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NASA NTRS1993

Airborne observations of the 1992 Arctic winter stratosphere by FTIR solar absorption spectroscopy

The JPL MkIV interferometer, a Fourier Transform Infra-Red (FTIR) spectrometer designed specifically for atmospheric remote sensing, made measurements of the composition of the Arctic stratosphere in January, February and March 1992. These measurements were made from the NASA DC-8 aircraft as part of the AASE2 campaign. The data reveal that despite 5 to 6 km of subsidence inside the vortex, which more than doubled the vertically integrated column amounts (burdens) of HF and HNO3 with respect to outside the vortex, considerable losses of NO2, HCl and ClNO3 were evident by mid-January. Temporary freeze-out of HNO3 was observed only on one occasion, Jan. 19, and was accompanied by substantial reductions in HCl and ClNO3. During February and March, ClNO3 and NO2 amounts increased dramatically. HCl also recovered but at a much slower rate, so that by March ClNO3 was the major reservoir of inorganic chlorine, at times exceeding HCl by a factor 2.

Toon, G. C.↗

NASA NTRS1994

On the relevance of the methane oxidation cycle to ozone hole chemistry

High concentrations of active chlorine are clearly responsible for the observed ozone depletion during the Antarctic polar spring. However, the mechanism behind the activation of chlorine from the reservoirs species HCl and ClONO2 and the maintenance of extremely high levels of active chlorine after polar sunrise is less well understood. Here, we focus on the influence of the methane oxidation cycle on 'ozone hole' chemistry through its effect on HOx and ClOx radicals. We demonstrate the great potential importance of the heterogeneous reaction HCl + HOCl yields Cl2 + H2O and the gasphase reaction ClO + CH3O2 yields ClOO + CH3O under sunlight conditions in polar spring. Under these conditions, the heterogeneous reaction is the main sink for HOx radicals. Through this channel, the HCl reservoir may be almost completely depleted. The gas phase reaction may control the levels of the CH3O2 radical, provided that high levels of ClO exist. Otherwise this radical initiates a sequence of reactions leading to a considerable loss of active chlorine. Moreover, the production of HOx radicals is reduced, and thereby the efficiency of the heterogeneous reaction limited. The two reactions together may accomplish the complete conversion of HCl into active chlorine, thereby leading to a rapid destruction of ozone.

Mueller, Rolf↗

NASA NTRS1993

In situ measurements of the ClO/HCl ratio: Heterogeneous processing on sulfate aerosols and polar stratospheric clouds

Simultaneous in situ measurements of stratospheric ClO and HCl have been made for the first time, during numerous flights of the ER-2 aircraft covering latitudes 24-90 deg N from October 1991 through March 1992. The ClO/HCl ratio is identified as a key indicator of heterogeneous processing both outside and within the Arctic polar vortex. For ClO mixing ratios below about 120 pptv, remarkably constant ClO/HCl values of about 15% characterize the lower stratosphere. The observed values are significantly higher than those derived from a 2-D model using either gas phase photochemistry alone (2%), or including heterogeneous sulfate chemistry (5-10%). During the Arctic early spring, after conversion of HCl into reactive chlorine has taken place, the vortex edge is poorly defined by ClO levels. Loss of HCl and its slow recovery following low-temperature polar heterogeneous chemistry distinguishes HCl as a new and unique dynamical tracer of polar stratospheric clouds (PSC)-processed air.

Webster, C. R.↗

NASA NTRS1993

In Situ Measurements of the ClO/HCl Ratio: Heterogeneous Processing on Sulfate Aerosols and Polar Stratospheric Clouds

Simultaneous in situ measurements of stratospheric ClO and HCl have been made for the first time, during numerous flights of the ER-2 aircraft covering latitudes 24-90 deg. N from October 1991 through March 1992. The ClO/HCl ratio is identified as a key indicator of heterogeneous processing both outside and within the Arctic polar vortex. For ClO mixing ratios below about 120 pptv, remarkably constant ClO/HCl values of about 15% characterize the lower stratosphere. The observed values are significantly higher than those derived from a 2-D model using either gas phase photochemistry alone (2%), or including heterogeneous sulfate chemistry (5-10%). During the Arctic early spring, after conversion of HCl into reactive chlorine has taken place, the vortex edge is poorly defined by ClO levels. Loss of HCl and its slow recovery following low-temperature polar heterogeneous chemistry distinguishes HCl as a new and unique dynamical tracer of PSC-processed air.

