE. The model was simplified by 1) basing the model on moles rather than mass, 2) simplifying the thermal conductivity model, and 3) implementing ARIA’s new phase change model. This memo briefly describes the model, implementation, and validation.

  8. 40 CFR 721.3680 - Ethylene oxide adduct of fatty acid ester with pentaerythritol.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Ethylene oxide adduct of fatty acid... New Uses for Specific Chemical Substances § 721.3680 Ethylene oxide adduct of fatty acid ester with... identified generically as ethylene oxide adduct of fatty acid ester with pentaerythritol (PMN P-91-442) is...

  9. Mass Spectrometric Analysis of Eight Common Chemical Explosives Using Ion Trap Mass Spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Park, Sehwan; Lee, Jihyeon; KIm, Jeongkwon [Chungnam National Univ., Daejeon (Korea, Republic of); Cho, Soo Gyeong; Goh, Eun Mee [Agency for Defense Development, Daejeon (Korea, Republic of); Lee, Sungman; Koh, Sungsuk [Sensor Tech Inc., Seoul (Korea, Republic of)

    2013-12-15

    Eight representative explosives (ammonium perchlorate (AP), ammonium nitrate (AN), trinitrotoluene (TNT), 2,4-dinitrotoluene (DNT), cyclonite (RDX), cyclotetramethylenetetranitramine (HMX), pentaerythritol tetranitrate (PETN), and hexanitrostilbene (HNS)) were comprehensively analyzed with an ion trap mass spectrometer in negative ion mode using direct infusion electrospray ionization. MS/MS experiments were performed to generate fragment ions from the major parent ion of each explosive. Explosives in salt forms such as AP or AN provided cluster parent ions with their own anions. Explosives with an aromatic ring were observed as either [M.H]{sup -} for TNT and DNT or [M]{sup ·-}. for HNS, while explosives without an aromatic ring such as RDX, HMX, and PETN were detected as an adduct ion with a formate anion, i. e., [M+HCOO]{sup -}. These findings provide a guideline for the rapid and accurate detection of explosives once portable MS instruments become more readily available.

  10. Mass Spectrometric Analysis of Eight Common Chemical Explosives Using Ion Trap Mass Spectrometer

    International Nuclear Information System (INIS)

    Park, Sehwan; Lee, Jihyeon; KIm, Jeongkwon; Cho, Soo Gyeong; Goh, Eun Mee; Lee, Sungman; Koh, Sungsuk

    2013-01-01

    Eight representative explosives (ammonium perchlorate (AP), ammonium nitrate (AN), trinitrotoluene (TNT), 2,4-dinitrotoluene (DNT), cyclonite (RDX), cyclotetramethylenetetranitramine (HMX), pentaerythritol tetranitrate (PETN), and hexanitrostilbene (HNS)) were comprehensively analyzed with an ion trap mass spectrometer in negative ion mode using direct infusion electrospray ionization. MS/MS experiments were performed to generate fragment ions from the major parent ion of each explosive. Explosives in salt forms such as AP or AN provided cluster parent ions with their own anions. Explosives with an aromatic ring were observed as either [M.H] - for TNT and DNT or [M] ·- . for HNS, while explosives without an aromatic ring such as RDX, HMX, and PETN were detected as an adduct ion with a formate anion, i. e., [M+HCOO] - . These findings provide a guideline for the rapid and accurate detection of explosives once portable MS instruments become more readily available

  11. First-principles studies of PETN molecular crystal vibrational frequencies under high pressure

    Science.gov (United States)

    Perger, Warren; Zhao, Jijun

    2005-07-01

    The vibrational frequencies of the PETN molecular crystal were calculated using the first-principles CRYSTAL03 program which employs an all-electron LCAO approach and calculates analytic first derivatives of the total energy with respect to atomic displacements. Numerical second derivatives were used to enable calculation of the vibrational frequencies at ambient pressure and under various states of compression. Three different density functionals, B3LYP, PW91, and X3LYP were used to examine the effect of the exchange-correlation functional on the vibrational frequencies. The pressure-induced shift of the vibrational frequencies will be presented and compared with experiment. The average deviation with experimental results is shown to be on the order of 2-3%, depending on the functional used.

  12. Oleic Acid Based Polyesters of Trimethylolpropane and Pentaerythritol for Bio lubricant Application

    International Nuclear Information System (INIS)

    Hamizah Ammarah Mahmud; Nadia Salih; Jumat Salimon

    2015-01-01

    The production of polyesters based on oleic acid and trimethylolpropane (TMP) or pentaerythritol (PE) as potential bio lubricant were carried out. The esterification processes between oleic acid with TMP or PE were carried out using sulfuric acid as a catalyst. The esterification process produced high yield between 92 %-94 % w/w respectively. The formation of polyesters was confirmed using gas chromatography (GC-FID), Fourier Transform Infrared Spectroscopy (FTIR) and Nuclear Magnetic Resonance (NMR). The polyesters were analyzed for basic lubrication physicochemical properties. The results showed that polyesters of both TMP and PE having high viscosity index between 200-309, good pour points ranging from -42 to -59 degree Celsius and high flash points of 280 - 300 degree Celsius respectively. The polyesters also showed good thermal oxidative stability with TGA onset temperatures above 180 degree Celsius. In general both products are plausible to be used as bio lubricant for industrial application. (author)

  13. Forensic analysis of explosives using isotope ratio mass spectrometry (IRMS)--preliminary study on TATP and PETN.

    Science.gov (United States)

    Benson, Sarah J; Lennard, Christopher J; Maynard, Philip; Hill, David M; Andrew, Anita S; Roux, Claude

    2009-06-01

    The application of isotopic techniques to investigations requiring the provision of evidence to a Court is limited. The objective of this research was to investigate the application of light stable isotopes and isotope ratio mass spectrometry (IRMS) to solve complex forensic cases by providing a level of discrimination not achievable utilising traditional forensic techniques. Due to the current threat of organic peroxide explosives, such as triacetone triperoxide (TATP), research was undertaken to determine the potential of IRMS to differentiate samples of TATP that had been manufactured utilising different starting materials and/or manufacturing processes. In addition, due to the prevalence of pentaerythritoltetranitrate (PETN) in detonators, detonating cord, and boosters, the potential of the IRMS technique to differentiate PETN samples from different sources was also investigated. Carbon isotope values were measured in fourteen TATP samples, with three definite groups appearing in the initial sample set based on the carbon data alone. Four additional TATP samples (in a second set of samples) were distinguishable utilising the carbon and hydrogen isotopic compositions individually, and also in combination with the oxygen isotope values. The 3D plot of the carbon, oxygen and hydrogen data demonstrated the clear discrimination of the four samples of TATP. The carbon and nitrogen isotope values measured from fifteen PETN samples, allowed samples from different sources to be readily discriminated. This paper demonstrates the successful application of IRMS to the analysis of explosives of forensic interest to assist in discriminating samples from different sources. This research represents a preliminary evaluation of the IRMS technique for the measurement of stable isotope values in TATP and PETN samples, and supports the dedication of resources for a full evaluation of this application in order to achieve Court reportable IRMS results.

  14. Surface characterization of an energetic material, pentaerythritoltetranitrate (PETN), having a thin coating achieved through a starved addition microencapsulation technique

    Energy Technology Data Exchange (ETDEWEB)

    Worley, C.M.

    1986-05-07

    The objective of this research was to: (1) determine the nature of a thin coating on an explosive material which was applied using a starved addition microencapsulation technique, (2) understand the coating/crystal bond, and (3) investigate the wettability/adhesion of plastic/solvent combinations using the coating process. The coating used in this work was a Firestone Plastic Company copolymer (FPC-461) of vinylchloride/trifluorochloroethylene in a 1.5/1.0 weight ratio. The energetic explosive examined was pentaerythritoltetranitrate (PETN). The coating process used was starved addition followed by a solvent evaporation technique. Surface analytical studies, completed for characterization of the coating process, show (1) evidence that the polymer coating is present, but not continuous, over the surface of PETN; (2) the average thickness of the polymer coating is between 16-32 A and greater than 44 A, respectively, for 0.5 and 20 wt % coated PETN; (3) no changes in surface chemistry of the polymer or the explosive material following microencapsulation; and (4) the presence of explosive material on the surface of 0.5 wt % FPC-461 coated explosives. 5 refs., 15 figs., 6 tabs.

  15. Forensic analysis of explosive residues from hand swabs

    International Nuclear Information System (INIS)

    Umi Khairul Ahmad; Sumathy Rajendran; Syahidah Abu Hassan

    2008-01-01

    In the forensic examination of physical evidence for organic explosives, cotton swabs are often used to collect residue from surfaces, such as skin and post-blast debris. A preliminary study has been conducted to develop extraction method of a common energetic compound, pentaerythritol tetranitrate (PETN) from hand swabs followed by direct analysis of the resulting extract solution using high-performance liquid chromatography (HPLC) with ultraviolet (UV) detector. Analysis was performed on an octadecylsilane-based (C 18 ) column using acetonitrile-water mixture (55:45) as mobile phase. The mobile phase was pumped at 1.0 mL/ min and separation affected using an isocratic mode with the detection wavelength of 230 nm. The explosive residue was extracted from cotton swabs using acetone in an ultrasonic cold bath. The developed method was later applied to the real hand swabs samples, which were taken from three army personnel who handled PETN during a munition disposal operation at Asahan Camp Military Firing range. The acetone extract obtained using sonication method was found to be effective in recovering PETN from cotton swabs with relatively high recovery (89.5 %) and good sensitivity with detection limit as low as 2 ng. The content of PETN in the real hand swab samples were found to be in the range of 4.7-130 mg. (author)

  16. ONE-DIMENSIONAL TIME TO EXPLOSION (THERMAL SENSITIVITY) TESTS ON PETN, PBX-9407, LX-10, AND LX-17

    Energy Technology Data Exchange (ETDEWEB)

    Hsu, Peter C. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Strout, Steve [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); McClelland, Matthew [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Ellsworth, Fred Ellsworth [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2016-01-28

    Incidents caused by fire and combat operations can heat energetic materials that may lead to thermal explosion and result in structural damage and casualty. Some explosives may thermally explode at fairly low temperatures (< 100 C) and the violence from thermal explosion may cause a significant damage. Thus it is important to understand the response of energetic materials to thermal insults. The One Dimensional Time to Explosion (ODTX) system at the Lawrence Livermore National Laboratory has been used for decades to measure times to thermal explosion, threshold thermal explosion temperature, and determine the kinetic parameters of thermal decomposition of energetic materials. Samples of different configurations (pressed part, powder, paste, and liquid) can be tested in the system. The ODTX testing can also provide useful data for assessing the thermal explosion violence of energetic materials. This report summarizes the results of our recent ODTX experiments on PETN powder, PBX-9407 pressed part, LX-10 pressed part, LX-17 pressed part and compares the test data that were obtained decades ago with the older version of ODTX system. Test results show the thermal sensitivity of various materials tested in the following order: PETN> PBX-9407 > LX-10 > LX-17.

  17. A novel polyester composite nanofiltration membrane formed by interfacial polymerization of pentaerythritol (PE) and trimesoyl chloride (TMC)

    Science.gov (United States)

    Cheng, Jun; Shi, Wenxin; Zhang, Lanhe; Zhang, Ruijun

    2017-09-01

    A novel polyester thin film composite nanofiltration (NF) membrane was prepared by interfacial polymerization of pentaerythritol (PE) and trimesoyl chloride (TMC) on polyethersulfone (PES) supporting membrane. The performance of the polyester composite NF membrane was optimized by regulating the preparation parameters, including reaction time, pH of the aqueous phase solution, pentaerythritol concentration and TMC concentration. A series of characterization, including permeation experiments, attenuated total reflectance-fourier transform infrared spectroscopy (ATR-FTIR), scanning electron microscope (SEM), atomic force microscopy (AFM), zeta potential analyzer and chlorine resistance experiments, were employed to study the properties of the optimized membrane. The results showed that the optimized polyester composite NF membrane exhibited very high rejection of Na2SO4 (98.1%), but the water flux is relatively low (6.1 L/m2 h, 0.5 MPa, 25 °C). The order of salt rejections is Na2SO4 > MgSO4 > MgCl2 > NaCl, which indicated the membrane was negatively charged, just consistent with the membrane zeta potential results. After treating by NaClO solutions with different concentrations (100 ppm, 500 ppm, 1000 ppm, 2000 ppm, 3000 ppm) for 48 h, the results demonstrated that the polyester NF membrane had good chlorine resistance. Additionally, the polyester TFC NF membrane exhibits good long-term stability.

  18. Unreacted equation of states of typical energetic materials under static compression: A review

    International Nuclear Information System (INIS)

    Zheng Zhaoyang; Zhao Jijun

    2016-01-01

    The unreacted equation of state (EOS) of energetic materials is an important thermodynamic relationship to characterize their high pressure behaviors and has practical importance. The previous experimental and theoretical works on the equation of state of several energetic materials including nitromethane, 1,3,5-trinitrohexahydro-1,3,5-triazine (RDX), 1,3,5,7-tetranitro-1,3,5,7-tetrazacyclooctane (HMX), hexanitrostilbene (HNS), hexanitrohexaazaisowurtzitane (HNIW or CL-20), pentaerythritol tetranitrate (PETN), 2,6-diamino-3,5-dinitropyrazine-1-oxide (LLM-105), triamino-trinitrobenzene (TATB), 1,1-diamino-2,2-dinitroethene (DADNE or FOX-7), and trinitrotoluene (TNT) are reviewed in this paper. The EOS determined from hydrostatic and non-hydrostatic compressions are discussed and compared. The theoretical results based on ab initio calculations are summarized and compared with the experimental data. (topical review)

  19. Long-term use of short- and long-acting nitrates in stable angina pectoris.

    Science.gov (United States)

    Kosmicki, Marek Antoni

    2009-05-01

    Long-acting nitrates are effective antianginal drugs during initial treatment. However, their therapeutic value is compromised by the rapid development of tolerance during sustained therapy, which means that their clinical efficacy is decreased during long-term use. Sublingual nitroglycerin (NTG), a short-acting nitrate, is suitable for the immediate relief of angina. In patients with stable angina treated with oral long-acting nitrates, NTG maintains its full anti-ischemic effect both after initial oral ingestion and after intermittent long-term oral administration. However, NTG attenuates this effect during continuous treatment, when tolerance to oral nitrates occurs, and this is called cross-tolerance. In stable angina long-acting nitrates are considered third-line therapy because a nitrate-free interval is required to avoid the development of tolerance. Nitrates vary in their potential to induce the development of tolerance. During long-lasting nitrate therapy, except pentaerythritol tetranitrate (PETN), one can observe the development of reactive oxygen species (ROS) inside the muscular cell of a vessel wall, and these bind with nitric oxide (NO). This leads to decreased NO activity, thus, nitrate tolerance. PETN has no tendency to form ROS, and therefore during long-term PETN therapy, there is probably no tolerance or cross-tolerance, as during treatment with other nitrates.

  20. Novel uses of detonator diagnostics

    Energy Technology Data Exchange (ETDEWEB)

    Gibson, John R. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Wilde, Zakary Robert [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Tasker, Douglas George [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Francois, Elizabeth Green [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Nakamoto, Teagan Kanakanui Junichi [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Smith, Dalton Kay [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Trujillo, Christopher J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-09-15

    A novel combination of diagnostics is being used to research the physics of detonator initiation. The explosive PETN (Pentaerythritol tetranitrate) commonly used in detonators, is also a piezo-electric material that, when sufficiently shocked, emits an electromagnetic field in the radio frequency (RF) range, along crystal fracture planes. In an effort to capture this RF signal, a new diagnostic was created. A copper foil, used as an RF antenna, was wrapped around a foam fixture encompassing a PETN pellet. Rogowski coils were used to obtain the change in current with respect to time (di/dt) the detonator circuit, in and polyvinylidene difluoride (PVDF) stress sensors were used to capture shockwave arrival time. The goal of these experiments is to use these diagnostics to study the reaction response of a PETN pellet of known particle size to shock loading with various diagnostics including an antenna to capture RF emissions. Our hypothesis is that RF feedback may signify the rate of deflagration to detonation transition (DDT) or lack thereof. The new diagnostics and methods will be used to determine the timing of start of current, bridge burst, detonator breakout timing and RF generated from detonation. These data will be compared to those of currently used diagnostics in order to validate the accuracy of these new methods. Future experiments will incorporate other methods of validation including dynamic radiography, optical initiation and use of magnetic field sensors.

  1. High explosive spot test analyses of samples from Operable Unit (OU) 1111

    Energy Technology Data Exchange (ETDEWEB)

    McRae, D.; Haywood, W.; Powell, J.; Harris, B.

    1995-01-01

    A preliminary evaluation has been completed of environmental contaminants at selected sites within the Group DX-10 (formally Group M-7) area. Soil samples taken from specific locations at this detonator facility were analyzed for harmful metals and screened for explosives. A sanitary outflow, a burn pit, a pentaerythritol tetranitrate (PETN) production outflow field, an active firing chamber, an inactive firing chamber, and a leach field were sampled. Energy dispersive x-ray fluorescence (EDXRF) was used to obtain semi-quantitative concentrations of metals in the soil. Two field spot-test kits for explosives were used to assess the presence of energetic materials in the soil and in items found at the areas tested. PETN is the major explosive in detonators manufactured and destroyed at Los Alamos. No measurable amounts of PETN or other explosives were detected in the soil, but items taken from the burn area and a high-energy explosive (HE)/chemical sump were contaminated. The concentrations of lead, mercury, and uranium are given.

  2. Forensic Analysis of High Explosive Residues from Selected Cloth

    International Nuclear Information System (INIS)

    Mohamad Afiq Mohamed Huri; Umi Kalthom Ahmad

    2014-01-01

    Increased terrorist activities around the Asian region have resulted in the need for improved analytical techniques in forensic analysis. High explosive residues from post-blast clothing are often encountered as physical evidence submitted to a forensic laboratory. Therefore, this study was initiated to detect high explosives residues of cyclotrimethylenetrinitramine (RDX) and pentaerythritol tetranitrate (PETN) on selected cloth in this study. Cotton swabbing technique was employed as a simple and rapid method in recovering analytes from the sample matrix. Analytes were analyzed using Griess spot test, TLC and HPLC. TLC separation employed toluene-ethyl acetate (9:1) as a good solvent system. Reversed phase HPLC separation employed acetonitrile-water (65:35) as the mobile phase and analytes detected using a programmed wavelength. RDX was detected at 235 nm for the first 3.5 min and then switched to 215 nm for PETN. Limits of detection (LODs) of analytes were in the low ppm range (0.05 ppm for RDX and 0.25 ppm for PETN). Analyte recovery studies revealed that the type of cloth has a profound effect on the extraction efficiency. Analytes were recovered better for nylon as compared to cotton cloth. However, no analytes could be recovered from denim cloth. For post-blast samples, only RDX was detected in low concentration for both nylon and cotton cloth. (author)

  3. High-pressure Raman investigations of phase transformations in pentaerythritol (C(CH sub 2 OH) sub 4)

    CERN Document Server

    Bhattacharya, T

    2002-01-01

    Our high-pressure Raman scattering experiments on pentaerythritol (C(CH sub 2 OH) sub 4) show that this compound undergoes at least three phase transformations up to 25 GPa. Splitting of various modes at approx 6.3, approx 8.2 and 10 GPa suggests that these phase transformations result in lowering of crystalline symmetry. A very small discontinuous change in slope of most of the Raman-active modes is observed at 0.3 GPa. However, no other signature of a phase transition was observed at this pressure. The observed correlation of the pressures for the onset of the two phase transformations with the limiting values of the distances between various non-bonded atoms in the parent phase suggests that the molecular rearrangements across the phase transformations are not very drastic. In addition, our earlier Fourier transform infrared and present Raman investigations indicate that high-pressure compression leads to increase in strength of the hydrogen bond present in this compound.

  4. Organic Nitrates and Nitrate Resistance in Diabetes: The Role of Vascular Dysfunction and Oxidative Stress with Emphasis on Antioxidant Properties of Pentaerithrityl Tetranitrate

    Directory of Open Access Journals (Sweden)

    Matthias Oelze

    2010-01-01

    Full Text Available Organic nitrates represent a class of drugs which are clinically used for treatment of ischemic symptoms of angina as well as for congestive heart failure based on the idea to overcome the impaired NO bioavailability by “NO” replacement therapy. The present paper is focused on parallels between diabetes mellitus and nitrate tolerance, and aims to discuss the mechanisms underlying nitrate resistance in the setting of diabetes. Since oxidative stress was identified as an important factor in the development of tolerance to organic nitrates, but also represents a hallmark of diabetic complications, this may represent a common principle for both disorders where therapeutic intervention should start. This paper examines the evidence supporting the hypothesis that pentaerithrityl tetranitrate may represent a nitrate for treatment of ischemia in diabetic patients. This evidence is based on the considerations of parallels between diabetes mellitus and nitrate tolerance as well as on preliminary data from experimental diabetes studies.

  5. Organic Nitrates and Nitrate Resistance in Diabetes: The Role of Vascular Dysfunction and Oxidative Stress with Emphasis on Antioxidant Properties of Pentaerithrityl Tetranitrate

    Science.gov (United States)

    Oelze, Matthias; Schuhmacher, Swenja; Daiber, Andreas

    2010-01-01

    Organic nitrates represent a class of drugs which are clinically used for treatment of ischemic symptoms of angina as well as for congestive heart failure based on the idea to overcome the impaired NO bioavailability by “NO” replacement therapy. The present paper is focused on parallels between diabetes mellitus and nitrate tolerance, and aims to discuss the mechanisms underlying nitrate resistance in the setting of diabetes. Since oxidative stress was identified as an important factor in the development of tolerance to organic nitrates, but also represents a hallmark of diabetic complications, this may represent a common principle for both disorders where therapeutic intervention should start. This paper examines the evidence supporting the hypothesis that pentaerithrityl tetranitrate may represent a nitrate for treatment of ischemia in diabetic patients. This evidence is based on the considerations of parallels between diabetes mellitus and nitrate tolerance as well as on preliminary data from experimental diabetes studies. PMID:21234399

  6. Sintesis de poliuretanos a partir de polioles obtenidos a partir del aceite de higuerilla modificado por transesterificación con pentaeritritol Polyurethanes sintetized of polyols obtained from castor oil modified by transesterification with pentaerythritol

    Directory of Open Access Journals (Sweden)

    Manuel F. Valero

    2008-01-01

    Full Text Available Castor oil was reacted by transesterification with various percentages in mass of pentaerythritol to obtain different esters of pentaerythritol. Alternatively, glycerol was also used instead of pentaerythritol for the same reaction in order to establish comparative reference products. The products of the reactions were characterized by matrix-assisted laser desorption/ionization time-of-flight mass spectroscopy in order to detect and quantify (in terms of the molecular mass and structural information the components of the products obtained. Analysis for hydroxyl value, acid value, viscosity and specific gravity were used to complete the characterization of the polyols obtained and also of the original castor oil. The polymer characterization was accomplished by tensile stress-strain tests, Shore A hardness, thermogravimetric analysis and chemical resistance to solvents.

  7. Characteristics of a New Plastic Explosive Named EPX-1

    Directory of Open Access Journals (Sweden)

    Ahmed Elbeih

    2015-01-01

    Full Text Available EPX-1 is a new plastic explosive (in the research stage which has been prepared for military and civilian applications. EPX-1 explosive contains pentaerythritol tetranitrate (PETN with different particle size as explosive filler bonded by nonenergetic thermoplastic binder plasticized by dibutyl phthalate (DBP. In this paper, the production method of EPX-1 was described. The crystal morphology was studied by scanning electron microscope (SEM. Heat of combustion was determined experimentally. The compatibility of PETN with the polymeric matrix was studied by vacuum stability test. Sensitivities to impact and friction were measured. The detonation velocity was measured experimentally and the detonation characteristics were calculated by EXPLO5 thermodynamic code. For comparison, Semtex 1A, Semtex 10, Formex P1, and Sprängdeg m/46 were studied. It was concluded that PEX-1 has compatible ingredients, it has the highest detonation velocity of all the studied plastic explosives, and its sensitivity is in the same level of the studied plastic explosives except Semtex 1A.

  8. Studies of the laser-induced fluorescence of explosives and explosive compositions.

    Energy Technology Data Exchange (ETDEWEB)

    Hargis, Philip Joseph, Jr. (,; .); Thorne, Lawrence R.; Phifer, Carol Celeste; Parmeter, John Ethan; Schmitt, Randal L.

    2006-10-01

    Continuing use of explosives by terrorists throughout the world has led to great interest in explosives detection technology, especially in technologies that have potential for standoff detection. This LDRD was undertaken in order to investigate the possible detection of explosive particulates at safe standoff distances in an attempt to identify vehicles that might contain large vehicle bombs (LVBs). The explosives investigated have included the common homogeneous or molecular explosives, 2,4,6-trinitrotoluene (TNT), pentaerythritol tetranitrate (PETN), cyclonite or hexogen (RDX), octogen (HMX), and the heterogeneous explosive, ammonium nitrate/fuel oil (ANFO), and its components. We have investigated standard excited/dispersed fluorescence, laser-excited prompt and delayed dispersed fluorescence using excitation wavelengths of 266 and 355 nm, the effects of polarization of the laser excitation light, and fluorescence imaging microscopy using 365- and 470-nm excitation. The four nitro-based, homogeneous explosives (TNT, PETN, RDX, and HMX) exhibit virtually no native fluorescence, but do exhibit quenching effects of varying magnitude when adsorbed on fluorescing surfaces. Ammonium nitrate and fuel oil mixtures fluoresce primarily due to the fuel oil, and, in some cases, due to the presence of hydrophobic coatings on ammonium nitrate prill or impurities in the ammonium nitrate itself. Pure ammonium nitrate shows no detectable fluorescence. These results are of scientific interest, but they provide little hope for the use of UV-excited fluorescence as a technique to perform safe standoff detection of adsorbed explosive particulates under real-world conditions with a useful degree of reliability.

  9. Characterization of nitrated sugar alcohols by atmospheric-pressure chemical-ionization mass spectrometry.

    Science.gov (United States)

    Ostrinskaya, Alla; Kelley, Jude A; Kunz, Roderick R

    2017-02-28

    The nitrated sugar alcohols mannitol hexanitrate (MHN), sorbitol hexanitrate (SHN) and xylitol pentanitrate (XPN) are in the same class of compounds as the powerful military-grade explosive pentaerythritol tetranitrate (PETN) and the homemade explosive erythritol tetranitrate (ETN) but, unlike for PETN and ETN, ways to detect MHN, SHN and XPN by mass spectrometry (MS) have not been fully investigated. Atmospheric-pressure chemical-ionization mass spectrometry (APCI-MS) was used to detect ions characteristic of nitrated sugar alcohols. APCI time-of-flight mass spectrometry (APCI-TOF MS) and collision-induced dissociation tandem mass spectrometry (CID MS/MS) were used for confirmation of each ion assignment. In addition, the use of the chemical ionization reagent dichloromethane was investigated to improve sensitivity and selectivity for detection of MHN, SHN and XPN. All the nitrated sugar alcohols studied followed similar fragmentation pathways in the APCI source. MHN, SHN and XPN were detectable as fragment ions formed by the loss of NO 2 , HNO 2 , NO 3 , and CH 2 NO 2 groups, and in the presence of dichloromethane chlorinated adduct ions were observed. It was determined that in MS/MS mode, chlorinated adducts of MHN and SHN had the lowest limits of detection (LODs), while for XPN the lowest LOD was for the [XPN-NO 2 ] - fragment ion. Partially nitrated analogs of each of the three compounds were also present in the starting materials, and ions attributable to these compounds versus those formed from in-source fragmentation of MHN, SHN, and XPN were distinguished and assigned using liquid chromatography APCI-MS and ESI-MS. The APCI-MS technique provides a selective and sensitive method for the detection of nitrated sugar alcohols. The methods disclosed here will benefit the area of explosives trace detection for counterterrorism and forensics. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  10. Thermal safety characterization on PETN, PBX-9407, LX-10-2, LX-17-1 and detonator in the LLNL's P-ODTX system

    Energy Technology Data Exchange (ETDEWEB)

    Hsu, P. C. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Strout, S. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Reynolds, J. G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Kahl, E. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Ellsworth, F. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Healy, T. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2017-09-21

    Incidents caused by fire and other thermal events can heat energetic materials that may lead to thermal explosion and result in structural damage and casualty. Thus, it is important to understand the response of energetic materials to thermal insults. The One-Dimensional-Time to Explosion (ODTX) system at the Lawrence Livermore National Laboratory (LLNL) has been used for decades to characterize thermal safety of energetic materials. In this study, an integration of a pressure monitoring element has been added into the ODTX system (P-ODTX) to perform thermal explosion (cook-off) experiments (thermal runaway) on PETN powder, PBX-9407, LX-10-2, LX-17-1, and detonator samples (cup tests). The P-ODTX testing generates useful data (thermal explosion temperature, thermal explosion time, and gas pressures) to assist with the thermal safety assessment of relevant energetic materials and components. This report summarizes the results of P-ODTX experiments that were performed from May 2015 to July 2017. Recent upgrades to the data acquisition system allows for rapid pressure monitoring in microsecond intervals during thermal explosion. These pressure data are also included in the report.

  11. Separation of alpha-, beta-, gamma-, delta-tocopherols and alpha-tocopherol acetate on a pentaerythritol diacrylate monostearate-ethylene dimethacrylate monolith by capillary electrochromatography.

    Science.gov (United States)

    Chaisuwan, Patcharin; Nacapricha, Duangjai; Wilairat, Prapin; Jiang, Zhengjin; Smith, Norman W

    2008-06-01

    This work reports the first use of a monolith with method development for the separation of tocopherol (TOH) compounds by CEC with UV detection. A pentaerythritol diacrylate monostearate-ethylene dimethacrylate (PEDAS-EDMA) monolithic column has been investigated for an optimised condition to separate alpha-, beta-, gamma- and delta-TOHs, and alpha-tocopherol acetate (TAc). The PEDAS-EDMA monolith showed a remarkably good selectivity for separation of the TOH isomers including the beta- and gamma-isomers which are not easily separated by standard C8 or C18 particle-packed columns. Retention studies indicated that an RP mechanism was involved in the separation on the PEDAS-EDMA column, but polar interactions with the underlying ester and hydroxyl groups enhanced the separation of the problematic beta- and gamma-isomers. Separation of all the compounds was achieved within 25 min using 3:10:87 v/v/v 100 mM Tris buffer (pH 9.3)/methanol/ACN as the mobile phase. The method was successfully applied to a pharmaceutical sample with recoveries from 93 to 99%. Intraday and interday precisions (%RSD) for peak area and retention time were less than 2.3. LODs for all four TOHs and TAc were below 1 ppm.

  12. The oxygen-rich pentaerythritol modified multi-walled carbon nanotube as an efficient adsorbent for aqueous removal of alizarin yellow R and alizarin red S

    Science.gov (United States)

    Yang, Jia-Ying; Jiang, Xin-Yu; Jiao, Fei-Peng; Yu, Jin-Gang

    2018-04-01

    A contrastive work on the removal of two organic dyes, alizarin yellow R (AYR) and alizarin red S (ARS), was carried out by utilizing pentaerythritol modified multi-walled carbon nanotubes (ox-MWCNT-PER) as a highly efficient adsorbent. Various characterization methods such as scanning electron microscopy (SEM), thermogravimetric analysis (TGA), Fourier transform infrared (FTIR) spectroscopy, the Brunauer-Emmett-Teller (BET) analysis and X-ray photoelectron spectroscopy (XPS), were applied for revealing the physical and chemical properties of the as-prepared material. In addition, the adsorption kinetics, isotherms and thermodynamic parameters were also discussed. The results showed that the time required to achieve the adsorption equilibrium for both dyes was about 30 min, and the increase in temperature was not favorable to the adsorption process. It was worth noting that the adsorption capacity of ox-MWCNT-PER towards ARS dye was more significant than that towards AYR dye. And the maximum adsorption capacities for ARS and AYR were 257.73 mg g-1 and 45.39 mg g-1, respectively. The possible adsorption mechanism was also proposed, and the synergistic effects of the hydrogen bonding and the π-π electron stacking interactions between the adsorbents and adsorbates both contributed to the adsorption. It could be proposed that the ox-MWCNT-PER nanocomposite might have some positive effects in removing organic dyes from water treatment in the future.

  13. Coefficients of sliding friction of single crystals of high explosives under different rubbing conditions

    International Nuclear Information System (INIS)

    Wu, Y Q; Chaudhri, M Munawar

    2013-01-01

    The coefficients of sliding friction of single crystals of commonly used high explosives pentaerythritol tetranitrate (PETN), cyclotrimethylene trinitramine (RDX) and beta-cyclotetramethylene tetranitramine (β-HMX) under several rubbing configurations and at a relative sliding speed of 0.22 mm s -1 were measured. The sliding configurations were (1) crystal-polished steel pairs, (2) like-crystal pairs and (3) unlike-crystal pairs. For every rubbing configuration the friction force showed oscillations, which are thought to be caused by the formation and shearing of the adhesive junctions formed at the surface of the rubbing crystals. This shearing of the adhesive junctions led to the formation of microscopic and sub-microscopic particles, which were confirmed by an environmental scanning electron microscope study. For every rubbing configuration and for relatively high normal loads pressing the rubbing crystals together, the coefficient of friction was generally in the range 0.2-0.25 and it has been concluded that the coefficient of friction is controlled by the adhesion with almost negligible contribution from the ploughing component. From a knowledge of the coefficient of friction and the uniaxial yield stress values of single crystals of RDX and β-HMX, the shear strength of these crystals were determined to be ∼13.4 MPa and ∼16.8 MPa, respectively.

  14. Direct analysis in real time mass spectrometry of potential by-products from homemade nitrate ester explosive synthesis.

    Science.gov (United States)

    Sisco, Edward; Forbes, Thomas P

    2016-04-01

    This work demonstrates the coupling of direct analysis in real time (DART) ionization with time-of-flight mass spectrometry (MS) in an off-axis configuration for the trace detection and analysis of potential partially nitrated and dimerized by-products of homemade nitrate ester explosive synthesis. Five compounds relating to the synthesis of nitroglycerin (NG) and pentaerythritol tetranitrate (PETN) were examined. Deprotonated ions and adducts with molecular oxygen, nitrite, and nitrate were observed in the mass spectral responses of these compounds. A global optimum temperature of 350 °C for the by-products investigated here enabled single nanogram to sub nanogram trace detection. Matrix effects were examined through a series of mixtures containing one or more compounds (sugar alcohol precursors, by-products, and/or explosives) across a range of mass loadings. The explosives MS responses experienced competitive ionization in the presence of all by-products. The magnitude of this influence corresponded to both the degree of by-product nitration and the relative mass loading of the by-product to the explosive. This work provides a characterization of potential by-products from homemade nitrate ester synthesis, including matrix effects and potential challenges that might arise from the trace detection of homemade explosives (HMEs) containing impurities. Detection and understanding of HME impurities and complex mixtures may provide valuable information for the screening and sourcing of homemade nitrate ester explosives. Published by Elsevier B.V.

  15. Synthesis of a new energetic nitrate ester

    Energy Technology Data Exchange (ETDEWEB)

    Chavez, David E [Los Alamos National Laboratory

    2008-01-01

    Nitrate esters have been known as useful energetic materials since the discovery of nitroglycerin by Ascanio Sobrero in 1846. The development of methods to increase the safety and utility of nitroglycerin by Alfred Nobel led to the revolutionary improvement in the utility of nitroglycerin in explosive applications in the form of dynamite. Since then, many nitrate esters have been prepared and incorporated into military applications such as double-based propellants, detonators and as energetic plasticizers. Nitrate esters have also been shown to have vasodilatory effects in humans and thus have been studied and used for treatments of ailments such as angina. The mechanism of the biological response towards nitrate esters has been elucidated recently. Interestingly, many of the nitrate esters used for military purposes are liquids (ethylene glycol dinitrate, propylene glycol dinitrate, etc). Pentaerythritol tetranitrate (PETN) is one of the only solid nitrate esters, besides nitrocellulose, that is used in any application. Unfortunately, PETN melting point is above 100 {sup o}C, and thus must be pressed as a solid for detonator applications. A more practical material would be a melt-castable explosive, for potential simplification of manufacturing processes. Herein we describe the synthesis of a new energetic nitrate ester (1) that is a solid at ambient temperatures, has a melting point of 85-86 {sup o}C and has the highest density of any known nitrate ester composed only of carbon, hydrogen, nitrogen and oxygen. We also describe the chemical, thermal and sensitivity properties of 1 as well as some preliminary explosive performance data.

