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At least 595 records · Page 33

Surface distribution of heterogenous clathrin assemblies in resorbing osteoclasts

Highlights: • Platinum replica microscopy has revealed new structural data on the clathrins on the ventralmembrane of osteoclasts. • Various clathrins were visualized, suggesting that they followed variations in the surface topography of the apatite. • Most of the flat clathrins may participate in the adhesive and mechnosensory functions in co-operation with podosomes. • The present findings in osteoclast biology reveal potential novel drug targets or treatment regimens. Osteoclasts seeded on either glass coverslips or apatite pellets have at least two morphologically distinct substrate adhesion sites: actin-based adhesion structures including podosome belts and sealing zones, and adjacent clathrin sheets. Clathrin-coated structures are exclusively localized at the podosome belts and sealing zone, in both of which the plasma membrane forms a tight attachment to the substrate surface. When cultured on apatite osteoclasts can degrade the apatite leading to the formation of resorption lacunae. The sealing zone divides the ventral membrane into different domains, outside and inside of the sealing zones. The former facing the smooth-surfaced intact apatite contains relatively solitary or networks of larger flat clathrin structures; and the latter, facing the rough-surfaced degraded apatite in the resorption lacunae contain clathrin in various shapes and sizes. Clathrin assemblies on the membrane domain facing not only a resorption lacuna, or trails but also intact apatite indeed were observed to be heterogeneous in size and intensity, suggesting that they appeared to follow variations in the surface topography of the apatite surface. These results provide a detailed insight into the flat clathrin sheets that have been suggested to be the sites of adhesion and mechanosensing in co-operation with podosomes.

60 APPLIED LIFE SCIENCES↗

Charge Transport in Zirconium-Based Metal–Organic Frameworks

Metal–organic frameworks (MOFs) are a class of crystalline porous materials characterized by inorganic nodes and multitopic organic linkers. Because of their molecular-scale porosity and periodic intraframework chemical functionality, MOFs are attractive scaffolds for supporting and/or organizing catalysts, photocatalysts, chemical-sensing elements, small enzymes, and numerous other functional-property-imparting, nanometer-scale objects. Notably, these objects can be installed after the synthesis of the MOF, eliminating the need for chemical and thermal compatibility of the objects with the synthesis milieu. Thus, postsynthetically functionalized MOFs can present three-dimensional arrays of high-density, yet well-separated, active sites. Depending on the application and corresponding morphological requirements, MOF materials can be prepared in thin-film form, pelletized form, isolated single-crystal form, polycrystalline powder form, mixed-matrix membrane form, or other forms. For certain applications, most obviously catalytic hydrolysis and electro- or photocatalytic water splitting, but also many others, an additional requirement is water stability. MOFs featuring hexa-zirconium(IV)-oxy nodes satisfy this requirement. For applications involving electrocatalysis, charge storage, photoelectrochemical energy conversion, and chemiresistive sensing, a further requirement is electrical conductivity, as embodied in electron or hole transport. As most MOFs, under most conditions, are electrically insulating, imparting controllable charge-transport behavior is both a chemically intriguing and chemically compelling challenge. Herein, we describe three strategies to render zirconium-based metal–organic frameworks (MOFs) tunably electrically conductive and, therefore, capable of transporting charge on the few nanometers (i.e., several molecular units) to few micrometers (i.e., typical dimensions for MOF microcrystallites) scale. The first strategy centers on redox-hopping between periodically arranged, chemically equivalent sites, essentially repetitive electron (or hole) self-exchange. Zirconium nodes are electrically insulating, but they can function as grafting sites for (a) redox-active inorganic clusters or (b) molecular redox couples. Alternatively, charge hopping based on linker redox properties can be exploited. Marcus’s theory of electron transfer has proven useful for understanding/predicting trends in redox-hopping based conductivity, most notably, in accounting for variations as great as 3000-fold depending on the direction of charge propagation through structurally anisotropic MOFs. In MOF environments, propagation of electronic charge via redox hopping is necessarily accompanied by movement of charge-compensating ions. Consequently, rates of redox hopping can depend on both the identity and concentration of ions permeating the MOF. In the context of electrocatalysis, an important goal is to transport electronic charge fast enough to match or exceed the inherent activity of MOF-based or MOF-immobilized catalysts. Bandlike electronic conductivity is the focus of an alternative strategy: one based on the introduction of molecular guests capable of forming donor–acceptor charge transfer complexes with the host framework. Theory again can be applied predictively to alter conductivity. A third strategy similarly emphasizes electronic conductivity, but it makes use of added bridges in the form of molecular oligomers or inorganic clusters that can then be linked to span the length of a MOF crystallite. For all strategies, retention of molecular-scale porosity is emphasized, as this property is key to many applications. Lastly, while our focus is on Zr-MOFs, the described approaches clearly are extendable to other MOF compositions, as has already been demonstrated, in part, in studies by others.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Thermally Driven Interfacial Degradation between Li 7 La 3 Zr 2 O 12 Electrolyte and LiNi 0.6 Mn 0.2 Co 0.2 O 2 Cathode