Webster, C. R.↗

NASA NTRS1996

ATMOS/ATLAS-3 Measurements of Stratospheric Chlorine and Reactive Nitrogen Partitioning Inside and Outside the November 1994 Antarctic Vortex

Partitioning between HCl and ClONO2 and among the main components of the reactive nitrogen family (NO, NO2, HNO3, ClONO2, N2O5, and HO2NO2) has been studied inside and outside the Antarctic stratospheric vortex based on ATMOS profiles measured at sunrise during the 3-12 November 1994 ATLAS-3 Shuttle mission. Elevated mixing ratios of HCl in the lower stratosphere with a peak of approximately 2.9 ppbv (10(exp -9) parts per volume) were measured inside the vortex near 500 K potential temperature (approximately 19 km). Maximum ClONO2 mixing ratios of approximately 1.2, approximately 1.4, and approximately 0.9 ppbv near 700 K (approximately 25 km) were measured inside, at the edge, and outside the vortex, respectively. Model calculations reproduce the higher levels of HCl and NO(x) (NO + NO2) inside the lower stratospheric vortex both driven by photochemical processes initiated by low O3. The high HCl at low O3 results from chemical production of HC1 via the reaction of enhanced Cl with CH4, limited production of ClONO2, and the descent of inorganic chlorine from higher altitudes.

Rinsland, C. P.↗

NASA NTRS1993

In Situ Measurements of the ClO/HCl Ratio: Heterogeneous Processing on Sulfate Aerosols and Polar Stratospheric Clouds

Webster, C. R.↗

NASA NTRS2006

Temporal Decrease in Upper Atmospheric Chlorine

We report a steady decrease in the upper stratospheric and lower mesospheric abundances of hydrogen chloride (HCl) from August 2004 through January 2006, as measured by the Microwave Limb Sounder (MLS) aboard the Aura satellite. For 60(deg)S to 60(deg)N zonal means, the average yearly change in the 0.7 to 0.1 hPa (approx.50 to 65 km) region is -27 +/- 3 pptv/year, or -0.78 +/- 0.08 percent/year. This is consistent with surface abundance decrease rates (about 6 to 7 years earlier) in chlorine source gases. The MLS data confirm that international agreements to reduce global emissions of ozone-depleting industrial gases are leading to global decreases in the total gaseous chlorine burden. Tracking stratospheric HCl variations on a seasonal basis is now possible with MLS data. Inferred stratospheric total chlorine (CITOT) has a value of 3.60 ppbv at the beginning of 2006, with a (2-sigma) accuracy estimate of 7%; the stratospheric chlorine loading has decreased by about 43 pptv in the 18-month period studied here. We discuss the MLS HCl measurements in the context of other satellite-based HCl data, as well as expectations from surface chlorine data. A mean age of air of approx. 5.5 years and an age spectrum width of 2 years or less provide a fairly good fit to the ensemble of measurements.

chlorine↗

NASA NTRS2020

High-temperature Hydrogen Chloride Releases from Mixtures of Sodium Chloride with Sulfates: Implications for the Chlorine-Mineralogy as Determined by the Sample Analysis at Mars Instrument on the Curiosity Rover in Gale Crater, Mars

Hydrogen chloride releases above 500 °C occurred in several samples analyzed by the Sample Analysis at Mars (SAM) evolved gas analyzer on the Curiosity rover in Gale crater. These have been attributed to reactions between chlorides (original or from oxychlorine decomposition) and water. Some of these HCl releases that peaked below the melting temperature of common chlorides did not co-evolve with oxygen or water, and were not explained by laboratory analog work (Figure 1). Therefore, these HCl releases were not caused by MgCl2 or soley due to reactions between water and melting chlorides. The goal of this work was to explain the HCl releases that did not co-evolve with oxygen or water and occurred below the melting point of common chlorides, which have not been explained by previous laboratory analog work. This work specifically evaluates the role of evolved SO2 in the production of HCl.

