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At least 235 records · Page 13

Disentangling Oxygen and Water Vapor Effects on Optoelectronic Properties of Monolayer Tungsten Disulfide

By understanding how the environmental composition impacts the optoelectronic properties of transition metal dichalcogenide monolayers, we demonstrate that simple photoluminescence (PL) measurements of tungsten disulfide (WS 2 ) monolayers can differentiate relative humidity environments. In this paper, we examine the PL and photoconductivity of chemical vapor deposition grown WS 2 monolayers under three carefully controlled environments: inert gas (N 2 ), dry air (O 2 in N 2 ), and humid nitrogen (H 2 O vapor in N 2 ). The WS 2 PL is measured as a function of 532 nm laser power and exposure time and can be decomposed into the exciton, trion, and lower energy state(s) contributions. Under continuous illumination in either O 2 or H 2 O vapor environment, we find dramatic (and reversible) increases in PL intensity relative to the PL in an inert environment. The PL bathochromically shifts in an O 2 environment and is dominated by increased trion emission and diminished exciton emission. In contrast, the WS 2 PL increase in a H 2 O environment results from an overall increase in emission from all spectral components where the exciton contribution dominates. The drastic increases in PL are anticorrelated with corresponding decreases in photoconductivity, as measured by time-resolved microwave conductivity. The results suggest that both O 2 and H 2 O react photochemically with the WS 2 monolayer surface, modifying the optoelectronic properties, but do so via distinct pathways. Thus, we use these optoelectronic differences to differentiate the amount of humidity in the air, which we show with 0%, 40%, and 80% relative humidity environments. This deeper understanding of how ambient conditions impact WS 2 monolayers enables novel humidity sensors as well as a better understanding of the correlation between TMDC surface chemistry, light emission, and photoconductivity. Moreover, these WS 2 measurements highlight the importance of considering the impact of the local environment on reported results.

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Middle Atmospheric Changes Caused by the January and March 2012 Solar Proton Events

The recent 23-30 January and 7-11 March 2012 solar proton event (SPE) periods were substantial and caused significant impacts on the middle atmosphere. These were the two largest SPE periods of solar cycle 24 so far. The highly energetic solar protons produced considerable ionization of the neutral atmosphere as well as HOx (H, OH, HO2) and NOx (N, NO, NO2). We compute a NOx production of 1.9 and 2.1 Gigamoles due to these SPE periods in January and March 2012, respectively, which places these SPE periods among the 12 largest in the past 50 years. Aura Microwave Limb Sounder (MLS) observations of the peroxy radical, HO2, show significant enhancements of 0.9 ppbv in the northern polar mesosphere as a result of these SPE periods. Both MLS measurements and Goddard Space Flight Center (GSFC) two-dimensional (2D) model predictions indicated middle mesospheric ozone decreases of 20 percent for several days in the northern polar region with maximum depletions 60 percent as a result of the HOx produced in both the January and March 2012 SPE periods. The SCISAT-1 Atmospheric Chemistry Experiment Fourier Transform Spectrometer (ACE) and the Envisat Michelson Interferometer for Passive Atmospheric Sounding (MIPAS) instruments measured NO and NO2 (NOx), which indicated enhancements of over 20 ppbv in most of the northern polar mesosphere for several days as a result of these SPE periods. The GSFC 2D model was used to predict the medium-term (months) influence and found that the polar Southern Hemisphere middle atmosphere ozone was most affected by these solar events due to the increased downward motion in the fall and early winter. The downward transport moved the SPE-produced NOy to lower altitudes and led to predicted modest destruction of ozone (5-9 percent) in the upper stratosphere days to weeks after the March 2012 event. Total ozone reductions were predicted to be a maximum of 1 percent in 2012 due to these SPEs.

ozone↗

AB Initio Study of the Structure and Spectroscopic Properties of Halogenated Thioperoxy Radicals

