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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Continuous-flow synthesis of thermochromic M-phase VO2 particles via rapid one-step hydrothermal reaction – effect of mixers

VO2 particles are promising materials for thermochromic smart windows that reduce building energy loss. Continuous-flow hydrothermal processes showcase advantages for synthesizing VO2 particles compared with traditional batch reaction systems. Mixers play a crucial role in particle fabrication in continuous-flow systems. In this study, a Center T-Mixer and a Collision Cross-Mixer are developed and implemented in a hot water fluidized suspension reaction (HWFSR) system. The influence of the resident time on the particle phase and size was evaluated, and properties of particles derived from systems equipped with differing mixers were compared. The resulting particles were characterized using techniques of X-ray powder diffraction (XRD) analysis, scanning electron microscopy (SEM), and differential scanning calorimetry (DSC). When compared with the Center T-Mixer, results indicate that the Collision Cross-Mixer has better control regarding the morphology and size distribution of resulting particles while improving the transition temperatures of the as-synthesized materials. HWFSR systems containing novel mixer designs are capable of producing pure M-phase VO2 particles in a single step contrary to the current reactor design that use a second postheat treatment step, and they are capable of synthesizing many other nanoparticle species, especially those requiring high temperature and pressure reaction conditions.

continuous-flow process↗
DOE OSTI2013

Alternate paddle configuration for improved wear resistance in the saltstone mixer

The Saltstone Production Facility has a 10-inch Readco-Kurimoto continuous mixer that mixes the premix dry feeds and low-level waste salt solution to make fresh (uncured) saltstone. Inspection of the mixer in January 2013 showed significant wear on the third, fourth and fifth paddle pairs after the conveying augers. A 2-inch Readco-Kurimoto continuous mixer was used to test alternate paddle configurations for use in the 10-inch mixer to decrease the wear rate on the paddles. Two wear tests were conducted to investigate a method of reducing wear on the mixer paddles. The first test (wear test 2a) had a paddle configuration similar to the currently installed 10-inch mixer in the SPF. This test established baseline wear. The second test (wear test 2b) had a reconfigured paddle arrangement that replaced the flat paddles with helical paddles for paddle pairs 2 - 6 and aligned paddle pair 1 with the augers. The intent of the reconfiguration was to more effectively convey the partially wetted dry feeds through the transition region and into the liquid feed where paddle wear is reduced due to dry feeds and salt solution being mixed at the intended water to premix ratio. The design of the helical paddles provides conveyance through the transition region to the liquid feed inlet. The alignment with the auger is aimed to provide a smoother transition (minimizing the discontinuity between the auger and paddle pair 1) into the downstream paddles. A soft metal with low wear resistance (6000 series aluminum) was used for the wear testing paddles to determine wear patterns while minimizing run time and maximizing wear rate. For the two paddle configurations tested using the scaled 2-inch Readco-Kurimoto continuous mixer, with the first six paddles after the augers replaced by the wear paddles and the remaining paddles were stainless steel. Since the 10-inch SPF mixer is designed with the liquid inlet centered over paddle pairs 5 and 6, the scaled 2-inch mixer was configured the same way. The wear rate from wear test 2a was approximately double the wear rate from wear test 2b for paddle pairs 4 and 5. For both configurations, there was little or no wear on paddle pairs 1, 2, 3 and 6 based on mass change, indicating that the un-wetted and fully wetted premix materials cause less wear than the partially wetted premix. Additionally, inspection of the wear surface of the paddles showed more deformation on the flat paddles than the helical paddles which was consistent with the wear rates. Aligning of the auger discharge flight with paddle pair 1 resulted in a lower wear rate paddle pair 1 rather than having them misaligned with the feed augers. During the paddle wear tests, polishing wear was observed on the inside barrel of the mixer. The polishing wear is evident on the upper housing clamshell and the lower housing clamshell primarily at paddle pairs 4 and 5, which is the transition region of the mixer. Wear on the mixer barrel increases the space between the paddles and the barrel, resulting in increased grout build up on the barrel. Since the mixer barrel cannot be reconfigured or replaced in the SPF, the method for mitigating wear on the barrel is to move the more viscous grout through the transition region as quickly as possible. In addition, the location of the liquid inlet does not allow for sufficient cleaning of the mixer since residual grout remains on paddle pairs 1 - 4. As the paddles continue to wear and the self-cleaning capability of the paddles is lost, the lack of sufficient flushing would aid in grout build up between the barrel and the paddles which could eventually lead to decreased throughput capacity of the dry feeds. Changing the paddle configuration from flat to helical resulted in no change to the rheological properties of the grout mixture. Both tests produced a grout that is within the processing range of the SPF. Based on the results of this testing, it is recommended for the currently installed SPF mixer that paddle pairs 1 through 6 be helical rather than flat, with the paddle pair 1 aligned with the feed augers in order to minimize the wear occurring in the SPF mixer. Based on the results of this testing, it is recommended that the mixer be inspected and critical measurements be taken whenever the SPF processing schedule allows in order to establish a wear rate of the 10-inch mixer paddles.5 Based on these measurements, the lifetime of paddles in the transition region can be established in order to set up a maintenance schedule for the mixer. Since replacing the entire mixer is very expensive and time intensive, replacing the worn paddles after a specific time period would allow for planned shutdowns as well as process optimization such that the mixer throughput is not compromised. In addition, further testing should be performed to determine an alternate liquid inlet location to better flush the mixer of residual grout at the end of processing. Sufficiently cleaning the mixer will help eliminate another potential source of wear. Another potential method for reducing the wear rate in the mixer is to reduce the mixer speed without affecting the throughput capacity. Since wear rate is a function of impact velocity of the grout and mixing paddles, testing could be done using the 2-inch mixer determine the optimum mixer speed to reduce wear but not adversely impact facility operations (e.g. throughput capacity and grout properties).