Clark, J.V.↗

NASA NTRSDate not supplied

Modeling the Uptake of Hydrogen Chloride onto Interior Spacecraft Materials

Hydrogen chloride (HCl) is a major combustion product from the pyrolysis of polyvinyl chloride (PVC) insulated electrical wires, a common spacecraft fire safety concern. Models at two different scales were developed to predict HCl uptake on anodized, chromate conversion coated (Iridite), and bare aluminum surfaces, as well as on Nomex fabric: a macroscopic one-step global surface reaction model where all the active sites are on the exterior surface, and a pore model where the interior active sites deeper into the oxide layer can also be accessed by HCl. Experiments were performed to calibrate kinetic and diffusion constants in the models. A cast acrylic test cell was used to measure the differences between the inlet and outlet concentration of HCl after inserting a sample rod of the test material. For the materials with a thin (< 200 µm) or no oxide layer, the macroscopic surface reaction model adequately predicts the experimental measurements. For the anodized aluminum with a thicker oxide layer, the pore model provided a better match to experimental results. The results will be discussed with respect to the spacecraft fire safety project (Saffire).

modeling↗

DOE OSTI2021

Visualizing plant cell wall changes proves the superiority of hydrochloric acid over sulfuric acid catalyzed γ-valerolactone pretreatment

Thermochemical pretreatment is one of the key steps to process lignocellulosic biomass for production of biofuels and biomaterials. γ-valerolactone (GVL) has been used as a green and renewable solvent to efficiently dissolve lignin under acidic conditions and enhance subsequent enzyme digestibility. Further improvement is still required to lower the pretreatment temperature in order to reduce sugar degradation and irreversible lignin condensation, as well as the capital cost. In this study, we compared the use of HCl and H 2 SO 4 as catalysts during GVL pretreatment, and found the performance of GVL-HCl at 100 °C was comparable to that of GVL-H 2 SO 4 at 120 °C in terms of xylan and lignin removal and enzyme digestibility. We further monitored the lignin removal and cellulose accessibility in the cell walls at different pretreatment time points by imaging the changes in lignin auto-fluorescence and in CtCBM3-GFP binding with confocal laser scanning microscopy (CLSM), respectively. We found GVL-HCl pretreatment at a relative low temperature (100 °C) could rapidly remove lignin in the compound middle lamella and cell corner areas, which concurred with the increase of CtCBM3-GFP binding in these areas. Real-time imaging of cell wall degradation by cellulases further revealed that the secondary cell walls could be digested from both cell lumen and CML sides, and eventually fully deconstructed within 24 h. Furthermore, our results provide new insight into the effects of chloride anions on plant cell wall structure during GVL pretreatment, and offer potential routes to further optimize and enhance the efficiency of GVL-based pretreatment.

09 BIOMASS FUELS↗

DOE OSTI2025

Highly crystalline, low-ash, graphite from coal using an Fe 2 O 3 -based catalytic process with recovery and reuse of catalyst and process acid

This study presents a sustainable process for producing highly crystalline, low-ash graphite from sub-bituminous coal using an Fe 2 O 3 -based catalytic method. The process integrates coal mineral removal, catalyst regeneration, and reagent recycling into a closed-loop system. Acid-soluble Fe-residue and mineral impurities are eliminated from the solid graphite through HCl treatment, followed by hydrolytic distillation to regenerate Fe 2 O 3 and recover HCl for reuse. Coal-derived silica is removed with a KOH rinse, yielding low-ash graphite suitable for high-performance applications. The closed-loop catalytic graphitization, where the recovered Fe 2 O 3 and HCl are used in subsequent graphitization runs, produces graphite with a degree of graphitization exceeding 95%. The L a and L c crystallite sizes reach 65–78 nm and 44–48 nm, respectively, with BET surface areas of 4–10 m 2 /g and an ash content below 0.1 wt.%. Lithium-ion battery testing reveals that anodes fabricated with this graphite deliver an initial discharge capacity between 384.5 and 421.2 mAh/g, averaging 395.0 ± 19.1 mAh/g, along with initial coulombic efficiencies of 85.0–89.1%. After 100 discharge–charge cycles at 0.25C, reversible capacities remain between 358.8 and 369.7 mAh/g, while coulombic efficiency stays above 99.9%. The findings highlight that coal can serve as a viable precursor for high-quality graphite production under relatively mild conditions, avoiding the need for extreme temperatures or aggressive reagents such as hydrofluoric acid, commonly employed in conventional processes. This work demonstrates both technical feasibility and environmental benefits, emphasizing its potential to support large-scale, sustainable graphite production for applications such as lithium-ion batteries.