Solid-state batteries offer higher energy density and enhanced safety compared to the present lithium-ion batteries using liquid electrolytes. A challenge to implement them is the high resistances, especially at the solid electrolyte interface with the cathode. Sintering at elevated temperature is needed in order to get good contact between the ceramic solid electrolyte and oxide cathodes and thus to reduce contact resistances. Many solid electrolyte and cathode materials react to form secondary phases. It is necessary to find out which phases arise as a result of interface sintering and evaluate their effect on electrochemical properties. Herein, we assessed the interfacial reactions between LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622) and Li 7 La 3 Zr 2 O 12 (LLZO) as a function of temperature in air. We prepared model systems by depositing thin-film NMC622 cathode layers on LLZO pellets. The thin-film cathode approach enabled us to use interface-sensitive techniques such as X-ray absorption spectroscopy in the near-edge as well as the extended regimes and identify the onset of detrimental reactions. We found that the Ni and Co chemical environments change already at moderate temperatures, on-setting from 500 °C and becoming especially prominent at 700 °C. By analyzing spectroscopy results along with X-ray diffraction, we identified Li 2 CO 3 , La 2 Zr 2 O 7 , and La(Ni,Co)O 3 as the secondary phases that formed at 700 °C. The interfacial resistance for Li transfer, measured by electrochemical impedance spectroscopy, increases significantly upon the onset and evolution of the detected interface chemistry. Our findings suggest that limiting the bonding temperature and avoiding CO 2 in the sintering environment can help to remedy the interfacial degradation.

36 MATERIALS SCIENCE↗

Multiscale Modeling of a Direct Nonoxidative Methane Dehydroaromatization Reactor with a Validated Model for Catalyst Deactivation

Due to the recent boom in shale gas production, aromatics production using direct nonoxidative methane dehydroaromatization (DHA) is being investigated extensively. However, due to rapid coke formation, catalysts in the nonoxidative methane DHA reactors get deactivated, which is one of the critical issues for the commercial success of the methane DHA process. In this paper, a model for catalyst deactivation is developed. Rate models for other DHA reactions are developed by considering the decrease in the catalyst activity with time. Due to the very fast coke formation rate on the fresh catalyst, there is coke formation immediately upon the introduction of the feed. Therefore, an algorithm is developed for estimation of the initial state of the reactor and the kinetic parameters by coupling an iterative direct substitution approach with an optimization approach. Transient experimental data from an in-house reactor are first reconciled and then used for developing the kinetic model including the coke formation model. Using the rate model, a dynamic, heterogeneous, multiscale reactor model with embedded heating is developed. Here, the model couples the catalyst pellet level model with a reactor level model. Impacts of temperature, L/D ratio, and scheduling of reactors on variability in conversion and yield with time are studied.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Enhancing the Chemical Energy Flux in a High-Temperature Tubular Counterflow Solid Fuel Synthesis Reactor Using a Bypass