Thioperoxy (XSO or XOS) radicals exist in a variety of chemical environments, and they have as a consequence drawn some interest. HSO, an important species in the chemistry of the troposphere, has been examined both experimentally. The halogenated (X = F, Cl or Br) peroxy species and isovalent thioperoxy species have been studied less, but they too are potentially interesting because oxidized sulfur species and halogen sources are present in the atmosphere. Learning the fate of XSO and XOS radicals is important to understanding the atmospheric oxidation chemistry of sulfur compounds. Of these, FSO and ClSO are particularly interesting because they have been directly detected spectroscopically. Recent studies in our laboratory on the photochemistry of thionyl halides (X2SO; where X = F or Cl) have suggested new ways to generate XSO species. The laser-induced photodissociation of thionyl fluoride, F2SO, at 193 nm and thionyl chloride, ClSO, at 248 nm is characterized by a radical mechanism, X2SO -> XSO + X. The structure of FSO has been characterized experimentally by Endo et cd. employing microwave spectroscopy. Using the unrestricted Hartree-Fock (UHF) self-consistent field (SCF) method, Sakai and Morokuma computed the electronic structure of the ground (sup 2)A" and the first excited (sup 2)A' states of FSO. Electron correlation was not taken into account in their study. In a laser photodissociation experiment, Huber et al. identified ClSO mass spectromctrically. ClSO has also been detected in low temperature matrices by EPR and in the gas phase by far IR laser magnetic resonance. Although the structure of FSO is known in detail, the only study, experimental or theoretical, of CISO has been an ab initio HFSCF study by Hinchliffe. Electron correlation corrections were also excluded from this study. In order to better understand the isomerization and dissociation dynamics of the radical species, we have performed ab initio correlated studies of the potential energy surfaces (PES) of ClSO and its isomer ClOS at the QCISD(T)/6-31 G* level of theory. For FSO and FOS, more extensive QCISD/6-31 1G(2df) calculations have been possible, and the results are summarized here.

Munoz, Luis A.↗

Quantum Dot–Organic Molecule Conjugates as Hosts for Photogenerated Spin Qubit Pairs

The inherent spin polarization present in photogenerated spin-correlated radical pairs makes them promising candidates for quantum computing and quantum sensing applications. The spin states of these systems can be probed and manipulated with microwave pulses using electron paramagnetic resonance spectrometers. However, to date, there are no reports on magnetic resonance-based spin measurements of photogenerated spin-correlated radical pairs hosted on quantum dots. In the current work, we prepare dye molecule-inorganic quantum dot conjugates and show that they can produce photogenerated spin-polarized states. The dye molecule, D131, is chosen for its ability to undergo efficient charge separation, and the nanoparticle materials, ZnO quantum dots, are chosen for their promising spin properties. Transient and steady state optical spectroscopy performed on ZnO quantum dot-D131 conjugates shows that reversible photogenerated charge separation is occurring. Transient and pulsed electron paramagnetic resonance experiments are then performed on the photogenerated radical pair, which demonstrate that (1) the radical pair is polarized at moderate temperatures and well modeled by existing theories and (2) the spin states can be accessed and manipulated with microwave pulses. In conclusion, this work opens the door to a new class of promising qubit materials that can be photogenerated in polarized states and hosted by highly tailorable inorganic nanoparticles.

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Comparison of the Arrhenius parameters between conventional hydrothermal and microwave-assisted synthesis methods for tin oxide nanoparticles

Microwave (MW) irradiation has emerged as a powerful tool for accelerating materials synthesis, yet the origins of its specific influence on reaction kinetics remain elusive. While multiple studies have attributed the observed enhancements in reaction rates under MW heating to reduced activation energies, other accounts have suggested modifications to the Arrhenius pre-exponential factor as the predominant cause. Distinguishing between these parameters in modern applications of MW processing in nanomaterials requires experimental approaches capable of resolving the dynamic and nuanced structural kinetics that govern MW-assisted chemistry. Here, we combine in-situ synchrotron X-ray total scattering with pair distribution function (PDF) analysis to track the structural evolution of SnO 2 nanoparticles synthesized via MW-assisted and conventional hydrothermal conditions. Avrami modeling and Arrhenius analysis suggest that although MW irradiation yields a higher apparent activation energy, the enhanced crystallization is better explained by a pre-exponential factor several orders of magnitude larger than that of conventional heating. These findings suggest that the MW field induces a higher frequency of successful molecular rearrangements rather than lowering the intrinsic activation barrier. The results contribute further insights clarifying the role of the applied MW field for materials design where MW-specific effects can be deliberately harnessed. Furthermore, this work presents a framework promoting the utility of in-situ PDF characterization coupled with kinetic analysis for developing more sophisticated descriptions of nanoscale transformations for MW-driven reaction kinetics.