  16. Forensic analysis of high explosives residues in post-blast water samples employing solid phase extraction for analyte pro-concentration

    International Nuclear Information System (INIS)

    Umi Kalsom Ahmad; Rajendran, Sumathy; Ling, Lee Woan

    2008-01-01

    Nitro aromatic, nitramine and nitrate ester compounds are a major group of high order explosive or better known as military explosives. Octahydro-1,3,5,7-tetrazocine (HMX), 1,3,5-hexahydro-1,3,5-trinitro triazine (RDX), 2,4,6-trinitro-toluene (TNT), pentaerythritol tetranitrate (PETN) and 2,4-dinitrotoluene (2,4-DNT) are secondary high explosives classified as most commonly used explosives components. There is an increasing demand for pre-concentration of these compounds in water samples as the sensitivity achieved by instrumental analytical methods for these high explosives residues are the main drawback in the application at trace levels for forensic analysis. Hence, a simple cartridge solid phase extraction (SPE) procedure was optimized as the off-line extraction and pre-concentration method to enhance the detection limit of high explosive residues using micellar electrokinetic chromatography (MEKC) and gas chromatography with electron-capture detection (GC-ECD) methods. The SPE cartridges utilized LiChrolut EN as the SPE adsorbent. By emplying pre-concentration using SPE, the detection limits of the target analytes in water sample were lowered by more than 1000 times with good percentage recovery (>87%) for MEKC method and lowered by 120 times with more than 2 % percentage recovery for GC-ECD methods. In order to test the feasibility of the developed method to real cases, post-blast water samples were analyzed. The post-blast water samples which were collected from Baling Bom training range, Ulu Kinta, Perak contained RDX and PETN in the range of 0.05 - 0.17 ppm and 0.0124 - 0.0390 ppm respectively. (author)

  17. Large-Scale Reactive Atomistic Simulation of Shock-induced Initiation Processes in Energetic Materials

    Science.gov (United States)

    Thompson, Aidan

    2013-06-01

    Initiation in energetic materials is fundamentally dependent on the interaction between a host of complex chemical and mechanical processes, occurring on scales ranging from intramolecular vibrations through molecular crystal plasticity up to hydrodynamic phenomena at the mesoscale. A variety of methods (e.g. quantum electronic structure methods (QM), non-reactive classical molecular dynamics (MD), mesoscopic continuum mechanics) exist to study processes occurring on each of these scales in isolation, but cannot describe how these processes interact with each other. In contrast, the ReaxFF reactive force field, implemented in the LAMMPS parallel MD code, allows us to routinely perform multimillion-atom reactive MD simulations of shock-induced initiation in a variety of energetic materials. This is done either by explicitly driving a shock-wave through the structure (NEMD) or by imposing thermodynamic constraints on the collective dynamics of the simulation cell e.g. using the Multiscale Shock Technique (MSST). These MD simulations allow us to directly observe how energy is transferred from the shockwave into other processes, including intramolecular vibrational modes, plastic deformation of the crystal, and hydrodynamic jetting at interfaces. These processes in turn cause thermal excitation of chemical bonds leading to initial chemical reactions, and ultimately to exothermic formation of product species. Results will be presented on the application of this approach to several important energetic materials, including pentaerythritol tetranitrate (PETN) and ammonium nitrate/fuel oil (ANFO). In both cases, we validate the ReaxFF parameterizations against QM and experimental data. For PETN, we observe initiation occurring via different chemical pathways, depending on the shock direction. For PETN containing spherical voids, we observe enhanced sensitivity due to jetting, void collapse, and hotspot formation, with sensitivity increasing with void size. For ANFO, we

  18. Preparation of a poly(3'-azido-3'-deoxythymidine-co-propargyl methacrylate-co-pentaerythritol triacrylate) monolithic column by in situ polymerization and a click reaction for capillary liquid chromatography of small molecules and proteins.

    Science.gov (United States)

    Lin, Zian; Yu, Ruifang; Hu, Wenli; Zheng, Jiangnan; Tong, Ping; Zhao, Hongzhi; Cai, Zongwei

    2015-07-07

    Combining free radical polymerization with click chemistry via a copper-mediated azide/alkyne cycloaddition (CuAAC) reaction in a "one-pot" process, a facile approach was developed for the preparation of a poly(3'-azido-3'-deoxythymidine-co-propargyl methacrylate-co-pentaerythritol triacrylate) (AZT-co-PMA-co-PETA) monolithic column. The resulting poly(AZT-co-PMA-co-PETA) monolith showed a relatively homogeneous monolithic structure, good permeability and mechanical stability. Different ratios of monomers and porogens were used for optimizing the properties of a monolithic column. A series of alkylbenzenes, amides, anilines, and benzoic acids were used to evaluate the chromatographic properties of the polymer monolith in terms of hydrophobic, hydrophilic and cation-exchange interactions, and the results showed that the poly(AZT-co-PMA-co-PETA) monolith exhibited more flexible adjustment in chromatographic selectivity than that of the parent poly(PMA-co-PETA) and AZT-modified poly(PMA-co-PETA) monoliths. Column efficiencies for toluene, DMF, and formamide with 35,000-48,000 theoretical plates per m could be obtained at a linear velocity of 0.17 mm s(-1). The run-to-run, column-to-column, and batch-to-batch repeatabilities of the retention factors were less than 4.2%. In addition, the proposed monolith was also applied to efficient separation of sulfonamides, nucleobases and nucleosides, anesthetics and proteins for demonstrating its potential.

  19. Sensitive detection of plastic explosives with self-assembled monolayer-coated microcantilevers

    Science.gov (United States)

    Pinnaduwage, L. A.; Boiadjiev, V.; Hawk, J. E.; Thundat, T.

    2003-08-01

    We report the detection of 10-30 parts-per-trillion levels of pentaerythritol tetranitrate and hexahydro-1,3,5-triazine within 20 s of exposure to a silicon microcantilever with its gold surface modified with a self-assembled monolayer of 4-mercaptobenzoic acid. These measurements correspond to a limit of detection of a few fg.

  20. Some analytical methods for explosives: Part 2

    Energy Technology Data Exchange (ETDEWEB)

    Selig, W.

    1965-12-08

    This report is the second compilation of methods for analyzing explosives. All the methods were developed for routine performance by techniques, and an attempt has therefore been made to keep them as simple as possible. Methods are presented for analyzing plastic-bonded explosives based on sym-cyclomethylenetetra-nitramine (HMX), based on viton in addition to HMX, and based on pentraerythritol tetranitrate (PETN).

  1. Destruction of energetic materials by supercritical water oxidation

    International Nuclear Information System (INIS)

    Beulow, S.J.; Dyer, R.B.; Harradine, D.M.; Robinson, J.M.; Oldenborg, R.C.; Funk, K.A.; McInroy, R.E.; Sanchez, J.A.; Spontarelli, T.

    1993-01-01

    Supercritical water oxidation is a relatively low-temperature process that can give high destruction efficiencies for a variety of hazardous chemical wastes. Results are presented examining the destruction of high explosives and propellants in supercritical water and the use of low temperature, low pressure hydrolysis as a pretreatment process. Reactions of cyclotrimethylene trinitramine (RDX), cyclotetramethylene tetranitramine (HMX), nitroguanidine (NQ), pentaerythritol tetranitrate (PETN), and 2,4,6-trinitrotoluene (TNT) are examined in a flow reactor operated at temperatures between 400 degrees C and 650 degrees C. Explosives are introduced into the reactor at concentrations below the solubility limits. For each of the compounds, over 99.9% is destroyed in less than 30 seconds at temperatures above 600 degrees C. The reactions produce primarily N 2 , N 2 O,CO 2 , and some nitrate and nitrite ions. The distribution of reaction products depends on reactor pressure, temperature, and oxidizer concentration. Kinetics studies of the reactions of nitrate and nitrite ions with various reducing reagents in supercritical water show that they can be rapidly and completely destroyed at temperatures above 525 degrees C. The use of slurries and hydrolysis to introduce high concentrations of explosives into a supercritical water reactor is examined. For some compounds the rate of reaction depends on particle size. The hydrolysis of explosives at low temperatures (<100 degrees C) and low pressures (<1 atm) under basic conditions produces water soluble, non-explosive products which are easily destroyed by supercritical water oxidation. Large pieces of explosives (13 cm diameter) have been successfully hydrolyzed. The rate, extent, and products of the hydrolysis depend on the type and concentration of base. Results from the base hydrolysis of triple base propellant M31A1E1 and the subsequent supercritical water oxidation of the hydrolysis products are presented

  2. 21 CFR 178.3690 - Pentaerythritol adipate-stearate.

    Science.gov (United States)

    2010-04-01

    ... fabrication of rigid and semi-rigid polyvinyl chloride and/or vinyl chloride-propylene copolymers complying... Conshohocken, Philadelphia, PA 19428-2959, or may be examined at the National Archives and Records... Conshohocken, Philadelphia, PA 19428-2959, or available for inspection at the National Archives and Records...

  3. Synthesis and Characterization of Mono-, Di-, and Tetranitrated 7,8-Disubstituted Glycolurils

    Science.gov (United States)

    2014-02-01

    Cheetah 7.0 [7] . All of the compounds 8–13 are predicted to have performance values less than TNT with 15 and 16 approaching the performance of TNT...0.25 1.25 0.25 a) Calculated values in brackets. b) Calculated using Cheetah 7.0. c) Peak decomposition temperature at 10 Kmin1 in a pinhole pan. d) Ex...118, 445–458. [7] S. Bastea, L. E. Fried, K. R. Glaesemann, W. M. Howard, I. W. Kuo, P. C. Souers, P. A. Vitello, Cheetah 7.0 User’s Manual, LLNL-SM

  4. A sensitive, handheld vapor sensor based on microcantilevers

    Science.gov (United States)

    Pinnaduwage, L. A.; Hedden, D. L.; Gehl, A.; Boiadjiev, V. I.; Hawk, J. E.; Farahi, R. H.; Thundat, T.; Houser, E. J.; Stepnowski, S.; McGill, R. A.; Deel, L.; Lareau, R. T.

    2004-11-01

    We report the development of a handheld sensor based on piezoresistive microcantilevers that does not depend on optical detection, yet has high detection sensitivity. The sensor is able to detect vapors from the plastic explosives pentaerythritol tetranitrate and hexahydro-1,3,5-triazine at levels below 10 parts per trillion within few seconds of exposure under ambient conditions. A differential measurement technique has yielded a rugged sensor that is unaffected by vibration and is able to function as a "sniffer." The microelectromechanical system sensor design allows for the incorporation of hundreds of microcantilevers with suitable coatings in order to achieve sufficient selectivity in the future, and thus could provide an inexpensive, unique platform for the detection of chemical, biological, and explosive materials.

  5. Water temperature and concentration measurements within the expanding blast wave of a high explosive

    International Nuclear Information System (INIS)

    Carney, J R; Lightstone, J M; Piecuch, S; Koch, J D

    2011-01-01

    We present an application of absorption spectroscopy to directly measure temperature and concentration histories of water vapor within the expansion of a high explosive detonation. While the approach of absorption spectroscopy is well established, the combination of a fast, near-infrared array, broadband light source, and rigid gauge allow the first application of time-resolved absorption measurements in an explosive environment. The instrument is demonstrated using pentaerythritol tetranitrate with a sampling rate of 20 kHz for 20 ms following detonation. Absorption by water vapor is measured between 1335 and 1380 nm. Water temperatures are determined by fitting experimental transmission spectra to a simulated database. Water mole fractions are deduced following the temperature assignment. The sources of uncertainty and their impact on the results are discussed. These measurements will aid the development of chemical-specific reaction models and the predictive capability in technical fields including combustion and detonation science

  6. A technique for measuring the quality of an elliptically bent pentaerythritol [PET(002)] crystal

    Energy Technology Data Exchange (ETDEWEB)

    Haugh, M. J., E-mail: haughmj@nv.doe.gov; Jacoby, K. D. [National Security Technologies, LLC, Livermore, California 94550 (United States); Barrios, M. A.; Thorn, D.; Emig, J. A.; Schneider, M. B. [Lawrence Livermore National Laboratory, 7000 East Avenue, Livermore, California 94550 (United States)

    2016-11-15

    We present a technique for determining the X-ray spectral quality from each region of an elliptically curved PET(002) crystal. The investigative technique utilizes the shape of the crystal rocking curve which changes significantly as the radius of curvature changes. This unique quality information enables the spectroscopist to verify where in the spectral range that the spectrometer performance is satisfactory and where there are regions that would show spectral distortion. A collection of rocking curve measurements for elliptically curved PET(002) has been built up in our X-ray laboratory. The multi-lamellar model from the XOP software has been used as a guide and corrections were applied to the model based upon measurements. But, the measurement of R{sub I} at small radius of curvature shows an anomalous behavior; the multi-lamellar model fails to show this behavior. The effect of this anomalous R{sub I} behavior on an X-ray spectrometer calibration is calculated. It is compared to the multi-lamellar model calculation which is completely inadequate for predicting R{sub I} for this range of curvature and spectral energies.

  7. Aspects of the behavior of some pentaerythritol ester base synlubes for turbo-engines

    Directory of Open Access Journals (Sweden)

    I.A. El-Magly

    2013-06-01

    Some physico-chemical behaviors and correlations have been deduced to characterize the prepared esters. Moreover, they shed the light on their suitability as base oils which may be used in formulations according to French Air specification 3514 (Nato 0–150 as compared with the commercial oil sample (Trubonycoil 13B used in this respect.

  8. Optimization of esterification of oleic acid and trimethylolpropane (TMP) and pentaerythritol (PE)

    Energy Technology Data Exchange (ETDEWEB)

    Mahmud, Hamizah Ammarah; Salimon, Jumat [School of Chemical Sciences and Food Technology, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor Darul Ehsan (Malaysia)

    2014-09-03

    Vegetable oil (VO) is the most potential alternative to replace mineral oil for lubricant due to better lubricating properties and great physicochemical properties. Chemical modification has to be done to overcome low temperature performance and low oxidation instability due to the presence of β-hydrogen atoms of glycerol molecule. The optimization of esterification of oleic acid and polyhydric alcohol with sulfuric acid catalyst was carried out to find the optimum conditions with the highest yield. Reeaction variables such as; molar ratio, temperature, duration and catalyst concentration. Two types of polyhydric alcohol have been used; TMP and PE. The optimum results showed oleic acid successfully converted 91.2% ester TMP and 92.7% ester PE at duration: 5 hours (Ester TMP), 6 hours (Ester PE); temperature: 150°C (ester TMP), 180°C (Ester PE); catalyst concentration: 1.5% (w/w); and mol ratio: 3.9:1 (ester TMP), 4.9:1 (ester PE). From the data obtained, mole ratio showed most influenced factors to the increasing yields of ester conversions.. The TMP/PE ester was confirmed using gas chromatography (GC-FID), Fourier Transform Infrared Spectroscopy (FTIR) and Nuclear Magnetic Resonance (NMR)

  9. A technique for measuring the quality of an elliptically bent pentaerythritol [PET(002)] crystal

    International Nuclear Information System (INIS)

    Haugh, M. J.; Jacoby, K. D.; Barrios, M. A.; Thorn, D.; Emig, J. A.; Schneider, M. B.

    2016-01-01

    We present a technique for determining the X-ray spectral quality from each region of an elliptically curved PET(002) crystal. The investigative technique utilizes the shape of the crystal rocking curve which changes significantly as the radius of curvature changes. This unique quality information enables the spectroscopist to verify where in the spectral range that the spectrometer performance is satisfactory and where there are regions that would show spectral distortion. A collection of rocking curve measurements for elliptically curved PET(002) has been built up in our X-ray laboratory. The multi-lamellar model from the XOP software has been used as a guide and corrections were applied to the model based upon measurements. But, the measurement of R I at small radius of curvature shows an anomalous behavior; the multi-lamellar model fails to show this behavior. The effect of this anomalous R I behavior on an X-ray spectrometer calibration is calculated. It is compared to the multi-lamellar model calculation which is completely inadequate for predicting R I for this range of curvature and spectral energies.

  10. Complexes of thorium tetranitrate with N-methylpiperazine, 2-methylpiperazine, N-phenylpiperazine and N,N'-dimethylpiperazine

    Energy Technology Data Exchange (ETDEWEB)

    Manhas, B S; Trikha, A K [Punjabi Univ., Patiala (India). Dept. of Chemistry; Singh, M [Guru Nanak Univ., Amritsar (India). Dept. of Chemistry

    1981-01-01

    Complexes of Th(NO/sub 3/)/sub 4/ with the title ligands have been synthesised and characterised on the basis of elemental analyses and IR spectral studies which indicate that the ligands in the complexes are in chair conformation and the nitrate group is bidentate. Coordination number is higher than ten in all the complexes.

  11. Spectral Characterization of RDX, ETN, PETN, TATP, HMTD, HMX, and C-4 in the Mid-Infrared Region

    Science.gov (United States)

    2014-04-01

    Germany, 1996. 12. Bertie, J.E. and Keefe , C.D. “Infrared intensities of liquids XXIV: Optical constants of liquid benzene-h6 at 25°C extended to...Bertie, J.E.; Apelblat, Y.; Keefe , C.D. “Infrared intensities of liquids XXV: Optical constants of liquid toluene at 25°C between 4800 and 400 cm−1

  12. Different-ligand boron complexes with gluconate-ions and pentaerythritol and gluconatoborates with B-O-B bridge bond

    International Nuclear Information System (INIS)

    Tel'zhenskaya, P.N.; Shvarts, E.M.; Vitola, I.M.

    1990-01-01

    Borogluconates differing in structure of the complex dimeric borogluconate ion from the described earlier have been synthesized. The results of physicochemical measurements (chemical and thermal analysis, IR-spectroscopy, titration according to Fisher, conductometry) allowed to propose formulas for the studied compounds

  13. 40 CFR 721.9400 - Reaction product of phenolic pentaerythritol tetraesters with fatty acid esters and oils, and...

    Science.gov (United States)

    2010-07-01

    ... information on methods for protectintg against such risk, into an MSDS as described in § 721.72(c) within 90... Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) TOXIC SUBSTANCES CONTROL ACT... substance is any manner or method of manufacture, import, or processing associated with any use of this...

  14. Organic Nitrate Therapy, Nitrate Tolerance, and Nitrate-Induced Endothelial Dysfunction: Emphasis on Redox Biology and Oxidative Stress

    Science.gov (United States)

    2015-01-01

    Abstract Organic nitrates, such as nitroglycerin (GTN), isosorbide-5-mononitrate and isosorbide dinitrate, and pentaerithrityl tetranitrate (PETN), when given acutely, have potent vasodilator effects improving symptoms in patients with acute and chronic congestive heart failure, stable coronary artery disease, acute coronary syndromes, or arterial hypertension. The mechanisms underlying vasodilation include the release of •NO or a related compound in response to intracellular bioactivation (for GTN, the mitochondrial aldehyde dehydrogenase [ALDH-2]) and activation of the enzyme, soluble guanylyl cyclase. Increasing cyclic guanosine-3′,-5′-monophosphate (cGMP) levels lead to an activation of the cGMP-dependent kinase I, thereby causing the relaxation of the vascular smooth muscle by decreasing intracellular calcium concentrations. The hemodynamic and anti-ischemic effects of organic nitrates are rapidly lost upon long-term (low-dose) administration due to the rapid development of tolerance and endothelial dysfunction, which is in most cases linked to increased intracellular oxidative stress. Enzymatic sources of reactive oxygen species under nitrate therapy include mitochondria, NADPH oxidases, and an uncoupled •NO synthase. Acute high-dose challenges with organic nitrates cause a similar loss of potency (tachyphylaxis), but with distinct pathomechanism. The differences among organic nitrates are highlighted regarding their potency to induce oxidative stress and subsequent tolerance and endothelial dysfunction. We also address pleiotropic effects of organic nitrates, for example, their capacity to stimulate antioxidant pathways like those demonstrated for PETN, all of which may prevent adverse effects in response to long-term therapy. Based on these considerations, we will discuss and present some preclinical data on how the nitrate of the future should be designed. Antioxid. Redox Signal. 23, 899–942. PMID:26261901

  15. Organic Nitrate Therapy, Nitrate Tolerance, and Nitrate-Induced Endothelial Dysfunction: Emphasis on Redox Biology and Oxidative Stress.

    Science.gov (United States)

    Daiber, Andreas; Münzel, Thomas

    2015-10-10

    Organic nitrates, such as nitroglycerin (GTN), isosorbide-5-mononitrate and isosorbide dinitrate, and pentaerithrityl tetranitrate (PETN), when given acutely, have potent vasodilator effects improving symptoms in patients with acute and chronic congestive heart failure, stable coronary artery disease, acute coronary syndromes, or arterial hypertension. The mechanisms underlying vasodilation include the release of •NO or a related compound in response to intracellular bioactivation (for GTN, the mitochondrial aldehyde dehydrogenase [ALDH-2]) and activation of the enzyme, soluble guanylyl cyclase. Increasing cyclic guanosine-3',-5'-monophosphate (cGMP) levels lead to an activation of the cGMP-dependent kinase I, thereby causing the relaxation of the vascular smooth muscle by decreasing intracellular calcium concentrations. The hemodynamic and anti-ischemic effects of organic nitrates are rapidly lost upon long-term (low-dose) administration due to the rapid development of tolerance and endothelial dysfunction, which is in most cases linked to increased intracellular oxidative stress. Enzymatic sources of reactive oxygen species under nitrate therapy include mitochondria, NADPH oxidases, and an uncoupled •NO synthase. Acute high-dose challenges with organic nitrates cause a similar loss of potency (tachyphylaxis), but with distinct pathomechanism. The differences among organic nitrates are highlighted regarding their potency to induce oxidative stress and subsequent tolerance and endothelial dysfunction. We also address pleiotropic effects of organic nitrates, for example, their capacity to stimulate antioxidant pathways like those demonstrated for PETN, all of which may prevent adverse effects in response to long-term therapy. Based on these considerations, we will discuss and present some preclinical data on how the nitrate of the future should be designed.

  16. Toxicological and pharmacological concerns on oxidative stress and related diseases

    Energy Technology Data Exchange (ETDEWEB)

    Saeidnia, Soodabeh [Medicinal Plants Research Center, Faculty of Pharmacy, Tehran University of Medical Sciences, Tehran 1417614411 (Iran, Islamic Republic of); College of Pharmacy and Nutrition, University of Saskatchewan, Saskatoon (Canada); Abdollahi, Mohammad, E-mail: Mohammad@TUMS.Ac.Ir [Department of Toxicology and Pharmacology, Faculty of Pharmacy, Pharmaceutical Sciences Research Center, Tehran University of Medical Sciences, Tehran 1417614411 (Iran, Islamic Republic of)

    2013-12-15

    Although reactive oxygen species (ROS) such as superoxide, hydrogen peroxide and hydroxyl radical are generated as the natural byproduct of normal oxygen metabolism, they can create oxidative damage via interaction with bio-molecules. The role of oxidative stress as a remarkable upstream part is frequently reported in the signaling cascade of inflammation as well as chemo attractant production. Even though hydrogen peroxide can control cell signaling and stimulate cell proliferation at low levels, in higher concentrations it can initiate apoptosis and in very high levels may create necrosis. So far, the role of ROS in cellular damage and death is well documented with implicating in a broad range of degenerative alterations e.g. carcinogenesis, aging and other oxidative stress related diseases (OSRDs). Reversely, it is cleared that antioxidants are potentially able to suppress (at least in part) the immune system and to enhance the normal cellular protective responses to tissue damage. In this review, we aimed to provide insights on diverse OSRDs, which are correlated with the concept of oxidative stress as well as its cellular effects that can be inhibited by antioxidants. Resveratrol, angiotensin converting enzyme inhibitors, angiotensin receptor blockers, statins, nebivolol and carvedilol, pentaerythritol tetranitrate, mitochondria-targeted antioxidants, and plant-derived drugs (alone or combined) are the potential medicines that can be used to control OSRD.

  17. Biocatalysis with thermostable enzymes: structure and properties of a thermophilic 'ene'-reductase related to old yellow enzyme.

    Science.gov (United States)

    Adalbjörnsson, Björn V; Toogood, Helen S; Fryszkowska, Anna; Pudney, Christopher R; Jowitt, Thomas A; Leys, David; Scrutton, Nigel S

    2010-01-25

    We report the crystal structure of a thermophilic "ene" reductase (TOYE) isolated from Thermoanaerobacter pseudethanolicus E39. The crystal structure reveals a tetrameric enzyme and an active site that is relatively large compared to most other structurally determined and related Old Yellow Enzymes. The enzyme adopts higher order oligomeric states (octamers and dodecamers) in solution, as revealed by sedimentation velocity and multiangle laser light scattering. Bead modelling indicates that the solution structure is consistent with the basic tetrameric structure observed in crystallographic studies and electron microscopy. TOYE is stable at high temperatures (T(m)>70 degrees C) and shows increased resistance to denaturation in water-miscible organic solvents compared to the mesophilic Old Yellow Enzyme family member, pentaerythritol tetranitrate reductase. TOYE has typical ene-reductase properties of the Old Yellow Enzyme family. There is currently major interest in using Old Yellow Enzyme family members in the preparative biocatalysis of a number of activated alkenes. The increased stability of TOYE in organic solvents is advantageous for biotransformations in which water-miscible organic solvents and biphasic reaction conditions are required to both deliver novel substrates and minimize product racemisation.

  18. Toxicological and pharmacological concerns on oxidative stress and related diseases

    International Nuclear Information System (INIS)

    Saeidnia, Soodabeh; Abdollahi, Mohammad

    2013-01-01

    Although reactive oxygen species (ROS) such as superoxide, hydrogen peroxide and hydroxyl radical are generated as the natural byproduct of normal oxygen metabolism, they can create oxidative damage via interaction with bio-molecules. The role of oxidative stress as a remarkable upstream part is frequently reported in the signaling cascade of inflammation as well as chemo attractant production. Even though hydrogen peroxide can control cell signaling and stimulate cell proliferation at low levels, in higher concentrations it can initiate apoptosis and in very high levels may create necrosis. So far, the role of ROS in cellular damage and death is well documented with implicating in a broad range of degenerative alterations e.g. carcinogenesis, aging and other oxidative stress related diseases (OSRDs). Reversely, it is cleared that antioxidants are potentially able to suppress (at least in part) the immune system and to enhance the normal cellular protective responses to tissue damage. In this review, we aimed to provide insights on diverse OSRDs, which are correlated with the concept of oxidative stress as well as its cellular effects that can be inhibited by antioxidants. Resveratrol, angiotensin converting enzyme inhibitors, angiotensin receptor blockers, statins, nebivolol and carvedilol, pentaerythritol tetranitrate, mitochondria-targeted antioxidants, and plant-derived drugs (alone or combined) are the potential medicines that can be used to control OSRD

  19. Trace explosives sensor testbed (TESTbed)

    Science.gov (United States)

    Collins, Greg E.; Malito, Michael P.; Tamanaha, Cy R.; Hammond, Mark H.; Giordano, Braden C.; Lubrano, Adam L.; Field, Christopher R.; Rogers, Duane A.; Jeffries, Russell A.; Colton, Richard J.; Rose-Pehrsson, Susan L.

    2017-03-01

    A novel vapor delivery testbed, referred to as the Trace Explosives Sensor Testbed, or TESTbed, is demonstrated that is amenable to both high- and low-volatility explosives vapors including nitromethane, nitroglycerine, ethylene glycol dinitrate, triacetone triperoxide, 2,4,6-trinitrotoluene, pentaerythritol tetranitrate, and hexahydro-1,3,5-trinitro-1,3,5-triazine. The TESTbed incorporates a six-port dual-line manifold system allowing for rapid actuation between a dedicated clean air source and a trace explosives vapor source. Explosives and explosives-related vapors can be sourced through a number of means including gas cylinders, permeation tube ovens, dynamic headspace chambers, and a Pneumatically Modulated Liquid Delivery System coupled to a perfluoroalkoxy total-consumption microflow nebulizer. Key features of the TESTbed include continuous and pulseless control of trace vapor concentrations with wide dynamic range of concentration generation, six sampling ports with reproducible vapor profile outputs, limited low-volatility explosives adsorption to the manifold surface, temperature and humidity control of the vapor stream, and a graphical user interface for system operation and testing protocol implementation.

  20. Organic nitrates: update on mechanisms underlying vasodilation, tolerance and endothelial dysfunction.

    Science.gov (United States)

    Münzel, Thomas; Steven, Sebastian; Daiber, Andreas

    2014-12-01

    Given acutely, organic nitrates, such as nitroglycerin (GTN), isosorbide mono- and dinitrates (ISMN, ISDN), and pentaerythrityl tetranitrate (PETN), have potent vasodilator and anti-ischemic effects in patients with acute coronary syndromes, acute and chronic congestive heart failure and arterial hypertension. During long-term treatment, however, side effects such as nitrate tolerance and endothelial dysfunction occur, and therapeutic efficacy of these drugs rapidly vanishes. Recent experimental and clinical studies have revealed that organic nitrates per se are not just nitric oxide (NO) donors, but rather a quite heterogeneous group of drugs considerably differing for mechanisms underlying vasodilation and the development of endothelial dysfunction and tolerance. Based on this, we propose that the term nitrate tolerance should be avoided and more specifically the terms of GTN, ISMN and ISDN tolerance should be used. The present review summarizes preclinical and clinical data concerning organic nitrates. Here we also emphasize the consequences of chronic nitrate therapy on the supersensitivity of the vasculature to vasoconstriction and on the increased autocrine expression of endothelin. We believe that these so far rather neglected and underestimated side effects of chronic therapy with at least GTN and ISMN are clinically important. Copyright © 2014 Elsevier Inc. All rights reserved.

  1. CCDC 948059: Experimental Crystal Structure Determination : catena-[(mu3-Oxo)-hexakis(mu3-isonicotonato)-triaqua-tri-chromium-tri-silver tetranitrate hydrate

    KAUST Repository

    Schoedel, Alexander; Wojtas, Lukasz; Kelley, Stephen P.; Rogers, Robin D.; Eddaoudi, Mohamed; Zaworotko, Michael J.

    2013-01-01

    An entry from the Cambridge Structural Database, the world’s repository for small molecule crystal structures. The entry contains experimental data from a crystal diffraction study. The deposited dataset for this entry is freely available from the CCDC and typically includes 3D coordinates, cell parameters, space group, experimental conditions and quality measures.

  2. Different-ligand boron complexes with gluconate-ions and pentaerythritol and gluconatoborates with B-O-B bridge bond. Raznoligandnye kompleksy bora s glyukonat-ionami i pentaehritritom i glyukonatoboraty s mostikovoj V-O-V svyaz'yu

    Energy Technology Data Exchange (ETDEWEB)

    Tel' zhenskaya, P N; Shvarts, E M; Vitola, I M [AN Latvijskoj SSR, Riga (USSR). Inst. Neorganicheskoj Khimii

    1990-01-01

    Borogluconates differing in structure of the complex dimeric borogluconate ion from the described earlier have been synthesized. The results of physicochemical measurements (chemical and thermal analysis, IR-spectroscopy, titration according to Fisher, conductometry) allowed to propose formulas for the studied compounds.

  3. Extending the range of compounds amenable for gas chromatography-mass spectrometric analysis.

    Science.gov (United States)

    Fialkov, Alexander B; Gordin, Alexander; Amirav, Aviv

    2003-04-04

    Gas chromatography-mass spectrometry (GC-MS) suffers from a major limitation in that an expanding number of thermally labile or low volatility compounds of interest are not amenable for analysis. We found that the elution temperatures of compounds from GC can be significantly lowered by reducing the column length, increasing the carrier gas flow rate, reducing the capillary column film thickness and lowering the temperature programming rate. Pyrene is eluted at 287 degrees C in standard GC-MS with a 30 m x 0.25 mm I.D. column with 1-microm DB5ms film and 1-ml/min He column flow rate. In contrast, pyrene is eluted at 79 degrees C in our "Supersonic GC-MS" system using a 1 m x 0.25 mm I.D. column with 0.1-microm DB5ms film and 100-ml/min He column flow rate. A simple model has been invoked to explain the significantly (up to 208 degrees C) lower elution temperatures observed. According to this model, every halving of the temperature programming rate, or number of separation plates (either through increased flow rate or due to reduced column length), results in approximately 20 degrees C lower elution temperature. These considerably lower elution temperatures enable the analysis of an extended range of thermally labile and low volatility compounds, that otherwise could not be analyzed by standard GC-MS. We demonstrate the analysis of large polycyclic aromatic hydrocarbons (PAHs) such as decacyclene with ten fused rings, well above the current GC limit of PAHs with six rings. Even a metalloporphirin such as magnesiumoctaethylporphin was easily analyzed with elution temperatures below 300 degrees C. Furthermore, a range of thermally labile compounds were analyzed including carbamates such as methomyl, aldicarb, aldicarbsulfone and oxamyl, explosives such as pentaerythritol tetranitrate, Tetryl and HMX, and drugs such as reserpine (608 a.m.u.). Supersonic GC-MS was used, based on the coupling of a supersonic molecular beam (SMB) inlet and ion sources with a bench

  4. Results, meta-analysis and a first evaluation of UNOxR, the urinary nitrate-to-nitrite molar ratio, as a measure of nitrite reabsorption in experimental and clinical settings.

    Science.gov (United States)

    Tsikas, Dimitrios; Hanff, Erik; Bollenbach, Alexander; Kruger, Ruan; Pham, Vu Vi; Chobanyan-Jürgens, Kristine; Wedekind, Dirk; Arndt, Tanja; Jörns, Anne; Berbée, Jimmy F P; Princen, Hans M G; Lücke, Thomas; Mariotti, François; Huneau, Jean-François; Ückert, Stefan; Frölich, Jürgen C; Lenzen, Sigurd

    2018-05-04

    We recently found that renal carbonic anhydrase (CA) is involved in the reabsorption of inorganic nitrite (NO 2 - ), an abundant reservoir of nitric oxide (NO) in tissues and cells. Impaired NO synthesis in the endothelium and decreased NO bioavailability in the circulation are considered major contributors to the development and progression of renal and cardiovascular diseases in different conditions including diabetes. Isolated human and bovine erythrocytic CAII and CAIV can convert nitrite to nitrous acid (HONO) and its anhydride N 2 O 3 which, in the presence of thiols (RSH), are further converted to S-nitrosothiols (RSNO) and NO. Thus, CA may be responsible both for the homeostasis of nitrite and for its bioactivation to RSNO/NO. We hypothesized that enhanced excretion of nitrite in the urine may contribute to NO-related dysfunctions in the renal and cardiovascular systems, and proposed the urinary nitrate-to-nitrite molar ratio, i.e., U NOx R, as a measure of renal CA-dependent excretion of nitrite. Based on results from clinical and experimental animal studies, here, we report on a first evaluation of U NOx R. We determined U NOx R values in preterm neonates, healthy children, and adults, in children suffering from type 1 diabetes mellitus (T1DM) or Duchenne muscular dystrophy (DMD), in elderly subjects suffering from chronic rheumatic diseases, type 2 diabetes mellitus (T2DM), coronary artery disease (CAD), or peripheral arterial occlusive disease (PAOD). We also determined U NOx R values in healthy young men who ingested isosorbide dinitrate (ISDN), pentaerythrityl tetranitrate (PETN), or inorganic nitrate. In addition, we tested the utility of U NOx R in two animal models, i.e., the LEW.1AR1-iddm rat, an animal model of human T1DM, and the APOE*3-Leiden.CETP mice, a model of human dyslipidemia. Mean U NOx R values were lower in adult patients with rheumatic diseases (187) and in T2DM patients of the DALI study (74) as compared to healthy elderly adults

  5. Synthesis of triazole-based and imidazole-based zinc catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Valdez, Carlos A.; Satcher, Jr., Joe H.; Aines, Roger D.; Baker, Sarah E.

    2013-03-12

    Various methods and structures of complexes and molecules are described herein related to a zinc-centered catalyst for removing carbon dioxide from atmospheric or aqueous environments. According to one embodiment, a method for creating a tris(triazolyl)pentaerythritol molecule includes contacting a pentaerythritol molecule with a propargyl halide molecule to create a trialkyne molecule, and contacting the trialkyne molecule with an azide molecule to create the tris(triazolyl)pentaerythritol molecule. In another embodiment, a method for creating a tris(imidazolyl)pentaerythritol molecule includes alkylating an imidazole 2-carbaldehyde molecule to create a monoalkylated aldehyde molecule, reducing the monoalkylated aldehyde molecule to create an alcohol molecule, converting the alcohol molecule to create an alkyl halide molecule using thionyl halide, and reacting the alkyl halide molecule with a pentaerythritol molecule to create a tris(imidazolyl)pentaerythritol molecule. In another embodiment, zinc is bound to the tris(triazolyl)pentaerythritol molecule to create a zinc-centered tris(triazolyl)pentaerythritol catalyst for removing carbon dioxide from atmospheric or aqueous environments.

  6. The Characterization of a Slurry Explosive--Teledet

    Science.gov (United States)

    1979-02-01

    weight PETN* 38.0 + .5 Ammonium nitrate** 27 T .5 Diethyleneglycol 9 T .5 Guar Gum .5 Water 25 + .5 *This is ultra-fine particle size, sensitive PETN. r...Diamond Laboratories ATTN: Technical Library I Branch 420, Mr. R.K. Warner 2800 Powder Mill Road Adelphi, MD 20783 P Commander US Army Engineers

  7. Modification of the Campylobacter jejuni N-linked glycan by EptC protein-mediated addition of phosphoethanolamine

    DEFF Research Database (Denmark)

    Scott, Nichollas E; Nothaft, Harald; Edwards, Alistair V G

    2012-01-01

    . Interrogation of these data allowed the identification of a phosphoethanolamine (pEtN)-modified variant of the N-glycan that was attached to multiple proteins. The pEtN moiety was attached to the terminal GalNAc of the canonical N-glycan. Deletion of the pEtN transferase eptC removed all evidence of the p......, yet above background levels of pEtN-glycan were also observed in E. coli not expressing eptC, suggesting that endogenous E. coli pEtN transferases can mediate the addition of pEtN to N-glycans. The addition of pEtN must be considered in the context of glycoengineering and may alter C. jejuni glycan...