Redox reactions of metal oxides offer a path towards using intermittent renewable resources for high-density thermochemical energy storage. Thermochemical energy storage often involves the flow of a particulate media. We describe a novel method to increase the throughput in a gravity-driven high-temperature thermochemical storage reactor flowing pelletized MgMnO. The moving bed reactor operates under counter-flow conditions and encounters particle flowability problems at temperatures of 1500 °C leading to sintering of the bed. Inertial forces of a counter-flowing gas can overcome the gravitational forces on the particles and limit the chemical energy storage rate of the reactor. We found that the insertion of a gas bypass (a slotted tube) into the reactor results in a 100% increase of the flow rates and achieved a 50% higher chemical energy storage flux compared to the operation without a bypass tube while mitigating the effects of sintering on the particles. As a result, the higher solid flow rates require a longer heated zone to reach a comparable residence time and extent of reduction compared to the lower flow rates.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Phase Change-Driven Negative Activation Energies in Pd/Carbon-Based/Organic Getter Hydrogenation Reactions

In this study, the hydrogenation of 1,4-diphenylbutadiyne (DPB) blended with carbon-supported Pd (DPB–Pd/C) in the form of pellets was investigated by isothermal–isobaric experiments at 1333 Pa of H 2 and in the temperature range of 291–315 K. The extracted kinetics were then used in conjunction with a complementary constant rate of H 2 input experimentation to model the performance of a DPB-catalysis/support system as a function of temperature and H 2 partial pressure. First-principles density functional theory (DFT) calculations were also performed to shed light on the molecular level energetics of DPB and its intermediate states. A seemingly puzzling formation of alternate positive activation energy barrier (higher reaction rate with higher temperature) and negative activation energy barrier (higher reaction rate with lower temperature) zones during the hydrogenation process was discovered. However, this observed phenomenon can be logically explained in terms of the associated phase changes and H 2 transport in the material. This work provides a good illustration of a rarely encountered chemical process with a negative activation energy barrier.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

X-ray Diffraction of Water in Polyvinylpyrrolidone

PVP is a hydrophilic polymer commonly used as an excipient in pharmaceutical formulations. Here we have performed time-resolved high-energy X-ray scattering experiments on pellets of PVP at different humidity conditions for 1-2 days. A two-phase exponential decay in water sorption is found with a peak in the differential pair distribution function at 2.85 Å, which is attributed to the average (hydrogen bonded) carbonyl oxygen-water oxygen distance. Additional scattering measurements on powders with fixed compositions ranging from 2 to 12.3 wt % H 2 O were modeled with Empirical Potential Structure Refinement (EPSR). Further, the models reveal approximately linear relations between the carbonyl oxygen-water oxygen coordination number (nO C - O W ) and the water oxygen-water oxygen coordination number (nO W - O W ) versus water content in PVP. A stronger preference for water-water hydrogen bonding over carbonyl-water bonding is found. At all the concentrations studied the majority of water molecules were found to be randomly isolated, but a wide distribution of coordination environments of water molecules is found within the PVP polymer strands at the highest concentrations. Overall, the EPSR models indicate a continuous evolution in structure versus water content with nO W - O W =1 occurring at similar to 12 wt % H 2 O, i.e., the composition where, on average, each watermolecule is surrounded by one other water molecule.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Improved Solid-State Reaction Method for Scaled-Up Synthesis of Ceramic Proton-Conducting Electrolyte Materials