36 MATERIALS SCIENCE↗

Carbon Dioxide Reduction Technology Trade Study

For long-term human missions, a closed-loop atmosphere revitalization system (ARS) is essential to minimize consumables. A carbon dioxide (CO2) reduction technology is used to reclaim oxygen (O2) from metabolic CO2 and is vital to reduce the delivery mass of metabolic O2. A key step in closing the loop for ARS will include a proper CO2 reduction subsystem that is reliable and with low equivalent system mass (ESM). Sabatier and Bosch CO2 reduction are two traditional CO2 reduction subsystems (CRS). Although a Sabatier CRS has been delivered to International Space Station (ISS) and is an important step toward closing the ISS ARS loop, it recovers only 50% of the available O2 in CO2. A Bosch CRS is able to reclaim all O2 in CO2. However, due to continuous carbon deposition on the catalyst surface, the penalties of replacing spent catalysts and reactors and crew time in a Bosch CRS are significant. Recently, technologies have been developed for recovering hydrogen (H2) from Sabatier-product methane (CH4). These include methane pyrolysis using a microwave plasma, catalytic thermal pyrolysis of CH4 and thermal pyrolysis of CH4. Further, development in Sabatier reactor designs based on microchannel and microlith technology could open up opportunities in reducing system mass and enhancing system control. Improvements in Bosch CRS conversion have also been reported. In addition, co-electrolysis of steam and CO2 is a new technology that integrates oxygen generation and CO2 reduction functions in a single system. A co-electrolysis unit followed by either a Sabatier or a carbon formation reactor based on Bosch chemistry could improve the overall competitiveness of an integrated O2 generation and CO2 reduction subsystem. This study evaluates all these CO2 reduction technologies, conducts water mass balances for required external supply of water for 1-, 5- and 10-yr missions, evaluates mass, volume, power, cooling and resupply requirements of various technologies. A system analysis and comparison among the technologies was made based on ESM, technology readiness level and reliability. Those technologies with potential were recommended for development.

Jeng, Frank F.↗

Microwave-assisted dehydrogenation of fossil fuels using iron-based alumina nanocomposites

Hydrogen is mainly produced via steam reforming of methane and gasification of coal, with enormous CO 2 emissions in both cases. Microwave-assisted thermocatalytic decomposition (pyrolysis) is of interest as a method for hydrogen production from fossil fuels with no CO 2 emissions. For successful implementation of this technology, it is necessary to develop decomposition catalysts that are also good microwave absorbers and can be produced from inexpensive materials via a robust synthetic route. Recently, iron-based alumina nanocomposites, fabricated by solution combustion synthesis (SCS), have shown promising microwave-absorbing and catalytic properties in the pyrolysis of plastics. The reported project explored the feasibilities of improving such catalysts and using them for the microwave-assisted pyrolysis of liquid fossil fuels, viz., diesel fuel, gasoline, and crude oil. The research focused on how SCS parameters affect the material properties and pyrolysis performance.

02 PETROLEUM↗

M2-SCREAM: A Stratospheric Composition Reanalysis of Aura MLS Data With MERRA-2 Transport

MERRA-2 Stratospheric Composition Reanalysis of Aura Microwave Limb Sounder (M2-SCREAM) is a new reanalysis of stratospheric ozone, water vapor, hydrogen chloride (HCl), nitric acid (HNO 3 ) and nitrous oxide (N 2 O) between 2004 and the present (with a latency of several months). The assimilated fields are provided at a 50-km horizontal resolution and at a three-hourly frequency. M2-SCREAM assimilates version 4.2 Microwave Limb Sounder (MLS) profiles of the five constituents alongside total ozone column from the Ozone Monitoring Instrument. Dynamics and tropospheric water vapor are constrained by the MERRA-2 reanalysis. The assimilated species are in excellent agreement with the MLS observations, except for HNO 3 in polar night, where data are not assimilated. Comparisons against independent observations show that the reanalysis realistically captures the spatial and temporal variability of all the assimilated constituents. In particular, the standard deviations of the differences between M2-SCREAM and constituent mixing ratio data from The Atmospheric Chemistry Experiment Fourier Transform Spectrometer are much smaller than the standard deviations of the measured constituents. Evaluation of the reanalysis against aircraft data and balloon-borne frost point hygrometers indicates a faithful representation of small-scale structures in the assimilated water vapor, HNO 3 and ozone fields near the tropopause. Comparisons with independent observations and a process-based analysis of the consistency of the assimilated constituent fields with the MERRA-2 dynamics and with large-scale stratospheric processes demonstrate the utility of M2-SCREAM for scientific studies of chemical and transport variability on time scales ranging from hours to decades. Analysis uncertainties and guidelines for data usage are provided.