  8. The effect of phosphoethanolamine intake on mortality and macrophage activity in mice with solid ehrlich tumors

    Directory of Open Access Journals (Sweden)

    Maria Sueli Parreira de Arruda

    2011-12-01

    Full Text Available The aim of the present study was to examine the effect of a diet rich in synthetic PEtn on the metabolism macrophages of tumor-bearing mice. The results demonstrated that PEtn increased the animals' survival time. In addition, the treated animals released smaller amounts of hydrogen peroxide (H2O2 and nitric oxide (NO than the non-treated animals, particularly after day 14. From the results it could be concluded that H2O2 and NO were important in the modulation of neoplastic growth, and pointed to a promising role of PEtn in the control of human neoplasms.

  9. Integrated Data Collection Analysis (IDCA) Program — Bullseye® Smokeless Powder

    Energy Technology Data Exchange (ETDEWEB)

    Sandstrom, Mary M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Geoffrey W. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Preston, Daniel N. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Pollard, Colin J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Warner, Kirstin F. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Sorensen, Daniel N. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Remmers, Daniel L. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Phillips, Jason J. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Shelley, Timothy J. [Bureau of Alcohol, Tobacco and Firearms, Redstone Arsenal, AL (United States); Reyes, Jose A. [Applied Research Associates, Tyndall AFB, FL (United States); Hsu, Peter C. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Reynolds, John G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2013-05-30

    The Integrated Data Collection Analysis (IDCA) program is conducting a proficiency study for Small- Scale Safety and Thermal (SSST) testing of homemade explosives (HMEs). Described here are the results for impact, friction, electrostatic discharge, and differential scanning calorimetry analysis of Bullseye® smokeless powder (Gunpowder). The participants found the Gunpowder: 1) to have a range of sensitivity to impact, from less than RDX to almost as sensitive as PETN, 2) to be moderately sensitive to BAM and ABL friction, 3) have a range for ESD, from insensitive to more sensitive than PETN, and 4) to have thermal sensitivity about the same as PETN and RDX.

  10. Integrated Data Collection Analysis (IDCA) Program - NaClO3/Icing Sugar

    Energy Technology Data Exchange (ETDEWEB)

    Sandstrom, Mary M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Geoffrey W. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Preston, Daniel N. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Pollard, Colin J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Warner, Kirstin F. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Sorensen, Daniel N. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Remmers, Daniel L. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Shelley, Timothy J. [Air Force Research Lab. (AFRL), Tyndall Air Force Base, FL (United States); Reyes, Jose A. [Applied Research Associates, Tyndall Air Force Base, FL (United States); Hsu, Peter C. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Reynolds, John G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2013-02-11

    The Integrated Data Collection Analysis (IDCA) program is conducting a proficiency study for Small- Scale Safety and Thermal (SSST) testing of homemade explosives (HMEs). Described here are the results for impact, friction, electrostatic discharge, and differential scanning calorimetry analysis of a mixture of NaClO3 and icing sugar—NaClO3/icing sugar mixture. The mixture was found to: be more sensitive than RDX but less sensitive than PETN in impact testing (180-grit sandpaper); be more sensitive than RDX and about the same sensitivity as PETN in BAM fiction testing; be less sensitive than RDX and PETN except for one participant found the mixture more sensitive than PETN in ABL ESD testing; and to have one to three exothermic features with the lowest temperature event occurring at ~ 160°C always observed in thermal testing. Variations in testing parameters also affected the sensitivity.

  11. Patterning high explosives at the nanoscale

    Energy Technology Data Exchange (ETDEWEB)

    Nafday, Omkar A.; Pitchimani, Rajasekar; Weeks, Brandon L. [Department of Chemical Engineering, Texas Tech University, Lubbock, TX 79409 (United States); Haaheim, Jason [NanoInk Inc., 8025 Lamon Ave., Skokie, IL 60077 (United States)

    2006-10-15

    For the first time, we have shown that spin coating and Dip pen nanolithography (DPN trademark) are simple methods of preparing energetic materials such as PETN and HMX on the nanoscale, requiring no heating of the energetic material. Nanoscale patterning has been demonstrated by the DPN method while continuous thin films were produced using the spin coating method. Results are presented for preparing continuous PETN thin films of nanometer thickness by the spin coating method and for controlling the architecture of arbitrary nanoscale patterns of PETN and HMX by the DPN method. These methods are simple for patterning energetic materials and can be extended beyond PETN and HMX, opening the door for fundamental studies at the nanoscale. (Abstract Copyright [2006], Wiley Periodicals, Inc.)

  12. Bio-based alkyds by direct enzymatic bulk polymerization

    DEFF Research Database (Denmark)

    Nguyen, Hiep Dinh

    to a corresponding classical reference. In a further development of the system, it has been found possible to use the esters of pentaerythritol and stearic acid in combination with the penta-aze derivative for the preparation of pseudo alkyds containing only pentaerythritol as polyol with high degree of branching....... Bio-based alkyds prepared from a combination of glycerol, and tall oil fatty acids, and azelaic acid by enzymatic polymerization show improved hydrophobicity and lower glass transition temperatures compared to an alkyd prepared from the same raw materials by a classical boiling method. The enzymatic...... of pentaerythritol derivatized with azelaic acid (or penta-aze) was examined and tested for the production of more branched alkyd systems. A photostability test validated the concept, and the method also resulted in alkyds with improved hydrophobicity and lower glass transition temperatures compared...

  13. 21 CFR 177.1580 - Polycarbonate resins.

    Science.gov (United States)

    2010-04-01

    ...′-iso-propylidenediphenol with molten diphenyl carbonate in the presence of the disodium salt of 4,4... chloride Monochlorobenzene Not to exceed 500 p.p.m. as residual solvent in finished resin. Pentaerythritol...-88-3) Not to exceed 800 parts per million as residual solvent in finished resin. Triethylamine (c...

  14. Synthesis of hyperbranched polystyrene and its fullerene end-capped derivates with multifunctional atom-transfer radical polymerization initiator

    NARCIS (Netherlands)

    Yang, J.W.; Wang, Changchun; Ming, W.

    2004-01-01

    A novel multifunctional A TRP initiator was synthesized by esterfication of a hyperbranched polyester Z5 [from pentaerythritol and 2, 2-bis Chydroxymethyl) propionic acid]. The macroinitiator contained approximately 19 initiating sites per molecule. It was used for the A TRP of styrene mediated by

  15. 40 CFR Table 1 to Subpart F of... - Synthetic Organic Chemical Manufacturing Industry Chemicals

    Science.gov (United States)

    2010-07-01

    ... 123637 II Pentachlorophenol 87865 III Pentaerythritol 115775 I Peracetic acid 79210 II Perchloromethyl... 83329 V Acetal 105577 V Acetaldehyde 75070 II Acetamide 60355 II Acetanilide 103844 II Acetic acid 64197... Acetonitrile 75058 I Acetophenone 98862 I Acrolein 107028 IV Acrylamide 79061 I Acrylic acid 79107 IV...

  16. Properties and thermal decomposition of the double salts of uranyl nitrate-ammonium nitrate

    International Nuclear Information System (INIS)

    Notz, K.J.; Haas, R.A.

    1989-01-01

    The formation of ammonium nitrate-uranyl nitrate double salts has important effects on the thermal denitration process for the preparation of UO 3 and on the physical properties of the resulting product. Analyses were performed, and properties and decomposition behavior were determined for three double salts: NH 4 UO 2 (NO 3 ) 3 , (NH 4 ) 2 UO 2 (NO 3 ) 4 , and (NH 4 ) 2 UO 2 (NO 3 ) 4 ·2H 2 O. The tinitrate salt decomposes without melting at 270-300 C to give a γ-UO 3 powder of ∼3-μm average size, with good ceramic properties for fabrication into UO 2 nuclear fuel pellets. The tetranitrate dihydrate melts at 48 C; it also dehydrates to the anhydrous salt. The anhydrous tetranitrate decomposes exothermically, without melting, at 170-270 C by losing one mole of ammonium nitrate to form the trinitrate salt

  17. Investigating a Drop-on-Demand Microdispenser for Standardized Sample Preparation

    Science.gov (United States)

    2012-09-01

    potassium chlorate were obtained from Sigma-Aldrich. 1,3,5-trinitro-1,3,5-triazine (RDX), octahydro-1,3,5,7- tetranitro-tetrazocine (HMX), 2,4,6... potassium chlorate , HMX, TNT, RDX, PETN, urea, and sugar. The analyte of interest was dissolved in the appropriate solvent and then diluted to various

  18. Laser-Induced Breakdown Spectroscopy for Detection of Explosives Residues: A Review of Recent Advances, Challenges, and Future Prospects

    Science.gov (United States)

    2013-04-01

    PETN), and nitrate and chlorate simulants mixed with sand (8%) at a distance of 50 m [104]. Early results for LIBS/Raman data originated in the art and...of black powder and its principle components (charcoal, sulfur, calcium sulfate, potassium nitrate, and ammonium nitrate) [22]. Although this ap

  19. Differential thermal analysis microsystem for explosive detection

    DEFF Research Database (Denmark)

    Olsen, Jesper Kenneth; Greve, Anders; Senesac, L.

    2011-01-01

    as a small silicon nitride membrane incorporating heater elements and a temperature measurement resistor. In this manuscript the DTA system is described and tested by measuring calorimetric response of 3 different kinds of explosives (TNT, RDX and PETN). This project is carried out under the framework...

  20. 77 FR 75243 - Self-Regulatory Organizations; Options Clearing Corporation; Order Approving Proposed Rule Change...

    Science.gov (United States)

    2012-12-19

    ... modeling and risk management procedures (``Risk Management Proposal'') \\9\\ is approved by the Commission... risk modeling enhancements with respect to longer-tenor options, including OTC S&P 500 Index Options... http://www.sec.gov/rules/petitions/2012/petn4-644.pdf . This Order does not address the relief...

  1. Effect of transesterification degree and post-treatment on the in-service performance of NCO-functionalized vegetable oil bituminous products

    OpenAIRE

    Cuadri Vega, Antonio Abad; García Morales, Moisés; Navarro Domínguez, Francisco Javier; Partal López, Pedro

    2014-01-01

    The bitumen modification through polyurethane prepolymers presents significant benefits for the manufacture of bituminous products for the paving industry. In this sense, this work explores the use, as bitumen modifier, of a novel reactive prepolymer synthesized by reaction of 4,4´,diphenylmethane diisocyanate (MDI) and a vegetable oil-based polyol, castor oil (CO), previously transesterified with pentaerythritol. On the one hand, thermal analysis on transesterified CO revealed a highly stabl...

  2. Highly Branched Bio-Based Unsaturated Polyesters by Enzymatic Polymerization

    DEFF Research Database (Denmark)

    Nguyen, Hiep Dinh; Löf, David; Hvilsted, Søren

    2016-01-01

    A one-pot, enzyme-catalyzed bulk polymerization method for direct production of highly branched polyesters has been developed as an alternative to currently used industrial procedures. Bio-based feed components in the form of glycerol, pentaerythritol, azelaic acid, and tall oil fatty acid (TOFA)...... stability, very high water contact angles of up to 141° and a glass transition temperature that could be controlled through the feed composition....

  3. Irradiatable polymer composition with improved oxidation resistance

    International Nuclear Information System (INIS)

    Lyons, B.J.

    1977-01-01

    A method is described for the incorporation of a substantially insoluble organic phosphite into a polymer composition such as polyolefin polymers or ethylene copolymers to prevent oxidation of the polymer at elevated temperatures after radiation-induced crosslinking. The crosslinking is readily achieved without affecting the antioxidant properties of the organic phosphite. Particularly suitable organic compounds are derivatives of pentaerythritol, dipentaerythritol, and tripentaerythritol in cooncentrations of 1 to 3% of the mixture to be irradiated

  4. Integrated Data Collection Analysis (IDCA) Program — KClO3/Icing Sugar (-100 mesh) Mixture

    Energy Technology Data Exchange (ETDEWEB)

    Sandstrom, Mary M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Geoffrey W. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Preston, Daniel N. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Pollard, Colin J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Warner, Kirstin F. [Naval Surface Warfare Center (IHD-NSWC), Indian Head, MD (United States). Indian Head Division; Sorenson, Daniel N. [Naval Surface Warfare Center (IHD-NSWC), Indian Head, MD (United States). Indian Head Division; Remmers, Daniel L. [Naval Surface Warfare Center (IHD-NSWC), Indian Head, MD (United States). Indian Head Division; Moran, Jesse S. [Naval Surface Warfare Center (IHD-NSWC), Indian Head, MD (United States). Indian Head Division; Shelley, Timothy J. [Air Force Research Lab. (AFRL/RXQF), Tyndall AFB, FL (United States); Hsu, Peter C. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Whipple, Richard E. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Reynolds, John G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2011-05-02

    The Integrated Data Collection Analysis (IDCA) program is conducting a proficiency study for Small-Scale Safety and Thermal (SSST) testing of homemade explosives (HMEs). Described here are the results for impact, friction, electrostatic discharge, and scanning calorimetry analysis of a mixture of KClO3 sized through a 100-mesh sieve mixed with icing sugar, also sized through a 100-mesh sieve—KClO3/icing sugar (-100) mixture. This material was selected because of the challenge of performing SSST testing of a mixture of two solid materials. The mixture was found to be: 1) more sensitive to impact than RDX, with sensitivity similar to PETN, 2) the same or more sensitive to friction than PETN, and 3) less sensitive to spark than RDX. The analysis showed that the mixture has thermally stability similar to RDX and is perhaps more energetic upon decomposition but variable results indicate sampling issues.

  5. Integrated Data Collection Analysis (IDCA) Program - KClO4/Aluminum Mixture

    Energy Technology Data Exchange (ETDEWEB)

    Sandstrom, Mary M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Geoffrey W. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Preston, Daniel N. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Pollard, Colin J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Warner, Kirstin F. [Naval Surface Warfare Center (NSWC IHD), Indian Head, MD (United States). Indian Head Division; Sorensen, Daniel N. [Naval Surface Warfare Center (NSWC IHD), Indian Head, MD (United States). Indian Head Division; Remmers, Daniel L. [Naval Surface Warfare Center (NSWC IHD), Indian Head, MD (United States). Indian Head Division; Whinnery, LeRoy L. [Sandia National Lab. (SNL-CA), Livermore, CA (United States); Shelley, Timothy J. [Air Force Research Lab. (AFRL), Tyndall AFB, FL (United States); Reyes, Jose A. [Applied Research Associates (ARA), Tyndall AFB, FL (United States); Hsu, Peter C. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Reynolds, John G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2012-01-17

    The Integrated Data Collection Analysis (IDCA) program is conducting a Proficiency Test for Small-Scale Safety and Thermal (SSST) testing of homemade explosives (HMEs). Described here are the results for impact, friction, electrostatic discharge, and differential scanning calorimetry analysis of a mixture of KClO4 and aluminum—KClO4/Al mixture. This material was selected because of the challenge of performing SSST testing of a mixture of two solids. The mixture was found to be: 1) much less sensitive to impact than RDX, (LLNL being the exception) and PETN, 2) more sensitive to friction than RDX and PETN, and 3) extremely sensitive to spark. The thermal analysis showed little or no exothermic character. One prominent endothermic feature was observed in the temperature range studied and identified as a phase transition of KClO4.

  6. Precursors in detonations in porous explosives

    International Nuclear Information System (INIS)

    Spaulding, R.L. Jr.

    1981-01-01

    Photographs of detonation waves in low-density HMX and PETN, made with an image-intensifier camera, show a brilliant band of light in front of the pressure jump. The radiation temperature is estimated to be 12,000 to 14,000 0 K. The spectrum of this light is continuous. A quartz gauge shows a gradual buildup of pressure from the material producing the light. The material has little effect on the propagation of detonation. Further observations, using pellets of plastic-bonded HMX and single crystals of PETN, show that the material thrown off the free surface is transparent, with a leading edge moving at approximately 20 mm/μs. Collision of this material with polymethyl methacrylate (PMMA) produces a brilliant light with a spectrum that is initially a narrow H/sub α/ line. Quartz gauges measure the rate of pessure buildup of this material

  7. Possible hazard reduction by using distributed phased nuclear explosions

    Energy Technology Data Exchange (ETDEWEB)

    Chilton, Frank [Theoretical Physics Program, Stanford Research Institute, Menio Park, CA (United States); [Department of Applied Science, University of California, Davis, CA (United States); Cheney, James A [Department of Civil Engineering, University of California, Davis, CA (United States)

    1970-05-15

    The use of two or more nuclear devices, phased together in order to constructively add their respective particle velocities, is proposed herein. By directing the seismic waves of the nuclear explosions to make them more efficient in accomplishing the intended construction, we hope to be able to reduce the radioactivity, seismic, and airblast hazards substantially. Experiments are being performed with one gram charges of PETN. (author)

  8. Standardized Sample Preparation Using a Drop-on-Demand Printing Platform

    Science.gov (United States)

    2013-05-07

    and Materials Ammonium nitrate (AN), methanol (MeOH), distilled water (H2O), acetonitrile, sugar, urea, and potassium chlorate (KClO3) were...various pre-determined energetic and interferent compounds. The evaluated analytes were: AN, potassium chlorate , HMX, TNT, RDX, PETN, urea, and...KClO3 molecules dissolving and then breaking into potassium and chlorate ions in H2O. An additional concern was the interaction of adjacent

  9. Unique Structural Modifications Are Present in the Lipopolysaccharide from Colistin-Resistant Strains of Acinetobacter baumannii

    Science.gov (United States)

    2013-10-01

    Selected reaction monitoring (SRM) studies were performed on a Thermo TSQ Quantum Ultra Triple Stage quadrupole mass spectrometer. The scans of the...well as a PmrC-dependent pEtN addition to the lipid A of E. coli O157:H7 (39). Surprisingly, the canine pathogen Capnocytophaga canimorsus and plant...variety of novel lipid A structures obtained from Francisella tula- rensis live vaccine strain. Innate Immun. 18:268 –278. 44. Balaji V, Jeremiah SS

  10. A review of Explosives Used in Explosive Excavation Research Laboratory Projects Since 1969

    Science.gov (United States)

    1974-12-01

    Boron compounds Potassium dichramat« Antimony compounds Bismuth compounds P«riodat«s Litharge Guar gum (polysaccSarid«) Storch Acrylomid... gum , and gelled with a cross- linking agent. The i-arliest slurries used Government surplus TNT as a fuel-sensitizer, but the majority o...Nonexplosive TNT PETN RDX Rentalite Composition B Guanidine nitrate Smokeless powder Nitres*: ch Alky’amine nitrates Nit.omannite Aluminum Sugar

  11. Additive Manufacture of Three Dimensional Nanocomposite Based Objects through Multiphoton Fabrication

    Directory of Open Access Journals (Sweden)

    Yaan Liu

    2016-09-01

    Full Text Available Three-dimensional structures prepared from a gold-polymer composite formulation have been fabricated using multiphoton lithography. In this process, gold nanoparticles were simultaneously formed through photoreduction whilst polymerisation of two possible monomers was promoted. The monomers, trimethylopropane triacrylate (TMPTA and pentaerythritol triacrylate (PETA were mixed with a gold salt, but it was found that the addition of a ruthenium(II complex enhanced both the geometrical uniformity and integrity of the polymerised/reduced material, enabling the first production of 3D gold-polymer structures by single step multiphoton lithography.

  12. Evaluation and Control of Thiol-ene/Thiol-epoxy Hybrid Networks

    OpenAIRE

    Carioscia, Jacquelyn A.; Stansbury, Jeffrey W.; Bowman, Christopher N.

    2007-01-01

    The development of thiol-ene/thiol-epoxy hybrid networks offers the advantage of tailorable polymerization kinetics while producing a highly crosslinked, high Tg polymer that has significantly reduced shrinkage stress. Stoichiometric mixtures of pentaerythritol tetra(3-mercaptopropionate) (PETMP)/triallyl-1,3,5-triazine-2,4,6-trione (TATATO) (thiol-ene, mixture 1) and PETMP/bisphenol a diglycidyl ether (BADGE) (thiol-epoxy, mixture 2) were prepared and hybrid mixtures of 75/25, 50/50, 25/75, ...

  13. Preparation of new biobased coatings from a triglycidyl eugenol derivative through thiol-epoxy click reaction

    OpenAIRE

    Guzman, Dailyn; Ramis Juan, Xavier; Fernández Francos, Xavier; de la Flor1 López, Sílvia; Serra Albet, Àngels

    2018-01-01

    © 2017 Elsevier B.V. A new triglycidyl eugenol derivative (3EPO-EU) was synthesized and characterized by spectroscopic techniques, and used as starting monomer in the preparation of novel bio-based thiol-epoxy thermosets. As thiols, commercially available tetrathiol derived from pentaerythritol (PETMP), a trithiol derived from eugenol (3SH-EU) and the hexathiol derived from squalene (6SH-SQ) were used in the presence of 4-(N,N-dimethylamino)pyridine as the basic catalyst. A flexible diglycidy...

  14. Integrated Data Collection Analysis (IDCA) Program - AN and Bullseye Smokeless Powder

    Energy Technology Data Exchange (ETDEWEB)

    Sandstrom, Mary M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Geoffrey W. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Preston, Daniel N. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Pollard, Colin J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Warner, Kirstin F. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States); Sorensen, Daniel N. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States); Remmers, Daniel L. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States); Phillips, Jason J. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Shelley, Timothy J. [Bureau of Alcohol, Tobacco, and Firearms, Redstone Arsenal, AL (United States); Reyes, Jose A. [Applied Research Associates, Tyndall Air Force Base, FL (United States); Hsu, Peter C. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Reynolds, John G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2013-07-17

    The Integrated Data Collection Analysis (IDCA) program is conducting a proficiency study for Small- Scale Safety and Thermal (SSST) testing of homemade explosives (HMEs). Described here are the results for impact, friction, electrostatic discharge, and differential scanning calorimetry analysis of ammonium nitrate (AN) mixed with Bullseye® smokeless powder (Gunpowder). The participants found the AN/Gunpowder to: 1) have a range of sensitivity to impact, comparable to or less than RDX, 2) be fairly insensitive to friction as measured by BAM and ABL, 3) have a range for ESD, from insensitive to more sensitive than PETN, and 4) have thermal sensitivity about the same as PETN and Gunpowder. This effort, funded by the Department of Homeland Security (DHS), is putting the issues of safe handling of these materials in perspective with standard military explosives. The study is adding SSST testing results for a broad suite of different HMEs to the literature. Ultimately the study has the potential to suggest new guidelines and methods and possibly establish the SSST testing accuracies needed when developing safe handling practices for HMEs. Each participating testing laboratory uses identical test materials and preparation methods. Note, however, the test procedures differ among the laboratories. The testing performers involved are Lawrence Livermore National Laboratory (LLNL), Los Alamos National Laboratory (LANL), Indian Head Division, Naval Surface Warfare Center, (NSWC IHD), Sandia National Laboratories (SNL), and Air Force Research Laboratory (AFRL/RXQL). These tests are conducted as a proficiency study in order to establish some consistency in test protocols, procedures, and experiments and to compare results when these testing variables cannot be made consistent. Keywords: Small-scale safety testing, proficiency test, impact-, friction-, spark discharge-, thermal testing, round-robin test, safety testing protocols, HME, RDX, potassium perchlorate, potassium

  15. Sandia National Laboratories Small-Scale Sensitivity Testing (SSST) Report: Calcium Nitrate Mixtures with Various Fuels.

    Energy Technology Data Exchange (ETDEWEB)

    Phillips, Jason Joe [Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)

    2014-07-01

    Based upon the presented sensitivity data for the examined calcium nitrate mixtures using sugar and sawdust, contact handling/mixing of these materials does not present hazards greater than those occurring during handling of dry PETN powder. The aluminized calcium nitrate mixtures present a known ESD fire hazard due to the fine aluminum powder fuel. These mixtures may yet present an ESD explosion hazard, though this has not been investigated at this time. The detonability of these mixtures will be investigated during Phase III testing.

  16. Explosion-induced combustion of hydrocarbon clouds in a chamber

    International Nuclear Information System (INIS)

    Neuwald, P; Reichenbach, H; Kuhl, A L

    2001-01-01

    The interaction of the detonation of a solid HE-charge with a non-premixed cloud of hydro-carbon fuel in a chamber was studied in laboratory experiments. Soap bubbles filled with a flammable gas were subjected to the blast wave created by the detonation of PETN-charges (0.2 g < mass < 0.5 g). The dynamics of the combustion system were investigated by means of high-speed photography and measurement of the quasi-static chamber pressure

  17. Dynamics of the formation of the condensed phase particles at detonation of high explosives

    CERN Document Server

    Evdokov, O V; Kulipanov, G N; Luckjanchikov, L A; Lyakhov, N Z; Mishnev, S I; Sharafutdinov, M R; Sheromov, M A; Ten, K A; Titov, V M; Tolochko, B P; Zubkov, P I

    2001-01-01

    The article presents the results of the experimental study SAXS on condensed carbon particles that appear at the detonation of a high explosive. It was shown that the SAXS signal rises for 1.5-4 mu s after the detonation front passing. The SAXS signal in trotyl and its alloys with hexogen starts just after the compression of the material in the detonation wave. In octogen, hexogen and PETN, the SAXS signal appears in 0.5 mu s and is much smaller than the signal at the detonation of trotyl and its alloys with hexogen.

  18. Fizičko-hemijske i detonacione karakteristike nitraminskih eksploziva - RDX, HMX i CL-20

    OpenAIRE

    Anđelković-Lukić Mirjana

    2002-01-01

    U radu su prikazane fizičko-hemijske i detonacione karakteristike nitraminskih brizantnih eksploziva, heksogena i oktogena, uporedene sa osobinama novog cikličnog nitraminskog eksploziva CL-20. Novi visokobrizantni eksploziv CL-20 postoji u četiri kristalne forme, stabilne na različitim temepraturama. Ima bolje detonacione karakteristike od heksogena i oktogena veću gustinu i brzinu detonacije, all mnogo veću osetljivost na udar i trenje, reda PETN. Zbog toga se ovaj eksploziv flegmatizuje sa...

  19. Imaging indicator for ESD safety testing.

    Energy Technology Data Exchange (ETDEWEB)

    Whinnery, LeRoy L.,; Nissen, April; Keifer, Patrick N.; Tyson, Alexander

    2013-05-01

    This report describes the development of a new detection method for electrostatic discharge (ESD) testing of explosives, using a single-lens reflex (SLR) digital camera and a 200-mm macro lens. This method has demonstrated several distinct advantages to other current ESD detection methods, including the creation of a permanent record, an enlarged image for real-time viewing as well as extended periods of review, and ability to combine with most other Go/No-Go sensors. This report includes details of the method, including camera settings and position, and results with wellcharacterized explosives PETN and RDX, and two ESD-sensitive aluminum powders.

  20. Comparing CTH simulations and experiments on explosively loaded rings

    Science.gov (United States)

    Braithwaite, C. H.; Aydelotte, Brady; Collins, Adam; Thadhani, Naresh; Williamson, David Martin

    2012-03-01

    A series of experiments were conducted on explosively loaded metallic rings for the purpose of studying fragmentation. In addition to the collection of fragments for analysis, the radial velocity of the expanding ring was measured with photon Doppler velocimetry (PDV) and the arrangement was imaged using high speed photography. Both the ring material and the material used as the explosive container were altered and the results compared with simulations performed in CTH. Good agreement was found between the simulations and the experiments. The maximum radial velocity attained was approximately 380 m/s, which was achieved through loading with a 5g PETN based charge.

  1. Recent Developments in the Field of Energetic Ionic Liquids

    Science.gov (United States)

    2014-10-07

    tetranitroaniline RDX 14,18,19,21 1,3,5-trinitro-1,3,5- triazacyclohexane PETN 14,15,21 [3-nitrooxy-2,2-bis(nitro oxymethyl) propyl ] nitrate CL20 21-25...was then proved to play a vital role since the chloride precursor (2a) was also found to be hypergolic. Therefore, the 45 anion is not solely... Synthesis , 1977, 1, 1. 91 C. D. Hurd, L. F. Audrieth and L. A. Nalefski, Inorganic Syntheses, ed. H. S. Booth, McGraw-Hill Book Company Inc., New York

  2. Comparative Assessment of Copper-Coated Kapton: Analysis of Microclad from Several Manufacturing Lots

    Energy Technology Data Exchange (ETDEWEB)

    Martz, Joseph Christopher [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Spearing, Dane Robert [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Labouriau, Andrea [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Judge, Elizabeth [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Kelly, Daniel [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Dirmyer, Matthew R. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Milenski, Helen Marie [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Patterson, Brian M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Sandoval, Cynthia Wathen [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Usov, Igor Olegovich [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Beaux, Miles Frank II [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Henderson, Kevin C. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Torres, Joseph Angelo [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Edwards, Stephanie Lynn [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Vodnik, Douglas R. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Keller, Jennie [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Mccabe, Rodney James [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Livescu, Veronica [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Cowan, Joseph Sarno [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Aragonez, Robert J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Tokash, Justin Charles [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Lawrence, Samantha Kay [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Leon Brito, Neliza [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-04-03

    Microclad is a composite material consisting of a thin copper coating applied on a single side over a Kapton substrate. Kapton is the commercial designator for polyimide supplied by DuPont. Microclad is a key material in detonator manufacture and function. Detonators which utilize Microclad function when a large current applied through a thin bridge etched into the copper produces a plasma, accelerating a Kapton flyer into an explosive (PETN) pellet. The geometry and properties of the Microclad are a critical element of this process.

  3. Experiments on cylindrically converging blast waves in atmospheric air

    Science.gov (United States)

    Matsuo, Hideo; Nakamura, Yuichi

    1980-06-01

    Cylindrically converging blast waves have been produced in normal atmospheric conditions by the detonation of the explosives, pentaerythritoltetranitrate, (PETN), over cylindrical surfaces. The shocks generated in this way are so strong that the fronts propagating through the air become luminous of themselves. The production and the propagation of the shocks have been monitored with a framing camera and a streak camera, and the time-space relations of the shock propagations have been determined using an electrical ionization probing system. The results have shown that the trajectory of the shock fronts near the axis of the cylinder can be approximately represented by the Guderley's formula.

  4. Full scale numerical analysis of high performance concrete columns designed to withstand severe blast impact

    DEFF Research Database (Denmark)

    Riisgaard, Benjamin; Georgakis, Christos; Stang, Henrik

    2007-01-01

    Polymer reinforced Compact Reinforced Composite, PCRC, is a Fiber reinforced Densified Small Particle system, FDSP, combined with a high strength longitudinal flexural rebar arrangement laced together with polymer lacing to avoid shock initiated disintegration of the structural element under blast...... of PETN (85/15) High Explosives at stand off 1600 mm. Additionally, a LS-DYNA material model suitable for predicting the response of Polymer reinforced Compact Reinforced Concrete improved for close-in detonation and a description of the LS-DYNA multi-material Eulerian method for modeling the blast event...

  5. Composite materials for thermal energy storage

    Science.gov (United States)

    Benson, D. K.; Burrows, R. W.; Shinton, Y. D.

    1985-01-01

    A composite material for thermal energy storage based upon polyhydric alcohols, such as pentaerythritol, trimethylol ethane (also known as pentaglycerine), neopentyl glycol and related compounds including trimethylol propane, monoaminopentaerythritol, diamino-pentaerythritol and tris(hydroxymethyl)acetic acid, separately or in combinations, which provide reversible heat storage through crystalline phase transformations are discussed. These PCM's do not become liquid during use and are in contact with at least one material selected from the group consisting of metals, carbon, siliceous, plastic, cellulosic, natural fiber, artificial fiber, concrete, gypsum, porous rock, and mixtures thereof. Particulate additions such as aluminum or graphite powders, as well as metal and carbon fibers can also be incorporated therein. Particulate and/or fibrous additions can be introduced into molten phase change materials which can then be cast into various shapes. After the phase change materials have solidified, the additions will remain dispersed throughout the matrix of the cast solid. The polyol is in contact with at least one material selected from the group consisting of metals, carbon, siliceous, plastic, cellulosic, natural fiber, artificial fiber, concrete, gypsum, and mixtures thereof.

  6. Crystallization and X-ray analysis of the salmon-egg lectin SEL24K

    Energy Technology Data Exchange (ETDEWEB)

    Murata, Kenji [Department of Animal Science, University of California, Davis 95616 (United States); Fisher, Andrew J. [Department of Chemistry, University of California, Davis 95616 (United States); Hedrick, Jerry L., E-mail: jlhedrick@ucdavis.edu [Department of Animal Science, University of California, Davis 95616 (United States)

    2007-05-01

    The 24 kDa egg lectin of Chinook salmon (Oncorhynchus tshawytscha) was purified by affinity chromatography from salmon eggs and crystallized by the hanging-drop vapor-diffusion method using 15/4 EO/OH (pentaerythritol ethoxylate) as a precipitant. The 24 kDa egg lectin of Chinook salmon (Oncorhynchus tshawytscha) is released from the egg during the cortical reaction. The lectin functions in blocking polyspermy during the fertilization process. The egg lectin was purified by affinity chromatography from salmon eggs and crystallized by the hanging-drop vapor-diffusion method using 15/4 EO/OH (pentaerythritol ethoxylate) as a precipitant. The crystal diffracted synchrotron-radiation X-rays to 1.63 Å resolution. The crystal belongs to the monoclinic space group P2{sub 1}, with unit-cell parameters a = 93.0, b = 73.6, c = 113.6 Å, α = 90, β = 92.82, γ = 90°. The crystal is likely to contain eight molecules in the asymmetric unit (V{sub M} = 2.3 Å{sup 3} Da{sup −1}), corresponding to a solvent content of 45.5%. A self-rotation function suggests an arrangement with 222 point symmetry within the asymmetric unit.

  7. Preparation and Property Recognition of Nimodipine Molecularly Imprinted Polymer

    Directory of Open Access Journals (Sweden)

    Fei-fei CHEN

    2015-09-01

    Full Text Available Objective: To explore the application of molecular imprinting technique in the separation and detection of nimodipine. Methods: Methacrylic acid as functional monomer, pentaerythritol triacrylate as cross-linking agent were used to prepare molecularly imprinted polymer (MIP with the feature of specific recognition performance on imprinting molecule nimodipine under condition of template molecule nimodipine. The preparation conditions, recognition performance of MIP on nimodipine, different proportions of template molecule and functional monomer, the selectivity to other substrate, and the relationship between adsorption quantity (Q and time were observed. Results: MIP was prepared successfully bynimodipine as template and pentaerythritol triacrylate as cross-linking agent, with the feature of specific recognition performance on nimodipine. The static adsorption distribution coefficient (KD was 0.2264. The equation of Q and the concentration of substrate of template MIP was y = -0.21x+0.2204. Combining capacity of template molecule at the same concentration enhanced with the increasing proportion of functional monomer.Conclusion: Nimodipine MIP based on molecular imprinting technique may become a new approach to chiral separation for nimodipine.

  8. Composite materials for thermal energy storage

    Science.gov (United States)

    Benson, D.K.; Burrows, R.W.; Shinton, Y.D.

    1985-01-04

    A composite material for thermal energy storage based upon polyhydric alcohols, such as pentaerythritol, trimethylol ethane (also known as pentaglycerine), neopentyl glycol and related compounds including trimethylol propane, monoaminopentaerythritol, diamino-pentaerythritol and tris(hydroxymethyl)acetic acid, separately or in combinations, which provide reversible heat storage through crystalline phase transformations. These PCM's do not become liquid during use and are in contact with at least one material selected from the group consisting of metals, carbon, siliceous, plastic, cellulosic, natural fiber, artificial fiber, concrete, gypsum, porous rock, and mixtures thereof. Particulate additions such as aluminum or graphite powders, as well as metal and carbon fibers can also be incorporated therein. Particulate and/or fibrous additions can be introduced into molten phase change materials which can then be cast into various shapes. After the phase change materials have solidified, the additions will remain dispersed throughout the matrix of the cast solid. The polyol is in contact with at least one material selected from the group consisting of metals, carbon, siliceous, plastic, cellulosic, natural fiber, artificial fiber, concrete, gypsum, and mixtures thereof.

  9. Aircraft Recirculation Filter for Air-Quality and Incident Assessment

    Science.gov (United States)

    Eckels, Steven J.; Jones, Byron; Mann, Garrett; Mohan, Krishnan R.; Weisel, Clifford P.