Protonic ceramic electrochemical cells (PCECs) represent promising technologies in the production of clean electricity, decarbonized hydrogen, chemicals, and fuels at intermediate temperatures. One of the challenges in commercializing PCECs is to produce the electrolyte materials on a large scale. The conventional solid-state reaction (SSR) method suffers from tedious synthesis procedures and low phase purity of the products due to the formation of unwanted secondary phases. Herein, we report an improved SSR (i-SSR) method for kilogram-scale production of high phase-purity electrolyte material BaZr 0.4 Ce 0.4 Y 0.1 Yb 0.1 O 3–δ (BZCYYb4411). In this method, the ball-milled precursor powders are pelletized prior to calcination, which effectively reduces the length of the diffusion paths between the components during perovskite phase formation. In this study, the synthesis procedure and calcination temperature are carefully optimized for efficient and repeatable production based on the powder crystallization behavior. A combined technoeconomic analysis and life cycle assessment modeling suggest that the i-SSR method could reduce the total production cost and greenhouse gas emissions by up to 19% and 39%, respectively, compared to the conventional SSR method. The high quality of the synthesized electrolyte material is corroborated by the excellent electrical conductivity and electrochemical performance of the fabricated PCEC cells.

36 MATERIALS SCIENCE↗

Surfactant Effects on Carbon Black Slurries for Aqueous Flow-Electrode Applications

Aqueous carbon black (CB) slurries are promising for flow-electrode applications due to their low cost and high electrical conductivity. Here, in this study, we investigate the impact of introducing a nonionic surfactant (Tween 20) on the rheological and electrical properties of 5 wt % Vulcan XC72R CB slurries in a 50 mM NaCl aqueous solution. We observe a Tween 20 critical concentration around 1.2 wt % that triggers an abrupt transition from a conductive gel to a high-resistance Newtonian fluid. This sudden network collapse coincides with a 250-fold reduction in settled mass, a 1–2 order of magnitude drop in viscosity, and a nearly 100-fold decrease in slurry conductivity. Centrifuged pellet conductivity measurements support the conclusion that this performance loss is largely due to the destruction of the gel network, rather than increased particle-to-particle resistance. SEM imaging suggests that the network is built from large 10 to 50 μm agglomerates that are fully dissolved above the critical surfactant concentration. We found that subcritical surfactant addition improved slurry shelf stability over 90 days, but that electrochemical cell testing revealed progressive performance degradation during operation. These results highlight the need for strategies that maximize long-term electrical conductivity without compromising viscosity, sedimentation stability, or resistance to accumulation on internal surfaces.

Materials science↗

Effect of Liquid Electrolyte Soaking on the Interfacial Resistance of Li 7 La 3 Zr 2 O 1 2 for All-Solid-State Lithium Batteries

In this work, the impact of liquid electrolyte soaking on the interfacial resistance between the garnet-structured Li 7 La 3 Zr 2 O 12 (LLZO) solid electrolyte and metallic lithium has been studied. Lithium carbonate (Li 2 CO 3 ) formed by inadvertent exposure of LLZO to ambient conditions is generally known to increase interfacial impedance and decrease lithium wettability. Soaking LLZO powders and pellets in the electrolyte containing lithium tetrafluoroborate (LiBF 4 ) shows a significantly reduced interfacial resistance and improved contact between lithium and LLZO. Raman spectroscopy, X-ray diffraction, and soft X-ray absorption spectroscopy reveal how Li 2 CO 3 is continuously removed with increasing soaking time. On-line mass spectrometry and free energy calculations show how LiBF 4 reacts with surface carbonate to form carbon dioxide. Using a very simple and scalable process that does not involve heat-treatment and expensive coating techniques, we show that the Li–LLZO interfacial resistance can be reduced by an order of magnitude.

25 ENERGY STORAGE↗

Electro-Chemo-Mechanical Evolution at the Garnet Solid Electrolyte–Cathode Interface