MERRA-2↗

T 1 Anisotropy Elucidates Spin Relaxation Mechanisms in an S = 1 Cr(IV) Optically Addressable Molecular Qubit

Paramagnetic molecules offer unique advantages for quantum information science owing to their spatial compactness, synthetic tunability, room-temperature quantum coherence, and potential for optical state initialization and readout. However, current optically addressable molecular qubits are hampered by rapid spin–lattice relaxation ( T 1 ) even at sub-liquid nitrogen temperatures. Here, we use temperature- and orientation-dependent pulsed electron paramagnetic resonance (EPR) to elucidate the negative sign of the ground state zero-field splitting (ZFS) and assign T 1 anisotropy to specific types of motion in an optically addressable S = 1 Cr(o-tolyl) 4 molecular qubit. The anisotropy displays a distinct sin 2 (2θ) functional form that is not observed in S = 1/2 Cu(acac) 2 or other Cu(II)/V(IV) microwave addressable molecular qubits. The Cr(o-tolyl) 4 T 1 anisotropy is ascribed to couplings between electron spins and rotational motion in low-energy acoustic or pseudoacoustic phonons. Our findings suggest that rotational degrees of freedom should be suppressed to maximize the coherence temperature of optically addressable qubits.

magnetic properties↗

Joint Assimilation of the Aura Microwave Limb Sounder and Ozone Mapping and Profiler Suite Limb Profiler Data: Towards a Reanalysis of Stratospheric Ozone for Trend Studies

The future trajectory of the stratospheric ozone recovery will be sensitive to greenhouse gas concentrations through thermal control of chemical loss and via stratospheric circulation changes. The latter in particular is subject to considerable uncertainty meriting continuing monitoring of the evolution of ozone throughout the depth of the stratosphere. Atmospheric reanalyses utilize the data assimilation methodology to obtain comprehensive representations of the state of the atmosphere, including its composition, on multidecadal scales by combining diverse measurements from satellite-borne and conventional data sources. Systematic biases among these various data types pose a challenge for assimilation by introducing spurious discontinuities that affect the utility of reanalyses for studies of long-term variability and trends.In this presentation we will outline an approach, developed at NASA's Global Modeling and Assimilation Office (GMAO), that allows joint assimilation of stratospheric ozone profiles from the Microwave Limb Sounder (MLS) on EOS Aura and the Ozone Mapping and Profiler Suite Limb Profiler (OMPS-LP) currently flying on the Suomi-NPP satellite with future missions projected into the 2030s. We will demonstrate that a simple offline correction significantly reduces biases between MLS and OMPS-LP ozone data providing a strategy for generating a long-term vertically resolved homogenized representation of stratospheric ozone in future reanalyses. One novel element of our approach compared to previous GMAO reanalysis is the use of a version of the Goddard Earth Observing System model with full stratospheric chemistry. We will show selected comparisons of MLS and OMPS-LP assimilation experiments with independent ozonesonde and satellite data as well as two examples of process-based evaluation focused on the 2016 QBO disruption and Arctic winter ozone loss focusing on the relative performance of the MLS and OMPS-LP analyses.

Wargan, K.↗

Spin Emitters beyond the Point Dipole Approximation in Nanomagnonic Cavities

Control over transition rates between spin states of emitters is crucial in a wide variety of fields ranging from quantum information science to the nanochemistry of free radicals. We present an approach to drive both electric and magnetic dipole-forbidden transitions of a spin emitter by placing it in a nanomagnonic cavity, requiring a description of both the spin emitter beyond the point dipole approximation and the vacuum magnetic fields of the nanomagnonic cavity with a large spatial gradient over the volume of the spin emitter. We specifically study the silicon vacancy (SiV – ) defect in diamond, whose Zeemansplit ground states comprise a logical qubit for solid-state quantum information processing, coupled to a magnetic nanoparticle serving as a model nanomagnonic cavity capable of concentrating microwave magnetic fields into deeply subwavelength volumes. Through first-principles modeling of the SiV – spin orbitals, we calculate the spin transition densities of magnetic dipole-allowed and -forbidden transitions and calculate their coupling rates to various multipolar modes of the nanomagnonic cavity. We envision using such a framework for manipulation of quantum spin states.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Gas-phase pyrolysis of trans 3-pentenenitrile: competition between direct and isomerization-mediated dissociation