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2012

Flashback resistant pre-mixer assembly

A pre-mixer assembly associated with a fuel supply system for mixing of air and fuel upstream from a main combustion zone in a gas turbine engine. The pre-mixer assembly includes a swirler assembly disposed about a fuel injector of the fuel supply system and a pre-mixer transition member. The swirler assembly includes a forward end defining an air inlet and an opposed aft end. The pre-mixer transition member has a forward end affixed to the aft end of the swirler assembly and an opposed aft end defining an outlet of the pre-mixer assembly. The aft end of the pre-mixer transition member is spaced from a base plate such that a gap is formed between the aft end of the pre-mixer transition member and the base plate for permitting a flow of purge air therethrough to increase a velocity of the air/fuel mixture exiting the pre-mixer assembly.

33 ADVANCED PROPULSION SYSTEMS↗
DOE OSTI2012

EVALUATION AND RECOMMENDATION OF SALTSTONE MIXER AUGER/PADDLES MATERIALS OF CONSTRUCTION FOR IMPROVED WEAR RESISTANCE

Wear and corrosion testing were conducted to evaluate alternate materials of construction for the Saltstone mixer auger and paddles. These components have been degraded by wear from the slurry processed in the mixer. Material test options included PVD coatings (TiN, TiCN, and ZrN), weld overlays (Stellite 12 and Ultimet) and higher hardness steels and carbides (D2 and tungsten carbide). The corrosion testing demonstrated that the slurry is not detrimental to the current materials of construction or the new candidates. The ASTM G75 Miller wear test showed that the high hardness materials and the Stellite 12 weld overlay provide superior wear relative to the Astralloy and CF8M stainless steel, which are the current materials of construction, as well as the PVD coatings and Ultimet. The following recommendations are made for selecting new material options and improving the overall wear resistance of the Saltstone mixer components: • A Stellite 12 weld overlay or higher hardness steel (with toughness equivalent to Astralloy) be used to improve the wear resistance of the Saltstone mixer paddles; other manufacturing specifications for the mixer need to be considered in this selection. • The current use of the Stellite 12 weld overlay be evaluated so that coverage of the 316 auger can be optimized for improved wear resistance of the auger. • The wear surfaces of the Saltstone mixer auger and paddles be evaluated so that laboratory data can be better correlated to actual service. • The 2-inch Saltstone mixer prototype be used to verify material performance.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Extending the lifetime of mixer paddles used in the production of a low-level radioactive cementitious waste form - 15624