    2015-01-01

    The current research examines the possibility of using recirculation filters from aircraft to document the nature of air-quality incidents on aircraft. These filters are highly effective at collecting solid and liquid particulates. Identification of engine oil contaminants arriving through the bleed air system on the filter was chosen as the initial focus. A two-step study was undertaken. First, a compressor/bleed air simulator was developed to simulate an engine oil leak, and samples were analyzed with gas chromatograph-mass spectrometry. These samples provided a concrete link between tricresyl phosphates and a homologous series of synthetic pentaerythritol esters from oil and contaminants found on the sample paper. The second step was to test 184 used aircraft filters with the same gas chromatograph-mass spectrometry system; of that total, 107 were standard filters, and 77 were nonstandard. Four of the standard filters had both markers for oil, with the homologous series synthetic pentaerythritol esters being the less common marker. It was also found that 90% of the filters had some detectable level of tricresyl phosphates. Of the 77 nonstandard filters, 30 had both markers for oil, a significantly higher percent than the standard filters. PMID:25641977

  10. Aircraft Recirculation Filter for Air-Quality and Incident Assessment.

    Science.gov (United States)

    Eckels, Steven J; Jones, Byron; Mann, Garrett; Mohan, Krishnan R; Weisel, Clifford P

    The current research examines the possibility of using recirculation filters from aircraft to document the nature of air-quality incidents on aircraft. These filters are highly effective at collecting solid and liquid particulates. Identification of engine oil contaminants arriving through the bleed air system on the filter was chosen as the initial focus. A two-step study was undertaken. First, a compressor/bleed air simulator was developed to simulate an engine oil leak, and samples were analyzed with gas chromatograph-mass spectrometry. These samples provided a concrete link between tricresyl phosphates and a homologous series of synthetic pentaerythritol esters from oil and contaminants found on the sample paper. The second step was to test 184 used aircraft filters with the same gas chromatograph-mass spectrometry system; of that total, 107 were standard filters, and 77 were nonstandard. Four of the standard filters had both markers for oil, with the homologous series synthetic pentaerythritol esters being the less common marker. It was also found that 90% of the filters had some detectable level of tricresyl phosphates. Of the 77 nonstandard filters, 30 had both markers for oil, a significantly higher percent than the standard filters.

  11. TUNG OIL BASED MONOMER FOR THERMOSETTING POLYMERS: SYNTHESIS, CHARACTERIZATION AND COPOLYMERIZATION WITH STYRENE

    Directory of Open Access Journals (Sweden)

    Chengguo Liu,

    2011-11-01

    Full Text Available A tung oil (TO based monomer for rigid thermosetting polymer was synthesized, characterized, and copolymerized with styrene in this study. Tung oil was alcoholyzed with pentaerythritol (PER to get tung oil pentaerythritol alcoholysis products (TOPER, and the optimized conditions were explored according to the yields of TOPER analyzed by gas chromatography-mass spectrometry (GC-MS. The resulting alcoholysis products were maleinated to form tung oil maleate half ester (TOPERMA, and the reaction conditions were determined by monitoring the reaction extents of TOPER and maleic anhydride (MA with 1HNMR spectroscopy. The TO alcoholysis and maleinization reaction products were characterized by IR, 1HNMR, and electrospray ionization-mass spectrometry (ESI-MS techniques. At last, the TOPERMA mixture was cured with styrene (St, and the initiator tert-butyl peroxy benzoate (TPB. Differential scanning calorimetry (DSC was employed to characterize the curing process. Mechanical properties of the cured TOPERMA/St resin further confirmed the best procedure for the maleinization reaction. The loading of TO reached about 30% weight of the resulting thermosetting polymer. This promising material from renewable resources can be a potential substitution for petroleum products when used as sheet molding compounds.

  12. Highly Branched Bio-Based Unsaturated Polyesters by Enzymatic Polymerization

    Directory of Open Access Journals (Sweden)

    Hiep Dinh Nguyen

    2016-10-01

    Full Text Available A one-pot, enzyme-catalyzed bulk polymerization method for direct production of highly branched polyesters has been developed as an alternative to currently used industrial procedures. Bio-based feed components in the form of glycerol, pentaerythritol, azelaic acid, and tall oil fatty acid (TOFA were polymerized using an immobilized Candida antarctica lipase B (CALB and the potential for an enzymatic synthesis of alkyds was investigated. The developed method enables the use of both glycerol and also pentaerythritol (for the first time as the alcohol source and was found to be very robust. This allows simple variations in the molar mass and structure of the polyester without premature gelation, thus enabling easy tailoring of the branched polyester structure. The postpolymerization crosslinking of the polyesters illustrates their potential as binders in alkyds. The formed films had good UV stability, very high water contact angles of up to 141° and a glass transition temperature that could be controlled through the feed composition.

  13. Rocket Solid Propellant Alternative Based on Ammonium Dinitramide

    Directory of Open Access Journals (Sweden)

    Grigore CICAN

    2017-03-01

    Full Text Available Due to the continuous run for a green environment the current article proposes a new type of solid propellant based on the fairly new synthesized oxidizer, ammonium dinitramide (ADN. Apart of having a higher specific impulse than the worldwide renowned oxidizer, ammonium perchlorate, ADN has the advantage, of leaving behind only nitrogen, oxygen and water after decomposing at high temperatures and therefore totally avoiding the formation of hydrogen chloride fumes. Based on the oxidizer to fuel ratios of the current formulations of the major rocket solid booster (e.g. Space Shuttle’s SRB, Ariane 5’s SRB which comprises mass variations of ammonium perchlorate oxidizer (70-75%, atomized aluminum powder (10-18% and polybutadiene binder (12-20% a new solid propellant was formulated. As previously stated, the new propellant formula and its variations use ADN as oxidizer and erythritol tetranitrate as fuel, keeping the same polybutadiene as binder.

  14. Experimental Studies on Improved Plastic Bonded Explosives Materials (PBXs for Controlled Fragmentation Warheads

    Directory of Open Access Journals (Sweden)

    Elsharkawy Karim

    2017-01-01

    Full Text Available This paper describes formulations of plastic bonded explosives (PBXs based on three highly brisant explosives, namely 1,3,5-trinitro-1,3,5-triazinane (RDX, 1,3,5,7-tetranitro-1,3,5,7-tetrazocane (HMX and pentaerythritoltetranitrate (PETN with polyurethane (PU based on Glycidyl azide polymer (GAP as an energetic binder in comparison with composition-B, which used in the fragmentation warheads. The sensitivity and performance properties of different types of PBXs were evaluated by experimental results of prepared selected PBX compositions. Casting technique was used to prepare the selected compositions containing 14% PU based on GAP. It has been observed that the brisance of the PBX based on HMX was higher than that of comp-B by 21.3 %, the detonation velocity showed a remarkable increase of the order of 8480 (m/s while that of comp-B was 7638 (m/s. A controlled fragmentation warhead with an outer grooving warhead case of dimensions 100x35x4 mm was used and arena test was carried out to determine the lethal zone of the fragmentation warhead. The lethal zone obtained from arena test for PBX composition based on HMX named PBXHG4 was higher than that based on RDX or PETN, and than that of comp-B by 40%.

  15. Integrated Data Collection Analysis (IDCA) Program — KClO3 (as received)/Icing Sugar

    Energy Technology Data Exchange (ETDEWEB)

    Sandstrom, Mary M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Geoffrey W. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Preston, Daniel N. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Pollard, Colin J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Warner, Kirstin F. [Naval Surface Warfare Center (NSWC IHD), Indian Head, MD (United States). Indian Head Division; Sorenson, Daniel N. [Naval Surface Warfare Center (NSWC IHD), Indian Head, MD (United States). Indian Head Division; Remmers, Daniel L. [Naval Surface Warfare Center (NSWC IHD), Indian Head, MD (United States). Indian Head Division; Shelley, Timothy J. [Air Force Research Lab. (AFRL/RXQL), Tyndall AFB, FL (United States); Reyes, Jose A. [Applied Research Associates, Inc., Tyndall AFB, FL (United States); Hsu, Peter C. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Whipple, Richard E. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Reynolds, John G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2011-05-23

    The Integrated Data Collection Analysis (IDCA) program is conducting a proficiency study for Small-Scale Safety and Thermal (SSST) testing of homemade explosives (HMEs). Described here are the results for impact, friction, electrostatic discharge, and differential scanning calorimetry analysis of a mixture of KClO3 as received from the manufacturer mixed with icing sugar, sized through a 100-mesh sieve—KClO3/icing sugar (AR) mixture. This material was selected because of the challenge of performing SSST testing of a mixture of two solid materials. The mixture was found to: 1) be more sensitive to impact than RDX, similar to PETN, 2) be the same or less sensitive to friction than PETN, and 3) to be less sensitive to spark than RDX. The thermal analysis showed that the mixture has thermally stability similar to RDX and is perhaps more energetic upon decomposition but variable results indicate sampling issues. Compared to the 100-mesh sieved counter part, the KClO3/icing sugar (-100) mixture, the AR mixture was found to be about the same sensitivity towards impact, friction and ESD.

  16. New Mix Explosives for Explosive Welding

    Science.gov (United States)

    Andreevskikh, Leonid

    2011-06-01

    Suggested and tested were some mix explosives--powder mixtures of a brisant high explosive (HE = RDX, PETN) and an inert diluent (baking soda)--for use in explosive welding. RDX and PETN were selected in view of their high throwing ability and low critical diameter. Since the decomposition of baking soda yields a huge amount of gaseous products, its presence ensures (even at a low HE percentage) a throwing speed that is sufficient for realization of explosive welding, at a reduced brisant action of charge. Mix chargers containing 30-70 wt % HE (the rest baking soda) have been tested experimentally and optimized. For study of possibility to reduce critical diameter of HE mixture, the mixture was prepared where HE crystal sizes did not exceed 10 μm. The tests, which were performed with this HE, revealed that the mixture detonated stably with the velocity D ~ 2 km/s, if the layer thickness was d = 2 mm. The above explosives afford to markedly diminish deformations within the oblique impact zone and thus to carry out explosive welding of hollow items and thin metallic foils.

  17. Fizičko-hemijske i detonacione karakteristike nitraminskih eksploziva - RDX, HMX i CL-20 / Physico-chemical and detonation properties of nitramine explosives: RDX, HMX and CL-20

    Directory of Open Access Journals (Sweden)

    Mirjana Anđelković-Lukić

    2002-11-01

    Full Text Available U radu su prikazane fizičko-hemijske i detonacione karakteristike nitraminskih brizantnih eksploziva, heksogena i oktogena, uporedene sa osobinama novog cikličnog nitraminskog eksploziva CL-20. Novi visokobrizantni eksploziv CL-20 postoji u četiri kristalne forme, stabilne na različitim temepraturama. Ima bolje detonacione karakteristike od heksogena i oktogena veću gustinu i brzinu detonacije, all mnogo veću osetljivost na udar i trenje, reda PETN. Zbog toga se ovaj eksploziv flegmatizuje sa polimerima etilenvinilacetatom (EVA i estanom. Da bi se povećale energetske performanse eksploziva i smanjila osetljivost na mehanička dejstva eksplozivu CL-20 dodaju se visokoenergetski materijali, fluoronitrojedinjenja (FEFO. / In this paper the physico-chemical and detonation properties of nitramine high explosives, hexogen and octogen, are presented and compared with a polycyclic nitramine high explosive CL-20. This new high explosive CL-20 exists in four crystalline forms, stable at different temperatures. CL-20 has better detonation properties than hexogen and octogen, higher density and detonation rate, but greater impact and friction sensitivity (of PETN class. So it is necessary to bond this explosive with polymers-ethylenvinil acetat (EVA and estane to reduce sensitivity to mechanical effects. CL-20 can be prepared by adding high energy materials-fluoro-nitro compounds (FEFO as regulators of energy performances.

  18. Molten salt destruction as an alternative to open burning of energetic material wastes

    International Nuclear Information System (INIS)

    Upadhye, R.S.; Watkins, B.E.; Pruneda, C.O.; Brummond, W.A.

    1994-01-01

    LLNL has built a small-scale (about 1 kg/hr throughput unit to test the destruction of energetic materials using the Molten Salt Destruction (MSD) process. We have modified the unit described in the earlier references to inject energetic waste material continuously into the unit. In addition to the HMX, other explosives we have destroyed include RDX, PETN, ammonium picrate, TNT, nitroguanadine, and TATB. We have also destroyed a liquid gun propellant comprising hydroxyl ammonium nitrate, triethanolammonium nitrate and water. In addition to these pure components, we have destroyed a number of commonly used formulations, such as LX-10 (HMX/Viton), LX-16 (PETN/FPC461, LX-17 (TATB/Kel F), and PBX-9404 (HMX)/CEF/Nitro cellulose). Our experiments have demonstrated that energetic materials can be safely and effectively treated by MSD.We have also investigated the issue of steam explosions in molten salt units, both experimentally and theoretically, and concluded that steam explosions can be avoided under proper design and operating conditions. We are currently building a larger unit (nominal capacity 5 kg/hr,) to investigate the relationship between residence time, temperature, feed concentration and throughputs, avoidance of back-burn, a;nd determination of the products of combustion under different operating conditions

  19. A novel plasmid-encoded serotype conversion mechanism through addition of phosphoethanolamine to the O-antigen of Shigella flexneri.

    Directory of Open Access Journals (Sweden)

    Qiangzheng Sun

    Full Text Available Shigella flexneri is the major pathogen causing bacillary dysentery in developing countries. S. flexneri is divided into at least 16 serotypes based on the combination of antigenic determinants present in the O-antigen. All the serotypes (except for serotype 6 share a basic O-unit containing one N-acetyl-d-glucosamine and three l-rhamnose residues, whereas differences between the serotypes are conferred by phage-encoded glucosylation and/or O-acetylation. Serotype Xv is a newly emerged and the most prevalent serotype in China, which can agglutinate with both MASF IV-1 and 7,8 monoclonal antibodies. The factor responsible for the presence of MASF IV-1 (E1037 epitope has not yet been identified. In this study, we analyzed the LPS structure of serotype Xv strains and found that the MASF IV-1 positive phenotype depends on an O-antigen modification with a phosphoethanolamine (PEtN group attached at position 3 of one of the rhamnose residues. A plasmid carried gene, lpt-O (LPS phosphoethanolamine transferase for O-antigen, mediates the addition of PEtN for serotype Xv and other MASF IV-1 positive strains. These findings reveal a novel serotype conversion mechanism in S. flexneri and show the necessity of further extension of the serotype classification scheme recognizing the MASF IV-1 positive strains as distinctive subtypes.

  20. New lipid family that forms inverted cubic phases in equilibrium with excess water: molecular structure-aqueous phase structure relationship for lipids with 5,9,13,17-tetramethyloctadecyl and 5,9,13,17-tetramethyloctadecanoyl chains.

    Science.gov (United States)

    Yamashita, Jun; Shiono, Manzo; Hato, Masakatsu

    2008-10-02

    With a view to discovering a new family of lipids that form inverted cubic phases, the aqueous phase behavior of a series of lipids with isoprenoid-type hydrophobic chains has been examined over a temperature range from -40 to 65 degrees C by using optical microscopy, DSC (differential scanning calorimetry), and SAXS (small-angle X-ray scattering) techniques. The lipids examined are those with 5,9,13,17-tetramethyloctadecyl and 5,9,13,17-tetramethyloctadecanoyl chains linked to a series of headgroups, that is, erythritol, pentaerythritol, xylose, and glucose. All of the lipid/water systems displayed a "water + liquid crystalline phase" two-phase coexistence state when sufficiently diluted. The aqueous phase structures of the most diluted liquid crystalline phases in equilibrium with excess water depend both on the lipid molecular structure and on the temperature. Given an isoprenoid chain, the preferred phase consistently follows a phase sequence of an H II (an inverted hexagonal phase) to a Q II (an inverted bicontinuous cubic phase) to an L alpha (a lamellar phase) as A* (cross-section area of the headgroup) increases. For a given lipid/water system, the phase sequence observed as the temperature increases is L alpha to Q II to H II. The present study allowed us to find four cubic phase-forming lipid species, PEOC 18+4 [mono- O-(5,9,13,17-tetramethyloctadecyl)pentaerythritol], beta-XylOC 18+4 [1- O-(5,9,13,17-tetramethyloctadecyl)-beta- d-xylopyranoside], EROCOC 17+4 [1- O-(5,9,13,17-tetramethyloctadecanoyl)erythritol], and PEOCOC 17+4 [mono- O-(5,9,13,17-tetramethyloctadecanoyl)pentaerythritol]. The values of T K (hydrated solid-liquid crystalline phase transition temperature) of the cubic phase-forming lipids are all below 0 degrees C. Quantitative analyses of the lipid molecular structure-aqueous phase structure relationship in terms of the experimentally evaluated "surfactant parameter" allow us to rationally select an optimum combination of hydrophilic

  1. Integrated Data Collection Analysis (IDCA) program--KClO4/Dodecane Mixture

    Energy Technology Data Exchange (ETDEWEB)

    Sandstrom, Mary M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Geoffrey W. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Preston, Daniel N. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Pollard, Colin J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Warner, Kirstin F. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Sorensen, Daniel N. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Remmers, Daniel L. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Shelley, Timothy J. [Air Force Research Lab. (AFRL), Tyndall AFB, FL (United States); Reyes, Jose A. [Applied Research Associates, Tyndall AFB, FL (United States); Hsu, Peter C. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Reynolds, John G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2012-05-11

    The Integrated Data Collection Analysis (IDCA) program is conducting a proficiency study for Small- Scale Safety and Thermal (SSST) testing of homemade explosives (HMEs). Described here are the results for impact, friction, electrostatic discharge, and differential scanning calorimetry analysis of a mixture of KClO4 and dodecane—KClO4/dodecane mixture. This material was selected because of the challenge of performing SSST testing of a mixture of solid and liquid materials. The mixture was found to: 1) be less sensitive to impact than RDX, and PETN, 2) less sensitive to friction than RDX and PETN, and 3) less sensitive to spark than RDX and PETN. The thermal analysis showed little or no exothermic features suggesting that the dodecane volatilized at low temperatures. A prominent endothermic feature was observed and assigned to a phase transition of KClO4. This effort, funded by the Department of Homeland Security (DHS), ultimately will put the issues of safe handling of these materials in perspective with standard military explosives. The study is adding SSST testing results for a broad suite of different HMEs to the literature. Ultimately the study has the potential to suggest new guidelines and methods and possibly establish the SSST testing accuracies needed to develop safe handling practices for HMEs. Each participating testing laboratory uses identical test materials and preparation methods wherever possible. Note, however, the test procedures differ among the laboratories. The results are compared among the laboratories and then compared to historical data from various sources. The testing performers involved for the KClO4/dodecane mixture are Lawrence Livermore National Laboratory (LLNL), Los Alamos National Laboratory (LANL), Indian Head Division, Naval Surface Warfare Center, (NSWC IHD), and Air Force Research Laboratory (AFRL/RXQL). These tests are conducted as a proficiency study in order to establish some

  2. Solid state phase change materials for thermal energy storage in passive solar heated buildings

    Science.gov (United States)

    Benson, D. K.; Christensen, C.

    1983-11-01

    A set of solid state phase change materials was evaluated for possible use in passive solar thermal energy storage systems. The most promising materials are organic solid solutions of pentaerythritol, pentaglycerine and neopentyl glycol. Solid solution mixtures of these compounds can be tailored so that they exhibit solid-to-solid phase transformations at any desired temperature within the range from less than 25 deg to 188 deg. Thermophysical properties such as thermal conductivity, density and volumetric expansion were measured. Computer simulations were used to predict the performance of various Trombe wall designs incorporating solid state phase change materials. Optimum performance was found to be sensitive to the choice of phase change temperatures and to the thermal conductivity of the phase change material. A molecular mechanism of the solid state phase transition is proposed and supported by infrared spectroscopic evidence.

  3. Unusual concentration-dependent microscopic dynamics of dendrimers in aqueous solution

    International Nuclear Information System (INIS)

    Wong, Kaikin; Wu, Chin Ming; Lam, Hak Fai; Chathoth, Suresh M.

    2016-01-01

    Dendrimers are novel three-dimensional, hyperbranched globular nanopolymeric macromolecules. The nanoscopic size, narrow polydispersity index, excellent control over molecular structure, availability of multiple functional groups at the periphery, and cavities in the interior made them very attractive candidate for drug delivery. In this communication, we have studied the microscopic dynamics of tetra-acid and pentaerythritol glycidyl ether dendrimers dissolved in aqueous solution with different concentrations. The effects of concentration and temperature to their long-range diffusion process are investigated by dynamic light scattering. Experimental results show a huge variation in the translational diffusion coefficient for the two dendrimers samples. Besides, the dependence of diffusion coefficients on concentration is unusually different in these dendrimer samples. Although the diffusion process follows Arrhenius relation with the temperature in both systems, the activation energy for the diffusion process has a distinct concentration dependence.

  4. Unusual concentration-dependent microscopic dynamics of dendrimers in aqueous solution

    Science.gov (United States)

    Wong, Kaikin; Wu, Chin Ming; Lam, Hak Fai; Chathoth, Suresh M.

    2016-05-01

    Dendrimers are novel three-dimensional, hyperbranched globular nanopolymeric macromolecules. The nanoscopic size, narrow polydispersity index, excellent control over molecular structure, availability of multiple functional groups at the periphery, and cavities in the interior made them very attractive candidate for drug delivery. In this communication, we have studied the microscopic dynamics of tetra-acid and pentaerythritol glycidyl ether dendrimers dissolved in aqueous solution with different concentrations. The effects of concentration and temperature to their long-range diffusion process are investigated by dynamic light scattering. Experimental results show a huge variation in the translational diffusion coefficient for the two dendrimers samples. Besides, the dependence of diffusion coefficients on concentration is unusually different in these dendrimer samples. Although the diffusion process follows Arrhenius relation with the temperature in both systems, the activation energy for the diffusion process has a distinct concentration dependence.

  5. Synthesis and Characterization of Optically Active Fractal Seed Mediated Silver Nickel Bimetallic Nanoparticles

    Directory of Open Access Journals (Sweden)

    Joseph Adeyemi Adekoya

    2014-01-01

    Full Text Available The synthesis of new seed mediated AgNi allied bimetallic nanocomposites was successfully carried out by the successive reduction of the metal ions in diethylene glycol, ethylene glycol, glycerol, and pentaerythritol solutions, with concomitant precipitation of Ag/Ni bimetal sols. The optical measurement revealed the existence of distinct band edge with surface plasmon resonance (SPR in the region of 400–425 nm and excitonic emission with maximum peak at 382 nm which were reminiscent of cluster-in-cluster surface enriched bimetallic silver-nickel sols. The morphological characterization by transmission electron microscopy, high resolution transmission electron microscopy, and X-ray diffraction analyses complimented by surface scan using X-ray photoelectron spectroscopy strongly supported the formation of intimately alloyed face-centered silver/nickel nanoclusters.

  6. Development and characterization of rosin-based polymer and its application as a cream base.

    Science.gov (United States)

    Dhanorkar, V T; Gawande, R S; Gogte, B B; Dorle, A K

    2002-01-01

    The literature contains many references to the wide range of uses of rosin-based polymers, but little has appeared in the area of rosin-based polymers used as cream bases. Various rosin polymers based on glycerol, sorbitol, and pentaerythritol were prepared and screened for efficacy as cream bases. Among these polymers, polymer 2 (glycerol-based) is reported in the present study as it produced creams with a better stability and release profile as compared to other creams. The creams were formulated employing polymer 2 (P2) and Tween 60 as surfactants. The stability of the prepared creams, as well as the diclofenac diethylammonium release pattern, was investigated using particle size analysis, conductivity, relative dielectric constant, spreadability, and irritation potential measurement, and was compared with that of creams containing Tween 60 (RT) prepared in the laboratory. The release of the drug, diclofenac diethylammonium, was measured after eight hours and compared with a standard cream (RT) and a marketed cream (RM).

  7. Unusual concentration-dependent microscopic dynamics of dendrimers in aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Wong, Kaikin; Wu, Chin Ming; Lam, Hak Fai; Chathoth, Suresh M., E-mail: smavilac@cityu.edu.hk [City University of Hong Kong, Department of Physics and Materials Science (Hong Kong, People’s Republic of China) (China)

    2016-05-15

    Dendrimers are novel three-dimensional, hyperbranched globular nanopolymeric macromolecules. The nanoscopic size, narrow polydispersity index, excellent control over molecular structure, availability of multiple functional groups at the periphery, and cavities in the interior made them very attractive candidate for drug delivery. In this communication, we have studied the microscopic dynamics of tetra-acid and pentaerythritol glycidyl ether dendrimers dissolved in aqueous solution with different concentrations. The effects of concentration and temperature to their long-range diffusion process are investigated by dynamic light scattering. Experimental results show a huge variation in the translational diffusion coefficient for the two dendrimers samples. Besides, the dependence of diffusion coefficients on concentration is unusually different in these dendrimer samples. Although the diffusion process follows Arrhenius relation with the temperature in both systems, the activation energy for the diffusion process has a distinct concentration dependence.

  8. Inorganic-Organic Thiol-ene Coated Mesh for Oil/Water Separation.

    Science.gov (United States)

    Chen, Qiyi; de Leon, Al; Advincula, Rigoberto C

    2015-08-26

    A highly efficient mesh for oil/water separation was fabricated by using a superhydrophobic and superoleophilic coating of thiol-ene hybrid, consisting of pentaerythritol tetra(3-mercaptopropionate) (PETMP), 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane (TMTVSi), and hydrophobic fumed silica nanoparticles, via a simple two-step fabrication process. Spray deposition and UV curing photopolymerization were sequentially performed, during which solvent evaporation provides microscale roughness while nanoparticle aggregation forms nanoscale roughness. The hierarchical morphologies were stabilized after UV curing photopolymerization. High contact angle (>150°) and low roll-off angle (<5°) were achieved due to the multiscale roughness structure of the hierarchical morphologies. These coatings also have excellent chemical resistance, as well as temperature and pH stability, after curing.

  9. Development of a ten inch manipulators-based, flexible, broadband two-crystal spectrometer

    Energy Technology Data Exchange (ETDEWEB)

    Steel, A. B., E-mail: steel1@llnl.gov; Dunn, J.; Emig, J.; Beiersdorfer, P.; Brown, G. V.; Shepherd, R.; Marley, E. V. [Lawrence Livermore National Laboratory, Livermore, California 94550 (United States); Hoarty, D. J. [Atomic Weapons Establishment, Aldermaston (United Kingdom)

    2014-11-15

    We have developed and implemented a broadband X-ray spectrometer with a variable energy range for use at the Atomic Weapons Establishment's Orion Laser. The spectrometer covers an energy bandwidth of ∼1–2 keV using two independently mounted, movable Bragg diffraction crystals. Using combinations of cesium hydrogen pthlate, ammonium dihydrogen phosphate, and pentaerythritol crystals, spectra covering the 1.4–2.5, 1.85–3.15, or 3.55–5.1 keV energy bands have been measured. Image plate is used for detection owing to its high dynamic range. Background signals caused by high energy X-rays and particles commonly produced in high energy laser experiments are reduced by a series of tantalum baffles and filters installed between the source and crystal and also between the crystals and detector.

  10. Development of a ten inch manipulators-based, flexible, broadband two-crystal spectrometer

    International Nuclear Information System (INIS)

    Steel, A. B.; Dunn, J.; Emig, J.; Beiersdorfer, P.; Brown, G. V.; Shepherd, R.; Marley, E. V.; Hoarty, D. J.

    2014-01-01

    We have developed and implemented a broadband X-ray spectrometer with a variable energy range for use at the Atomic Weapons Establishment's Orion Laser. The spectrometer covers an energy bandwidth of ∼1–2 keV using two independently mounted, movable Bragg diffraction crystals. Using combinations of cesium hydrogen pthlate, ammonium dihydrogen phosphate, and pentaerythritol crystals, spectra covering the 1.4–2.5, 1.85–3.15, or 3.55–5.1 keV energy bands have been measured. Image plate is used for detection owing to its high dynamic range. Background signals caused by high energy X-rays and particles commonly produced in high energy laser experiments are reduced by a series of tantalum baffles and filters installed between the source and crystal and also between the crystals and detector

  11. Poliuretanos obtenidos a partir de aceite de higuerilla modificado y poli-isocianatos de lisina: síntesis, propiedades mecánicas y térmicas y degradación in vitro

    Directory of Open Access Journals (Sweden)

    Manuel F. Valero

    2014-01-01

    Full Text Available Biodegradable polyurethanes (PUR were prepared from polyols derived from castor oil by transesterification of pentaerythritol-modified castor oil and lysine polyisocyanates (LDI and LTI. The polyurethanes obtained were characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis (TGA, and dynamic mechanical thermal analysis (DMTA. The mechanical behavior of the polyurethanes was measured by Shore A hardness and tensile testing (stress-strain curves. The biodegradable nature of the material was determined by contact angle, water absorption tests, and in vitro degradation in PBS solution. This study aims to examine the effect of the structure and functionality of diisocyanate on the mechanical properties and in vitro degradation of the material. The results were compared with homologous materials obtained from isophorone diisocyanate (IPDI used in previous works. The objective was to evaluate candidate materials that can be potentially used in tissue engineering.

  12. Superhydrophobic hybrid inorganic-organic thiol-ene surfaces fabricated via spray-deposition and photopolymerization.

    Science.gov (United States)

    Sparks, Bradley J; Hoff, Ethan F T; Xiong, Li; Goetz, James T; Patton, Derek L

    2013-03-13

    We report a simple and versatile method for the fabrication of superhydrophobic inorganic-organic thiol-ene coatings via sequential spray-deposition and photopolymerization under ambient conditions. The coatings are obtained by spray-deposition of UV-curable hybrid inorganic-organic thiol-ene resins consisting of pentaerythritol tetra(3-mercaptopropionate) (PETMP), triallyl isocyanurate (TTT), 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane (TMTVSi), and hydrophobic fumed silica nanoparticles. The spray-deposition process and nanoparticle agglomeration/dispersion provide surfaces with hierarchical morphologies exhibiting both micro- and nanoscale roughness. The wetting behavior, dependent on the concentration of TMTVSi and hydrophobic silica nanoparticles, can be varied over a broad range to ultimately provide coatings with high static water contact angles (>150°), low contact angle hysteresis, and low roll off angles (spray-deposition and UV-cure process on a variety of substrate surfaces including glass, paper, stone, and cotton fabric.

  13. Fireproofing and heat insulating performance improvement of EG/ATH modified intumescent flame retardant coating treated under Co-60 radiation

    Science.gov (United States)

    Zhang, Yuehong; Luan, Weiling; Jiang, Tao

    2017-12-01

    New intumescent flame retardant (IFR) coatings with different fire retardants were prepared in this paper. Expandable graphite (EG) and Aluminium hydroxide (ATH) were respectively added into the conventional IFR coating system, which included ammonium polyphosphate (APP) / pentaerythritol (PER) / melamine (MEL). The fireproofing time and heat insulating properties of the additives acted as fire retardants were investigated via thermogravimetry analysis (TGA) and fire resistance test of homemade big panel test. The morphology of the char layer structure was achieved by scanning electron microscopy (SEM). The highlight of the paper was that the coating samples were pretreated under Co-60 radiation. The influence of radiation on the fire resistance time and char layer height was investigated. The results showed that the prepared IFR coatings can be used in Co-60 radiation for more than 90 min when encountering fire. It would be a reference for radiation shielding in nuclear environment.

  14. Effect of mixing mode and emulsifying agents on micro/nanoencapsulation of low viscosity self-healing agents in polymethyl methacrylate shell

    Science.gov (United States)

    Ahangaran, Fatemeh; Navarchian, Amir H.; Hayaty, Mehran; Esmailpour, Karim

    2016-09-01

    In this study, epoxy prepolymer (EC 157) and pentaerythritol tetrakis (3-mercaptopropionate) (PETMP) as hardener were encapsulated separately in polymethyl methacrylate (PMMA) shells through an internal phase separation method. Chemical structures, morphologies, and thermal properties of healing agent micro/nanocapsules were characterized by Fourier transform infrared (FT-IR) spectroscopy, field emission scanning electron microscopy (FESEM), and thermal gravimetric analysis (TGA) respectively. The effects of encapsulation processing conditions such as mechanical mixing rate, ultrasonication, emulsifier type, and co-emulsifier concentration on encapsulation yield, capsule mean diameter and core content were studied using the Taguchi experimental design approach. The results indicated that the main significant factors affecting the yield of encapsulation are emulsifier type and ultrasonication. The most important factors which affect the mean diameter of capsules are emulsifier type and mechanical mixing rate. The core content was influenced by ultrasonication and mechanical mixing rate. The relative optimum condition of encapsulation was also determined using overall evaluation criteria.

  15. The sensitizing capacity of multifunctional acrylates in the guinea pig.

    Science.gov (United States)

    Björkner, B

    1984-10-01

    The multifunctional acrylates used in ultraviolet (UV) curable resins act as cross-linkers and "diluents". They are usually based on di(meth)acrylate esters of dialcohols or tri- and tetra-acrylate esters of polyalcohols. In UV-curable coatings, the most commonly used are pentaerythritol triacrylate (PETA), trimethylolpropane triacrylate (TMPTA) and 1,6-hexanediol diacrylate (HDDA). In other uses, such as dental composite resin materials, the dimethacrylic monomers based on n-ethylene glycol are the most useful. The sensitizing capacity of various multifunctional acrylates and their cross-reactivity pattern have been investigated with the guinea pig maximization test. The tests show that BUDA (1,4-butanediol diacrylate) and HDDA are moderate to strong sensitizers and that they probably cross-react with each other. The n-ethylene glycol diacrylates and methacrylates tested are weak or non-sensitizers. Tripropylene glycol diacrylate (TPGDA) is a moderate and neopentyl glycol diacrylate (NPGDA) a strong sensitizer, whereas neopentyl glycol dimethacrylate is a non-sensitizer. The commercial PETA is a mixture of pentaerythritol tri- and tetra-acrylate (PETA-3 and PETA-4). PETA-3 is a much stronger sensitizer than PETA-4. Simultaneous reactions were seen between PETA-3, PETA-4 and TMPTA. The oligotriacrylate OTA 480 is a moderate sensitizer, but no concomitant reactions were seen with PETA-3, PETA-4 or TMPTA. Of the multifunctional acrylates tested, the di- and triacrylic compounds should be regarded as potent sensitizers. The methacrylated multifunctional acrylic compounds are weak or non-sensitizers.

  16. Amino acid-incorporated polymer network by thiol-ene polymerization

    Directory of Open Access Journals (Sweden)

    R. Yokose

    2015-08-01

    Full Text Available Triallyl L-alanine (A3A and triallyl L-phenylalanine (A3F were synthesized by reactions of L-alanine and L-phenylalanine with allyl bromide in the presence of sodium hydroxide, respectively. Thiol-ene thermal polymerization of A3A or A3F with pentaerythritol-based primary tetrathiol (pS4P or pentaerythritol-based secondary tetrathiol (S4P at allyl/SH 1/1 in the presence of 2,2'-azobis(isobutyronitrile produced an amino acid-incorporated polymer network (A3ApS4P, A3A-S4P or A3F-S4P. Although the thermally cured resins were homogeneous and flat films, the corresponding thiol-ene photopolymerization did not give a successful result. Degree of swelling for each thermally cured film in N,Ndimethylformamide was much higher than that in water. The glass transition and 5% weight loss temperatures (Tg and T5 of A3F-pS4P and A3F-S4P were higher than those of A3A-pS4P and A3A-S4P, respectively. Also, A3F-pS4P and A3F-S4P exhibited much higher tensile strengths and moduli than A3A-pS4P and A3A-S4P did, respectively. Consequently, A3FpS4P displayed the highest Tg (38.7°C, T5 (282.0°C, tensile strength (9.5 MPa and modulus (406 MPa among all the thermally cured resins.

  17. Boron doped diamond synthesized from detonation nanodiamond in a C-O-H fluid at high pressure and high temperature

    Science.gov (United States)

    Shakhov, Fedor M.; Abyzov, Andrey M.; Takai, Kazuyuki

    2017-12-01

    Boron doped diamond (BDD) was synthesized under high pressure and high temperature (HPHT) of 7 GPa, 1230 °C in a short time of 10 s from a powder mixtures of detonation nanodiamond (DND), pentaerythritol C5H8(OH)4 and amorphous boron. SEM, TEM, XRD, XPS, FTIR and Raman spectroscopy indicated that BDD nano- and micro-crystals have formed by consolidation of DND particles (4 nm in size). XRD showed the enlargement of crystallites size to 6-80 nm and the increase in diamond lattice parameter by 0.02-0.07% without appearance of any microstrains. Raman spectroscopy was used to estimate the content of boron atoms embedded in the diamond lattice. It was found that the Raman diamond peak shifts significantly from 1332 cm-1 to 1290 cm-1 without appearance of any non-diamond carbon. The correlation between Raman peak position, its width, and boron content in diamond is proposed. Hydrogenated diamond carbon in significant amount was detected by IR spectroscopy and XPS. Due to the doping with boron content of about 0.1 at%, the electrical conductivity of the diamond achieved approximately 0.2 Ω-1 cm-1. Reaction mechanism of diamond growth (models of recrystallization and oriented attachment) is discussed, including the initial stages of pentaerythritol pyrolysis and thermal desorption of functional groups from the surface of DND particles with the generation of supercritical fluid of low-molecular substances (H2O, CH4, CO, CO2, etc.), as well as byproducts formation (B2O3, B4C).