The flash pyrolysis of trans 3-pentenenitrile (3-PN, CH 3 –$CH=CH$–CH 2 –CN) was studied by combining the results of VUV photoionization mass spectra with broadband microwave spectra recorded as a function of the temperature of the pyrolysis tube. The two separated functional groups (vinyl and nitrile) open up isomerization as an initial step in competition with unimolecular dissociation. Primary products were detected by keeping the 3-PN concentration low and limiting reaction times to the traversal time of the gas in the pyrolysis tube (~100 μs). The reaction is quenched and products are cooled by expansion into vacuum before interrogation over the 8–18 GHz region using chirped-pulse broadband methods. 118 nm VUV photoionization of the same reaction mixture provides a means of detecting all products with ionization potentials below 10.5 eV with minimal fragmentation. These results are combined with a detailed computational investigation of the C 5 H 7 N and related potential energy surfaces, leading to a consistent picture of the unimolecular decomposition of 3-PN. Loss of two H-atoms to form a 79 amu product is proven from its microwave transitions to contain trans-Z-2,4-pentadienenitrile, while no pyridine is observed. Methyl loss, HCN loss, and breaking the central C(2)–C(3) bond all occur following isomerization of the position of the double bond, thereby opening up low-energy pathways to these decomposition channels.

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Methanol and hydrogen sulfide in comet P/Halley

The Neutral Mass Spectrometer on the Giotto spacecraft measured the gas and ion composition in the coma of comet P/Halley. A detailed model of the ion chemistry inside the contact surface located at 4660 km is used to interpret the measured ion desnity profiles in the 32 to 35 amu/e mass range. The masses 33 and 35 amu/e are dominated by the protonated methanol and hydrogen sulfide ions CH3OH2(+) and H3S(+). Both profiles are essentially compatible with CH3OH and H2S originating from the nucleus only. The production rates relative to water are Y(CH3OH) = Q(CH3OH)/Q(H2O) = 1.7% and Y(H2S) = 0.41%. Our Y(CH3OH) agrees well with a determination from IR spectra obtained about 6 weeks after the Giotto encounter with P/Halley. In 7 other comets IR and microwave observations give Y(CH3OH) values between about 0.7 and 6%, indicating that the methanol abundance shows a strong variability from comet to comet. In three other comets Y(H2S) values between 0.2 and 0.5% have been reported. In addition to H2S(+), only ions containing minor isotopes of H, C, O and S contribute to mass 34 amu/e (e.g. (34)S(+), (13)CH3OH2(+), CH4DO(+)). These contributions can be calculated from the measured densities of the ions containing the major isotopes and the H2S(+) contribution from the measured H3S(+) density. From mass 34 amu/e we can also derive an upper limit of 1% for the abundance of deuterated methanol. This limit is at most marginally compatible with a direct interstellar origin of the CH3OH in P/Halley as the measured interstellar abundance of deuterated methanol is 1 to 6%.

Eberhardt, P.↗

Selective and Scalable Control of Spin Quantum Memories in a Photonic Circuit

A central goal in many quantum information processing applications is a network of quantum memories that can be entangled with each other while being individually controlled and measured with high fidelity. This goal has motivated the development of programmable photonic integrated circuits (PICs) with integrated spin quantum memories using diamond color center spin-photon interfaces. However, this approach introduces a challenge into the microwave control of individual spins within closely packed registers. Here, we present a quantum memory-integrated photonics platform capable of (i) the integration of multiple diamond color center spins into a cryogenically compatible, high-speed programmable PIC platform, (ii) selective manipulation of individual spin qubits addressed via tunable magnetic field gradients, and (iii) simultaneous control of qubits using numerically optimized microwave pulse shaping. The combination of localized optical control, enabled by the PIC platform, together with selective spin manipulation opens the path to scalable quantum networks on intrachip and interchip platforms.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Microwave Spectroscopy of Complex Molecules Around the Young Protostar Chamaeleon MMS1