The salt-stone Production Facility (SPF) at the Savannah River Site (SRS) immobilizes low-level radioactive salt solution as a cementitious waste form known as salt-stone. The mixer used in the SPF is a '10-inch' Readco-Kurimoto continuous mixer with paddles fabricated from a high toughness steel. salt-stone is processed daily at a rate of 9.46 E-03 m{sup 3}/s (150 gallons per minute) in a caustic and radioactive environment. The paddles have degraded much quicker than expected which limits production rates and increases outage times. Due to the high cost of the mixer and the limited maintenance due to the radioactive environment, a combination of material properties and paddle configuration must be employed to extend the lifetime of the paddles. This paper will discuss two wear tests conducted by the Savannah River National Laboratory (SRNL) to determine the optimum paddle configuration to reduce wear on the mixer paddles. The first wear test used the mixer design operated up to December 2011 as the baseline and the second test used the mixer design installed after December 2011 as its baseline. As a result of these tests, the SPF will be implementing a new paddle configuration in the mixer currently installed in the SPF process room. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2015

Applying Hanford Tank Mixing Data to Define Pulse Jet Mixer Operation

Pulse jet mixed (PJM) process vessels are being developed for storing, blending, and chemical processing of nuclear waste slurries at the Waste Treatment and Immobilization Plant (WTP) to be built at Hanford, Washington. These waste slurries exhibit variable process feed characteristics including Newtonian to non-Newtonian rheologies over a range of solids loadings. Waste feed to the WTP from the Hanford Tank Farms will be accomplished via the Waste Feed Delivery (WFD) system which includes million-gallon underground storage double-shell tanks (DSTs) with dual-opposed jet mixer pumps. Experience using WFD type jet mixer pumps to mobilize actual Hanford waste in DSTs may be used to establish design threshold criteria of interest to pulse jet mixed process vessel operation. This paper describes a method to evaluate the pulse jet mixed vessel capability to process waste based on information obtained during mobilizing and suspending waste by the WFD system jet mixer pumps in a DST. Calculations of jet velocity and wall shear stress in a specific pulse jet mixed process vessel were performed using a commercial computational fluid dynamics (CFD) code. The CFD-modelled process vessel consists of a 4.9-m- (16-ft-) diameter tank with a 2:1 semi-elliptical head, a single, 10-cm (4-in.) downward facing 60-degree conical nozzle, and a 0.61-m (24-in.) inside diameter PJM. The PJM is located at 70% of the vessel radius with the nozzle stand-off-distance 14 cm (6 in.) above the vessel head. The CFD modeled fluid velocity and wall shear stress can be used to estimate vessel waste-processing performance by comparison to available actual WFD system process data. Test data from the operation of jet mixer pumps in the 23-m (75-ft) diameter DSTs have demonstrated mobilization, solid particles in a sediment matrix were moved from their initial location, and suspension, mobilized solid particles were moved to a higher elevation in the vessel than their initial location, of waste solids. Jet mixer pumps were used in Hanford waste tank 241-AZ-101, and at least 95% of the 0.46-m (18-in.) deep sediment, with a shear strength of 1,500 to 4,200 Pa, was mobilized. Solids with a median particle size of 43 μm, 90th percentile of 94μm, were suspended in tank 241-AZ-101 to at least 5.5 m (216 in.) above the vessel bottom. Analytical calculations for this jet mixer pump test were used to estimate the velocities and wall shear stress that mobilized and suspended the waste. These velocities and wall shear stresses provide design threshold criteria which are metrics for system performance that can be evaluated via testing. If the fluid motion in a specific pulse jet mixed process vessel meets or exceeds the fluid motion of the demonstrated performance in the WFD system, confidence is provided that that vessel will similarly mobilize and suspend those solids if they were within the WTP. The single PJM CFD-calculated jet velocity and wall shear stress compare favorably with the design threshold criterion estimated for the tank 241-AZ-101 process data. Therefore, for both mobilization and suspension, the performance data evaluated from the WFD system testing increases confidence that the performance of the pulse jet mixed process vessels will be sufficient to process that waste even if that waste is not fully characterized.