  18. Integrated Data Collection Analysis (IDCA) Program — Ammonium Nitrate

    Energy Technology Data Exchange (ETDEWEB)

    Sandstrom, Mary M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Geoffrey W. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Preston, Daniel N. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Pollard, Colin J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Warner, Kirstin F. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Sorensen, Daniel N. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Remmers, Daniel L. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Phillips, Jason J. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Shelley, Timothy J. [Bureau of Alcohol, Tobacco and Firearms, Redstone Arsenal, AL (United States); Reyes, Jose A. [Applied Research Associates, Tyndall AFB, FL (United States); Hsu, Peter C. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Reynolds, John G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2013-05-17

    The Integrated Data Collection Analysis (IDCA) program is conducting a proficiency study for Small- Scale Safety and Thermal (SSST) testing of homemade explosives (HMEs). Described here are the results for impact, friction, electrostatic discharge, and differential scanning calorimetry analysis of ammonium nitrate (AN). AN was tested, in most cases, as both received from manufacturer and dried/sieved. The participants found the AN to be: 1) insensitive in Type 12A impact testing (although with a wide range of values), 2) completely insensitive in BAM friction testing, 3) less sensitive than the RDX standard in ABL friction testing, 4) less sensitive than RDX in ABL ESD testing, and 5) less sensitive than RDX and PETN in DSC thermal analyses.

  19. Computations on Internal Blast from Titanium-Cased Charges in Air

    Science.gov (United States)

    1984-07-01

    formation and considerable temperature- dependent polymorphic transition . Oxygen is soluble in titanium metal to the extent of about 25 atom-percent, yielding...15 CSH8N4O1 2 NC Nitrocellulose, 13.3% N; -812.9 +3 C6H7N2.5010 HMX symn-Cyclotetramnethylene- + 77.4 0 tetranitramine, C4HSNBO8 Pentolite 50% PETN, 50...TNT; -97.9 -5 C6.1 6H6 .2 5N3.41085. Comp 8 65% RDX , 35% TNT; + 11.47 -9 C1 .96H2. 53N2.2202.68 TNT 2,4,6-Trinitrotoluene, +30.7 -25 p C7R 5N306 N2

  20. Photoactive energetic materials

    Science.gov (United States)

    Chavez, David E.; Hanson, Susan Kloek; Scharff, Robert Jason; Veauthier, Jacqueline Marie; Myers, Thomas Winfield

    2018-02-27

    Energetic materials that are photoactive or believed to be photoactive may include a conventional explosive (e.g. PETN, nitroglycerine) derivatized with an energetic UV-absorbing and/or VIS-absorbing chromophore such as 1,2,4,5-tetrazine or 1,3,5-triazine. Absorption of laser light having a suitably chosen wavelength may result in photodissociation, decomposition, and explosive release of energy. These materials may be used as ligands to form complexes. Coordination compounds include such complexes with counterions. Some having the formula M(L).sub.n.sup.2+ were synthesized, wherein M is a transition metal and L is a ligand and n is 2 or 3. These may be photoactive upon exposure to a laser light beam having an appropriate wavelength of UV light, near-IR and/or visible light. Photoactive materials also include coordination compounds bearing non-energetic ligands; in this case, the counterion may be an oxidant such as perchlorate.

  1. Dynamic response of single hexagonal LMFBR core subassembly wrappers

    Energy Technology Data Exchange (ETDEWEB)

    Ash, J. E.; Marciniak, T. J.; (Argonne National Lab., IL (United States))

    1977-07-01

    To analyze the dynamic structural response of the LMFBR core subassembly hexagonal wrappers to postulated local energy releases and the sensitivity of the response to variations in both the pressure loading and the material properties of the stainless steel, a finite-element computer code STRAW has been developed. A series of experiments was performed to study the effects of variations in material properties. The amount of coldworking to which the Type 316 stainless steel is subjected has a strong influence upon the ductility and the elastic yield point. The usual fabrication process produced a nominally 20% coldworking with a yield point of about 680 MPa. By designing a special set of dies for the drawing process, a very low ductility hexcan was produced for which the yield point was raised to 820 MPa. Conversely, the yield point was lowered to 170 MPa by a solution annealing process producing a highly ductile test hexcan. A metallurgical study was conducted to find a representative brittle simulant material for the irradiated end-of-life steel properties. An aging treatment for Type 446 stainless steel was developed which reproduced the expected tensile-flow behavior of the in-pile subassembly. Further study is underway to investigate the fracture properties of the simulant material. The pressure pulses were generated by the controlled expansion of high-pressure detonation poducts from low-density explosives detonated inside a vented steel cannister. The orifice configuration of the cannister and the charge mixture ratio were designed to produce two specified pulse shapes. A charge containing 37,7 g PETN mixed with 35 wt % inert, hollow-glass microballoons developed a pressure pulse peak of 9.5 MPa at 1.0 ms. Increasing the PETN to 41 g resulted in a 14.6 MPa peak pressure, and increasing the explosive concentration to 90 wt % in the mixture increased the burning rate and the pulse risetime, so that the peak occurred at 0.6 ms.

  2. Integrated Data Collection Analysis (IDCA) Program - KClO3/Dodecane Mixture

    Energy Technology Data Exchange (ETDEWEB)

    Sandstrom, Mary M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Brown, Geoffrey W. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Preston, Daniel N. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Pollard, Colin J. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Warner, Kirstin F. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Sorenson, Daniel N. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Remmers, Daniel L. [Naval Surface Warfare Center (NSWC), Indian Head, MD (United States). Indian Head Division; Shelley, Timothy J. [Air Force Research Lab. (AFRL), Tyndall AFB, FL (United States); Whinnery, LeRoy L. [Sandia National Lab. (SNL-CA), Livermore, CA (United States); Hsu, Peter C. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Reynolds, John G. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2011-05-23

    The Integrated Data Collection Analysis (IDCA) program is conducting a proficiency study for Small-Scale Safety and Thermal (SSST) testing of homemade explosives (HMEs). Described here are the results for impact, friction, electrostatic discharge, and differential scanning calorimetry analysis of a mixture of KClO3 and dodecane—KClO3/dodecane mixture. This material was selected because of the challenge of performing SSST testing of a mixture of solid and liquid materials. The mixture was found to: 1) be more sensitive to impact than RDX, and PETN, 2) less sensitive to friction than PETN, and 3) less sensitive to spark than RDX. The thermal analysis showed little or no exothermic features suggesting that the dodecane volatilized at low temperatures. A prominent endothermic feature was observed assigned to melting of KClO3. This effort, funded by the Department of Homeland Security (DHS), ultimately will put the issues of safe handling of these materials in perspective with standard military explosives. The study is adding SSST testing results for a broad suite of different HMEs to the literature. Ultimately the study has the potential to suggest new guidelines and methods and possibly establish the SSST testing accuracies needed to develop safe handling practices for HMEs. Each participating testing laboratory uses identical test materials and preparation methods wherever possible. Note, however, the test procedures differ among the laboratories. The results are compared among the laboratories and then compared to historical data from various sources. The testing performers involved for the KClO3/dodecane mixture are Lawrence Livermore National Laboratory (LLNL), Los Alamos National Laboratory (LANL), and Indian Head Division, Naval Surface Warfare Center, (NSWC IHD). These tests are conducted as a proficiency study in order to establish some consistency in test protocols, procedures, and experiments and to understand

  3. Standoff laser-induced thermal emission of explosives

    Science.gov (United States)

    Galán-Freyle, Nataly Y.; Pacheco-Londoño, Leonardo C.; Figueroa-Navedo, Amanda; Hernandez-Rivera, Samuel P.

    2013-05-01

    A laser mediated methodology for remote thermal excitation of analytes followed by standoff IR detection is proposed. The goal of this study was to determine the feasibility of using laser induced thermal emission (LITE) from vibrationally excited explosives residues deposited on surfaces to detect explosives remotely. Telescope based FT-IR spectral measurements were carried out to examine substrates containing trace amounts of threat compounds used in explosive devices. The highly energetic materials (HEM) used were PETN, TATP, RDX, TNT, DNT and ammonium nitrate with concentrations from 5 to 200 μg/cm2. Target substrates of various thicknesses were remotely heated using a high power CO2 laser, and their mid-infrared (MIR) thermally stimulated emission spectra were recorded. The telescope was configured from reflective optical elements in order to minimize emission losses in the MIR frequencies and to provide optimum overall performance. Spectral replicas were acquired at a distance of 4 m with an FT-IR interferometer at 4 cm- 1 resolution and 10 scans. Laser power was varied from 4-36 W at radiation exposure times of 10, 20, 30 and 60 s. CO2 laser powers were adjusted to improve the detection and identification of the HEM samples. The advantages of increasing the thermal emission were easily observed in the results. Signal intensities were proportional to the thickness of the coated surface (a function of the surface concentration), as well as the laser power and laser exposure time. For samples of RDX and PETN, varying the power and time of induction of the laser, the calculated low limit of detections were 2 and 1 μg/cm2, respectively.

  4. Ultraviolet Resonant Raman Enhancements in the Detection of Explosives

    Energy Technology Data Exchange (ETDEWEB)

    Short Jr., Billy Joe [Naval Postgraduate School, Monterey, CA (United States)

    2009-06-01

    Raman-based spectroscopy is potentially militarily useful for standoff detection of high explosives. Normal (non-resonance) and resonance Raman spectroscopies are both light scattering techniques that use a laser to measure the vibrational spectrum of a sample. In resonance Raman, the laser is tuned to match the wavelength of a strong electronic absorbance in the molecule of interest, whereas, in normal Raman the laser is not tuned to any strong electronic absorbance bands. The selection of appropriate excitation wavelengths in resonance Raman can result in a dramatic increase in the Raman scattering efficiency of select band(s) associated with the electronic transition. Other than the excitation wavelength, however, resonance Raman is performed experimentally the same as normal Raman. In these studies, normal and resonance Raman spectral signatures of select solid high explosive (HE) samples and explosive precursors were collected at 785 nm, 244 nm and 229 nm. Solutions of PETN, TNT, and explosive precursors (DNT & PNT) in acetonitrile solvent as an internal Raman standard were quantitatively evaluated using ultraviolet resonance Raman (UVRR) microscopy and normal Raman spectroscopy as a function of power and select excitation wavelengths. Use of an internal standard allowed resonance enhancements to be estimated at 229 nm and 244 nm. Investigations demonstrated that UVRR provided ~2000-fold enhancement at 244 nm and ~800-fold improvement at 229 nm while PETN showed a maximum of ~25-fold at 244 nm and ~190-fold enhancement at 229 nm solely from resonance effects when compared to normal Raman measurements. In addition to the observed resonance enhancements, additional Raman signal enhancements are obtained with ultraviolet excitation (i.e., Raman scattering scales as !4 for measurements based on scattered photons). A model, based partly on the resonance Raman enhancement results for HE solutions, is presented for estimating Raman enhancements for solid HE samples.

  5. Synthesis and characterization of triglyceride based thermosetting polymers

    Science.gov (United States)

    Can, Erde

    2005-07-01

    Plant oils, which are found in abundance in all parts of the world and are easily replenished annually, have the potential to replace petroleum as a chemical feedstock for making polymers. Within the past few years, there has been growing interest to use triglycerides as the basic constituent of thermosetting polymers with the necessary rigidity, strength and glass transition temperatures required for engineering applications. Plant oils are not polymerizable in their natural form, however various functional groups that can polymerize can easily be attached to the triglyceride structure making them ideal cross-linking monomers for thermosetting liquid molding resins. Through this research project a number of thermosetting liquid molding resins based on soybean and castor oil, which is a specialty oil with hydroxyls on its fatty acids, have been developed. The triglyceride based monomers were prepared via the malination of the alcoholysis products of soybean and castor oil with various polyols, such as pentaerythritol, glycerol, and Bisphenol A propoxylate. The malinated glycerides were then cured in the presence of a reactive diluent, such as styrene, to form rigid glassy materials with a wide range of properties. In addition to maleate half-esters, methacrylates were also introduced to the glyceride structure via methacrylation of the soybean oil glycerolysis product with methacrylic anhydride. This product, which contains methacrylic acid as by-product, and its blends with styrene also gave rigid materials when cured. The triglyceride based monomers were characterized via conventional spectroscopic techniques. Time resolved FTIR analysis was used to determine the curing kinetics and the final conversions of polymerization of the malinated glyceride-styrene blends. Dynamic Mechanical Analysis (DMA) was used to determine the thermomechanical behavior of these polymers and other mechanical properties were determined via standard mechanical tests. The use of lignin

  6. Surface-modified multifunctional MIP nanoparticles

    Science.gov (United States)

    Moczko, Ewa; Poma, Alessandro; Guerreiro, Antonio; Perez de Vargas Sansalvador, Isabel; Caygill, Sarah; Canfarotta, Francesco; Whitcombe, Michael J.; Piletsky, Sergey

    2013-04-01

    The synthesis of core-shell molecularly imprinted polymer nanoparticles (MIP NPs) has been performed using a novel solid-phase approach on immobilised templates. The same solid phase also acts as a protective functionality for high affinity binding sites during subsequent derivatisation/shell formation. This procedure allows for the rapid synthesis, controlled separation and purification of high-affinity materials, with each production cycle taking just 2 hours. The aim of this approach is to synthesise uniformly sized imprinted materials at the nanoscale which can be readily grafted with various polymers without affecting their affinity and specificity. For demonstration purposes we grafted anti-melamine MIP NPs with coatings which introduce the following surface characteristics: high polarity (PEG methacrylate); electro-activity (vinylferrocene); fluorescence (eosin acrylate); thiol groups (pentaerythritol tetrakis(3-mercaptopropionate)). The method has broad applicability and can be used to produce multifunctional imprinted nanoparticles with potential for further application in the biosensors, diagnostics and biomedical fields and as an alternative to natural receptors.The synthesis of core-shell molecularly imprinted polymer nanoparticles (MIP NPs) has been performed using a novel solid-phase approach on immobilised templates. The same solid phase also acts as a protective functionality for high affinity binding sites during subsequent derivatisation/shell formation. This procedure allows for the rapid synthesis, controlled separation and purification of high-affinity materials, with each production cycle taking just 2 hours. The aim of this approach is to synthesise uniformly sized imprinted materials at the nanoscale which can be readily grafted with various polymers without affecting their affinity and specificity. For demonstration purposes we grafted anti-melamine MIP NPs with coatings which introduce the following surface characteristics: high polarity

  7. In-situ Fabrication of a Freestanding Acrylate-based Hierarchical Electrolyte for Lithium-sulfur Batteries

    International Nuclear Information System (INIS)

    Liu, M.; Jiang, H.R.; Ren, Y.X.; Zhou, D.; Kang, F.Y.; Zhao, T.S.

    2016-01-01

    Graphical abstract: We present a freestanding acrylate-based hierarchical electrolyte. This quasi-solid electrolyte is assembled by in-situ gelation of a pentaerythritol tetraacrylate (PETEA)-based gel polymer electrolyte (GPE) into a polymethyl methacrylate (PMMA)-based electrospun network. The prepared polymer battery renders a suppressed shuttle effect and much enhanced cycle life. - Highlights: • A freestanding Acrylate-based Hierarchical Electrolyte was in-situ crafted. • The high conductivity is due to strong uptake ability and elimination of separator. • The polymer battery renders a superior high rate capability and excellent retention. • First-principle calculations prove anchoring ability of ester functional groups. • Cell modeling shows geometric design effectively suppresses polysulfide flux. - Abstract: A number of methods have been attempted to suppress the shuttle effect in lithium-sulfur (Li-S) batteries to improve battery performance. Conventional methods, however, reduce the ionic conductivity, sacrifice the overall energy density and increase the cost of production. Here, we report a facile synthesis of an acrylate-based hierarchical electrolyte (AHE). This quasi-solid electrolyte is assembled by in-situ gelation of a pentaerythritol tetraacrylate (PETEA)-based gel polymer electrolyte (GPE) into a polymethyl methacrylate (PMMA)-based electrospun network. The structural similarity and synergetic compatibility between the electrospun network and GPE provide the AHE an ester-rich robust structure with a high ionic conductivity of 1.02 × 10 −3 S cm −1 due to the strong uptake ability and the elimination of commercial separator. The S/AHE/Li polymer battery also renders a high rate capability of 645 mAh g −1 at 3C, while maintaining excellent retention at both high and low current densities (80.3% after 500 cycles at 0.3C and 91.9% after 500 cycles at 3C). First-principle calculations reveal that the reduced shuttle effect can be

  8. Composting of soils/sediments and sludges containing toxic organics including high energy explosives. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Doyle, R.C.; Kitchens, J.F.

    1993-07-01

    Laboratory and pilot-scale experimentation were conducted to evaluate composting as an on-site treatment technology to remediate soils contaminated with hazardous waste at DOE`s PANTEX Plant. Suspected contaminated sites within the PANTEX Plant were sampled and analyzed for explosives, other organics, and inorganic wastes. Soils in drainage ditches and playas at PANTEX Plant were found to be contaminated with low levels of explosives (including RDX, HMX, PETN and TATB). Additional sites previously used for solvent disposal were heavily contaminated with solvents and transformation products of the solvent, as well as explosives and by-products of explosives. Laboratory studies were conducted using {sup 14}C-labeled explosives and {sup 14}C-labeled diacetone alcohol contaminated soil loaded into horse manure/hay composts at three rates: 20, 30, and 40%(W/W). The composts were incubated for six weeks at approximately 60{degree}C with continuous aeration. All explosives degraded rapidly and were reduced to below detection limits within 3 weeks in the laboratory studies. {sup 14}C-degradates from {sup 14}C-RDX, {sup 14}C-HMX and {sup 14}C-TATB were largely limited to {sup 14}CO{sub 2} and unextracted residue in the compost. Volatile and non-volatile {sup 14}C-degradates were found to result from {sup 14}C-PETN breakdown, but these compounds were not identified. {sup 14}C-diacetone alcohol concentrations were significantly reduced during composting. However, most of the radioactivity was volatilized from the compost as non-{sup 14}CO{sub 2} degradates or as {sup 14}C-diacetone alcohol. Pilot scale composts loaded with explosives contaminated soil at 30% (W/W) with intermittent aeration were monitored over six weeks. Data from the pilot-scale study generally was in agreement with the laboratory studies. However, the {sup 14}C-labeled TATB degraded much faster than the unlabeled TATB. Some formulations of TATB may be more resistant to composting activity than others.

  9. Materials research for passive solar systems: Solid-state phase-change materials

    Science.gov (United States)

    Benson, D. K.; Webb, J. D.; Burrows, R. W.; McFadden, J. D. O.; Christensen, C.

    1985-03-01

    A set of solid-state phase-change materials is being evaluated for possible use in passive solar thermal energy storage systems. The most promising materials are organic solid solutions of pentaerythritol (C5H12O4), pentaglycerinve (C5H12O3), and neopentyl glycol (C5H12O2). Solid solution mixtures of these compounds can be tailored so that they exhibit solid-to-solid phase transformations at any desired temperature between 25 C and 188 C, and have latent heats of transformation etween 20 and 70 cal/g. Transformation temperatures, specific heats, and latent heats of transformation have been measured for a number of these materials. Limited cyclic experiments suggest that the solid solutions are stable. These phase-change materials exhibit large amounts of undercooling; however, the addition of certain nucleating agents as particulate dispersions in the solid phase-change material greatly reduces this effect. Computer simulations suggest that the use of an optimized solid-state phase-change material in a Trombe wall could provide better performance than a concrete Trombe wall four times thicker and nine times heavier.

  10. Dermal oncogenicity bioassays of monofunctional and multifunctional acrylates and acrylate-based oligomers.

    Science.gov (United States)

    DePass, L R; Maronpot, R R; Weil, C S

    1985-01-01

    Several important components of photocurable coatings were studied for dermal tumorigenic activity by repeated application to the skin of mice. The substances tested were 2-ethylhexyl acrylate (EHA) and methylcarbamoyloxyethyl acrylate (MCEA) (monomers); neopentyl glycol diacrylate (NPGDA), esterdiol-204-diacrylate (EDDA), and pentaerythritol tri(tetra)acrylate (PETA) (cross-linkers); and three acrylated urethane oligomers. For each bioassay, 40 C3H/HeJ male mice were dosed 3 times weekly on the dorsal skin for their lifetime with the highest dose of the test agent that caused no local irritation or reduction in body weight gain. Two negative control groups received acetone (diluent) only. A positive control group received 0.2% methylcholanthrene (MC). NPGDA and EHA had significant tumorigenic activity with tumor yields of eight and six tumor-bearing mice (three and two malignancies), respectively. The MC group had 34 mice with carcinomas and 1 additional mouse with a papilloma. MCEA had no dermal tumorigenic activity but resulted in early mortality. No skin tumors in the treatment area were observed in the other groups. Additional studies will be necessary to elucidate possible relationships between structure and tumorigenic activity for the acrylates.

  11. PEGDA hydrogels as a replacement for animal tissues in mucoadhesion testing.

    Science.gov (United States)

    Eshel-Green, Tal; Eliyahu, Shaked; Avidan-Shlomovich, Shlomit; Bianco-Peled, Havazelet

    2016-06-15

    Utilization of animal parts in ex-vivo mucoadhesion assays is a common approach that presents many difficulties due to animal rights issues and large variance between animals. This study examines the suitability of two PEGDA (poly(ethylene glycol) diacrylate) based hydrogels to serve as tissue mimetics for mucoadhesion evaluation. One hydrogel, termed PEGDA-QT, was composed of pentaerythritol tetrakis (3-mercaptopropionate) and PEG and contained free thiol groups mimicking those found in natural mucosa. The other hydrogel was formed by UV (ultraviolet) curing of PEGDA and mimicked the mechanical property of mucosa but not its chemical constitute. When ranking different first generation mucoadhesive polymers using a tensile assay, both hydrogels showed good agreement with the ranking achieved for porcine small intestine. However, only PEGDA-QT and porcine small intestine shared a similar displacement curve. The same ranking for PEGDA-QT and porcine small intestine was also observed when comparing a second-generation mucoadhesive polymer, thiolated alginate, to native alginate. Our findings suggest that PEGDA-QT could serve as a replacement for porcine small intestine in both mucoadhesion evaluations using a tensile machine and the flow-through method for first and second-generation mucoadhesive polymers. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. PLA-based biodegradable and tunable soft elastomers for biomedical applications

    International Nuclear Information System (INIS)

    Harrane, Amine; Leroy, Adrien; Nouailhas, Hélène; Garric, Xavier; Coudane, Jean; Nottelet, Benjamin

    2011-01-01

    Although desirable for biomedical applications, soft degradable elastomers having balanced amphiphilic behaviour are rarely described in the literature. Indeed, mainly highly hydrophobic elastomers or very hydrophilic elastomers with hydrogel behaviours are found. In this work, we developed thermoset degradable elastomers based on the photo-cross-linking of poly(lactide)-poly(ethylene glycol)-poly(lactide) (PLA-PEG-PLA) triblock prepolymers. The originality of the proposed elastomers comes from the careful choice of the prepolymer amphiphilicity and from the possible modulation of their mechanical properties and degradation rates provided by cross-linkers of different nature. This is illustrated with the hydrophobic and rigid 2,4,6-triallyloxy-1,3,5-triazine compared to the hydrophilic and soft pentaerythritol triallyl ether. Thermal properties, mechanical properties, swelling behaviours, degradation rates and cytocompatibility have been evaluated. Results show that it is possible to generate a family of degradable elastomers covering a broad range of properties from a single biocompatible and biodegradable prepolymer.

  13. Bio-Based Nano Composites from Plant Oil and Nano Clay

    Science.gov (United States)

    Lu, Jue; Hong, Chang K.; Wool, Richard P.

    2003-03-01

    We explored the combination of nanoclay with new chemically functionalized, amphiphilic, plant oil resins to form bio-based nanocomposites with improved physical and mechanical properties. These can be used in many new applications, including the development of self-healing nanocomposites through controlled reversible exfoliation/intercalation, and self-assembled nano-structures. Several chemically modified triglyceride monomers of varying polarity, combined with styrene (ca 30include acrylated epoxidized soybean oil (AESO), maleated acrylated epoxidized soybean oil (MAESO) and soybean oil pentaerythritol glyceride maleates (SOPERMA), containing either hydroxyl group or acid functionality or both. The clay used is a natural montmorillonite modified with methyl tallow bis-2-hydroxyethyl quaternary ammonium chloride, which has hydroxyl groups. Both XRD and TEM showed a completely exfoliated structure at 3 wtwhen the clay content is above 5 wtconsidered a mix of intercalated and partially exfoliated structure. The controlled polarity of the monomer has a major effect on the reversible dispersion of clay in the polymer matrix. The bio-based nanocomposites showed a significant increase in flexural modulus and strength. Supported by EPA and DoE

  14. A Novel Methodology for the Synthesis of Acyloxy Castor Polyol Esters: Low Pour Point Lubricant Base Stocks.

    Science.gov (United States)

    Kamalakar, Kotte; Mahesh, Goli; Prasad, Rachapudi B N; Karuna, Mallampalli S L

    2015-01-01

    Castor oil, a non-edible oil containing hydroxyl fatty acid, ricinoleic acid (89.3 %) was chemically modified employing a two step procedure. The first step involved acylation (C(2)-C(6) alkanoic anhydrides) of -OH functionality employing a green catalyst, Kieselguhr-G and solvent free medium. The catalyst after reaction was filtered and reused several times without loss in activity. The second step is esterification of acylated castor fatty acids with branched mono alcohol, 2-ethylhexanol and polyols namely neopentyl glycol (NPG), trimethylolpropane (TMP) and pentaerythritol (PE) to obtain 16 novel base stocks. The base stocks when evaluated for different lubricant properties have shown very low pour points (-30 to -45°C) and broad viscosity ranges 20.27 cSt to 370.73 cSt, higher viscosity indices (144-171), good thermal and oxidative stabilities, and high weld load capacities suitable for multi-range industrial applications such as hydraulic fluids, metal working fluids, gear oil, forging and aviation applications. The study revealed that acylated branched mono- and polyol esters rich in monounsaturation is desirable for developing low pour point base stocks.

  15. Characterization of red mud-epoxy intumescent char using surface imaging and micro analysis

    Energy Technology Data Exchange (ETDEWEB)

    Arogundade, A. I., E-mail: ajiunolorioba@gmail.com; Megat-Yusoff, P. S. M., E-mail: puteris@petronas.com.my; Faiz, A. [Department of Mechanical Engineering, Universiti Tecknologi Petronas (Malaysia); Bhat, A. H. [Department of Fundamental and Applied Science, Universiti Tecknologi Petronas (Malaysia)

    2015-07-22

    In this study, red mud (RM), an oxide waste was proposed as reinforcing, synergistic filler for the traditional epoxy intumescent coating (IC). 5.5 wt% of acid-modified and unmodified red mud were introduced into the basic intumescent formulation of ammonium polyphosphate (APP), pentaerythritol (PER) and melamine (MEL). In order to predict effect of modification on its suitability, Field emission electron scanning microscopy and Fourier transform infra red were used to obtain detailed characteristics such as the cell size, pore distribution, homogeneity and chemical composition of the red mud-epoxy carbonaceous char. Both acid-modified and unmodified RM-filled ICs produced chars with smaller and more closely packed cells compared to chars from the unfilled coating. Both coating types had hard carbonaceous metal phosphate coverings that could act as heat barriers. The unmodified red mud was found to be antagonistic to the intumescent action with an expansion of only 2 times the initial thickness. The leached, low iron-red mud produced an expansion of 15 times the initial thickness, but possessed a hollow interior. From these findings, it may be deduced that while acid leaching of red mud may improve intumescent expansion, it would be necessary to optimize the percent filler loading to improve residual mass.

  16. Preparation and Characterization of UV-Curable Cyclohexanone-Formaldehyde Resin and Its Cured Film Properties

    Directory of Open Access Journals (Sweden)

    Guang Yang

    2014-01-01

    Full Text Available UV-curable cyclohexanone-formaldehyde (UVCF resin was prepared with cyclohexanone-formaldehyde (CF resin, isophorone diisocyanate (IPDI, and pentaerythritol triacrylate (PETA as base substance, bridging agent, and functional monomer, respectively. The structure of UVCF was characterized by Fourier transform infrared spectroscopy (FT-IR, 1H-nuclear magnetic resonance spectroscopy (1H-NMR, and gel permeation chromatography (GPC. The viscosity and photopolymerization behavior of the UV-curable formulations were studied. The thermal stability and mechanical properties of the cured films were also investigated. The results showed that UVCF resin was successfully prepared, the number of average molecular weight was about 2010, and its molecular weight distribution index was 2.8. With the increase of UVCF resin content, the viscosity of the UV-curable formulations increased. After exposure to UV irradiation for 230 s, the photopolymerization conversion of the UV-curable formulations was above 80%. Moreover, when the UVCF content was 60%, the formulations had high photopolymerization rate, and the cured UVCF films showed good thermal stability and mechanical properties.

  17. The synthesis of weak acidic type hybrid monolith via thiol-ene click chemistry and its application in hydrophilic interaction chromatography.

    Science.gov (United States)

    Zeng, Jiao; Liu, Shengquan; Wang, Menglin; Yao, Shouzhuo; Chen, Yingzhuang

    2017-05-01

    In this work, a porous structure and good permeability monolithic column was polymerized in UV transparent fused-silica capillaries via photo-initiated thiol-ene click polymerization of 2,4,6,8-tetravinyl-2,4,6,8-tetramethylcyclotetrasiloxane (TMTVS), pentaerythritol tetra(3-mercaptopropionate)(PETMP), itaconic acid, respectively, in the presence of porogenic solvents (tetrahydrofuranand methanol) and an initiator (2,2-dimethoxy-2-phenylacetophenone) (DMPA) within 30 min. The physical properties of this monolith were characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and nitrogen adsorption/desorption measurements. For an overall evaluation of the monolith in chromatographic application, separations of polycyclic aromatic hydrocarbons (PAHs), phenols, amides and bases were carried out. The column efficiency of this monolith could be as high as 112 560 N/m. It also possesses a potential application in fabrication of monoliths with high efficiency for c-LC. In addition, the resulting monolithic column demonstrated the potential use in analysis of environment waters. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Effect of Crosslinking Agent Concentration on the Properties of Unmedicated Hydrogels

    Directory of Open Access Journals (Sweden)

    Rachel Shet Hui Wong

    2015-09-01

    Full Text Available Novel polyethylene oxide (PEO hydrogel films were synthesized via UV crosslinking with varying concentrations of pentaerythritol tetra-acrylate (PETRA as crosslinking agent. The aim was to study the effects of the crosslinking agent on the material properties of hydrogel films intended for dermatological applications. Fabricated film samples were characterized using swelling studies, scanning electron microscopy, tensile testing and rheometry. Films showed rapid swelling and high elasticity. The increase of PETRA concentration resulted in significant increase in the gel fraction and crosslinking density (ρc, while causing a significant decrease in the equilibrium water content (EWC, average molecular weight between crosslinks (\\({\\overline{M}}_{c}\\, and mesh size (ζ of films. From the scanning electron microscopy, cross-linked PEO hydrogel network appeared as cross-linked mesh-like structure with interconnected micropores. Rheological studies showed PEO films required a minimum of 2.5% w/w PETRA to form stable viscoelastic solid gels. Preliminary studies concluded that a minimum of 2.5% w/w PETRA is required to yield films with desirable properties for skin application.

  19. Fabrication, thermal properties and thermal stabilities of microencapsulated n-alkane with poly(lauryl methacrylate) as shell

    International Nuclear Information System (INIS)

    Qiu, Xiaolin; Lu, Lixin; Wang, Ju; Tang, Guoyi; Song, Guolin

    2015-01-01

    Highlights: • Microencapsulation of octadecane and paraffin by crosslinked poly(lauryl methacrylate). • Octadecane microcapsules have a melting enthalpy of about 118 J g −1 . • Weight loss temperatures of the microcapsules were increased by 67 °C and 28 °C. • Phase change enthalpies decreased by around 10 wt% after 500 thermal cycles. • Foams with microcapsules can be applied for passive temperature control. - Abstract: Microencapsulation of n-octadecane or paraffin with poly(lauryl methacrylate) (PLMA) shell was performed by a suspension-like polymerization. The polymer shell was crosslinked by pentaerythritol tetraacrylate (PETRA). The surface morphologies of microcapsules were investigated by scanning electron microscopy (SEM). Phase change properties, thermal reliabilities and thermal stabilities of microcapsules were determined by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). The n-octadecane microcapsule exhibits higher melting enthalpy (118.0 J g −1 ) and crystallization enthalpy (108.3 J g −1 ) compared with the paraffin microcapsule. The thermal resistant temperatures were enhanced by more than 25 °C when n-alkanes were microencapsulated by PLMA. The PCM contents of microcapsules decreased by less than 4 wt% and 6 wt% after 500 and 1000 thermal cycles, respectively. Heat-up experiments indicated that microcapsule-treated foams exhibited upgraded thermal regulation capacities. Consequently, microencapsulated n-octadecane or paraffin with PLMA as shell possesses good potentials for heat storage and thermal regulation.

  20. Effect of Drug Loading Method and Drug Physicochemical Properties on the Material and Drug Release Properties of Poly (Ethylene Oxide Hydrogels for Transdermal Delivery

    Directory of Open Access Journals (Sweden)

    Rachel Shet Hui Wong

    2017-07-01

    Full Text Available Novel poly (ethylene oxide (PEO hydrogel films were synthesized via UV cross-linking with pentaerythritol tetra-acrylate (PETRA as cross-linking agent. The purpose of this work was to develop a novel hydrogel film suitable for passive transdermal drug delivery via skin application. Hydrogels were loaded with model drugs (lidocaine hydrochloride (LID, diclofenac sodium (DIC and ibuprofen (IBU via post-loading and in situ loading methods. The effect of loading method and drug physicochemical properties on the material and drug release properties of medicated film samples were characterized using scanning electron microscopy (SEM, swelling studies, differential scanning calorimetry (DSC, fourier transform infrared spectroscopy (FT-IR, tensile testing, rheometry, and drug release studies. In situ loaded films showed better drug entrapment within the hydrogel network and also better polymer crystallinity. High drug release was observed from all studied formulations. In situ loaded LID had a plasticizing effect on PEO hydrogel, and films showed excellent mechanical properties and prolonged drug release. The drug release mechanism for the majority of medicated PEO hydrogel formulations was determined as both drug diffusion and polymer chain relaxation, which is highly desirable for controlled release formulations.

  1. Thiol-acrylate nanocomposite foams for critical size bone defect repair: A novel biomaterial.

    Science.gov (United States)

    Garber, Leah; Chen, Cong; Kilchrist, Kameron V; Bounds, Christopher; Pojman, John A; Hayes, Daniel

    2013-12-01

    Bone tissue engineering approaches using polymer/ceramic composites show promise as effective biocompatible, absorbable, and osteoinductive materials. A novel class of in situ polymerizing thiol-acrylate based copolymers synthesized via an amine-catalyzed Michael addition was studied for its potential to be used in bone defect repair. Both pentaerythritol triacrylate-co-trimethylolpropane tris(3-mercaptopropionate) (PETA-co-TMPTMP) and PETA-co-TMPTMP with hydroxyapatite (HA) composites were fabricated in solid cast and foamed forms. These materials were characterized chemically and mechanically followed by an in vitro evaluation of the biocompatibility and chemical stability in conjunction with human adipose-derived mesenchymal pluripotent stem cells (hASC). The solid PETA-co-TMPTMP with and without HA exhibited compressive strength in the range of 7-20 MPa, while the cytotoxicity and biocompatibility results demonstrate higher metabolic activity of hASC on PETA-co-TMPTMP than on a polycaprolactone control. Scanning electron microscope imaging of hASC show expected spindle shaped morphology when adhered to copolymer. Micro-CT analysis indicates open cell interconnected pores. Foamed PETA-co-TMPTMP HA composite shows promise as an alternative to FDA-approved biopolymers for bone tissue engineering applications. Copyright © 2013 Wiley Periodicals, Inc., a Wiley Company.

  2. Use of the CSD program package for structure determination from powder data

    International Nuclear Information System (INIS)

    Akselrud, L.G.; Zavalii, P.Yu.; Grin, Yu.N.; Pecharski, V.K.; Baumgartner, B.; Woelfel, E.

    1993-01-01

    Although Rietveld's method of full profile structure refinement of powder data is a much-used tool today, ab initio structure solution from powder data is still not a routine task. One of the reasons for this is that fully overlapped peaks usually cannot be handled by routine structure determination programs. This shortcoming is not present in the Crystal Structure Determination (CSD) package which accepts intensities from powder diagrams as well as single crystal data. In order to demonstrate the possibilities of the CSD package, powder diagrams of five substances with already known crystal structure were collected and evaluated with the CSD package. The samples were scheelite (CaWO 4 ), pentaerythritol (C(CH 2 OH) 4 ), sodium sulfite (Na 2 SO 3 ), copper sulfate pentahydrate (CuSO 4 .5H 2 O) and silver germanium phosphide (Ag 6 Ge 10 P 12 ) and showed problems typical for powder work like preferred orientation and heavy peak overlapping. For four of the samples, correct atomic positions for some atoms could be found from the automatic MULTAN solution, which were then used in subsequent least squares- and difference Fourier calculations to locate the remaining atoms. Surprisingly, the cubic Ag 6 Ge 10 P 12 posed the most problems for the structure solution although one third of the observed intensities was single-indexed and the final R-value was as low as 4%. (orig.)