Observations are presented of emission lines from organic molecules at frequencies 30-100 GHz in the vicinity of the extremely young, chemically rich, very low-luminosity protostar and candidate first hydrostatic core Chamaeleon MMS1. Column densities are derived and emission maps are presented for species including polyynes, cyanopolyynes, sulphuretted carbon-chains and methanol. Emission from the carbon-chain-bearing species peaks very near to the protostar; methanol peaks about 0.1 pc further away. The mean molecular hydrogen number density is calculated to be 10(exp 6) per cc. and the gas kinetic temperature is in the range 4-7 K. The abundances of long carbon chains (including C6H and HC7N) are very large -- similar to those found in the most carbon-chain-rich regions of the Galaxy, and indicative of a non-equilibrium carbon chemistry. The observed methanol and acetaldehyde abundances indicate active grain-surface chemistry and desorption processes. The carbon-chain anions C4H- and C6H- were not detected and the upper limit on the anion-to-neutral ratio for C4H- is less than 0.02% and for C6H-, less than 10%. These values are consistent with previous observations in interstellar clouds and low-mass protostars. Deuterated HC3N and c-C3H2 were detected, with fractionation ratios of about 4%, and 22%, respectively. A low c-C3H2 ortho-to-para ratio was measured, which is consistent with a molecular hydrogen ortho-to-para ratio of close to zero and implies a relatively young chemical age (less than about 10(exp 5) yr) for the matter surrounding Cha-MMS1. These observations show that a high level of chemical complexity can be present in star-forming gas.

Cordiner, Martin A.↗

Spectroscopy and chemistry of the atmosphere of Uranus

A comprehensive review of the chemistry and spectroscopy of the Uranian atmosphere is presented by means of earth-based, earth-orbital, and Voyager 2 observations covering the UV, visible, infrared, and radio wavelength regions. It is inferred from these observations, in concert with the average density of about 1.3 g/cu cm, that the Uranian atmosphere is enriched in heavy elements relative to solar composition. Pre-Voyager earth-based observations of CH4 bands in the visible region and Voyager radio occultation data imply a CH4/H2 volume mixing ratio of about 2 percent corresponding to an enrichment of approximately 24 times the solar value of 0.000835. In contrast to CH4, microwave observations indicate an apparent depletion of NH3 in the 155-to-200-K region of the atmosphere by 100 to 200 times relative to the solar NH3/H2 mixing ratio of -0.000174. It is suggested that the temporal and latitudinal variations deduced for the NH3/H2 mixing ratio in this region of the Uranian atmosphere are due to atmospheric circulation effects.

Fegley, Bruce, Jr.↗

Decline in Antarctic Ozone Depletion and Lower Stratospheric Chlorine Determined From Aura Microwave Limb Sounder Observations

Attribution of Antarctic ozone recovery to the Montreal protocol requires evidence that (1)Antarctic chlorine levels are declining and (2) there is a reduction in ozone depletion in response to achlorine decline. We use Aura Microwave Limb Sounder measurements of O3, HCl, and N2O to demonstratethat inorganic chlorine (Cly) from 2013 to 2016 was 223 ± 93 parts per trillion lower in the Antarctic lowerstratosphere than from 2004 to 2007 and that column ozone depletion declined in response. The mean Clydecline rate, ~0.8%/yr, agrees with the expected rate based on chlorofluorocarbon lifetimes. N2Omeasurements are crucial for identifying changes in stratospheric Cly loading independent of dynamicalvariability. From 2005 to 2016, the ozone depletion and Cly time series show matching periods of decline,stability, and increase. The observed sensitivity of O3 depletion to changing Cly agrees with the sensitivitysimulated by the Global Modeling Initiative chemistry transport model integrated

Ozone recovery↗

Optimized Microwave Digestion and Quantification Procedure for Boron Carbide samples

A microwave-assisted HNO3-H2SO4-HF digestion system was explored/optimized for the total dissolution of Boron Carbide samples followed by multi-elemental determination using ICP-MS and ICP OES, in order to improve the methods used in a previous try using a microwave-assisted H2O2-HNO3-HF digestion system. The samples were microwave digested to accomplish complete dissolution needed to perform quantitative analysis of their metal content. Two Boron Carbide samples were provided to us: JM10 and JM11. The Boron Carbide samples were completely dissolved at the end of the optimized microwave digestion procedure that was developed. The digested samples were analyzed for metals mostly by ICP MS; few elements were analyzed by ICP-OES. Microwave digestion reactions were performed in a Titan MPS instrument (Perkin Elmer, USA). Titan MPS instrument is equipped with Temperature and Pressure regulations and controlled by software. Each microwave digestion batch contained the samples of interest along with a reagent blank and one certified standard (1632e) in order to (i) compensate for the contaminations present in the reagents, (ii) ensure that the digestion was complete and (iii) that there was a good recovery of all the constituents. The certified standard used (1632e) was provided with USGS certificates of analysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