mixing' slurry↗
DOE OSTI2016

A Chemistry Based Criticality Safety Evaluation of the HM-Process Mixer Settlers

The criticality safety of Savannah River Site's H Canyon two cycle uranium extraction and purification process, called the HM process, is examined. Explicit Monte Carlo models of the multi-stage mixer-settlers are generated for the first time using the KENO-VI module of the SCALE 6.1 code package and spanning normal operating conditions and a wide range of potential upset conditions with stagewise compositions based directly on SEPHIS Mod-4 chemistry models of the same conditions. To achieve industrial scale processing, mixer-settlers are often not geometrically favorable to prevent criticality so other means must be used for criticality safety, namely control of fissile concentration and mass. Historically, the worst case upset is a reflux condition resulting from a stream flow rate, temperature, or composition that is off from the normal operating conditions. A reflux is considered to be the state in which the fissile material is not proceeding in the desired direction, i.e. is stripping rather than extracting or vice versa. The criticality safety analyses which set the current operational limits were conducted many years ago with less sophisticated codes and only loosely tied criticality to chemistry. Those analyses conservatively assumed that a reflux changed the behavior of the mixer-settler such that the fissile content collected continuously in only three stages of the mixer-settler, at a rate based on the SEPHIS modeling, until criticality occurred. This implies that under some condition the distribution coefficient of the fissile material either goes to infinity or zero, which is not physically achievable. In such a scenario, the operator would have some amount of time to react and correct the problem before sufficient fissile material built up in the mixer-settler and caused a criticality. In reality, an upset in a stream would cause the process to transition to a new, though undesired, equilibrium state of operation. The distribution coefficients would change, but would not diverge. In this work, aqueous and organic streams are modeled for both the mixer and the settler region of each stage of each bank using chemical distribution data from SEPHIS and solving the chemical equations for a wide range of operational parameters spanning normal and upset conditions. Conservative assumptions are made regarding enrichment and reflection and the whole bank multiplication factor is evaluated using discrete stage-wise compositions. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2016

Experimental Evaluation of Dual-Opposed Jet Mixer Pump Performance for Slurry Mixing

Million-gallon double-shell tanks at Hanford are used to store transuranic, high-level, and low-level radioactive wastes. These wastes consist of a large volume of salt-laden solution covering a smaller volume of settled sludge primarily containing metal hydroxides. These wastes will be retrieved and processed into immobile waste forms suitable for permanent disposal. Retrieval is an important step in implementing these disposal scenarios. The retrieval concept evaluated is to use submerged dual-nozzle jet mixer pumps with horizontally oriented nozzles located near the tank floor that produce horizontal jets of fluid to mobilize the settled solids. The mixer pumps are oscillated through 180 about a vertical axis so the high velocity fluid jets sweep across the floor of the tank. After the solids are mobilized, the pumps will continue to operate at a reduced flow rate producing lower velocity jets sufficient to maintain the particles in a uniform suspension (concentration uniformity). Several types of waste and tank configurations exist at Hanford. The jet mixer pump systems and operating conditions required to mobilize sludge and maintain slurry uniformity will be a function of the waste type and tank configuration. The focus of this work was to conduct a 1/12-scale experiment to develop an analytical model to relate slurry uniformity to tank and mixer pump configurations, operating conditions, and sludge properties. This experimental study evaluated concentration uniformity in a 1/12-scale experiment varying the Reynolds number (Re), Froude number (Fr), and gravitational settling parameter (Gs) space. Simulant physical properties were chosen to obtain the required Re and Gs where Re and Gs were varied by adjusting the kinematic viscosity and mean particle diameter, respectively. Test conditions were achieved by scaling the jet nozzle exit velocity in a 75-in. diameter tank using a mock-up of a centrally located dual-opposed jet mixer pump located just above the tank floor. Concentration measurements at sampling locations throughout the tank were used to assess the degree of uniformity achieved during each test. Concentration data was obtained using a real time in-situ ultrasonic attenuation probe and post-test analysis of discrete batch samples. The undissolved solids concentration at these locations was analyzed to determine whether the tank contents were uniform (≤ ±10% variation about mean) or nonuniform (> ±10% variation about mean) in concentration. Concentration inhomogeneity was modeled as a function of dimensionless parameters. The parameters that best describe the maximum solids volume fraction that can be suspended were found to be 1) the Fr based on nozzle average discharge velocity and tank contents level and 2) the dimensionless particle size based on nozzle diameter. The dependence on the jet Re does not appear to be statistically significant.