  3. Fire Propagation Performance of Intumescent Fire Protective Coatings Using Eggshells as a Novel Biofiller

    Directory of Open Access Journals (Sweden)

    M. C. Yew

    2014-01-01

    Full Text Available This paper aims to synthesize and characterize an effective intumescent fire protective coating that incorporates eggshell powder as a novel biofiller. The performances of thermal stability, char formation, fire propagation, water resistance, and adhesion strength of coatings have been evaluated. A few intumescent flame-retardant coatings based on these three ecofriendly fire retardant additives ammonium polyphosphate phase II, pentaerythritol and melamine mixed together with flame-retardant fillers, and acrylic binder have been prepared and designed for steel. The fire performance of the coatings has conducted employing BS 476: Part 6-Fire propagation test. The foam structures of the intumescent coatings have been observed using field emission scanning electron microscopy. On exposure, the coated specimens’ B, C, and D had been certified to be Class 0 due to the fact that their fire propagation indexes were less than 12. Incorporation of ecofriendly eggshell, biofiller into formulation D led to excellent performance in fire stopping (index value, (I=4.3 and antioxidation of intumescent coating. The coating is also found to be quite effective in water repellency, uniform foam structure, and adhesion strength.

  4. Preparation, thermal properties and thermal reliabilities of microencapsulated n-octadecane with acrylic-based polymer shells for thermal energy storage

    Energy Technology Data Exchange (ETDEWEB)

    Qiu, Xiaolin [Advanced Materials Institute and Clearer Production Key Laboratory, Graduate School at Shenzhen, Tsinghua University, Shenzhen 518055 (China); Key Laboratory of Advanced Materials, Department of Materials Science and Engineering, Tsinghua University, Haidian District, Beijing 100084 (China); Song, Guolin; Chu, Xiaodong; Li, Xuezhu [Advanced Materials Institute and Clearer Production Key Laboratory, Graduate School at Shenzhen, Tsinghua University, Shenzhen 518055 (China); Tang, Guoyi, E-mail: tanggy@tsinghua.edu.cn [Advanced Materials Institute and Clearer Production Key Laboratory, Graduate School at Shenzhen, Tsinghua University, Shenzhen 518055 (China); Key Laboratory of Advanced Materials, Department of Materials Science and Engineering, Tsinghua University, Haidian District, Beijing 100084 (China)

    2013-01-10

    Highlights: Black-Right-Pointing-Pointer n-Octadecane was encapsulated by p(butyl methacrylate) (PBMA) and p(butyl acrylate). Black-Right-Pointing-Pointer Microcapsules using divinylbenzene as crosslinking agent have better quality. Black-Right-Pointing-Pointer Microcapsule with butyl methacrylate-divinylbenzene has highest latent heat. Black-Right-Pointing-Pointer Microcapsule with butyl methacrylate-divinylbenzene has greatest thermal stability. Black-Right-Pointing-Pointer Phase change temperatures and enthalpies of the microcapsules varied little after thermal cycle. - Abstract: Microencapsulation of n-octadecane with crosslinked p(butyl methacrylate) (PBMA) and p(butyl acrylate) (PBA) as shells for thermal energy storage was carried out by a suspension-like polymerization. Divinylbenzene (DVB) and pentaerythritol triacrylate (PETA) were employed as crosslinking agents. The surface morphologies of the microencapsulated phase change materials (microPCMs) were studied by scanning electron microscopy (SEM). Thermal properties, thermal reliabilities and thermal stabilities of the as-prepared microPCMs were investigated by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). The microPCMs prepared by using DVB exhibit greater heat capacities and higher thermal stabilities compared with those prepared by using PETA. The thermal resistant temperature of the microPCM with BMA-DVB polymer was up to 248 Degree-Sign C. The phase change temperatures and latent heats of all the as-prepared microcapsules varied little after 1000 thermal cycles.

  5. Influence of expandable graphite on fire resistance and water resistance of flame-retardant coatings

    International Nuclear Information System (INIS)

    Wang, Zhenyu; Han, Enhou; Ke, Wei

    2007-01-01

    Expandable graphite (EG) coating and ammonium polyphosphate-pentaerythritol-melamine (APP-PER-MEL) coating were prepared. Thermal degradation and char formation of the coatings were investigated by differential thermal analysis (DTA), thermogravimetry (TG), X-ray diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The results have shown that the anti-oxidation and fire-resistant properties of expandable graphite coating containing EG with size of 74 μm are better than those of APP-PER-MEL coating. The static immersion test was applied to study water resistance of the coatings, and the fire protection test and mechanical test were used to analyse heat insulation and mechanical properties of coatings before and after water immersion. The fire-resistant and mechanical properties of APP-PER-MEL coating were severely damaged by water immersion, whereas EG coating containing 8.5% EG with size of 74 μm could retain the good fire resistance even after 500 h water immersion

  6. Structure-activity relationship studies on a Trp dendrimer with dual activities against HIV and enterovirus A71. Modifications on the amino acid.

    Science.gov (United States)

    Martínez-Gualda, Belén; Sun, Liang; Rivero-Buceta, Eva; Flores, Aida; Quesada, Ernesto; Balzarini, Jan; Noppen, Sam; Liekens, Sandra; Schols, Dominique; Neyts, Johan; Leyssen, Pieter; Mirabelli, Carmen; Camarasa, María-José; San-Félix, Ana

    2017-03-01

    We have recently described a new class of dendrimers with tryptophan (Trp) on the surface that show dual antiviral activities against HIV and EV71 enterovirus. The prototype compound of this family is a pentaerythritol derivative with 12 Trps on the periphery. Here we complete the structure-activity relationship studies of this family to identify key features that might be significant for the antiviral activity. With this aim, novel dendrimers containing different amino acids (aromatic and non-aromatic), tryptamine (a "decarboxylated" analogue of Trp) and N-methyl Trp on the periphery have been prepared. Dendrimer with N-Methyl Trp was the most active against HIV-1 and HIV-2 while dendrimer with tyrosine was endowed with the most potent antiviral activity against EV71. This tyrosine dendrimer proved to inhibit a large panel of EV71 clinical isolates (belonging to different clusters) in the low nanomolar/high picomolar range. In addition, a new synthetic procedure (convergent approach) has been developed for the synthesis of the prototype and some other dendrimers. This convergent approach proved more efficient (higher yields, easier purification) than the divergent approach previously reported. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

  7. Thiol-ene reaction as tool for crosslinking of polynorbornene micelles in the nanoscale

    Science.gov (United States)

    Rupp, Barbara; Bauer, Thomas; Slugovc, Christian

    2009-08-01

    The thiol-ene reaction is a established photoreaction of multifunctional thiols and enes. Virtually any type of ene will participate in a free radical polymerisation process with a thiol. An advantage over many other photochemical reactions is that the reaction proceeds almost as rapidly in ambient conditions as in inert atmosphere. In this work we introduce the UV-crosslinking of polynorbornenes made by ring opening metathesis polymerization making use of the residual double bond in the polymer backbone. The crosslinking experiments were done in thin films and were followed by FTIR measurements, to proof the accessibility of double-bonds in the polymers for the addition of the thiols. As a result of these pre-experiments we created flexible and light transmitting films. To further increase the scope of this reaction, amphiphilic block copolymers were prepared and used to form block copolymer micelles in a selective solvent, which were subsequently crosslinked with pentaerythritol tetra(3-mercaptopropionate) (PETMP). FT-IR, DLS and SEM-measurements were used to prove the successful crosslinking and thus nanoparticle formation.

  8. Synthesis of Upconverting Hydrogel Nanocomposites Using Thiol-Ene Click Chemistry: Template for the Formation of Dendrimer-Like Gold Nanoparticle Assemblies.

    Science.gov (United States)

    Meesaragandla, Brahmaiah; Mahalingam, Venkataramanan

    2015-11-16

    The synthesis of upconverting hydrogel nanocomposites by base-catalyzed thiol-ene click reaction between 10-undecenoic acid capped Yb(3+)/Er(3+)-doped NaYF4 nanoparticles and pentaerythritol tetrakis(3-mercaptopropionate) (PETMP) as tetrathiol monomer is reported. This synthetic strategy for nanocomposite gels is quite different from works where usually the preformed gels are mixed with the nanoparticles. Developing nanocomposites by surface modification of capping ligands would allow tuning and controlling of the separation of the nanoparticles inside the gel network. The hydrogel nanocomposites prepared by thiol-ene click reaction show strong enhancement in luminescence intensity compared to 10-undecenoic acid-capped Yb(3+)/Er(3+)-doped NaYF4 nanoparticles through the upconversion process (under 980 nm laser excitation). The hydrogel nanocomposites display strong swelling characteristics in water resulting in porous structures. Interestingly, the resulting nanocomposite gels act as templates for the synthesis of dendrimer-like Au nanostructures when HAuCl4 is reduced in the presence of the nanocomposite gels. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. An oxygen-insensitive degradable resist for fabricating metallic patterns on highly curved surfaces by UV-nanoimprint lithography.

    Science.gov (United States)

    Hu, Xin; Huang, Shisong; Gu, Ronghua; Yuan, Changsheng; Ge, Haixiong; Chen, Yanfeng

    2014-10-01

    In this paper, an oxygen-insensitive degradable resist for UV-nanoimprint is designed, com-prising a polycyclic degradable acrylate monomer, 2,10-diacryloyloxymethyl-1,4,9,12-tetraoxa-spiro [4.2.4.2] tetradecane (DAMTT), and a multifunctional thiol monomer pentaerythritol tetra(3-mercaptopropionate) (PETMP). The resist can be quickly UV-cured in the air atmosphere and achieve a high monomer conversion of over 98%, which greatly reduce the adhesion force between the resist and the soft mold. High conversion, in company with an adequate Young's modulus (about 1 GPa) and an extremely low shrinkage (1.34%), promises high nanoimprint resolution of sub-50 nm. The cross-linked resist is able to break into linear molecules in a hot acid solvent. As a result, metallic patterns are fabricated on highly curved surfaces via the lift off process without the assistance of a thermoplastic polymer layer. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Evaluation and Control of Thiol-ene/Thiol-epoxy Hybrid Networks.

    Science.gov (United States)

    Carioscia, Jacquelyn A; Stansbury, Jeffrey W; Bowman, Christopher N

    2007-03-08

    The development of thiol-ene/thiol-epoxy hybrid networks offers the advantage of tailorable polymerization kinetics while producing a highly crosslinked, high T(g) polymer that has significantly reduced shrinkage stress. Stoichiometric mixtures of pentaerythritol tetra(3-mercaptopropionate) (PETMP)/triallyl-1,3,5-triazine-2,4,6-trione (TATATO) (thiol-ene, mixture 1) and PETMP/bisphenol a diglycidyl ether (BADGE) (thiol-epoxy, mixture 2) were prepared and hybrid mixtures of 75/25, 50/50, 25/75, and 10/90 w/w of mixtures 1 and 2 were polymerized using a combination of both radical and anionic initiation. The light exposure timing and the relative initiation conditions of the two types were used to control the order and relative rates of the radical and anionic polymerizations. The 50/50 w/w thiol-ene/thiol-epoxy hybrid material exhibited a final stress of only 0.2 MPa, which is 90 % lower than the stress developed in a control dimethacrylate resin. Kinetic analysis indicates composition affects network development in thiol-ene/thiol-epoxy hybrid networks and produces materials with robust mechanical properties.

  11. A Scalable Method toward Superhydrophilic and Underwater Superoleophobic PVDF Membranes for Effective Oil/Water Emulsion Separation.

    Science.gov (United States)

    Yuan, Tao; Meng, Jianqiang; Hao, Tingyu; Wang, Zihong; Zhang, Yufeng

    2015-07-15

    A superhydrophilic and underwater superoleophobic PVDF membrane (PVDFAH) has been prepared by surface-coating of a hydrogel onto the membrane surface, and its superior performance for oil/water emulsion separation has been demonstrated. The coated hydrogel was constructed by an interfacial polymerization based on the thiol-epoxy reaction of pentaerythritol tetrakis (3-mercaptopropionate) (PETMP) with diethylene glycol diglycidyl ether (PEGDGE) and simultaneously tethered on an alkaline-treated commercial PVDF membrane surface via the thio-ene reaction. The PVDFAH membranes can be fabricated in a few minutes under mild conditions and show superhydrophilic and underwater superoleophobic properties for a series of organic solvents. Energy dispersive X-ray (EDX) analysis shows that the hydrogel coating was efficient throughout the pore lumen. The membrane shows superior oil/water emulsion separation performance, including high water permeation, quantitative oil rejection, and robust antifouling performance in a series oil/water emulsions, including that prepared from crude oil. In addition, a 24 h Soxhlet-extraction experiment with ethanol/water solution (50:50, v/v) was conducted to test the tethered hydrogel stability. We see that the membrane maintained the water contact angle below 5°, indicating the covalent tethering stability. This technique shows great promise for scalable fabrication of membrane materials for handling practical oil emulsion purification.

  12. Network type sp3 boron-based single-ion conducting polymer electrolytes for lithium ion batteries

    Science.gov (United States)

    Deng, Kuirong; Wang, Shuanjin; Ren, Shan; Han, Dongmei; Xiao, Min; Meng, Yuezhong

    2017-08-01

    Electrolytes play a vital role in modulating lithium ion battery performance. An outstanding electrolyte should possess both high ionic conductivity and unity lithium ion transference number. Here, we present a facile method to fabricate a network type sp3 boron-based single-ion conducting polymer electrolyte (SIPE) with high ionic conductivity and lithium ion transference number approaching unity. The SIPE was synthesized by coupling of lithium bis(allylmalonato)borate (LiBAMB) and pentaerythritol tetrakis(2-mercaptoacetate) (PETMP) via one-step photoinitiated in situ thiol-ene click reaction in plasticizers. Influence of kinds and content of plasticizers was investigated and the optimized electrolytes show both outstanding ionic conductivity (1.47 × 10-3 S cm-1 at 25 °C) and high lithium transference number of 0.89. This ionic conductivity is among the highest ionic conductivity exhibited by SIPEs reported to date. Its electrochemical stability window is up to 5.2 V. More importantly, Li/LiFePO4 cells with the prepared single-ion conducting electrolytes as the electrolyte as well as the separator display highly reversible capacity and excellent rate capacity under room temperature. It also demonstrates excellent long-term stability and reliability as it maintains capacity of 124 mA h g-1 at 1 C rate even after 500 cycles without obvious decay.

  13. Actividad antibacteriana, degradación hidrolítica y microbiana y citotoxicidad in vitro de poliuretanos sintetizados con polioles derivados del aceite de higuerilla

    Directory of Open Access Journals (Sweden)

    Yomaira L. Uscategui

    Full Text Available Biological activities from polyurethanes (PUs synthesized from polyols (derived from castor oil and isophorone diisocyanate were evaluated. In vitro degradability was evaluated by phosphate buffered saline (PBS and antibacterial degradation with Escherichia coli and Pseudomonas aeruginosa. The biocompatibility was analyzed by: i the antimicrobial activity against E. coli, S. aureus and P. aeruginosa, and ii in vitro cytotoxicity assays using mouse embryonic fibroblast cell line L-929 in direct contact with the PUs and with NIH/3T3 cells in indirect contact with the PUs degradation products. PUs with polyol P1 (2,64% molar relation of pentaerythritol and castor oil was the material with better biodegradation properties: 1.125±0.110% in 72 h by PBS at 100 ºC. In general, all materials were degraded up to 1.000±0.223% and 2.251±0.010% in 72 h by E. coli and P. aeruginosa, respectively. On the other hand, it was determined a close relationship between functionality of polyol and bacterial inhibition. The antibacterial effect of the PUs decreased by 67% for E. coli, 55% for S. aureus and 56% for P. aeruginosa after 24 h. Chemical modification of castor oil did not generate a cytotoxic effect on the tested cell lines. The evaluated materials are suggested as candidates to obtain biomaterials due to their mechanical properties and biocompatibility presented in untransformed cells.

  14. Preparation of Magnetic Iron Oxide Nanoparticles (MIONs with Improved Saturation Magnetization Using Multifunctional Polymer Ligand

    Directory of Open Access Journals (Sweden)

    Muhammad Irfan Majeed

    2016-11-01

    Full Text Available This paper describes the preparation of ultra-small magnetic iron oxide (Fe3O4 nanoparticles (MIONs coated with water-soluble thioether end-functionalized polymer ligand pentaerythritol tetrakis 3-mercaptopropionate-polymethacrylic acid (PTMP-PMAA. The MIONs were prepared by co-precipitation of aqueous iron precursor solution at a high temperature. The polymer modified MIONs were characterized by dynamic light scattering (DLS, transmission electron microscopy (TEM, Fourier transform infrared spectroscopy (FTIR, X-ray powder diffraction (XRD, thermogravimetric analysis (TGA, and vibrating sample magnetometery (VSM. It was found that these MIONs were successfully modified by this water-soluble polymer ligand with a fairly uniform size and narrow size distribution. The dried powder of MIONs could be stored for a long time and re-dispersed well in water without any significant change. Additionally, the polymer concentration showed a significant effect on size and magnetic properties of the MIONs. The saturation magnetization was increased by optimizing the polymer concentration. Furthermore, the 3-(4,5-dimethylthiazol-2-yl-2-5-diphenyltetrazolium bromide (MTT-assay demonstrated that these MIONs were highly biocompatible and they could be successfully coupled with fluorescent dye Rhodamine due to the formation of amide bond between carboxylic acid groups of MIONs and amine groups of dye. The obtained results indicated that these multifunctional MIONs with rich surface chemistry exhibit admirable potential in biomedical applications.

  15. Crystallization and preliminary characterization of three different crystal forms of human saposin C heterologously expressed in Pichia pastoris

    International Nuclear Information System (INIS)

    Schultz-Heienbrok, Robert; Remmel, Natascha; Klingenstein, R.; Rossocha, Maksim; Sandhoff, Konrad; Saenger, Wolfram; Maier, Timm

    2006-01-01

    Three different crystal forms were obtained of human saposin C. The structures could not be determined by molecular replacement using known solution structures of the protein as search models, supporting the notion of a highly flexible protein. The amphiphilic saposin proteins (A, B, C and D) act at the lipid–water interface in lysosomes, mediating the hydrolysis of membrane building blocks by water-soluble exohydrolases. Human saposin C activates glucocerebrosidase and β-galactosylceramidase. The protein has been expressed in Pichia pastoris, purified and crystallized in three different crystal forms, diffracting to a maximum resolution of 2.5 Å. Hexagonal crystals grew from 2-propanol-containing solution and contain a single molecule in the asymmetric unit according to the Matthews coefficient. Orthorhombic and tetragonal crystals were both obtained with pentaerythritol ethoxylate and are predicted to contain two molecules in the asymmetric unit. Attempts to determine the respective crystal structures by molecular replacement using either the known NMR structure of human saposin C or a related crystal structure as search models have so far failed. The failure of the molecular-replacement method is attributed to conformational changes of the protein, which are known to be required for its biological activity. Crystal structures of human saposin C therefore might be the key to mapping out the conformational trajectory of saposin-like proteins

  16. Synthesis of Cu/SiO2 Core-Shell Particles Using Hyperbranched Polyester as Template and Dispersant

    Science.gov (United States)

    Han, Wensong

    2017-07-01

    Third-generation hyperbranched polyester (HBPE3) was synthesized by stepwise polymerization with N, N-diethylol-3-amine methylpropionate as AB2 monomer and pentaerythritol as core molecule. Then, Cu particles were prepared by reduction of copper nitrate with ascorbic acid in aqueous solution using HBPE3 as template. Finally, Cu/SiO2 particles were prepared by coating silica on the surface of Cu particles. The structure and morphology of the samples were characterized by Fourier-transform infrared (FT-IR) spectrometry, x-ray diffraction (XRD) analysis, transmission electron microscopy (TEM), scanning electron microscopy (SEM), and thermogravimetric analysis (TGA). The results confirmed the formation of the silica coating on the surface of Cu and that the Cu/SiO2 particles had spherical shape with particle size in the range of 0.8 μm to 2 μm. Compared with pure Cu, the synthesized Cu/SiO2 core-shell particles exhibited better oxidation resistance at high temperature. Moreover, the oxidation resistance of the Cu/SiO2 particles increased significantly with increasing tetraethyl orthosilicate (TEOS) concentration.

  17. The MDI-Mediated Lateral Crosslinking of Polyurethane Copolymer and the Impact on Tensile Properties and Shape Memory Effect

    International Nuclear Information System (INIS)

    Chung, Yong Chan; Chung, Hyang Mi; Choi, Jae Won; Chun, Byoung Chul

    2012-01-01

    The maximum stress and strain at break remained high and stable after MDI-mediated crosslinking. Similarly, shape recovery and shape retention tests also showed excellent and reproducible results. The MDI-mediated crosslinking was responsible for the interesting tensile and shape memory results. Therefore, it was demonstrated in this investigation that the allophanate type crosslinking, unlike previous misleading information, was possible under the mild reaction conditions. Polyurethane (PU) has long been investigated due to its excellent mechanical properties, shape memory effect, and biocompatibility, and was grafted with pendant functional groups to tailor the polymer characteristics without affecting their basic structure. Actually, polyethyleneglycol has been grafted to polyurethane to improve biocompatibility in biomedical applications, and low temperature flexibility could be improved by the pendant naphthol group grafted to PU. In the field of shape memory polyurethane, mechanical and shape memory properties could be improved by terminal crosslinking with glycerol, pentaerythritol, and dextrin. Alternatively, a flexible crosslinking method was devised to demonstrate both high mechanical strength and shape recovery

  18. Fabrication, thermal properties and thermal stabilities of microencapsulated n-alkane with poly(lauryl methacrylate) as shell

    Energy Technology Data Exchange (ETDEWEB)

    Qiu, Xiaolin, E-mail: shirleyqiu2009@gmail.com [Jiangsu Key Laboratory of Advanced Food Manufacturing Equipment and Technology, School of Mechanical Engineering, Jiangnan University, Wuxi 214122 (China); Lu, Lixin; Wang, Ju [Jiangsu Key Laboratory of Advanced Food Manufacturing Equipment and Technology, School of Mechanical Engineering, Jiangnan University, Wuxi 214122 (China); Tang, Guoyi [Advanced Materials Institute and Clearer Production Key Laboratory, Graduate School at Shenzhen, Tsinghua University, Shenzhen 518055 (China); Key Laboratory of Advanced Materials, Department of Materials Science and Engineering, Tsinghua University, Haidian District, Beijing 100084 (China); Song, Guolin [Advanced Materials Institute and Clearer Production Key Laboratory, Graduate School at Shenzhen, Tsinghua University, Shenzhen 518055 (China)

    2015-11-20

    Highlights: • Microencapsulation of octadecane and paraffin by crosslinked poly(lauryl methacrylate). • Octadecane microcapsules have a melting enthalpy of about 118 J g{sup −1}. • Weight loss temperatures of the microcapsules were increased by 67 °C and 28 °C. • Phase change enthalpies decreased by around 10 wt% after 500 thermal cycles. • Foams with microcapsules can be applied for passive temperature control. - Abstract: Microencapsulation of n-octadecane or paraffin with poly(lauryl methacrylate) (PLMA) shell was performed by a suspension-like polymerization. The polymer shell was crosslinked by pentaerythritol tetraacrylate (PETRA). The surface morphologies of microcapsules were investigated by scanning electron microscopy (SEM). Phase change properties, thermal reliabilities and thermal stabilities of microcapsules were determined by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). The n-octadecane microcapsule exhibits higher melting enthalpy (118.0 J g{sup −1}) and crystallization enthalpy (108.3 J g{sup −1}) compared with the paraffin microcapsule. The thermal resistant temperatures were enhanced by more than 25 °C when n-alkanes were microencapsulated by PLMA. The PCM contents of microcapsules decreased by less than 4 wt% and 6 wt% after 500 and 1000 thermal cycles, respectively. Heat-up experiments indicated that microcapsule-treated foams exhibited upgraded thermal regulation capacities. Consequently, microencapsulated n-octadecane or paraffin with PLMA as shell possesses good potentials for heat storage and thermal regulation.

  19. Preparation, thermal properties and thermal reliabilities of microencapsulated n-octadecane with acrylic-based polymer shells for thermal energy storage

    International Nuclear Information System (INIS)

    Qiu, Xiaolin; Song, Guolin; Chu, Xiaodong; Li, Xuezhu; Tang, Guoyi

    2013-01-01

    Highlights: ► n-Octadecane was encapsulated by p(butyl methacrylate) (PBMA) and p(butyl acrylate). ► Microcapsules using divinylbenzene as crosslinking agent have better quality. ► Microcapsule with butyl methacrylate–divinylbenzene has highest latent heat. ► Microcapsule with butyl methacrylate–divinylbenzene has greatest thermal stability. ► Phase change temperatures and enthalpies of the microcapsules varied little after thermal cycle. - Abstract: Microencapsulation of n-octadecane with crosslinked p(butyl methacrylate) (PBMA) and p(butyl acrylate) (PBA) as shells for thermal energy storage was carried out by a suspension-like polymerization. Divinylbenzene (DVB) and pentaerythritol triacrylate (PETA) were employed as crosslinking agents. The surface morphologies of the microencapsulated phase change materials (microPCMs) were studied by scanning electron microscopy (SEM). Thermal properties, thermal reliabilities and thermal stabilities of the as-prepared microPCMs were investigated by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). The microPCMs prepared by using DVB exhibit greater heat capacities and higher thermal stabilities compared with those prepared by using PETA. The thermal resistant temperature of the microPCM with BMA–DVB polymer was up to 248 °C. The phase change temperatures and latent heats of all the as-prepared microcapsules varied little after 1000 thermal cycles.

  20. A novel intumescent flame retardant-functionalized graphene: Nanocomposite synthesis, characterization, and flammability properties

    International Nuclear Information System (INIS)

    Huang, Guobo; Chen, Suqing; Tang, Shouwan; Gao, Jianrong

    2012-01-01

    An intumescent flame retardant, poly(piperazine spirocyclic pentaerythritol bisphosphonate) (PPSPB), has been covalently grafted onto the surfaces of graphene oxide (GO) to obtain GO–PPSPB and according nanocomposites were prepared via solvent blending. The X-ray diffraction (XRD) and transmission electron microscopy (TEM) results show that the chemically reduced GO–PPSPB (CRG–PPSPB) can achieve better dispersion in the ethylene vinyl acetate copolymer (EVA) matrix and exfoliated EVA/CRG–PPSPB nanocomposites are formed. The results from thermogravimetric analysis (TGA) and cone calorimeter tests indicate that CRG–PPSPB improve thermal stability and reduce obviously the flammability (including peak heat release rate (PHRR), total heat release (THR), average mass loss rate (AMLR), etc.) of EVA. Compared with pure EVA resin, the PHRR of the EVA/CRG–PPSPB nanocomposites filled with 1 wt% CRG–PPSPB is reduced by about 56%. The SEM images show that a compact, dense and uniform intumescent char is formed for EVA/CRG–PPSPB nanocomposites after combustion. The functionalization of graphene by intumescent flame retardant PPSPB can improve both the dispersion of graphene sheets in the polymer matrix and flame retardancy of the nanocomposites. -- Highlights: ► Graphene oxide were modified with intumescent flame retardant PPSPB. ► EVA/CRG–PPSPB nanocomposites were prepared via solvent blending. ► CRG–PPSPB improved the flame retardancy of EVA nanocomposites.

  1. Synthesis and carbonization chemistry of a phosphorous–nitrogen based intumescent flame retardant

    International Nuclear Information System (INIS)

    Ma, Haiyun; Fang, Zhengping

    2012-01-01

    Graphical abstract: The carbonization chemistry and mechanism of a novel synthesized intumescent flame retardant. The final chars showed a complex P-O-Ph and aromatic/graphitic structure containing architecture. Highlights: ► The IFR synthesized is polymeric and has high molecular weight. ► The IFR has a higher thermal stability than most of the commercial IFRs. ► The final chars of IFR showed a complex P-O-Ph and aromatic/graphitic structure. - Abstract: In this work, a polymeric phosphorous–nitrogen containing intumescent flame retardant, named poly(diaminodiphenyl methane spirocyclic pentaerythritol bisphosphonate) (PDSPB), was synthesized. The carbonization chemistry was investigated. FTIR and 1 H NMR were used to confirm the chemical structure of PDSPB. Thermogravimetric analysis (TGA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), in situ FTIR and energy dispersive X-ray (EDX) were used to investigate and monitor the chemical structural changes during thermal degradation. PDSPB demonstrated a three-step degradation behavior. PDSPB oligomers continuously polymerized and generated a higher macromolecular weight during the first step (200–250 °C). The phosphate ester bonds were broken down and phosphoric acid was released which dehydrated the carbon source to form chars during the second step (280–320 °C). The residues will be further degraded and form final chars during the final weight loss step (400–450 °C). The final chars showed a complex P-O-Ph and aromatic/graphitic structure containing architecture.

  2. Recognition of explosives fingerprints on objects for courier services using machine learning methods and laser-induced breakdown spectroscopy.

    Science.gov (United States)

    Moros, J; Serrano, J; Gallego, F J; Macías, J; Laserna, J J

    2013-06-15

    During recent years laser-induced breakdown spectroscopy (LIBS) has been considered one of the techniques with larger ability for trace detection of explosives. However, despite of the high sensitivity exhibited for this application, LIBS suffers from a limited selectivity due to difficulties in assigning the molecular origin of the spectral emissions observed. This circumstance makes the recognition of fingerprints a latent challenging problem. In the present manuscript the sorting of six explosives (chloratite, ammonal, DNT, TNT, RDX and PETN) against a broad list of potential harmless interferents (butter, fuel oil, hand cream, olive oil, …), all of them in the form of fingerprints deposited on the surfaces of objects for courier services, has been carried out. When LIBS information is processed through a multi-stage architecture algorithm built from a suitable combination of 3 learning classifiers, an unknown fingerprint may be labeled into a particular class. Neural network classifiers trained by the Levenberg-Marquardt rule were decided within 3D scatter plots projected onto the subspace of the most useful features extracted from the LIBS spectra. Experimental results demonstrate that the presented algorithm sorts fingerprints according to their hazardous character, although its spectral information is virtually identical in appearance, with rates of false negatives and false positives not beyond of 10%. These reported achievements mean a step forward in the technology readiness level of LIBS for this complex application related to defense, homeland security and force protection. Copyright © 2013 Elsevier B.V. All rights reserved.

  3. Design Considerations for a Portable Raman Probe Spectrometer for Field Forensics

    Directory of Open Access Journals (Sweden)

    James F. Kelly

    2012-01-01

    Full Text Available Raman spectroscopy has been shown to be a viable method for explosives detection. Currently most forensic Raman systems are either large, powerful instruments for laboratory experiments or handheld instruments for in situ point detection. We have chosen to examine the performance of certain benchtop Raman probe systems with the goal of developing an inexpensive, portable system that could be used to operate in a field forensics laboratory to examine explosives-related residues or samples. To this end, a rugged, low distortion line imaging dispersive Raman spectrograph was configured to work at 830 nm laser excitation and was used to determine whether the composition of thin films of plastic explosives or small (e.g., ≤10 μm particles of RDX or other explosives or oxidizers can be detected, identified, and quantified in the field. With 300 mW excitation energy, concentrations of RDX and PETN can be detected and reconstructed in the case of thin Semtex smears, but further work is needed to push detection limits of areal dosages to the ~1 μg/cm2 level. We describe the performance of several probe/spectrograph combinations and show preliminary data for particle detection, calibration and detection linearity for mixed compounds, and so forth.

  4. Advanced recognition of explosives in traces on polymer surfaces using LIBS and supervised learning classifiers.

    Science.gov (United States)

    Serrano, Jorge; Moros, Javier; Sánchez, Carlos; Macías, Jorge; Laserna, J Javier

    2014-01-02

    The large similarity existing in the spectral emissions collected from organic compounds by laser-induced breakdown spectroscopy (LIBS) is a limiting factor for the use of this technology in the real world. Specifically, among the most ambitious challenges of today's LIBS involves the recognition of an organic residue when neglected on the surface of an object of identical nature. Under these circumstances, the development of an efficient algorithm to disclose the minute differences within this highly complex spectral information is crucial for a realistic application of LIBS in countering explosive threats. An approach cemented on scatter plots of characteristic emission features has been developed to identify organic explosives when located on polymeric surfaces (teflon, nylon and polyethylene). By using selected spectral variables, the approach allows to design a concise classifier for alerting when one of four explosives (DNT, TNT, RDX and PETN) is present on the surface of the polymer. Ordinary products (butter, fuel oil, hand cream, olive oil and motor oil) cause no confusion in the decisions taken by the classifier. With rates of false negatives and false positives below 5%, results demonstrate that the classification algorithm enables to label residues according to their harmful nature in the most demanding scenario for a LIBS sensor. Copyright © 2013 Elsevier B.V. All rights reserved.

  5. Long-Wave Infrared (LWIR) Molecular Laser-Induced Breakdown Spectroscopy (LIBS) Emissions of Thin Solid Explosive Powder Films Deposited on Aluminum Substrates.

    Science.gov (United States)

    Yang, Clayton S-C; Jin, Feng; Trivedi, Sudhir B; Brown, Ei E; Hommerich, Uwe; Tripathi, Ashish; Samuels, Alan C

    2017-04-01

    Thin solid films made of high nitro (NO 2 )/nitrate (NO 3 ) content explosives were deposited on sand-blasted aluminum substrates and then studied using a mercury-cadmium-telluride (MCT) linear array detection system that is capable of rapidly capturing a broad spectrum of atomic and molecular laser-induced breakdown spectroscopy (LIBS) emissions in the long-wave infrared region (LWIR; ∼5.6-10 µm). Despite the similarities of their chemical compositions and structures, thin films of three commonly used explosives (RDX, HMX, and PETN) studied in this work can be rapidly identified in the ambient air by their molecular LIBS emission signatures in the LWIR region. A preliminary assessment of the detection limit for a thin film of RDX on aluminum appears to be much lower than 60 µg/cm 2 . This LWIR LIBS setup is capable of rapidly probing and charactering samples without the need for elaborate sample preparation and also offers the possibility of a simultaneous ultraviolet visible and LWIR LIBS measurement.

  6. Ambient Pressure Laser Desorption—Chemical Ionization Mass Spectrometry for Fast and Reliable Detection of Explosives, Drugs, and Their Precursors

    Directory of Open Access Journals (Sweden)

    René Reiss

    2018-06-01

    Full Text Available Fast and reliable information is crucial for first responders to draw correct conclusions at crime scenes. An ambient pressure laser desorption (APLD mass spectrometer is introduced for this scenario, which enables detecting substances on surfaces without sample pretreatment. It is especially useful for substances with low vapor pressure and thermolabile ones. The APLD allows for the separation of desorption and ionization into two steps and, therefore, both can be optimized separately. Within this work, an improved version of the developed system is shown that achieves limits of detection (LOD down to 500 pg while remaining fast and flexible. Furthermore, realistic scenarios are applied to prove the usability of this system in real-world issues. For this purpose, post-blast residues of a bomb from the Second World War were analyzed, and the presence of PETN was proven without sample pretreatment. In addition, the analyzable substance range could be expanded by various drugs and drug precursors. Thus, the presented instrumentation can be utilized for an increased number of forensically important compound classes without changing the setup. Drug precursors revealed a LOD ranging from 6 to 100 ng. Drugs such as cocaine hydrochloride, heroin, (3,4-methylendioxy-methamphetamine hydrochloride (MDMA hydrochloride, and others exhibit a LOD between 10 to 200 ng.

  7. Development of ab initio techniques critical for future science-based explosives R&D

    Energy Technology Data Exchange (ETDEWEB)

    Wixom, Ryan R. [Sandia National Lab. (SNL-CA), Livermore, CA (United States); Mattsson, Ann Elisabet [Sandia National Lab. (SNL-CA), Livermore, CA (United States)

    2013-10-01

    Density Functional Theory (DFT) has emerged as an indispensable tool in materials research, since it can accurately predict properties of a wide variety of materials at both equilibrium and extreme conditions. However, for organic molecular crystal explosives, successful application of DFT has largely failed due to the inability of current exchange-correlation functionals to correctly describe intermolecular van der Waals (vdWs) forces. Despite this, we have discovered that even with no treatment of vdWs bonding, the AM05 functional and DFT based molecular dynamics (MD) could be used to study the properties of molecular crystals under compression. We have used DFT-MD to predict the unreacted Hugoniots for PETN and HNS and validated the results by comparison with crystalline and porous experimental data. Since we are also interested in applying DFT methods to study the equilibrium volume properties of explosives, we studied the nature of the vdWs bonding in pursuit of creating a new DFT functional capable of accurately describing equilibrium bonding of molecular crystals. In this report we discuss our results for computing shock Hugoniots of molecular crystals and also what was learned about the nature of bonding in these materials.

  8. Fessibility Study on Nitrogen in Explosives using X-ray Photoelectron Spectroscopy: Chemical Fertilizer

    International Nuclear Information System (INIS)

    Dararutana, P.

    2014-01-01

    It was known that an explosive is defined as a material which contains a large amount of energy stored in chemical bonds. The energetic stability of gaseous products, and hence, their generation come from the strong bond formation of carbon (mono/di)oxide and (di)nitrogen. Consequently, most commercial explosives are contained -NO 2 , -ONO 2 and/or -NHNO 2 groups which when detonated release gases like the aforementioned ones, e.g., nitroglycerin, TNT, HMX, PETN, nitrocellulose, etc. It was revealed that the elemental compositions, especially N was found in most of the explosive and fertilizer. Chemical fertilizers that used as explosive stimulants were analyzed using X-ray photoelectron spectroscopy (XPS) and scanning electron microscope coupled with energy-dispersive X-ray fluorescence spectroscopy (SEM-EDS). XPS spectra showed relatively high amount of nitrogen (N) in the various samples, especially sample #6 and #7. In addition, the elemental analysis revealed the presence of trace elements. Explosives and fertilizers have differences in specific compositions. It can be concluded that these methods seem to be used as a fingerprint examination to identify various kinds of explosives and fertilizers.