Catalytic graphitization↗

DOE OSTI2025

A Novel Solid Form of Erlotinib: Synthesis by Heterogeneous Complexation and Characterization by NMR Crystallography

We describe the synthesis of a novel complex of the anticancer "active pharmaceutical ingredient erlotinib (ERL) via heterogeneous nucleation on polished zinc tiles. The resulting product, ERL 2 ·ZnCl 2 , is characterized by single-crystal X-ray diffraction, multinuclear solid-state NMR (ssNMR) spectroscopy, and density functional theory (DFT) calculations. Also characterized are the hydrochloride salt (ERL·HCl) and monohydrate free base (ERL·H 2 O) forms of erlotinib. 13 C ssNMR spectroscopy is useful for site-by-site assignment and rapid fingerprinting, while also providing preliminary structural interpretations, such as the number of molecules in the asymmetric unit. 35 Cl ssNMR can readily differentiate between the chloride ions in ERL·HCl and the covalently bonded chlorine in ERL 2 ·ZnCl 2 . 15 N ssNMR proves to be critical here because of the large isotropic chemical shift differences between ERL·H 2 O, ERL·HCl, and ERL 2 ·ZnCl 2 . The 15 N chemical shift tensors are linked directly to differences in structure and bonding with the aid of DFT calculations. Together, these results demonstrate the utility of multinuclear NMR crystallography for the characterization of solid forms of APIs, especially when other analytical techniques face significant challenges.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Unsaturated Sulfur Crown Ethers Can Extract Mercury(II) and Show Promise for Future Copernicium(II) Studies: A Combined Experimental and Computational Study

The unsaturated hexathia-18-crown-6 (UHT18C6) molecule was investigated for the extraction of Hg(II) in HCl and HNO3 media. This extractant can be directly compared to the recently studied saturated hexathia-18-crown-6 (HT18C6). The default conformation of the S lone pairs in UHT18C6 is endodentate, where the pocket of the charge density, according to the crystal structures, is oriented toward the center of the ring, which should allow better extraction for Hg(II) compared to the exodentate HT18C6. Batch study experiments showed that Hg(II) had better extraction at low acid molarity (ca. 99% in HCl and ca. 95% in HNO 3 ), while almost no extraction was observed above 0.4 M HCl and 4 M HNO 3 (<5%). Speciation studies were conducted with the goal of delineating a plausible extraction mechanism. Density functional theory calculations including relativistic effects were carried out on both Hg(II)-encapsulated HT18C6 and UHT18C6 complexes to shed light on the binding strength and the nature of bonding. Our calculations offer insights into the extraction mechanism. In addition to Hg(II), calculations were performed on the hypothetical divalent Cn(II) ion, and showed that HT18C6 and UHT18C6 could extract Cn(II). Finally, the extraction kinetics were explored to assess whether this crown can extract the short-lived Cn(II) species in a future online experiment.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2023

Modeling–Experiment–Theory Analysis of Reactions Initiated from Cl + Methyl Formate

