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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Thin Film Electrodes for Anodic Stripping Voltammetry: A Mini-Review

Anodic stripping voltammetry (ASV) is a powerful electrochemical analytical technique that allows for the detection and quantification of a variety of metal ion species at very low concentrations in aqueous media. While early, traditional ASV measurements relied on macroscopic electrodes like Hg drop electrodes to provide surfaces suitable for plating/stripping, more recent work on the technique has replaced these electrodes with thin film metal electrodes generated in situ . Such electrodes are plated alongside the analyte species onto the surface of a primary electrode, producing a composite metal electrode from which the analyte(s) can then be stripped, identified, and quantified. In this minireview, we will explore the development and use of these unique electrodes in a variety of different applications. A number of metals (e.g., Hg, Bi, Sn, etc.) have shown promise as thin film ASV electrodes in both acidic and alkaline media, and frequently multiple metals in addition to the analyte of interest are deposited together to optimize the plating/stripping behavior, improving sensitivity. Due to the relatively simple nature of the measurement and its suitability for a wide range of pH, it has been used broadly: To measure toxic metals in the environment, characterize battery materials, and enable biological assays, among other applications. We will discuss these applications in greater detail, as well as provide perspective on future development and uses of these thin film electrodes in ASV measurements.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Bismuth Detection in Alkaline Electrolyte via Anodic Stripping Voltammetry for Battery Separator Evaluation

Abstract Anodic stripping voltammetry (ASV) has been widely used for the detection of several heavy metal ions in neutral and acidic solution, in many cases employing electrodes and/or solutions incorporating Bi. In this work we demonstrate that Bi(OH) 4 − ion concentration can be measured in highly alkaline 8.5 M KOH solution using ASV. The addition of Pb in similar concentrations to the Bi(OH) 4 − being measured is shown to improve both the sensitivity and precision of the method. When the Pb additive is employed, a formal limit of detection of 8.5 ppb is achieved, compared to 17.3 ppb when the Pb additive is not used. Due to the use of Bi additives in alkaline battery chemistries, it follows that separators which limit Bi(OH) 4 − diffusion into the bulk electrolyte and away from the electrodes are of interest. For this purpose, we utilize ASV to determine Bi(OH) 4 − diffusion rates through Celgard 3501, cellophane 350P00, and Nafion 211. Bi(OH) 4 − crossover rates, as determined by ASV, are shown to be repeatable and consistent with expectations from the known separator structure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Multiplexed Anodic Stripping Voltammetry Detection of Heavy Metals in Water Using Nanocomposites Modified Screen-Printed Electrodes Integrated With a 3D-Printed Flow Cell

In this study, we present multiplexed anodic stripping voltammetry (ASV) detection of heavy metal ions (HMIs)—As(III), Cd(II), and Pb(II)—using a homemade electrochemical cell consisting of dual working, reference and counter screen-printed electrodes (SPE) on polyimide substrate integrated with a 3D-printed flow cell. Working and counter electrodes were fabricated by the screen-printing of graphite paste while the Ag/AgCl paste was screen-printed as a reference electrode (Ag/AgCl quasi-reference electrode). The working electrodes were modified with (BiO) 2 CO 3 -reduced graphene oxide (rGO)-Nafion [(BiO) 2 CO 3 -rGO-Nafion] and Fe 3 O 4 magnetic nanoparticles (Fe 3 O 4 MNPs) decorated Au nanoparticles (AuNPs)-ionic liquid (IL) (Fe 3 O 4 -Au-IL) nanocomposites separately to enhance HMIs sensing. Electrochemical detection was achieved using square wave ASV technique. The desired structure of the flow electrochemical cell was optimized by the computational fluid dynamic (CFD). Different experimental parameters for stripping analysis of HMIs were optimized including deposition time, deposition potential and flow rate. The linear range of calibration curves with the sensing nanocomposites modified SPE for the three metal ions was from 0–50 μg/L. The limits of detection (S/N = 3) were estimated to be 2.4 μg/L for As(III), 1.2 μg/L for Pb(II) and 0.8 μg/L for Cd(II). Furthermore, the homemade flow anodic stripping sensor platform was used to detect HMIs in simulated river water with a 95–101% recovery, indicating high selectivity and accuracy and great potential for applicability even in complex matrices.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1989

Development and testing of a prototype mosaic wedge-and-strip anode detector

A preliminary laboratory study of a prototype mosaic wedge-and-strip anode, a new class of readout system that will furnish large format, high resolution microchannel plate detectors with comparatively simple readout electronics is described. The goals of this study were to demonstrate the linearity of the mosaic anode algorithm, and to verify the predicted resolution performance in a realistic detector configuration. It is found that the nonlinearity introduced at the boundary between two anodes is limited to 50-100 microns. It is also shown that the spatial resolution of the detector is limited mainly by partition noise to about 35 microns (FWHM) at a gain of 2 x 10 to the 7th. A systematic investigation of the charge distribution arriving at the anode is also described. Using the relative charges arriving on the two anodes of the mosaic pattern, the detailed shape of the distribution and its dependence on MCP-anode voltage, MCP voltage, and pulse height are determined. A significant dependence of the profile on pulse height, which can introduce a pulse height dependence to the centroid calculation, particularly near the anode edges is found. Improved anode designs which will achieve the optimal performance are discussed.