correlation↗
DOE OSTI2018

An all-dielectric metasurface as a broadband optical frequency mixer

A frequency mixer is a nonlinear device that combines electromagnetic waves to create waves at new frequencies. Mixers are ubiquitous components in modern radio-frequency technology and microwave signal processing. The development of versatile frequency mixers for optical frequencies remains challenging: such devices generally rely on weak nonlinear optical processes and, thus, must satisfy phase-matching conditions. Here we utilize a GaAs-based dielectric metasurface to demonstrate an optical frequency mixer that concurrently generates eleven new frequencies spanning the ultraviolet to near-infrared. The even and odd order nonlinearities of GaAs enable our observation of second-harmonic, third-harmonic, and fourth-harmonic generation, sum-frequency generation, two-photon absorption-induced photoluminescence, four-wave mixing and six-wave mixing. The simultaneous occurrence of these seven nonlinear processes is assisted by the combined effects of strong intrinsic material nonlinearities, enhanced electromagnetic fields, and relaxed phase-matching requirements. In conclusion, such ultracompact optical mixers may enable a plethora of applications in biology, chemistry, sensing, communications, and quantum optics.

47 OTHER INSTRUMENTATION↗
DOE OSTI2014

Evaluation of static mixer flow enhancements for cryogenic viscous compressor prototype for ITER vacuum system

As part of the U.S. ITER contribution to the vacuum systems for the ITER fusion project, a cryogenic viscous compressor (CVC) is being designed and fabricated to cryopump hydrogenic gases in the torus and neutral beam exhaust streams and to regenerate the collected gases to controlled pressures such that they can be mechanically pumped with controlled flows to the tritium reprocessing facility. One critical element of the CVC design that required additional investigation was the determination of flow rates of the low pressure (up to 1000 Pa) exhaust stream that would allow for complete pumping of hydrogenic gases while permitting trace levels of helium to pass through the CVC to be pumped by conventional vacuum pumps. A sub-scale prototype test facility was utilized to determine the effectiveness of a static mixer pump tube concept, which consisted of a series of rotated twisted elements brazed into a 2-mm thick, 5-cm diameter stainless steel tube. Cold helium gas flow provided by a dewar and helium transfer line was used to cool the exterior of the static mixer pump tube. Deuterium gas was mixed with helium gas through flow controllers at different concentrations while the composition of the exhaust gas was monitored with a Penning gauge and optical spectrometer to determine the effectiveness of the static mixer. It was found that with tube wall temperatures between 6 K and 9 K, the deuterium gas was completely cryopumped and only helium passed through the tube. These results have been used to design the cooling geometry and the static mixer pump tubes in the full-scale CVC prototype.

42 ENGINEERING↗
DOE OSTI2014

Evaluation of Static Mixer Flow Enhancements for Cryogenic Viscous Compressor Prototype for ITER Vacuum System

As part of the U.S. ITER contribution to the vacuum systems for the ITER fusion project, a cryogenic viscous compressor (CVC) is being designed and fabricated to cryopump hydrogenic gases in the torus and neutral beam exhaust streams and to regenerate the collected gases to controlled pressures such that they can be mechanically pumped with controlled flows to the tritium reprocessing facility. One critical element of the CVC design that required additional investigation was the determination of flow rates of the low pressure (50 to 1000 Pa) exhaust stream that would allow for complete pumping of hydrogenic gases while permitting trace levels of helium to pass through the CVC to be pumped by conventional vacuum pumps. A sub-scale prototype test facility was utilized to determine the effectiveness of a static mixer pump tube concept, which consisted of a series of rotated twisted elements brazed into a 2-mm thick, 5-cm diameter stainless steel tube. Cold helium gas flow provided by a dewar and helium transfer line was used to cool the exterior of the static mixer pump tube. Deuterium gas was mixed with helium gas through flow controllers at different concentrations while the composition of the exhaust gas was monitored with a Penning gauge and optical spectrometer to determine the effectiveness of the static mixer. It was found that with tube wall temperatures between 6 K and 9 K, the deuterium gas was completely cryopumped and only helium passed through the tube. These results have been used to design the cooling geometry and the static mixer pump tubes in the full-scale CVC prototype