Methyl formate (MF; CH 3 OCHO) is the smallest representative of esters, which are common components of biodiesel. The present study characterizes the thermal dissociation kinetics of the radicals formed by H atom abstraction from MF—CH 3 OCO and CH 2 OCHO—through a combination of modeling, experiment, and theory. For the experimental effort, excimer laser photolysis of Cl 2 was used as a source of Cl atoms to initiate reactions with MF in the gas phase. Time-resolved species profiles of MF, Cl 2 , HCl, CO 2 , CH 3 , CH 3 Cl, CH 2 O, and CH 2 ClOCHO were measured and quantified using photoionization mass spectrometry at temperatures of 400–750 K and 10 Torr. The experimental data were simulated using a kinetic model, which was informed by ab initio-based theoretical kinetics calculations and included chlorine chemistry and secondary reactions of radical decomposition products. Here, we calculated the rate coefficients for the H-abstraction reactions Cl + MF → HCl + CH 3 OCO (R1a) and Cl + MF → HCl + CH 2 OCHO (R1b): k 1a,theory = 6.71 × 10 –15 ·T 1.14 ·exp(—606/T) cm 3 /molecule·s; k 1b,theory = 4.67 × 10 –18 ·T 2.21 ·exp(—245/T) cm 3 /molecule·s over T = 200–2000 K. Electronic structure calculations indicate that the barriers to CH 3 OCO and CH 2 OCHO dissociation are 13.7 and 31.6 kcal/mol and lead to CH 3 + CO 2 (R3) and CH 2 O + HCO (R5), respectively. The master equation-based theoretical rate coefficients are k 3,theory (P = ∞) = 2.94 × 10 9 ·T 1.21 ·exp(—6209/T) s –1 and k 5,theory (P = ∞) = 8.45 × 10 8 ·T 1.39 ·exp(—15132/T) s –1 over T = 300–1500 K. The calculated branching fractions into R1a and R1b and the rate coefficient for R5 were validated by modeling of the experimental species time profiles and found to be in excellent agreement with theory. Additionally, we found that the bimolecular reactions CH 2 OCHO + Cl, CH 2 OCHO + Cl 2 , and CH 3 + Cl 2 were critical to accurately model the experimental data and constrain the kinetics of MF-radicals. Inclusion of the kinetic parameters determined in this study showed a significant impact on combustion simulations of larger methyl esters, which are considered as biodiesel surrogates.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Resolving Heterogeneous Dynamics of Excess Protons in Aqueous Solution with Rate Theory

Rate theories have found great utility across the chemical sciences by providing a physically transparent way to analyze dynamical processes. Here we demonstrate the benefits of using transition state theory and Marcus theory to study the rate of proton transfer in HCl solutions. By using long ab initio molecular dynamics simulations we show that good agreement is obtained between these two different formulations of rate theory and how they can be used to study the pathways and life-time of proton transfer in aqueous solution. Since both rate theory formulations utilize identical sets of molecular data, this provides a self-consistent theoretical picture of the rates of aqueous phase proton transfer. Specifically, we isolate and quantify the rates of proton transfer, ion-pair dissociation, and solvent exchange in concentrated HCl solutions. Our analysis predicts a concentration dependence to both proton transfer and ion-pairing. Moreover, our estimate of the life-time for the Zundel species is 0.8 ps and 1.3 ps for 2M and 8M HCl, respectively. In this paper, we demonstrate that concentration effects, can indeed be quantified through the combination of state-of-the-art simulation and theory and provides a picture of the important correlations between the cation (hydronium) and the counter-ion in acid solutions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Kinetic Study of Polyvinyl Chloride Pyrolysis with Characterization of Dehydrochlorinated PVC

In this paper, we study the kinetics of polyvinyl chloride (PVC) decomposition using a combination of experimental and computational approaches. Here, we develop a simplified kinetic model that contains only two steps: dehydrochlorination of PVC and further decomposition of the PVC residue. The model is consistent with density functional theory (DFT) calculations and experimental data. Dehydrochlorination is an autocatalytic reaction that starts with a tertiary chloride (Cl) and generates hydrogen chloride (HCl) and benzene as the main products. Benzene and HCl formation rates showed similar trends, indicating that HCl likely catalyzes a homolytic carbon-carbon (C-C) bond cleavage, which gives rise to benzene and an aliphatic fragment. We characterized the structure of dehydrochlorinated PVC (PVC residue) by using thermal gravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FTIR), and nuclear magnetic resonance spectroscopy (NMR). FTIR and NMR results indicate that the PVC residue contains 20% quaternary carbon content, indicating a high concentration of cross-linked molecules. We predict that the most probable structure in the cross-linked centers of the PVC residue is cyclohexadiene, which is supported by DFT calculations, FTIR, and NMR.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Strong mutual increase in the efficiency of isotope-selective laser IR dissociation of molecules under nonequilibrium thermodynamic conditions of the compression shock under irradiation in a bimolecular mixture