Solid-state batteries promise higher energy density and improved safety compared with lithium-ion batteries. However, electro-chemomechanical instabilities at the solid electrolyte interface with the cathode and the anode hinder their large scale implementation. Here, in this study, we focus on resolving electro-chemo-mechanical instability mechanisms and their onset conditions between a state-of-the-art cathode, LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622), and the garnet Li 7 La 3 Zr 2 O 12 (LLZO) solid electrolyte. We used thin-film NMC622 on LLZO pellets to place the interfacial region within the detection depth of the X-ray characterization techniques. The experimental probes of the near-interface region included in operando X-ray absorption spectroscopy and ex situ focused ion beam scanning electron microscopy. Electrochemical degradation was not observable during cycling at room temperature with 4.3 V versus Li/Li + charge voltage cutoff, or with stepwise potentiostatic hold up to 4.1 V versus Li/Li + . In contrast, secondary phases including reduced transition metal species (Ni 2+ , Co 2+ ) were found after cycling up to 4.3 V versus Li/Li + at 80 °C and during potentiostatic hold at 4.3 V versus Li/Li + (Ni 2+ ). Intergranular cracks between NMC622 grains and delamination at the NMC622|LLZO interface occurred readily after the first charge. These interface reaction products and mechanical failure lowered the capacity and cell efficiency due to partial loss of the NMC622 phase, partial loss of contact at the interface, and a higher polarization resistance. Electrochemical instability between delithiated NMC622 and LLZO could be mitigated by using a low charge voltage cutoff or cycling at lower temperature. Ways to engineer the mechanical properties to avoid crack deflection and delamination at the interface are also discussed for enhancing mechanical stability.

36 MATERIALS SCIENCE↗

ThO 2 and Th 1– x U x O 2 Nanoscale Materials and Thin Films for Nuclear Science Applications

This study investigates the dynamics and mechanisms of solution combustion synthesis (SCS) for the preparation of nanoscale ThO 2 and Th 1–x U x O 2 materials, utilizing metal nitrates (Th(NO 3 ) 4 and UO 2 (NO 3 ) 2 ) and acetylacetone (C 5 H 8 O 2 ) as reactants dissolved in a 2-methoxyethanol (C 3 H 8 O 2 ) solvent. By combining thermodynamic calculations, dynamic time–temperature profile measurements with differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA), this research reveals how variations in acetylacetone concentration and uranium content influence the structural parameters of the synthesized oxides. The time–temperature measurements show that the heating rate and maximum combustion temperatures are sensitive to acetylacetone concentration. DSC-TGA results indicate shifts in exothermic peak temperatures as the uranium content changes. The complexation between thorium and acetylacetone emerges as a critical factor, impacting combustion parameters and the structural characteristics of the final products. The uniform distribution of Th and U in the Th 1–x U x O 2 solid solution and the formation of nanoscale particles with strained crystallites are considered essential for the low-temperature densification of these materials for nuclear fuel pellet applications. Additionally, high-quality ThO 2 and Th 1–x U x O 2 thin (100–150 nm) films are successfully synthesized via electrospray deposition of combustible solutions followed by a brief period of heat treatment. Furthermore, these films exhibit excellent structural and morphological uniformity, making them ideal candidates for nuclear measurements, irradiation damage studies, and investigations into the physical properties of both pure and mixed oxides.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Virgin-like High-Density Polyethylene from Recycled Mixed Polyolefins

Reported herein is the compatibilization of mixed polyolefins containing a rheology modifier (M-PO RM ) derived from municipal solid waste (MSW) by using different types of compatibilizers. One compatibilizer was produced “in situ” during reactive extrusion (REX), and the other compatibilizers were commercial styrenic block copolymer and maleated polymer-based compatibilizers. Both “in situ” and commercial compatibilizers were first used in laboratory-controlled polyolefins containing a rheology modifier (denoted as L-PO RM ) and were investigated for their mechanical properties. The study was then extended to a rheology modifier containing recycled mixed polyolefins (M-PO RM ), where the effects of both compatibilizers were evaluated. Compared to the in situ and other commercial compatibilizers, the styrenic block copolymer offered superior performance, as it enabled the synthesis of virgin-like high-density polyethylene (HDPE) from the M-PO RM . The findings suggest that M-PO RM can be transformed into blends with virgin HDPE-like properties, thus offering an industrially relevant approach for the re- and upcycling of mixed polyolefins. Finally, the M-PO RM pellets with uniform MFI and good mechanical properties can be used as injection mold feedstocks for different applications such as in the construction and automotive sectors.