  9. The dynamic pressure measurements of the nuclear reactor coolant for condition-based maintenance of the reactor

    International Nuclear Information System (INIS)

    Es-Saheb, M.H.H.

    1990-01-01

    The condition-based maintenance of the nuclear reactor, by monitoring and measuring the instantaneous dynamic pressure distribution of the coolant (water) impact on the solid surfaces of the reactor during operation is presented. The behaviour of water domes (jets) produced by underwater explosions of small changes of P.E.T.N. at various depths in two different size cylindrical containers, which simulate the nuclear reactor, is investigated. Water surface domes (jets) from the underwater explosions are photographed. Depending on the depth of the charge, curved and flat top jets of up to 455 mm diameter and impact speeds of up to 70 m/sec. are observed. The instabilities in the dome surfaces are observed and the instantaneous profiles are analysed. It is found that, in all cases tested, the maximum pressure takes place at the center of the jet and could reach up to 3.0 times the on-dimensional impact pressure value. The use of their measurements, as online monitoring for condition-based maintenance and design-out maintenance is discussed. 18 refs

  10. Combustion of Shock-Dispersed Flake Aluminum - High-Speed Visualization

    Energy Technology Data Exchange (ETDEWEB)

    Neuwald, P; Reichenbach, H; Kuhl, A

    2006-06-19

    Charges of 0.5 g PETN were used to disperse 1 g of flake aluminum in a rectangular test chamber of 4 liter inner volume and inner dimensions of approximately 10 cm x 10 cm x 40 cm. The subsequent combustion of the flake aluminum with the ambient air in the chamber gave rise to a highly luminous flame. The evolution of the luminous region was studied by means of high-speed cinematography. The high-speed camera is responsive to a broad spectral range in the visible and near infra-red. For a number of tests this response range was narrowed down by means of a band-pass filter with a center wavelength of 488 nm and a half-width of 23 nm. The corresponding images were expected to have a stronger temperature dependence than images obtained without the filter, thus providing better capability to highlight hot-spots. Emission in the range of the pass-band of the filter can be due to continuous thermal radiation from hot Al and Al{sub 2}O{sub 3} particles or to molecular band emission from gaseous AlO. A time-resolving spectrometer was improvised to inspect this topic. The results suggest that AlO emission occurs, but that the continuous spectrum is the dominating effect in our experiments.

  11. Effectiveness of laser sources for contactless sampling of explosives

    Science.gov (United States)

    Akmalov, Artem E.; Chistyakov, Alexander A.; Kotkovskii, Gennadii E.

    2016-05-01

    A mass-spectrometric study of photo processes initiated by ultraviolet (UV) laser radiation in explosives adsorbed on metal and dielectric substrates has been performed. A calibrated quadrupole mass spectrometer was used to determine a value of activation energy of desorption and a quantity of explosives desorbed by laser radiation. A special vacuumoptical module was elaborated and integrated into a vacuum mass-spectrometric system to focus the laser beam on a sample. It has been shown that the action of nanosecond laser radiation set at q= 107 - 108 W/cm2, λ=266 nm on adsorbed layers of molecules of trinitrotoluene (TNT ) and pentaerytritoltetranitrate (PETN) leads not only to an effective desorption, but also to the non-equilibrium dissociation of molecules with the formation of nitrogen oxide NO. The cyclotrimethylenetrinitramine (RDX) dissociation products are observed only at high laser intensities (q> 109 W/cm2) thus indicating the thermal nature of dissociation, whereas desorption of RDX is observed even at q> 107 W/cm2 from all substrates. Desorption is not observed for cyclotetramethylenetetranitramine (HMX) under single pulse action: the dissociation products NO and NO2 are registered only, whereas irradiation at 10Hz is quite effective for HMX desorption. The results clearly demonstrate a high efficiency of nanosecond laser radiation with λ = 266 nm, q ~ 107 - 108 W/cm2, Epulse= 1mJ for desorption of molecules of explosives from various surfaces.

  12. New directions in the science and technology of advanced sheet explosive formulations and the key energetic materials used in the processing of sheet explosives: Emerging trends.

    Science.gov (United States)

    Talawar, M B; Jangid, S K; Nath, T; Sinha, R K; Asthana, S N

    2015-12-30

    This review presents the work carried out by the international community in the area of sheet explosive formulations and its applications in various systems. The sheet explosive is also named as PBXs and is a composite material in which solid explosive particles like RDX, HMX or PETN are dispersed in a polymeric matrix, forms a flexible material that can be rolled/cut into sheet form which can be applied to any complex contour. The designed sheet explosive must possess characteristic properties such as flexible, cuttable, water proof, easily initiable, and safe handling. The sheet explosives are being used for protecting tanks (ERA), light combat vehicle and futuristic infantry carrier vehicle from different attacking war heads etc. Besides, sheet explosives find wide applications in demolition of bridges, ships, cutting and metal cladding. This review also covers the aspects such as risks and hazard analysis during the processing of sheet explosive formulations, effect of ageing on sheet explosives, detection and analysis of sheet explosive ingredients and the R&D efforts of Indian researchers in the development of sheet explosive formulations. To the best of our knowledge, there has been no review article published in the literature in the area of sheet explosives. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Rapid expansion and fracture of metallic cylinders driven by explosive loads

    International Nuclear Information System (INIS)

    Hiroe, T.; Fujiwara, K.; Abe, T.; Yoshida, M.

    2004-01-01

    Smooth walled tubular specimens of stainless steel and low-carbon steels were explosively expanded to fragmentation. The driver was a column of the high explosive PETN inserted into the central bore and initiated by exploding a fine copper wire using a discharge current from a high-voltage capacitor bank. The variation of wall thickness and the effect of different explosive driver diameters are reported. A fully charged casing model was also exploded with initiation at the end surface for comparison. Streak and framing photos show both radially and axially symmetric expansion of cylinders at average strain rates of above 104 s-1 and a wall velocity of 417-1550 m/s. Some framing photos indicate the initiation and spacing of fractures during the bursting of the cylinders. Hydro codes have been applied to simulate the experimental behavior of the cylinders, examining numerical stresses, deformation and fracture criteria. Most of the fragments were successfully recovered inside a cushion-filled chamber, and the circumferential fracture spacing of measured fragments is investigated using a fragmentation model

  14. Computer simulation for prediction of performance and thermodynamic parameters of high energy materials

    International Nuclear Information System (INIS)

    Muthurajan, H.; Sivabalan, R.; Talawar, M.B.; Asthana, S.N.

    2004-01-01

    A new code viz., Linear Output Thermodynamic User-friendly Software for Energetic Systems (LOTUSES) developed during this work predicts the theoretical performance parameters such as density, detonation factor, velocity of detonation, detonation pressure and thermodynamic properties such as heat of detonation, heat of explosion, volume of explosion gaseous products. The same code also assists in the prediction of possible explosive decomposition products after explosion and power index. The developed code has been validated by calculating the parameters of standard explosives such as TNT, PETN, RDX, and HMX. Theoretically predicated parameters are accurate to the order of ±5% deviation. To the best of our knowledge, no such code is reported in literature which can predict a wide range of characteristics of known/unknown explosives with minimum input parameters. The code can be used to obtain thermochemical and performance parameters of high energy materials (HEMs) with reasonable accuracy. The code has been developed in Visual Basic having enhanced windows environment, and thereby advantages over the conventional codes, written in Fortran. The theoretically predicted HEMs performance can be directly printed as well as stored in text (.txt) or HTML (.htm) or Microsoft Word (.doc) or Adobe Acrobat (.pdf) format in the hard disk. The output can also be copied into the Random Access Memory as clipboard text which can be imported/pasted in other software as in the case of other codes

  15. Explosives and chemical warfare agents - detection and analysis with PTR-MS

    Energy Technology Data Exchange (ETDEWEB)

    Sulzer, Philipp; Juerschik, Simone; Jaksch, Stefan; Jordan, Alfons; Hanel, Gernot; Hartungen, Eugen; Seehauser, Hans; Maerk, Lukas; Haidacher, Stefan; Schottkowsky, Ralf [IONICON Analytik GmbH, Innsbruck (Austria); Petersson, Fredrik [Institut fuer Ionenphysik und Angewandte Physik, Leopold-Franzens Universitaet Innsbruck (Austria); Maerk, Tilmann [IONICON Analytik GmbH, Innsbruck (Austria); Institut fuer Ionenphysik und Angewandte Physik, Leopold-Franzens Universitaet Innsbruck (Austria)

    2010-07-01

    We utilized a recently developed high sensitivity PTR-MS instrument equipped with a high resolution time-of-flight mass analyzer for detailed investigations on explosives and chemical warfare agents (CWAs). We show that with this so called PTR-TOF 8000 it is possible to identify solid explosives (RDX, TNT, HMX, PETN and Semtex A) by analyzing the headspace above small quantities of samples at room temperature and from trace quantities not visible to the naked eye placed on surfaces. As the mentioned solid explosives possess very low vapor pressures, the main challenge for detecting them in the gas phase is to provide an instrument with a sufficient sensitivity. CWAs on the other side have very high vapor pressures but are difficult to identify unambiguously as their nominal molecular masses are usually comparably small and therefore hard to distinguish from harmless everyday-compounds (e.g. mustard gas: 159 g/mol). In the present work we demonstrate that we can detect a broad range of dangerous substances, ranging from the CWA mustard gas to the explosive HMX.

  16. Polymyxin susceptibility testing, interpretative breakpoints and resistance mechanisms: An update.

    Science.gov (United States)

    Bakthavatchalam, Yamuna Devi; Pragasam, Agila Kumari; Biswas, Indranil; Veeraraghavan, Balaji

    2018-03-01

    Emerging multidrug-resistant (MDR) nosocomial pathogens are a great threat. Polymyxins, an old class of cationic polypeptide antibiotic, are considered as last-resort drugs in treating infections caused by MDR Gram-negative bacteria. Increased use of polymyxins in treating critically ill patients necessitates routine polymyxin susceptibility testing. However, susceptibility testing both of colistin and polymyxin B (PMB) is challenging. In this review, currently available susceptibility testing methods are briefly discussed. The multicomponent composition of colistin and PMB significantly influences susceptibility testing. In addition, poor diffusion in the agar medium, adsorption to microtitre plates and the synergistic effect of the surfactant polysorbate 80 with polymyxins have a great impact on the performance of susceptibility testing methods This review also describes recently identified chromosomal resistance mechanisms, including modification of lipopolysaccharide (LPS) with 4-amino-4-deoxy-l-arabinose (L-Ara4-N) and phosphoethanolamine (pEtN) resulting in alteration of the negative charge, as well as the plasmid-mediated colistin resistance determinants mcr-1, mcr-1.2, mcr-2 and mcr-3. Copyright © 2017 International Society for Chemotherapy of Infection and Cancer. Published by Elsevier Ltd. All rights reserved.

  17. A comparison of the efficacy of various antioxidants on the oxidative stability of irradiated polyethylene.

    Science.gov (United States)

    Hope, Natalie; Bellare, Anuj

    2015-03-01

    Ultrahigh-molecular-weight polyethylene (UHMWPE) is subjected to radiation crosslinking to form highly crosslinked polyethylene (HXLPE), which has improved wear resistance. First-generation HXLPE was subjected to thermal treatment to reduce or quench free radicals that can induce long-term oxidative degeneration. Most recently, antioxidants have been added to HXLPE to induce oxidative resistance rather than by thermal treatment. However, antioxidants can interfere with the efficiency of radiation crosslinking. We sought to identify (1) which antioxidant from among those tested (vitamin E, β-carotene, butylated hydroxytoluene, or pentaerythritol tetrakis [methylene-3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate]) causes the least reduction of crosslinking; (2) which promotes the greatest oxidative stability; and (3) which had the lowest ratio of oxidation index to crosslink density. Medical-grade polyethylene (PE) resin was blended with 0.1 weight % of the following stabilizers: alpha tocopherol (vitamin E), β-carotene, butylated hydroxytoluene (BHT), and pentaerythritol tetrakis [methylene-3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] (a hindered phenol antioxidant [HPAO]). These blends were compression-molded into sheets and subjected to electron beam irradiation to a dose of 100 kGy. Equilibrium swelling experiments were conducted to calculate crosslink density. Each PE was subjected to accelerated aging for a period of 2 weeks and Fourier transform infrared spectroscopy was used to measure the maximum oxidation. Statistical analysis was conducted using analysis of variance with Fisher's protected least significant difference in which a p value of tested (1.49, ES = 1.94; 95% CI, 1.32-1.66) followed by HPAO-PE (1.70, ES = 1.52; 95% CI, 1.61-1.80), vitamin E-PE (2.21, ES = 0.52; 95% CI, 2.05-2.38), and β-carotene-PE (2.69, ES = -0.43; 95% CI, 2.46-2.93) compared with control PE (2.47, 95% CI, 2.07-2.88) with β-carotene (p = 0.208) and vitamin E (p = 0

  18. 聚苯乙烯包覆正十四醇微胶囊的制备及表征%Preparation and Characterization of Myristyl Alcohol Microcapsules Coated with Polystyrene

    Institute of Scientific and Technical Information of China (English)

    黄云峰; 闵洁; 叶琳; 王丽萍; 李帅涛; 宋晓秋

    2017-01-01

    选用过硫酸钾(K2S2O8)为引发剂,司班80(Span 80)和吐温80(Tween80)为复配乳化剂,聚乙烯吡咯烷酮K30(PVP-K30)为分散剂,季戊四醇四丙烯酸酯(PETA)为交联剂,采用乳液聚合法制备出了以正十四醇(MA)为芯材,聚苯乙烯(PS)为壁材的正十四醇-聚苯乙烯相变微胶囊(MA/PS微胶囊);通过差示扫描量热仪、扫描电镜、傅里叶变换红外光谱仪和热重分析仪等仪器对制备的微胶囊进行检测袁征.结果表明,当聚乙烯吡咯烷酮K30和复配乳化剂(m(Span80):m(Tween80)=3:13)加入量分别为正十四醇质量的5%和4%,过硫酸钾和季戊四醇四丙烯酸酯加入量分别为苯乙烯单体质量的10%和37.5%,芯壁比为2.5:1,搅拌速度为1000 r/min时,所制备的MA/PS微胶囊具有良好的热稳定性和致密性.%Myristyl alcohol-polystyrene phase change microcapsules (MA/PS microcapsules) were prepared by emulsion polymerization with myristyl alcohol (MA) as core material,polystyrene (PS) as outer shell,potassium peroxodisulfate (K2S2O8) as initiator,Span 80 and Tween 80 as complex emulsifiers,the polyvinyl pyrrolidone K30 (PVP-K30) as dispersant and pentaerythritol tetraacrylate (PETA) as crosslinking agent.The microcapsules were characterized by differential scanning calorimetry (DSC),scanning electron microscopy (SEM),Fourier transform infrared spectroscopy (FT-IR),thermogravimetric analyzer (TGA),et al.The results show that the prepared MA/ PS microcapsules have good thermal stability and compactness when the amount of polyvinylpyrrolidone K30 and compound emulsifier (m(Span80):m(Tween80)=3:13) is 5% and 4% of the mass of myristyl alcohol,respectively,potassium persulfate and pentaerythritol tetraacrylate are added 10 % and 37.5 % of the mass of styrene monomer respectively,the ratio of core to wall is 2.5:1 and the stirring speed is 1000 r/min.

  19. 壁材交联对相变微胶囊的性能调控%Performance regulation of phase change microcapsules by cross-linking of wall material

    Institute of Scientific and Technical Information of China (English)

    管羽; 张维; 刘金树

    2017-01-01

    In order to investigate the effect of wall material composition on the performance of phase change microcapsules,a mixture of solid and liquid paraffin is used as the core material and methyl methacrylate as the wall material to prepare phase change material microcapsules by suspension polymerization method.Pentaerythritol tetraacrylate and allyl methacrylate are crosslinked with methyl methacrylate to obtain phase change microcapsules with different wall materials,and then to achieve the regulation of microcapsule performance.The results of scanning electron microscopy (SEM) show that the addition of crosslinking agents can effectively improve the regularity and surface smoothness of phase change microcapsules,as well as the uniformity of particle size distribution.The results of thermogravimetric analysis (TG) and differential scanning calorimetry (DSC) analysis show that the crosslinking agents can significantly reduce the mass loss rate of the microcapsules at high temperature,increase the decomposition temperature range,enhance the stability of the wall material and improve the coating efficiency of the wall material.Compared with the untreated microcapsules,the phase change enthalpy decreased.When adding 1.0 g pentaerythritol tetraacrylate,the obtained microcapsules have good dispersibility,regular spherical shap.e,smooth surface,particle size of 1.0~1.5 μm,good thermal stability,can withstand 155 ℃ high temperature,and the maximum enthalpy of phase change is 29.643 J/g.%为探讨壁材组成对相变微胶囊性能的调控作用,选用固液混合石蜡为芯材,甲基丙烯酸甲酯为壁材,利用悬浮聚合法制备相变材料微胶囊.加入季戊四醇四丙烯酸酯和甲基丙烯酸烯丙酯作为交联剂,与甲基丙烯酸甲酯进行交联共聚,得到不同壁材组成的相变微胶囊,进而实现对微胶囊性能的调控.扫描电镜(SEM)结果表明,交联剂的加入能够有效提高相变微胶囊的规整性和表

  20. In-situ Polymerization-modification Process and Foaming of Poly(ethylene terephthalate)

    Institute of Scientific and Technical Information of China (English)

    仲华; 奚桢浩; 刘涛; 赵玲

    2013-01-01

    Most of traditional linear poly(ethylene terephthalate) (PET) resins of relatively low molecular mass and narrow molecular mass distribution have low melt strength at foaming temperatures, which are not enough to support and keep cells. An in-situ polymerization-modification process with esterification and polycondensation stages was performed in a 2 L batch stirred reactor using pyromellitic dianhydride (PMDA) or pentaerythritol (PENTA) as modifying monomers to obtain PETs with high melt strength. The influence of amounts of modifying monomers on the properties of modified PET was investigated. It was found that the selected modifying monomers could effectively introduce branched structures into the modified PETs and improve their melt strength. With in-creasing the amount of the modifying monomer, the melt strength of the modified PET increased. But when the amount of PENTA reached 0.35%or PMDA reached 0.9%, crosslinking phenomenon was observed in the modified PET. Supercritical carbon dioxide (ScCO2) was employed as physical foaming agent to evaluate the foaming ability of modified PETs. The modified PETs had good foaming properties at 14 MPa of CO2 pressure with foaming tem-perature ranging from 265 °C to 280 °C. SEM micrographs demonstrated that both modified PET foams had ho-mogeneous cellular structures, with cell diameter ranging from 35 μm to 49 μm for PENTA modified PETs and 38μm to 57μm for PMDA modified ones. Correspondingly, the cell density had a range of 3.5×107 cells·cm-3 to 7×106 cells·cm-3 for the former and 2.8×107 cells·cm-3 to 5.8×106 cells·cm-3 for the latter.

  1. Preparation of polymer monolithic column functionalized by arsonic acid groups for mixed-mode capillary liquid chromatography.

    Science.gov (United States)

    Qin, Zhang-Na; Yu, Qiong-Wei; Wang, Ren-Qi; Feng, Yu-Qi

    2018-04-27

    A mixed-mode polymer monolithic column functionalized by arsonic acid groups was prepared by single-step in situ copolymerization of monomers p-methacryloylaminophenylarsonic acid (p-MAPHA) and pentaerythritol triacrylate (PETA). The prepared poly(p-MAPHA-co-PETA) monolithic column has a homogeneous monolithic structure with good permeability and mechanical stability. Zeta potential measurements reveal that the monolithic stationary phase holds a negative surface charge when the mobile phase resides in the pH range of 3.0-8.0. The retention mechanisms of prepared monolithic column are explored by the separation of selected polycyclic aromatic hydrocarbons (PAHs), nucleosides, and three basic compounds. The results indicate that the column functions in three different separation modes associated with reversed-phase chromatography based on hydrophobic interaction, hydrophilic interaction chromatography, and cation-exchange chromatography. The column efficiency of prepared monolithic column is estimated to be 70,000 and 76,000 theoretical plates/m for thiourea and naphthalene, respectively, at a linear flow velocity of 0.85 mm/s using acetonitrile/H 2 O (85/15, v/v) as the mobile phase. Furthermore, an analysis of the retention factors obtained for the PAHs indicates that the prepared monolithic column exhibits good reproducibility with relative standard deviations of 2.9%, 4.0%, and 4.7% based on run-to-run injections, column-to-column preparation, and batch-to-batch preparation, respectively. Finally, we investigate the separation performance of the proposed monolithic column for select phenols, sulfonamides, nucleobases and nucleosides. Copyright © 2018 Elsevier B.V. All rights reserved.

  2. Process for hardening an alkyd resin composition using ionizing radiation. [electron beams, gamma radiation

    Energy Technology Data Exchange (ETDEWEB)

    Watanabe, T; Murata, K; Maruyama, T

    1969-11-27

    In an alkyd resin composition having free hydroxide radicals and containing a conjugated unsaturated fatty acid and/or oil as a component thereof, a process for hardening an alkyd resin composition comprises the steps of dissolving into a vinyl monomer, the product obtained by the semi-esterification reaction of said hydroxide radicals with acid anhydrides having polymerizable radicals and hardening by ionizing radiation to provide a coating with a high degree of cross-linking, with favorable properties such as toughness, hardness, chemical resistance and resistance to weather and with the feasibility of being applied as the ground and finish coat on metals, wood, paper, outdoor construction or the like. Any kind of ionization radiation, particularly accelerated electron beams, ..gamma.. radiation can be used at 50/sup 0/C to -5/sup 0/C for a few seconds or minutes, permitting continuous operation. In one example, 384 parts of phthalic anhydride, 115 parts of pentaerythritol, 233 parts of trimethylol ethane, 288 parts of tung fatty acid and 49 parts of para-tertiary-butyl benzoic acid are mixed and heated with 60 parts of xylene to an acid value of 12. In addition, 271 parts of maleic anhydride and 0.6 parts of hydroquinone are admixed with the content and heated to terminate the reaction. 100 parts of a 50% stylene solution of this alkyd resin are mixed with 1 part of a 60% toluene solution of cobalt naphthenate, and then coated on a glass plate and irradiated with high energy electron beams of 300 kV with a dose of 5 Mrad for 1 sec.

  3. Microencapsulated n-octadecane with different methylmethacrylate-based copolymer shells as phase change materials for thermal energy storage

    International Nuclear Information System (INIS)

    Qiu, Xiaolin; Li, Wei; Song, Guolin; Chu, Xiaodong; Tang, Guoyi

    2012-01-01

    Microcapsules containing n-octadecane with different methylmethacrylate (MMA (methyl methacrylate))-based copolymer shells were fabricated by a suspension-like polymerization. Butyl acrylate (BA), butyl methacrylate (BMA), lauryl methacrylate (LMA) and stearyl methacrylate (SMA) were employed as monomers to copolymerize with MMA. Pentaerythritol tetraacrylate (PETRA) was employed as a crosslinking agent. The (microencapsulted phase change materials) MicroPCMs were characterized using Fourier transformed infrared (FTIR) spectroscopy and scanning electron microscopy (SEM). Thermal properties and thermal resistances of MicroPCMs were investigated by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), respectively. Phase change enthalpies and PCM contents of MicroPCMs increased with the length decreasing of the side chain of the monomers. The n-octadecane content of as much as 77.3% can be obtained in the crosslinked MicroPCMs with P(MMA-co-BMA) as shell, and accompanied by the highest melting enthalpy (173.7 J/g) and crystallization enthalpy (174.4 J/g). Heat capacities of crosslinked MicroPCMs are higher than those of their uncrosslinked counterparts. The crosslinked MicroPCMs exhibit significantly greater thermal stabilities compared with their uncrosslinked counterparts and the n-ontadecane bulk. The crosslinked MicroPCMs with P(MMA-co-SMA) displays the highest thermal resistance temperature up to 255 °C. Therefore, MicroPCMs with MMA-based copolymer as shells, especially crosslinked copolymer shells, show excellent potentials for thermal energy storage. -- Highlights: ► n-Octadecane was encapsulated with methylmethacrylate(MMA)-based copolymer shells. ► n-Octadecane content of Microcapsules increased with length decreasing of side chain of monomers. ► Microcapsule with P(MMA-co-butyl methacrylate) has the highest latent heat. ► Microcapsule with P(MMA-co-stearyl methacrylate) has the greatest thermal stability.

  4. Synthesis and carbonization chemistry of a phosphorous-nitrogen based intumescent flame retardant

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Haiyun, E-mail: mahaiyun@gmail.com [College of Chemistry and Environmental Science, HeBei University, Baoding, Hebei Province 071002 (China); Fang, Zhengping [MOE Key Laboratory of Macromolecular Synthesis and Functionalization, Institute of Polymer Composites, Zhejiang University, Hangzhou 310027 (China); Laboratory of Polymer Materials and Engineering, Ningbo Institute of Technology, Zhejiang University, Ningbo 315100 (China)

    2012-09-10

    Graphical abstract: The carbonization chemistry and mechanism of a novel synthesized intumescent flame retardant. The final chars showed a complex P-O-Ph and aromatic/graphitic structure containing architecture. Highlights: Black-Right-Pointing-Pointer The IFR synthesized is polymeric and has high molecular weight. Black-Right-Pointing-Pointer The IFR has a higher thermal stability than most of the commercial IFRs. Black-Right-Pointing-Pointer The final chars of IFR showed a complex P-O-Ph and aromatic/graphitic structure. - Abstract: In this work, a polymeric phosphorous-nitrogen containing intumescent flame retardant, named poly(diaminodiphenyl methane spirocyclic pentaerythritol bisphosphonate) (PDSPB), was synthesized. The carbonization chemistry was investigated. FTIR and {sup 1}H NMR were used to confirm the chemical structure of PDSPB. Thermogravimetric analysis (TGA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), in situ FTIR and energy dispersive X-ray (EDX) were used to investigate and monitor the chemical structural changes during thermal degradation. PDSPB demonstrated a three-step degradation behavior. PDSPB oligomers continuously polymerized and generated a higher macromolecular weight during the first step (200-250 Degree-Sign C). The phosphate ester bonds were broken down and phosphoric acid was released which dehydrated the carbon source to form chars during the second step (280-320 Degree-Sign C). The residues will be further degraded and form final chars during the final weight loss step (400-450 Degree-Sign C). The final chars showed a complex P-O-Ph and aromatic/graphitic structure containing architecture.

  5. Thio-urethane oligomers improve the properties of light-cured resin cements.

    Science.gov (United States)

    Bacchi, Ataís; Consani, Rafael L; Martim, Gedalias C; Pfeifer, Carmem S

    2015-05-01

    Thio-urethanes were synthesized by combining 1,6-hexanediol-diissocyante (aliphatic) with pentaerythritol tetra-3-mercaptopropionate (PETMP) or 1,3-bis(1-isocyanato-1-methylethyl)benzene (aromatic) with trimethylol-tris-3-mercaptopropionate (TMP), at 1:2 isocyanate:thiol, leaving pendant thiols. Oligomers were added at 10-30 phr to BisGMA-UDMA-TEGDMA (5:3:2, BUT). 25 wt% silanated inorganic fillers were added. Commercial cement (Relyx Veneer, 3M-ESPE) was also evaluated with 10-20 phr of aromatic oligomer. Near-IR was used to follow methacrylate conversion (DC) and rate of polymerization (Rpmax). Mechanical properties were evaluated in three-point bending (ISO 4049) for flexural strength/modulus (FS/FM, and toughness), and notched specimens (ASTM Standard E399-90) for fracture toughness (KIC). Polymerization stress (PS) was measured on the Bioman. Volumetric shrinkage (VS, %) was measured with the bonded disk technique. Results were analyzed with ANOVA/Tukey's test (α=5%). In general terms, for BUT cements, conversion and mechanical properties in flexure increased for selected groups with the addition of thio-urethane oligomers. The aromatic versions resulted in greater FS/FM than aliphatic. Fracture toughness increased by two-fold in the experimental groups (from 1.17 ± 0.36 MPam(1/2) to around 3.23 ± 0.22 MPam(1/2)). Rpmax decreased with the addition of thio-urethanes, though the vitrification point was not statistically different from the control. VS and PS decreased with both oligomers. For the commercial cement, 20 phr of oligomer increased DC, vitrification, reduced Rpmax and also significantly increased KIC, and reduced PS and FM. Thio-urethane oligomers were shown to favorably modify conventional dimethacrylate networks. Significant reductions in polymerization stress were achieved at the same time conversion and fracture toughness increased. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

  6. Characterization of methacrylate-based composites containing thio-urethane oligomers.

    Science.gov (United States)

    Bacchi, Atais; Nelson, Morgan; Pfeifer, Carmem S

    2016-02-01

    To evaluate the ability of thio-urethane oligomers to improve the properties of restorative composite resins. Oligomers were synthesized by combining 1,6-hexanediol-diissocyante (aliphatic) with pentaerythritol tetra-3-mercaptopropionate (PETMP) or 1,3-bis(1-isocyanato-1-methylethyl)benzene (aromatic) with trimethylol-tris-3-mercaptopropionate (TMP), at 1:2 isocyanate:thiol, leaving pendant thiols. Oligomers were added at 0-20 wt% to BisGMA-TEGDMA (70-30 wt%). Silanated inorganic fillers were added (70 wt%). Materials were photoactivated at 800 mW/cm(2) filtered to 320-500 nm. Near-IR was used to follow degree of methacrylate conversion (DC). Mechanical properties were evaluated in three-point bending with 2 mm × 2 mm × 25 mm bars for flexural strength/modulus and toughness (FS/E, and T) according to ISO 4049, and 2 mm × 5 mm × 25 mm notched specimens for fracture toughness (KIC). Polymerization stress (PS) was measured on the Bioman. Results were analyzed with ANOVA/Tukey's test (α=5%). Significant increase in DC was observed in thio-urethane-containing materials especially for the group with 20 wt% of aliphatic version. Materials composed by oligomers also promoted higher FS, E, and KIC in comparison to controls irrespective of thio-urethane type. A significant increase in toughness was detected by ANOVA, but not distinguished in the groups. The PS was significantly reduced by the presence of thio-urethane for almost all groups. The use of thio-urethane oligomer to compose methacrylate-based restorative composite promote increase in DC, FS, E and KIC while significant reduces PS. A simple additive was shown to reduce stress while increasing convrersion and mechanical properties, mainly fracture toughness. This has he potential of increasing the service life of dental composites, without changing current operatory procedures. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

  7. Investigations of step-growth thiol-ene polymerizations for novel dental restoratives.

    Science.gov (United States)

    Lu, Hui; Carioscia, Jacquelyn A; Stansbury, Jeffery W; Bowman, Christopher N

    2005-12-01

    The goal of this work was to investigate the feasibility of formulating novel dental restorative materials that utilize a step-growth thiol-ene photopolymerization. Particularly, we are aiming to significantly reduce the polymerization shrinkage and shrinkage stress while retaining adequate physical properties as compared to current dimethacrylatre-based systems. The thiol-ene system is composed of a 4:3 molar mixture of triallyl-1,3,5-triazine-2,4,6-trione (TATATO) and pentaerythritol tetramercaptopropionate (PETMP). The simultaneous measurement of shrinkage stress and functional group conversion was performed. Solvent extraction of unreacted monomers and dynamic mechanical analysis on the polymer networks that were formed were also studied. Flexural strength was measured for both filled and unfilled PETMP/TATATO and Bis-GMA/TEGDMA systems. Photopolymerization of PETMP/TATATO occurs at a much higher rate, with the maximum polymerization rate six times faster, than Bis-GMA/TEGDMA cured under the identical conditions. The results from the simultaneous measurement of shrinkage stress and conversion showed that the onset of shrinkage stress coincides with the delayed gel point conversion, which is predicted to be 41% for the 3:4 stoichiometric PETMP/TATATO resin composition. The maximum shrinkage stress developed for PETMP/TATATO was about 0.4 MPa, which was only approximately 14% of the maximum shrinkage stress of the Bis-GMA/TEGDMA system. Adequate flexural strength and flexural modulus values were obtained for both filled and unfilled PETMP/TATATO systems. The dramatically reduced shrinkage stress, increased polymerization rate, significance increased functional group conversion, and decreased leachable species are all benefits for the use-of thiol-ene systems as potential dental restorative materials.

  8. Synthesis of Programmable Main-chain Liquid-crystalline Elastomers Using a Two-stage Thiol-acrylate Reaction.

    Science.gov (United States)

    Saed, Mohand O; Torbati, Amir H; Nair, Devatha P; Yakacki, Christopher M

    2016-01-19

    This study presents a novel two-stage thiol-acrylate Michael addition-photopolymerization (TAMAP) reaction to prepare main-chain liquid-crystalline elastomers (LCEs) with facile control over network structure and programming of an aligned monodomain. Tailored LCE networks were synthesized using routine mixing of commercially available starting materials and pouring monomer solutions into molds to cure. An initial polydomain LCE network is formed via a self-limiting thiol-acrylate Michael-addition reaction. Strain-to-failure and glass transition behavior were investigated as a function of crosslinking monomer, pentaerythritol tetrakis(3-mercaptopropionate) (PETMP). An example non-stoichiometric system of 15 mol% PETMP thiol groups and an excess of 15 mol% acrylate groups was used to demonstrate the robust nature of the material. The LCE formed an aligned and transparent monodomain when stretched, with a maximum failure strain over 600%. Stretched LCE samples were able to demonstrate both stress-driven thermal actuation when held under a constant bias stress or the shape-memory effect when stretched and unloaded. A permanently programmed monodomain was achieved via a second-stage photopolymerization reaction of the excess acrylate groups when the sample was in the stretched state. LCE samples were photo-cured and programmed at 100%, 200%, 300%, and 400% strain, with all samples demonstrating over 90% shape fixity when unloaded. The magnitude of total stress-free actuation increased from 35% to 115% with increased programming strain. Overall, the two-stage TAMAP methodology is presented as a powerful tool to prepare main-chain LCE systems and explore structure-property-performance relationships in these fascinating stimuli-sensitive materials.

  9. Continuous solid-state phase transitions in energy storage materials with orientational disorder – Computational and experimental approach

    International Nuclear Information System (INIS)

    Singh, Harpreet; Talekar, Anjali; Chien, Wen-Ming; Shi, Renhai; Chandra, Dhanesh; Mishra, Amrita; Tirumala, Muralidhar; Nelson, Daryl J.

    2015-01-01

    We report on TES (thermal energy storage) in new CT (continuous phase transitions) in multicomponent tetrahederally configured (orientationally disordered) crystals of NPG-neopentylglycol-C 5 H 12 O 2 , PG-pentaglycerine-C 5 H 12 O 3 , and PE-pentaerythritol-C 5 H 12 O 4 . This discovery is applicable in thermal energy storage in many systems which do not require conventional isothermal first-order phase transition energy storage. The above compounds exhibit polymorphs of orientationally disordered phases in which O–H…O bond rotation around the C–C bond stores significant amount of energy; for example, in PE 41.26 kJ/mol are absorbed isothermally during solid–solid transitions. In this paper we show, anisothermal continuous phase transitions (CT), due to compositional changes with changes in temperature, associated with a measurable amount of energy, not reported earlier. The correlation of phase stability regions in pseudo-binaries, calculated from ternary NPG–PG–PE phase diagrams, is validated by experimental ternary DSC (differential scanning calorimetry) and in-situ x-ray diffraction data. We established equations for determining the CT in a temperature range, and their respective enthalpies of transitions for any composition of the ternaries. Thermodynamic calculations of the Gibbs energies of the solution phases are modeled as substitutional solid solutions, in which the excess Gibbs energies are expressed by the Redlich–Kister–Muggianu polynomial. There is excellent agreement between the experimental and CALPHAD calculated data. - Highlights: • Continuous phase transition (CT) thermal energy storage in organic ternary system. • Anisothermal temperature ramping leads to CT transitions as per lever rule. • Orientationally disordered phases store energy in O–H…O bond rotation/oscillation. • Validated calculated data with measured thermodynamic properties in ternary system. • Used CALPHAD methodology to calculate Gibbs energies of

  10. A novel rat model of blast-induced traumatic brain injury simulating different damage degree: implications for morphological, neurological, and biomarker changes

    Directory of Open Access Journals (Sweden)

    Mengdong eLiu

    2015-05-01

    Full Text Available In current military conflicts and civilian terrorism, blast-induced traumatic brain injury (bTBI is the primary cause of neurotrauma. However, the effects and mechanisms of bTBI are poorly understood. Although previous researchers have made significant contributions to establishing animal models for the simulation of bTBI, the precision and controllability of blast-induced injury in animal models must be improved. Therefore, we established a novel rat model to simulate blast-wave injury to the brain. To simulate different extents of bTBI injury, the animals were divided into moderate and severe injury groups. The miniature spherical explosives (PETN used in each group were of different sizes (2.5 mm diameter in the moderate injury group and 3.0 mm diameter in the severe injury group. A specially designed apparatus was able to precisely adjust the positions of the miniature explosives and create eight rats with bTBI simultaneously, using a single electric detonator. Neurological functions, gross pathologies, histopathological changes and the expression levels of various biomarkers were examined after the explosion. Compared with the moderate injury group, there were significantly more neurological dysfunctions, cortical contusions, intraparenchymal hemorrhages, cortical expression of S-100β, MBP, NSE, IL-8, IL-10, iNOS and HIF-1α in the severe injury group. These results demonstrate that we have created a reliable and reproducible bTBI model in rats. This model will be helpful for studying the mechanisms of bTBI and developing strategies for clinical bTBI treatment.