We have revealed a strong (by a factor of 2 to 5) mutual increase in the yield of IR molecular dissociation (by the example of CF{sub 2}HCl and CF{sub 3}Br) and a significant (by a factor of 1.5 to 3) lowering of dissociation thresholds in the nonequilibrium thermodynamic conditions of compression shock in the irradiation of the molecules by resonance IR laser radiation in the bimolecular mixture in comparison with their individual irradiation. This opens up the possibility to perform efficient isotope-selective IR dissociation of molecules at lower excitation energy densities (Φ ⩽ 1.5 – 2.0 J cm{sup −2}) and thereby to improve the dissociation selectivity. This was demonstrated by the example of chlorine- and bromine-isotope selective dissociation of the specified molecules, which are characterised by quite small (less than 0.25 cm{sup −1}) isotope shifts in the IR vibrational absorption spectra excited by laser radiation. The enrichment coefficients K {sub enr}({sup 35}Cl / {sup 37}Cl) = 0.90 ± 0.05 in the residual CF{sub 2}HCl gas and K {sub enr}({sup 79}Br / {sup 81}Br) in the resultant Br{sub 2} product are obtained when the CF{sub 2}HCl : CF{sub 3}Br = 1 : 1 molecular mixture and CF{sub 3}Br molecules, respectively, are irradiated by the 9R(30) CO{sub 2} laser line (frequency, 1084.635 cm{sup −1}) at an energy density Φ ≈ 1.3 J cm{sup −2}. (laser isotope separation)

36 MATERIALS SCIENCE↗

DOE OSTI2022

In Situ High-Temperature TEM Observation of Inconel Corrosion by Molten Chloride Salts with N 2 , O 2 , or H 2 O

Here, in situ transmission electron microscopy (TEM) diffraction and imaging techniques are used to monitor and quantify corrosion of Inconel-625 by pure molten chloride salts (MgCl 2 – NaCl – KCl) at 500 °C–800 °C in 1.0 atm inert N 2 or pure O2, or by salts which are controllably hydrated in a high vacuum chamber. The isothermal corrosion rate R in inert N 2 increases from 203 ± 30 μ m year –1 at 700 °C to 463 ± 30 μ m year –1 at 800 °C. An oxygen ambient causes a six-fold increase to R = 1261 ± 170 μ m year –1 at 700 °C. Salt hydration dramatically accelerates corrosion to R > 3 × 10 5 μ m year –1 at 700 °C while it leads to a more moderate R = 95 ± 20 and 486 ± 30 μ m year –1 at 500 °C and 600 °C, respectively. These isothermal corrosion rates indicate that the molten chloride corrosion is significantly accelerated by salt hydration at temperatures above 600 °C, where corrosion is aggravated by increased generation and solubility of corrosive HCl gases. Hence, to reduce rate of corrosion it is important to both avoid incorporation of H 2 O into the system at each stage and ensure proper flushing of the system before increasing the temperature beyond 600 °C. Compositional analysis of the corroded cells indicate that corrosion in O 2 ambient is dominated by oxidation of metals by O 2 gas dissolved in the chloride melt, but corrosion in H 2 O ambients is caused by chlorination of metals by dissolved HCl gas and MgOH + ions. So, to reduce rate of corrosion, steps should be taken to tailor chloride melt compositions that has low solubility for HCl and O 2 . All of our corroded samples exhibit passive-protective oxide layers of Cr, Mg, and Ni. In addition, distinct volatile compounds of Ni, Mo and Cr involving NiCl 2 , (Na,K) 2 MoO 4 and CrO 2 (OH) 2 are detected in N 2 , H 2 O, and O 2 ambients, respectively. We believe that corrosion acceleration can be minimized by minimizing formation of volatile by-products or promoting reactions that could convert these volatile compounds to solid phases, as these volatile compounds led to destruction of protective oxide layers.

14 SOLAR ENERGY↗