compatibilization↗

Role of Amorphous Chains in Nanoplastic Formation from Semicrystalline Polymers

Semicrystalline polymers, e.g., polyethylene terephthalate (PET), release micro- (100 nm to 1 mm) and nanoplastics (up to 100 nm) [MNPL] when they are degraded under quiescent conditions. However, the exact molecular mechanisms leading to material fragmentation into MNPL are unknown. Here, we monitor the evolution of chain molecular weight and the MNPL production kinetics during hydrolysis of PET pellets. We find that only ~0.6% of the amorphous phase ester bonds are hydrolyzed at the onset of MNPL release. Then, by combining a random scission model with measured amorphous spacings, we estimate that only ~15% of the stress transmitters in the amorphous phase, namely, bridges and entangled loops, have failed by this point. Thus, spontaneous fragmentation of the semicrystalline nanostructure occurs despite significant intercrystalline connectivity. We resolve this apparent contradiction by proposing that fragmentation can only occur when progressive tie-chain scission causes the material to undergo the ductile/brittle transition. Mechanistically, we speculate that the internal stresses responsible for material fragmentation are caused by processing (i.e., residual stresses) and/or sample densification induced by chemi-crystallization. We discuss additional factors that may affect our analysis and thus require further investigation, such as skin-core effects, preferential degradation of stress transmitters and/or recrystallization processes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Conjugated Metal–Organic Macrocycles: Synthesis, Characterization, and Electrical Conductivity

The dimensional reduction of solids into smaller fragments provides a route to achieve new physical properties and gain deeper insight into the extended parent structures. Here, we report the synthesis of CuTOTP-OR (TOTP n – = 2,3,6,7-tetraoxidotriphenylene), a family of copper-based macrocycles that resemble truncated fragments of the conductive 2D metal–organic framework Cu 3 (HHTP) 2 (HHTP = 2,3,6,7,10,11-hexahydroxytriphenylene). The planar metal–organic macrocycles self-assemble into ordered nanotubes with internal diameters of ~2 nm and short interlayer distances of ~3.20 Å. Strong π–π stacking interactions between macrocycles facilitate out-of-plane charge transport, and pressed pellet conductivities as high as 2(1)×10 -3 S cm -1 are observed. Peripheral alkyl functionalization enhances solution processability and enables the fabrication of thin-film field-effect transistor devices. Ambipolar charge transport is observed, suggesting similar behavior may be operative in Cu 3 (HHTP) 2 . By coupling the attractive features of metal–organic frameworks with greater processability, these macrocycles enable facile device integration and a more nuanced understanding of out-of-plane charge transport in 2D conductive metal–organic frameworks.

36 MATERIALS SCIENCE↗

Unconventional Charge Transport in MgCr 2 O 4 and Implications for Battery Intercalation Hosts

Ion transport in solid-state cathode materials prescribes a fundamental limit to the rates batteries can operate; therefore, an accurate understanding of ion transport is a critical missing piece to enable new battery technologies, such as magnesium batteries. Based on our conventional understanding of lithium-ion materials, MgCr 2 O 4 is a promising magnesium-ion cathode material given its high capacity, high voltage against an Mg anode, and acceptable computed diffusion barriers. Electrochemical examinations of MgCr 2 O 4 , however, reveal significant energetic limitations. Motivated by these disparate observations; herein, we examine long-range ion transport by electrically polarizing dense pellets of MgCr 2 O 4 . Our conventional understanding of ion transport in battery cathode materials, e.g., Nernst-Einstein conduction, cannot explain the measured response since it neglects frictional interactions between mobile species and their nonideal free energies. In this work, we propose an extended theory that incorporates these interactions and reduces to the Nernst-Einstein conduction under dilute conditions. This theory describes the measured response, and we report the first study of long-range ion transport behavior in MgCr 2 O 4 . We conclusively show that the Mg chemical diffusivity is comparable to lithium-ion electrode materials, whereas the total conductivity is rate-limiting. Given these differences, energy storage in MgCr 2 O 4 is limited by particle-scale voltage drops, unlike lithium-ion particles that are limited by concentration gradients. Future materials design efforts should consider the interspecies interactions described in this extended theory, particularly with respect to multivalent-ion systems and their resultant effects on continuum transport properties.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Probing Terra Incognita of Ni–P Catalysts: Operando Explorations during Hydrogen Evolution Reaction