Duckworth, Robert C↗
DOE OSTI2023

Comparison of nanocomposite dispersion and distribution for several melt mixers

Breakup (dispersion) and distribution of nanoparticles are the chief hurdles towards taking advantage of nanoparticles in polymer nanocomposites for reinforcement, flame retardancy, conductivity, chromaticity, and other properties. Microscopy is often used to quantify mixing, but it has a limited field of view, does not average over bulk samples, and fails to address nano-particle hierarchical structures. Ultra-small-angle X-ray scattering (USAXS) can provide a macroscopic statistical average of nanoscale dispersion (breakup) and emergent hierarchical structure, as well as the distribution on the nanoscale. Here, this work compares several common mixer geometries for carbon black-polystyrene nanocomposites. Two twin-screw extruder geometries, typical for industrial processing of melt blends, are compared with a laboratory-scale single screw extruder and a Banbury mixer. It is found that for a given mixer, nanoscale distribution increases following a van der Waals function using accumulated strain as an analogue for temperature while macroscopic distribution/dispersion, using microscopy, does not follow this dependency. Breakup and aggregation in dispersive mixing follow expected behavior on the nanoscale. Across these drastically different mixing geometries an unexpected dependency is observed for nanoscale distributive mixing (both nano and macroscopic) as a function of accumulated strain that may reflect a transition from distributive turbulent to dispersive laminar mixing as the mixing gap is reduced.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Fluid flow structure around the mixer in a reactor with mechanical mixing

Fluid flow structure around the mixer in a cylindrical reactor with mechanical mixing is studied and numerical results are presented in this article. The model area is complex because of the presence of convex corners of the mixer in the fluid flow. Proper boundary conditions for the vorticity calculated on the base of the stream function values near solid boundaries of the examined area are presented. The boundary value problem of motion of swirling incompressible viscous fluid in a vertical tank reactor with a mixer is solved numerically. The calculations are made by a computer code, written in MATLAB. The complex structure of the flow around the mixing disk is described and commented.

42 ENGINEERING↗
DOE OSTI2012

Evaluation Of Saltstone Mixer Paddle Configuration For Improved Wear Resistance

A soft metal with low wear resistance (6000 series aluminum), was used to minimize run time while maximizing wear rate. Two paddle configurations were tested, with the first four paddles after the augers replaced by the wear paddles. The first configuration was all flat paddles, with the first paddle not aligned with the augers and is consistent with present SPF mixer. The second configuration had helical paddles for the first three stages after the augers and a flat paddle at the fourth stage. The first helical paddle was aligned with the auger flight for the second configuration. The all flat paddle configuration wear rate was approximately double the wear rate of the helical paddles for the first two sets of paddles after the augers. For both configurations, there was little or no wear on the third and fourth paddle sets based on mass change, indicating that the fully wetted premix materials are much less abrasive than the un-wetted or partially wetted premix. Additionally, inspection of the wear surface of the paddles at higher magnification showed the flat paddles were worn much more than the helical and is consistent with the wear rates. Aligning the auger discharge flight with the first set of helical paddles was effective in reducing the wear rate as compared to the flat paddle configuration. Changing the paddle configuration from flat to helical resulted in a slight increase in rheological properties. Although, both tests produced grout-like material that is within the processing rage of the SPF, it should be noted that cement is not included in the premix and water was used rather than salt solution, which does affect the rheology of the fresh grout. The higher rheological properties from the helical wear test are most likely due to the reduced number of shearing paddles in the mixer. In addition, there is variation in the rheological data for each wear test. This is most likely due to the way that the dry feeds enter the mixer from the dry feeder. The premix is discharged from the hopper in an unsteady fashion, where irregular sized clumps were observed leaving the discharge of the auger, though the auger speed is constant.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2016