  11. Laser-induced breakdown spectroscopy for the remote detection of explosives at level of fingerprints

    Science.gov (United States)

    Almaviva, S.; Palucci, A.; Lazic, V.; Menicucci, I.; Nuvoli, M.; Pistilli, M.; De Dominicis, L.

    2016-04-01

    We report the results of the application of Laser-Induced Breakdown Spectroscopy (LIBS) for the detection of some common military explosives and theirs precursors deposited on white varnished car's external and black car's internal or external plastic. The residues were deposited by an artificial silicon finger, to simulate material manipulation by terrorists when preparing a car bomb, leaving traces of explosives on the parts of a car. LIBS spectra were acquired by using a first prototype laboratory stand-off device, developed in the framework of the EU FP7 313077 project EDEN (End-user driven DEmo for CBRNe). The system operates at working distances 8-30 m and collects the LIBS in the spectral range 240-840 nm. In this configuration, the target was moved precisely in X-Y direction to simulate the scanning system, to be implemented successively. The system is equipped with two colour cameras, one for wide scene view and another for imaging with a very high magnification, capable to discern fingerprints on a target. The spectral features of each examined substance were identified and compared to those belonging to the substrate and the surrounding air, and those belonging to possible common interferents. These spectral differences are discussed and interpreted. The obtained results show that the detection and discrimination of nitro-based compounds like RDX, PETN, ammonium nitrate (AN), and urea nitrate (UN) from organic interfering substances like diesel, greasy lubricants, greasy adhesives or oils in fingerprint concentration, at stand-off distance of some meters or tenths of meters is feasible.

  12. Optimization of biological and instrumental detection of explosives and ignitable liquid residues including canines, SPME/ITMS and GC/MSn

    Science.gov (United States)

    Furton, Kenneth G.; Harper, Ross J.; Perr, Jeannette M.; Almirall, Jose R.

    2003-09-01

    A comprehensive study and comparison is underway using biological detectors and instrumental methods for the rapid detection of ignitable liquid residues (ILR) and high explosives. Headspace solid phase microextraction (SPME) has been demonstrated to be an effective sampling method helping to identify active odor signature chemicals used by detector dogs to locate forensic specimens as well as a rapid pre-concentration technique prior to instrumental detection. Common ignitable liquids and common military and industrial explosives have been studied including trinitrotoluene, tetryl, RDX, HMX, EGDN, PETN and nitroglycerine. This study focuses on identifying volatile odor signature chemicals present, which can be used to enhance the level and reliability of detection of ILR and explosives by canines and instrumental methods. While most instrumental methods currently in use focus on particles and on parent organic compounds, which are often involatile, characteristic volatile organics are generally also present and can be exploited to enhance detection particularly for well-concealed devices. Specific examples include the volatile odor chemicals 2-ethyl-1-hexanol and cyclohexanone, which are readily available in the headspace of the high explosive composition C-4; whereas, the active chemical cyclo-1,3,5-trimethylene-2,4,6-trinitramine (RDX) is not. The analysis and identification of these headspace 'fingerprint' organics is followed by double-blind dog trials of the individual components using certified teams in an attempt to isolate and understand the target compounds to which dogs are sensitive. Studies to compare commonly used training aids with the actual target explosive have also been undertaken to determine their suitability and effectiveness. The optimization of solid phase microextraction (SPME) combined with ion trap mobility spectrometry (ITMS) and gas chromatography/mass spectrometry/mass spectrometry (GC/MSn) is detailed including interface development

  13. Effect of cetuximab combined with paclitaxel + cisplatin neoadjuvant chemotherapy on esophageal cancer cell proliferation and invasion

    Directory of Open Access Journals (Sweden)

    Yu-Lin Zhao

    2017-07-01

    Full Text Available Objective: To study the effect of cetuximab combined with paclitaxel + cisplatin neoadjuvant chemotherapy on esophageal cancer cell proliferation and invasion. Methods: A total of 62 patients with esophageal cancer who were treated in the hospital between January 2015 and December 2016 were collected and divided into control group and observation group according to random number table, with 31 cases in each group. Control group of patients received paclitaxel + cisplatin neoadjuvant chemotherapy + surgery, and observation group of patients accepted cetuximab combined with paclitaxel + cisplatin neoadjuvant chemotherapy + surgery. The differences in proliferation and invasion gene expression in the tumor tissue were compared between two groups of patients before and after chemotherapy. Results: Before chemotherapy, differences in proliferation and invasion gene expression in tumor tissue were not statistically significant between two groups of patients. After chemotherapy, proproliferation genes FOXA1, ABCE1, USP39 and Nestin mRNA expression in tumor tissue of observation group were significantly lower than those of control group; anti-proliferation genes PETN, KLF4, TSLC1 and AnnexinA2 mRNA expression were significantly higher than those of control group; pro-invasion genes γ-synuclein, CXCR4 and Snail mRNA expression were significantly lower than those of control group; anti-invasion genes CIAPIN1, Fez and Lrig1 mRNA expression were significantly higher than that of control group. Conclusions: Cetuximab combined with paclitaxel + cisplatin neoadjuvant chemotherapy can effectively inhibit the malignant degree of esophageal cancer cells and inhibit its proliferation and invasion.

  14. Gaseous byproducts from high-temperature thermal conversion elemental analysis of nitrogen- and sulfur-bearing compounds with considerations for δ2H and δ18O analyses.

    Science.gov (United States)

    Hunsinger, Glendon B; Tipple, Christopher A; Stern, Libby A

    2013-07-30

    High-temperature, conversion-reduction (HTC) systems convert hydrogen and oxygen in materials into H2 and CO for δ(2)H and δ(18)O measurements by isotope ratio mass spectrometry. HTC of nitrogen- and sulfur-bearing materials produces unintended byproduct gases that could affect isotope analyses by: (1) allowing isotope exchange reactions downstream of the HTC reactor, (2) creating isobaric or co-elution interferences, and (3) causing deterioration of the chromatography. This study characterizes these HTC byproducts. A HTC system (ThermoFinnigan TC/EA) was directly connected to a gas chromatograph/quadrupole mass spectrometer in scan mode (m/z 8 to 88) to identify the volatile products generated by HTC at conversion temperatures of 1350 °C and 1450 °C for a range of nitrogen- and sulfur-bearing solids [keratin powder, horse hair, caffeine, ammonium nitrate, potassium nitrate, ammonium sulfate, urea, and three nitrated organic explosives (PETN, RDX, and TNT)]. The prominent HTC byproduct gases include carbon dioxide, hydrogen cyanide, methane, acetylene, and water for all nitrogen-bearing compounds, as well as carbon disulfide, carbonyl sulfide, and hydrogen sulfide for sulfur-bearing compounds. The 1450 °C reactor temperature reduced the abundance of most byproduct gases, but increased the significant byproduct, hydrogen cyanide. Inclusion of a post-reactor chemical trap containing Ascarite II and Sicapent, in series, eliminated the majority of byproducts. This study identified numerous gaseous HTC byproducts. The potential adverse effects of these gases on isotope ratio analyses are unknown but may be mitigated by higher HTC reactor temperatures and purifying the products with a purge-and-trap system or with chemical traps. Published in 2013. This article is a U.S. Government work and is in the public domain in the USA.

  15. Reduced amino acids in the bovine uterine lumen of cloned versus in vitro fertilized pregnancies prior to implantation.

    Science.gov (United States)

    Groebner, Anna E; Zakhartchenko, Valeri; Bauersachs, Stefan; Rubio-Aliaga, Isabel; Daniel, Hannelore; Büttner, Mathias; Reichenbach, Horst D; Meyer, Heinrich H D; Wolf, Eckhard; Ulbrich, Susanne E

    2011-10-01

    Fetal overgrowth and placental abnormalities frequently occur in pregnancies following somatic cell nuclear transfer (SCNT). An optimal intrauterine supply of amino acids (AA) is of specific importance for the development of the bovine preimplantation embryo, and a defective regulation of AA supply might contribute to pregnancy failures. Thus, we analyzed 41 AA and derivatives by liquid chromatography-tandem mass spectrometry in uterine flushings of day 18 pregnant heifers carrying in vitro fertilized (IVF) or SCNT embryos, which were cultured under identical conditions until transfer to recipients. The concentrations of several AA were reduced in samples from SCNT pregnancies: L-leucine (1.8-fold), L-valine (1.6-fold), L-isoleucine (1.9-fold), L-phenylalanine (1.5-fold), L-glutamic acid (3.9-fold), L-aspartic acid (4.0-fold), L-proline (2.6-fold), L-alanine (2.0-fold), L-arginine (2.5-fold), and L-lysine (1.9-fold). The endometrial transcript abundance for the AA transporter solute carrier family 7 (amino acid transporter, L-type), member 8 (SLC7A8) was also 2.4-fold lower in SCNT pregnancies. O-phosphoethanolamine (PetN) was 11-fold (p=0.0001) reduced in the uterine fluid of animals carrying an SCNT conceptus, pointing toward changes of the phospholipid metabolism. We provide evidence for disturbed embryo-maternal interactions in the preimplantation period after transfer of SCNT embryos, which may contribute to developmental abnormalities. These are unlikely related to the major embryonic pregnancy recognition signal interferon-tau, because similar activities were detected in uterine flushings of the SCNT and IVF groups.

  16. Recent advances in the molten salt technology for the destruction of energetic materials

    International Nuclear Information System (INIS)

    Upadhye, R.S.; Watkins, B.E.; Pruneda, C.O.

    1995-11-01

    The DOE has thousands of pounds of energetic materials which result from dismantlement operations at the Pantex Plant. The authors have demonstrated the Molten Salt Destruction (MSD) Process for the treatment of explosives and explosive-containing wastes on a 1.5 kilogram of explosive per hour scale and are currently building a 5 kilogram per hour unit. MSD converts the organic constituents of the waste into non-hazardous substances such as carbon dioxide, nitrogen and water. Any inorganic constituents of the waste, such as binders and metallic particles, are retained in the molten salt. The destruction of energetic material waste is accomplished by introducing it, together with air, into a crucible containing a molten salt, in this case a eutectic mixture of Na, K, and Li carbonates. The following pure component DOE and DoD explosives have been destroyed in LLNL's experimental unit at their High Explosives Applications Facility (HEAF): ammonium picrate, HMX, K-6, NQ, NTO, PETN, RDX, TATB, and TNT. In addition, the following formulations were also destroyed: Comp B, LX-10, LX-16, LX-17, PBX-9404, and XM46, a US Army liquid gun propellant. In this 1.5 kg/hr unit, the fractions of carbon converted to CO and of chemically bound nitrogen converted to NOx were found to be well below 1T. In addition to destroying explosive powders and molding powders the authors have also destroyed materials that are typical of real world wastes. These include shavings from machined pressed parts of plastic bonded explosives and sump waste containing both explosives and non-explosive debris. Based on the information obtained on the smaller unit, the authors have constructed a 5 kg/hr MSD unit, incorporating LLNL's advanced chimney design. This unit is currently under shakedown tests and evaluation

  17. Gasdynamic Model of Turbulent Combustion in TNT Explosions

    Energy Technology Data Exchange (ETDEWEB)

    Kuhl, A L; Bell, J B; Beckner, V E

    2010-01-08

    A model is proposed to simulate turbulent combustion in confined TNT explosions. It is based on: (i) the multi-component gasdynamic conservation laws, (ii) a fast-chemistry model for TNT-air combustion, (iii) a thermodynamic model for frozen reactants and equilibrium products, (iv) a high-order Godunov scheme providing a non-diffusive solution of the governing equations, and (v) an ILES approach whereby adaptive mesh refinement is used to capture the energy bearing scales of the turbulence on the grid. Three-dimensional numerical simulations of explosion fields from 1.5-g PETN/TNT charges were performed. Explosions in six different chambers were studied: three calorimeters (volumes of 6.6-l, 21.2-l and 40.5-l with L/D = 1), and three tunnels (L/D = 3.8, 4.65 and 12.5 with volumes of 6.3-l) - to investigate the influence of chamber volume and geometry on the combustion process. Predicted pressures histories were quite similar to measured pressure histories for all cases studied. Experimentally, mass fraction of products, Y{sub p}{sup exp}, reached a peak value of 88% at an excess air ratio of twice stoichiometric, and then decayed with increasing air dilution; mass fractions Y{sub p}{sup calc} computed from the numerical simulations followed similar trends. Based on this agreement, we conclude that the dominant effect that controls the rate of TNT combustion with air is the turbulent mixing rate; the ILES approach along with the fast-chemistry model used here adequately captures this effect.

  18. Multi-functional Textiles for Military Applications

    Science.gov (United States)

    Malshe, Priyadarshini

    The objective of this research was to develop the standard rip-stop weave military uniform fabric made of 50/50 nylon/cotton (NyCo) to achieve a repellent front surface and an antibacterial bulk for protection from chemical-biological warfare agents. Diallyldimethylammonium chloride (DADMAC), a quaternary ammonium salt monomer was graft polymerized on NyCo fabric to impart antimicrobial capability using atmospheric pressure glow discharge plasma. Plasma was used to induce free radical chain polymerization of the DADMAC monomer to introduce a graft polymerized network on the fabric with durable antimicrobial properties. Pentaerythritol tertraacrylate was used as a cross-linking agent to obtain a highly cross-linked, durable polymer network. The presence of polyDADMAC on the fabric surface was confirmed using acid dye staining, SEM, and TOF-SIMS. Antibacterial performance was evaluated using standard AATCC test method 100 for both gram positive and gram negative bacteria. Results showed 99.9% reduction in the bacterial activities of K. pneumoniae and S. aureus. To achieve repellency on NyCo front surface, an environmentally benign C6 fluorocarbon monomer, 2-(perfluorohexyl) ethyl acrylate was graft polymerized using plasma on the front surface of the NyCo fabric which was already grafted with polyDADMAC for anti-microbial properties. The surface was characterized by IR spectroscopy and XPS. The presence of fluorine on the surface was mapped and confirmed by TOF-SIMS. SEM images showed a uniform layer of fluorocarbon polymer on the fiber surface. High water contact angle of 144° was obtained on the surface. The surface also achieved a high AATCC Test Method 193 rating of 9 and AATCC Test Method 118 rating of 5, indicating that the surface could repel a fluid with surface tension as low as 24 dynes/cm. Appropriate experimental designs and statistical modeling of data helped identify the experimental space and optimal factor combinations for best response. The study

  19. Resin cements formulated with thio-urethanes can strengthen porcelain and increase bond strength to ceramics.

    Science.gov (United States)

    Bacchi, Atais; Spazzin, Aloisio Oro; de Oliveira, Gabriel Rodrigues; Pfeifer, Carmem; Cesar, Paulo Francisco

    2018-06-01

    The use of thio-urethane oligomers has been shown to significantly improve the mechanical properties of resin cements (RCs). The aim of this study was to use thio-urethane-modified RC to potentially reinforce the porcelain-RC structure and to improve the bond strength to zirconia and lithium disilicate. Six oligomers were synthesized by combining thiols - pentaerythritol tetra-3-mercaptopropionate (PETMP, P) or trimethylol-tris-3-mercaptopropionate (TMP, T) - with di-functional isocyanates - 1,6-Hexanediol-diissocyante (HDDI) (aliphatic, AL) or 1,3-bis(1-isocyanato-1-methylethyl)benzene (BDI) (aromatic, AR) or Dicyclohexylmethane 4,4'-Diisocyanate (HMDI) (cyclic, CC). Thio-urethanes (20 wt%) were added to a BisGMA/UDMA/TEGDMA organic matrix. Filler was introduced at 60 wt%. The microshear bond strength (μSBS), Weibull modulus (m), and failure pattern of RCs bonded to zirconia (ZR) and lithium disilicate (LD) ceramics was evaluated. Biaxial flexural test and fractographic analysis of porcelain discs bonded to RCs were also performed. The biaxial flexural strength (σ bf ) and m were calculated in the tensile surfaces of porcelain and RC structures (Z = 0 and Z = -t 2 , respectively). The μSBS was improved with RCs formulated with oligomers P_AL or T_AL bonded to LD and P_AL, P_AR or T_CC bonded to zirconia in comparison to controls. Mixed failures predominated in all groups. σ bf had superior values at Z = 0 with RCs formulated with oligomers P_AL, P_AR, T_AL, or T_CC in comparison to control; σ bf increased with all RCs composed by thio-urethanes at Z = -t 2 . Fractographic analysis revealed all fracture origins at Z = 0. The use of specific thio-urethane oligomers as components of RCs increased both the biaxial flexural strength of the porcelain-RC structure and the μSBS to LD and ZR. The current investigation suggests that it is possible to reinforce the porcelain-RC pair and obtain higher bond strength to LD and ZR with RCs

  20. Rheological and mechanical properties and interfacial stress development of composite cements modified with thio-urethane oligomers.

    Science.gov (United States)

    Bacchi, Ataís; Pfeifer, Carmem S

    2016-08-01

    Thio-urethane oligomers have been shown to reduce stress and increase toughness in highly filled composite materials. This study evaluated the influence of thio-urethane backbone structure on rheological and mechanical properties of resin cements modified with a fixed concentration of the oligomers. Thio-urethane oligomers (TU) were synthesized by combining thiols - pentaerythritol tetra-3-mercaptopropionate (PETMP) or trimethylol-tris-3-mercaptopropionate (TMP) - with isocyanates - 1,6-hexanediol-diissocyante (HDDI) (aliphatic) or 1,3-bis(1-isocyanato-1-methylethyl)benzene (BDI) (aromatic) or dicyclohexylmethane 4,4'-diisocyanate (HMDI) (cyclic), at 1:2 isocyanate:thiol, leaving pendant thiols. 20wt% TU were added to BisGMA-UDMA-TEGDMA (5:3:2). 60wt% silanated inorganic fillers were added. Near-IR was used to follow methacrylate conversion and rate of polymerization ( [Formula: see text] ). Mechanical properties were evaluated in three-point bending (ISO 4049) for flexural strength/modulus (FS/FM, and toughness), and notched specimens (ASTM Standard E399-90) for fracture toughness (KIC). PS was measured on the Bioman. Viscosity (V) and gel-points (defined as the crossover between storage and loss shear moduli (G'/G″)) were obtained with rheometry. Glass transition temperature (Tg), cross-link density and homogeneity of the network were obtained with dynamic mechanical analysis. Film-thickness was evaluated according to ISO 4049. DC and mechanical properties increased and [Formula: see text] and PS decreased with the addition of TUs. Gelation (G'/G″) was delayed and DC at G'/G″ increased in TU groups. Tg and cross-link density dropped in TU groups, while oligomers let to more homogenous networks. An increase in V was observed, with no effect on film-thickness. Significant reductions in PS were achieved at the same time conversion and mechanical properties increased. The addition of thio-urethane oligomers proved successful in improving several key properties

  1. Nanogel-crosslinked nanoparticles increase the inhibitory effects of W9 synthetic peptide on bone loss in a murine bone resorption model

    Directory of Open Access Journals (Sweden)

    Sato T

    2015-05-01

    Full Text Available Toshimi Sato,1 Neil Alles,1,2 Masud Khan,1,3 Kenichi Nagano,1,4 Mariko Takahashi,1 Yukihiko Tamura,1 Asako Shimoda,5,6 Keiichi Ohya,1 Kazunari Akiyoshi,5,6 Kazuhiro Aoki1 1Department of Bio-Matrix (Pharmacology, Graduate School, Tokyo Medical and Dental University, Tokyo, Japan; 2Department of Biochemistry, Faculty of Medicine, University of Peradeniya, Peradeniya, Sri Lanka; 3Department of Dental Pharmacology, City Dental College and Hospital, Dhaka, Bangladesh; 4Department of Oral Medicine, Infection and Immunity, Harvard School of Dental Medicine, Boston, MA, USA; 5Department of Polymer Chemistry, Graduate School of Engineering, Kyoto University, Katsura, 6ERATO Akiyoshi Bio-Nanotransporter Project, Japan Science and Technology Agency, Katsura Int’tech Center Kyotodaigaku-Katsura, Nishikyo-ku, Kyoto, Japan Abstract: We investigated the biological activity of W9, a bone resorption inhibitor peptide, using NanoClik nanoparticles as an injectable carrier, where acryloyl group-modified cholesterol-bearing pullulan (CHPOA nanogels were crosslinked by pentaerythritol tetra (mercaptoethyl polyoxyethylene. Thirty 5-week-old male C57BL/6J mice were fed a low calcium diet and received once-daily subcutaneous injections of the carrier alone, W9 24 mg/kg/day alone, W9 24 mg/kg/day incorporated in cholesterol bearing pullulan (CHP nanogels, or W9 (8 and 24 mg/kg/day incorporated in NanoClik nanoparticles for 4 days (n=5. Mice that received a normal calcium diet with NanoClik nanoparticle injections without W9 were used as a control group. Radiological analyses showed that administration of W9 24 mg/kg/day significantly prevented low calcium-induced reduction of bone mineral density in the long bones and lumbar vertebrae, but only when the NanoClik nanoparticles were used as a carrier. Histomorphometric analyses of the proximal tibiae revealed that W9 24 mg/kg/day incorporated in NanoClik nanoparticles prevented the increase in bone resorption indices

  2. The complete chloroplast genome sequence of strawberry (Fragaria  × ananassa Duch.) and comparison with related species of Rosaceae.

    Science.gov (United States)

    Cheng, Hui; Li, Jinfeng; Zhang, Hong; Cai, Binhua; Gao, Zhihong; Qiao, Yushan; Mi, Lin

    2017-01-01

    Compared with other members of the family Rosaceae, the chloroplast genomes of Fragaria species exhibit low variation, and this situation has limited phylogenetic analyses; thus, complete chloroplast genome sequencing of Fragaria species is needed. In this study, we sequenced the complete chloroplast genome of F . ×  ananassa 'Benihoppe' using the Illumina HiSeq 2500-PE150 platform and then performed a combination of de novo assembly and reference-guided mapping of contigs to generate complete chloroplast genome sequences. The chloroplast genome exhibits a typical quadripartite structure with a pair of inverted repeats (IRs, 25,936 bp) separated by large (LSC, 85,531 bp) and small (SSC, 18,146 bp) single-copy (SC) regions. The length of the F . ×  ananassa 'Benihoppe' chloroplast genome is 155,549 bp, representing the smallest Fragaria chloroplast genome observed to date. The genome encodes 112 unique genes, comprising 78 protein-coding genes, 30 tRNA genes and four rRNA genes. Comparative analysis of the overall nucleotide sequence identity among ten complete chloroplast genomes confirmed that for both coding and non-coding regions in Rosaceae, SC regions exhibit higher sequence variation than IRs. The Ka/Ks ratio of most genes was less than 1, suggesting that most genes are under purifying selection. Moreover, the mVISTA results also showed a high degree of conservation in genome structure, gene order and gene content in Fragaria , particularly among three octoploid strawberries which were F . ×  ananassa 'Benihoppe', F . chiloensis (GP33) and F . virginiana (O477). However, when the sequences of the coding and non-coding regions of F . ×  ananassa 'Benihoppe' were compared in detail with those of F . chiloensis (GP33) and F . virginiana (O477), a number of SNPs and InDels were revealed by MEGA 7. Six non-coding regions ( trnK - matK , trnS - trnG , atpF - atpH , trnC - petN , trnT - psbD and trnP - psaJ ) with a percentage of variable sites greater than

  3. DNA甲基化抑制剂对涎腺腺样囊性癌中PTEN基因表达的影响%Effects of DNA methylation inhibitor on the expression of PTEN in adenoid cystic carcinoma cells

    Institute of Scientific and Technical Information of China (English)

    张华昌; 向学熔; 范小平; 徐军; 杨明聪; 吴静

    2011-01-01

    MSP).Using The expression of mRNA and protein of PTEN were analyzed by RT-PCR,western blot after treatment with methyltransferase inhibitor 5-aza-2'-deoxycytidine(5-Aza-dc).Results:RT-PCR analysis showed that the expression of PTEN in ACC-2 cells was significantly lower than that in the normal salivary gland epithelial cells(p0.05).Using "Methprimer"software predicted,the CpG islands were found in the promoter region of PETN.The existence of CpG island methylation in PETN promoter region in ACC-2 cells was super-expression by Methylation-Specific PCR(MSP) analysis.After the treatment with methyltransferase inhibitor 5-aza-2'-deoxycytidine(5-Aza-dc),the levels of mRNA and protein of PTEN in adenoid cystic carcinoma cells were increased dramatically(p0.05),the levels of PTEN mRNA and protein is consistent.Conclusion:The low expression of PTEN in adenoid cystic carcinoma cells may be related to The hypermethylation of CpG island in promoter of PTEN.

  4. Antibiofouling hybrid dendritic Boltorn/star PEG thiol-ene cross-linked networks.

    Science.gov (United States)

    Bartels, Jeremy W; Imbesi, Philip M; Finlay, John A; Fidge, Christopher; Ma, Jun; Seppala, Jonathan E; Nystrom, Andreas M; Mackay, Michael E; Callow, James A; Callow, Maureen E; Wooley, Karen L

    2011-06-01

    A series of thiol-ene generated amphiphilic cross-linked networks was prepared by reaction of alkene-modified Boltorn polyesters (Boltorn-ene) with varying weight percent of 4-armed poly(ethylene glycol) (PEG) tetrathiol (0-25 wt%) and varying equivalents of pentaerythritol tetrakis(3-mercaptopropionate) (PETMP) (0-64 wt%). These materials were designed to present complex surface topographies and morphologies, with heterogeneity of surface composition and properties and robust mechanical properties, to serve as nontoxic antibiofouling coatings that are amenable to large-scale production for application in the marine environment. Therefore, a two-dimensional matrix of materials compositions was prepared to study the physical and mechanical properties, over which the compositions spanned from 0 to 25 wt% PEG tetrathiol and 0-64 wt% PETMP (the overall thiol/alkene (SH/ene) ratios ranged from 0.00 to 1.00 equiv), with both cross-linker weight percentages calculated with respect to the weight of Boltorn-ene. The Boltorn-ene components were prepared through the esterification of commercially available Boltorn H30 with 3-butenoic acid. The subsequent cross-linking of the Boltorn-PEG-PETMP films was monitored using IR spectroscopy, where it was found that near-complete consumption of both thiol and alkene groups occurred when the stoichiometry was ca. 48 wt% PETMP (0.75 equiv SH/ene, independent of PEG amount). The thermal properties of the films showed an increase in T(g) with an increase in 4-armed PEG-tetrathiol wt%, regardless of the PETMP concentration. Investigation of the bulk mechanical properties in dry and wet states found that the Young's modulus was the greatest at 48 wt% PETMP (0.75 equiv of SH/ene). The ultimate tensile strength increased when PETMP was constant and the PEG concentration was increased. The Young's modulus was slightly lower for wet films at constant PEG or constant PETMP amounts, than for the dry samples. The nanoscopic surface features were

  5. Shrinkage / stress reduction and mechanical properties improvement in restorative composites formulated with thio-urethane oligomers.

    Science.gov (United States)

    Bacchi, Atais; Yih, Jonathan A; Platta, Jacqueline; Knight, Joseph; Pfeifer, Carmem S

    2018-02-01

    Thio-urethane oligomers (TUs) have been shown to favorably modify methacrylate networks to reduce stress and significantly increase fracture toughness. Since those are very desirable features in dental applications, the objective of this work was to characterize restorative composites formulated with the addition of TUs. TUs were synthesized by combining thiols - pentaerythritol tetra-3-mercaptopropionate (PETMP) or trimethylol-tris-3-mercaptopropionate (TMP) - with isocyanates - 1,6-Hexanediol-diissocyante (HDDI) (aliphatic) or 1,3-bis(1-isocyanato-1-methylethyl)benzene (BDI) (aromatic) or dicyclohexylmethane 4,4'-Diisocyanate (HMDI) (cyclic), at 1:2 isocyanate:thiol, leaving pendant thiols. 20wt% TU were added to BisGMA-TEGDMA (70-30%). To this organic matrix, 70wt% silanated inorganic fillers were added. Near-IR was used to follow methacrylate conversion and rate of polymerization (Rp max ). Mechanical properties were evaluated in three-point bending (ISO 4049) for flexural strength/modulus (FS/FM) and toughness (T), and notched specimens (ASTM Standard E399-90) for fracture toughness (K IC ). Polymerization stress (PS) was measured on the Bioman. Volumetric shrinkage (VS) was measured with the bonded disk technique. Glass transition temperature (Tg) and heterogeneity of network were obtained with dynamic mechanical analysis. The addition of TUs led to an increase in mechanical properties (except for Tg and FS). Fracture toughness ranged from 1.6-1.94MPam 1/2 for TU-modified groups, an increase of 33-61% in relation to the control (1.21 ± 0.1MPam 1/2 ). Toughness showed a two-fold increase in relation to the control: from 0.91MPa to values ranging from 1.70-1.95MPa. Flexural modulus was statistically higher for the TU-modified groups. The Tg, as expected, decreased for all TU groups due to the greater flexibility imparted to the network (which also explains the increase in toughness and fracture toughness). Narrower tan-delta peaks suggest more homogeneous

  6. A Novel Technique for Assessing Antioxidant Concentration in Retrieved UHMWPE.

    Science.gov (United States)

    Currier, Barbara H; Van Citters, Douglas W

    2017-05-01

    Antioxidants added to UHMWPE to prevent in vivo oxidation are important to the long-term performance of hip and knee arthroplasty. Diffused vitamin E antioxidant polyethylene raised questions about potential in vivo elution that could cause inflammatory reactions in periprosthetic tissues and also potentially leave the implant once again prone to oxidation. Currently, there is no information on the elution, if any, of antioxidants from implant polyethylene materials in vivo. (1) Do antioxidants, especially diffused vitamin E, elute from antioxidant polyethylene in vivo? (2) Can extraction of the retrieved antioxidant polyethylene (to remove absorbed species from the in vivo environment near the articular and nonarticular surfaces) improve the identification of antioxidant content? (3) Can actual antioxidant content be estimated from calculated antioxidant indices by accounting for ester content (from absorbed species) near the articular and nonarticular surfaces? An institutional review board-approved retrieval laboratory received 39 antioxidant polyethylene hip and knee retrievals at revision from 25 surgeons with in vivo time of 0.02 to 3.6 years (median, 1.3 years). These consecutive antioxidant polyethylene retrievals, received between May 2010 and February 2016, were made from three different antioxidant highly crosslinked polyethylene materials: diffused vitamin E, blended vitamin E, and hindered phenol antioxidant pentaerythritol tetrakis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)] propionate (here and after referred to as PBHP). Retrievals were analyzed using Fourier transform infrared (FTIR) spectroscopy. Absorbed ester index (1725-1740 cm -1 normalized to 1365-1371 cm -1 ), and vitamin E index (1245-1275 cm -1 ) and PBHP index (1125-1150 cm -1 ), normalized to 1850-1985 cm -1 , were defined. Microtomed thin sections of PBHP and vitamin E retrievals were hexane-extracted to remove absorbed species from the in vivo environment in an effort to improve

  7. Thumba (Citrullus colocynthis L. seed oil: a potential bio-lubricant base-stock

    Directory of Open Access Journals (Sweden)

    Kamalakar, K.

    2015-03-01

    Full Text Available Thumba seed oil, a minor, renewable tree borne oil, was exploited for the preparation of biolubricant base-stocks. The different base-stocks prepared were epoxy thumba oil (ETO, branched, 2-ethylhexyl ester (T2-EtHE, and polyol esters, namely, neopentyl glycol (TNPGE, trimethylolpropane (TTMPE and pentaerythritol (TPEE esters of thumba fatty acids. All the base-stocks were thoroughly characterized using spectral techniques. When evaluated for lubricant properties, ETO showed much higher viscosity (216.9 cSt, good oxidative stability (RBOT Method, ASTM D 2272 (20 min and weld load (ASTM IP 239 (180 kg behavior when compared to the branched and polyol esters. Polyol esters, T2-EtHE, TNPGE and TTMPE (−9 to −18 °C showed low pour points compared to ETO and TPEE. The thermal stabilities (Thermo gravimetric analysis, TGA of ETO and TPEE (425 °C were higher compared to other base-stocks. The lubricant properties of ETO matched well with ISO VG 220 and Aviation Grade 100 lubricant specifications, while polyol esters can be well exploited for hydraulic and metal working fluid applications.Las semillas de thumba producen un aceite de escasa importancia que ha sido explotado como base para la preparación de biolubricantes. Los diferentes derivados de thumba preparados fueron: éteres epoxi (ETO, éteres ramificados, éster de 2-etilhexilo (T2-ETHE, y los ésteres de poliol:, neopentil glicol (TNPGE, trimetilolpropano (TTMPE y pentaeritritol (TPEE. Todas las bases se caracterizaron en su totalidad utilizando técnicas espectrales. Cuando se evaluaron las propiedades del lubricante, ETO mostró una viscosidad mucho más alta (216,9 cSt, buena estabilidad a la oxidación (RBOT Método, ASTM D 2272 (20 min y buena carga (239 ASTM IP (180 kg en comparación con el comportamiento de los ésteres de poliol y los ramificados. Los ésteres de poliol, T2-EEl, TNPGE y TTMPE (−9 a −18 °C mostraron bajos puntos de fluidez en comparación con ETO y TPE. Las

  8. Electromagnetic Effects in SDF Explosions

    Energy Technology Data Exchange (ETDEWEB)

    Reichenbach, H; Neuwald, P; Kuhl, A L

    2010-02-12

    The notion of high ion and electron concentrations in the detonation of aluminized explosive mixtures has aroused some interest in electro-magnetic effects that the SDF charges might generate when detonated. Motivated by this interest we have started to investigate whether significant electro-magnetic effects show up in our small-scale experiments. However, the design of instrumentation for this purpose is far from straightforward, since there are a number of open questions. Thus the main aim of the feasibility tests is to find - if possible - a simple and reliable method that can be used as a diagnostic tool for electro-magnetic effects. SDF charges with a 0.5-g PETN booster and a filling of 1 g aluminum flakes have been investigated in three barometric bomb calorimeters with volumes ranging from 6.3 l to of 6.6 l. Though similar in volume, the barometric bombs differed in the length-to-diameter ratio. The tests were carried out with the bombs filled with either air or nitrogen at ambient pressure. The comparison of the test in air to those in nitrogen shows that the combustion of TNT detonation products or aluminum generates a substantial increase of the quasi-steady overpressure in the bombs. Repeated tests in the same configuration resulted in some scatter of the experimental results. The most likely reason is that the aluminum combustion in most or all cases is incomplete and that the amount of aluminum actually burned varies from test to test. The mass fraction burned apparently decreases with increasing aspect ratio L/D. Thus an L/D-ratio of about 1 is optimal for the performance of shock-dispersed-fuel combustion. However, at an L/D-ratio of about 5 the combustion still yields appreciable overpressure in excess of the detonation. For a multi-burst scenario in a tunnel environment with a number of SDF charges distributed along a tunnel section a spacing of 5 tunnel diameter and a fuel-specific volume of around 7 l/g might provide an acceptable compromise

  9. Combustion characteristics of SMX and SMX based propellants

    Science.gov (United States)

    Reese, David A.

    This work investigates the combustion of the new solid nitrate ester 2,3-hydroxymethyl-2,3-dinitro-1,4-butanediol tetranitrate (SMX, C6H 8N6O16). SMX was synthesized for the first time in 2008. It has a melting point of 85 °C and oxygen balance of 0% to CO 2, allowing it to be used as an energetic additive or oxidizer in solid propellants. In addition to its neat combustion characteristics, this work also explores the use of SMX as a potential replacement for nitroglycerin (NG) in double base gun propellants and as a replacement for ammonium perchlorate in composite rocket propellants. The physical properties, sensitivity characteristics, and combustion behaviors of neat SMX were investigated. Its combustion is stable at pressures of up to at least 27.5 MPa (n = 0.81). The observed flame structure is nearly identical to that of other double base propellant ingredients, with a primary flame attached at the surface, a thick isothermal dark zone, and a luminous secondary flame wherein final recombination reactions occur. As a result, the burning rate and primary flame structure can be modeled using existing one-dimensional steady state techniques. A zero gas-phase activation energy approximation results in a good fit between modeled and observed behavior. Additionally, SMX was considered as a replacement for nitroglycerin in a double base propellant. Thermochemical calculations indicate improved performance when compared with the common double base propellant JA2 at SMX loadings above 40 wt-%. Also, since SMX is a room temperature solid, migration may be avoided. Like other nitrate esters, SMX is susceptible to decomposition over long-term storage due to the presence of excess acid in the crystals; the addition of stabilizers (e.g., derivatives of urea) during synthesis should be sufficient to prevent this. the addition of Both unplasticized and plasticized propellants were formulated. Thermal analysis of unplasticized propellant showed a distinct melt