We have developed two Ni phosphide preparation methods allowing operando XAS surface-sensitive studies of well-defined bulk systems. For Ni K-edge XAS, a Ni 2 P phase-pure powder was sintered into a high-density pellet and polished for grazing incidence XAS. Ni sites were mildly affected by the acidic electrolyte prior to the HER, while the applied cathodic potential caused the reduction of Ni surface states beyond the states of as-prepared Ni 2 P. The computed fully H-covered Ni 2 P [0001] model describes the difference in the operando Ni K-edge GIXAS spectrum well. Upon turning the applied bias off, the Ni sites became immediately oxidized, forming NiO on the surface. Thus, the active phase during the HER is covalent Ni 0 close to that in the intermetallic phosphides, and Ni 2+ oxides formed after, and not during, the HER. For P K-edge XAS, Ni foam was phosphorized to form a thin Ni 3 P layer while preserving its high surface area. Upon immersion in the acidic electrolyte, the P sites underwent removal of P 5+ phosphates and formed new P coordination, possibly due to the adsorption of protons from the electrolyte. These new P surface states were not affected by turning the cathodic current on and off as soon as the sample was immersed in the acidic electrolyte. However, the removal of the sample from the electrochemical cell and drying in air resulted in substantial depletion and oxidation of surface P. Echoing the observed Ni site chemistry during HER, XAS and XPS suggest that the in situ active P sites are different from the oxidized P states observed under ex situ conditions.

Kong, Seongyoung [Iowa State Univ., Ames, IA (Unit↗

High-Throughput Characterization and Optimization of Polyamide Hydrolase Activity Using Open Port Sampling Interface Mass Spectrometry

Enzymatic biodegradation of polymers, such as polyamides (PA), has the potential to cost-effectively reduce plastic waste, but enhancements in degradation efficiency are needed. Engineering enzymes through directed evolution is one pathway toward identification of critical domains needed for improving activity. However, screening such enzymatic libraries (100s-to-1000s of samples) is time-consuming. Here we demonstrate the use of robotic autosampler (PAL) and immediate drop on demand technology (I.DOT) liquid handling systems coupled with open-port sampling interface-mass spectrometry (OPSI-MS) to screen for PA6 and PA66 hydrolysis by 6-aminohexanoate-oligomer endo-hydrolase (nylon hydrolase, NylC) in a high-throughput (8–20 s/sample) manner. The OPSI-MS technique required minimal sample preparation and was amenable to 96-well plate formats for automated processing. Enzymatic hydrolysis of PA characteristically produced soluble linear oligomer products that could be identified by OPSI-MS. Incubation temperatures and times were optimized for PA6 (65 °C, 24 h) and PA66 (75 °C, 24 h) over 108 experiments. In addition, the I.DOT/OPSI-MS quantified production of PA6 linear dimer (8.3 ± 1.6 μg/mL) and PA66 linear monomer (13.5 ± 1.5 μg/mL) by NylC with a lower limit of detection of 0.029 and 0.032 μg/mL, respectively. For PA6 and PA66, linear oligomer production corresponded to 0.096 ± 0.018% and 0.204 ± 0.028% conversion of dry pellet mass, respectively. The developed methodology is expected to be utilized to assess enzymatic hydrolysis of engineered enzyme libraries, comprising hundreds to thousands of individual samples.

47 OTHER INSTRUMENTATION↗