Effects of molecular confinement and crowding on horseradish peroxidase kinetics using a nanofluidic gradient mixer

Here, we studied the effects of molecular confinement and crowding on enzyme kinetics at length scales and under conditions similar to those found in biological cells. These experiments were carried out using a nanofluidic network of channels constituting a nanofluidic gradient mixer, providing the basis for measuring multiple experimental conditions simultaneously. Furthermore, the 100 nm × 40 μm nanochannels were wet etched directly into borosilicate glass, then annealed and characterized with fluorescein emission prior to kinetic measurements. The nanofluidic gradient mixer was then used to measure the kinetics of the conversion of the horseradish peroxidase (HRP)-catalyzed conversion of non-fluorescent Amplex Red (AR) to the fluorescent product resorufin in the presence of hydrogen peroxide (H 2 O 2 ). The design of the gradient mixer allows reaction kinetics to be studied under multiple (five) unique solution compositions in a single experiment. In order to characterize the efficiency of the device the effects of confinement on HRP-catalyzed AR conversion kinetics were studied by varying the starting ratio of AR : H 2 O 2 . Equimolar concentrations of Amplex Red and H 2 O 2 yielded the highest reaction rates followed by 2 : 1, 1 : 2, 5 : 1, and finally 1 : 5 [AR] : [H 2 O 2 ]. Under all conditions, initial reaction velocities were decreased by excess H 2 O 2 . Crowding effects on kinetics were studied by increasing solution viscosity in the nanochannels in the range 1.0–1.6 cP with sucrose. Increasing the solution viscosities in these confined geometries decreases the initial reaction velocity at the highest concentration from 3.79 μM min -1 at 1.00 cP to 0.192 μM min -1 at 1.59 cP. Variations in reaction velocity are interpreted in the context of models for HRP catalysis and for molecular crowding.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Infrared compatible rapid mixer to probe millisecond chemical kinetics

Fast microfluidic mixers are a valuable tool for studying solution-phase chemical reaction kinetics and molecular processes with spectroscopy. However, microfluidic mixers that are compatible with infrared vibrational spectroscopy have seen only limited development due to the poor infrared transparency of the current microfabrication material. We describe the design, fabrication, and characterization of CaF2-based continuous flow turbulent mixers, which are capable of measuring kinetics in the millisecond time window with infrared spectroscopy, when integrated into an infrared microscope. Kinetics measurements demonstrate the ability to resolve relaxation processes with 1 millisecond time resolution, and straightforward improvements are described that should result in sub-100 µs time-resolution.

Instruments & Instrumentation↗
DOE OSTI2021

Millisecond timescale reactions observed via X-ray spectroscopy in a 3D microfabricated fused silica mixer

Determination of electronic structures during chemical reactions remains challenging in studies which involve reactions in the millisecond timescale, toxic chemicals, and/or anaerobic conditions. Here, a three-dimensionally (3D) microfabricated microfluidic mixer platform that is compatible with time-resolved X-ray absorption and emission spectroscopy (XAS and XES, respectively) is presented. This platform, to initiate reactions and study their progression, mixes a high flow rate (0.50–1.5 ml min –1 ) sheath stream with a low-flow-rate (5–90 µl min –1 ) sample stream within a monolithic fused silica chip. The chip geometry enables hydro­dynamic focusing of the sample stream in 3D and sample widths as small as 5 µm. The chip is also connected to a polyimide capillary downstream to enable sample stream deceleration, expansion, and X-ray detection. In this capillary, sample widths of 50 µm are demonstrated. Further, convection–diffusion-reaction models of the mixer are presented. The models are experimentally validated using confocal epifluorescence microscopy and XAS/XES measurements of a ferricyanide and ascorbic acid reaction. The models additionally enable prediction of the residence time and residence time uncertainty of reactive species as well as mixing times. Residence times (from initiation of mixing to the point of X-ray detection) during sample stream expansion as small as 2.1 ± 0.3 ms are also demonstrated. Importantly, an exploration of the mixer operational space reveals a theoretical minimum mixing time of 0.91 ms. The proposed platform is applicable to the determination of the electronic structure of conventionally inaccessible reaction intermediates.

3D microfabrication↗