Rasmussen, A.↗
DOE OSTI2024

Performance of a triple-GEM detector with capacitive-sharing 3-coordinate (X–Y–U)-strip anode readout

The concept of capacitive-sharing readout, described in detail in a previous study, offers the possibility for the development of high-performance three-coordinates (X--Y--U)-strip readout for Micro Pattern Gaseous Detectors (MPGDs) using simple standard PCB fabrication techniques. Capacitive-sharing (X--Y--U)-strip readout allows simultaneous measurement of the Cartesian coordinates x and y of the position of the particles together with a third coordinate u along the diagonal axis in a single readout PCB. This provides a powerful tool to address multiple-hit ambiguity and enable pattern recognition capabilities in moderate particle flux environment of collider or fixed target experiments in high energy physics HEP) and nuclear physics (NP). We present in this paper the performance of a 10 cm × 10 cm triple-GEM detector with capacitive-sharing (X--Y--U)-strip anode readout. Spatial resolutions of the order of $\sigma_{x}^{res}$ = 71.6 $\pm$ 0.8 $\mu$m for X-strips, $\sigma_{y}^{res}$ = 56.2 $\pm$ 0.9 $\mu$m for Y-strips and $\sigma_{u}^{res}$ = 75.2 $\pm$ 0.9 $\mu$m for U-strips have been obtained at a beam test at Thomas Jefferson National Accelerator Facility (Jefferson Lab). Modifications of the readout design of future prototypes to improve the spatial resolution and challenges in scaling to large-area MPGDs are discussed.

(X-Y-U) strip↗
NASA NTRS1981

Wedge-and-strip anodes for centroid-finding position-sensitive photon and particle detectors

The paper examines geometries employing position-dependent charge partitioning to obtain a two-dimensional position signal from each detected photon or particle. Requiring three or four anode electrodes and signal paths, images have little distortion and resolution is not limited by thermal noise. An analysis of the geometrical image nonlinearity between event centroid location and the charge partition ratios is presented. In addition, fabrication and testing of two wedge-and-strip anode systems are discussed. Images obtained with EUV radiation and microchannel plates verify the predicted performance, with further resolution improvements achieved by adopting low noise signal circuitry. Also discussed are the designs of practical X-ray, EUV, and charged particle image systems.

Martin, C.↗
NASA NTRS1969

A method for precision anodize stripping

Felt templates saturated with etch solution remove anodized finish from aluminum without damage to the surface. The solution is a combination of nitric acid, chromic acid, and hydrofluoric acid.

Peters, R. L.↗
NASA NTRS1993

Chemical Strips Anodic Film From Aluminum

Phosphoric acid solution offers advantages over other stripping solutions. More effective than other strippers and safer to use. Relatively environmentally benign, phosphoric acid stripper ceases its chemical attack so less process control is needed in its use.

Eichinger, Eric C.↗
DOE OSTI2021

Applying Anodic Stripping Voltammetry to Complex Wastewater Streams for Rapid Metal Detection (Final Report)

The overall objective of this project is the development of a lab-on-a-chip (LOC) electrochemical sensor capable of accurately measuring heavy metal (lead (Pb), cadmium (Cd), and arsenic (As)) concentrations in complex aqueous streams such as wastewater. The specific goals include: i) identify how heavy metal speciate and transform during the different stages of the wastewater treatment train, and explore pre-treatment methods that will de-complex heavy metals, making them available to ASV, ii) develop appropriate electrodes for ASV using organic/inorganic nanomaterials, and iii) integrate pre-treatment steps and specialized electrodes into an LOC sensor device capable of autonomously determining heavy metal concentrations in complex wastewater streams.

99 GENERAL AND MISCELLANEOUS↗
NASA NTRS2001

Three axis pulsed plasma thruster with angled cathode and anode strip lines

A spacecraft attitude and altitude control system utilizes sets of three pulsed plasma thrusters connected to a single controller. The single controller controls the operation of each thruster in the set. The control of a set of three thrusters in the set makes it possible to provide a component of thrust along any one of three desired axes. This configuration reduces the total weight of a spacecraft since only one controller and its associated electronics is required for each set of thrusters rather than a controller for each thruster. The thrusters are positioned about the spacecraft such that the effect of the thrusters is balanced.

Cassady, R. Joseph↗
NASA NTRS1989

Imaging characteristics of the Extreme Ultraviolet Explorer microchannel plate detectors

The Extreme Ultraviolet Explorer (EUVE) satellite will conduct an all-sky survey over the wavelength range from 70 A to 760 A using four grazing-incidence telescopes and seven microchannel-plate (MCP) detectors. The imaging photon-counting MCP detectors have active areas of 19.6 cm2. Photon arrival position is determined using a wedge-and-strip anode and associated pulse-encoding electronics. The imaging characteristics of the EUVE flight detectors are presented including image distortion, flat-field response, and spatial differential nonlinearity. Also included is a detailed discussion of image distortions due to the detector mechanical assembly, the wedge-and-strip anode, and the electronics. Model predictions of these distortions are compared to preflight calibration images which show distortions less than 1.3 percent rms of the detector diameter of 50 mm before correction. The plans for correcting these residual detector image distortions to less than 0.1 percent rms are also presented.

Vallerga, J. V.↗
NASA NTRS1989

Photon counting detectors for Fabry-Perot interferometers

Sealed channel plate photomultipliers with multiple discrete anodes for use as photon counting detectors in the image plane of Fabry-Perot interferometers are described. The influence of design and construction on performance of completed devices is discussed. Effects on spatial resolution, lifetime, and counting efficiency are described. It is shown that devices can be optimized for particular applications. The results should be generally applicable to resistive anode and wedge and strip anode types of sealed detectors.

Darlington, E. H.↗
DOE OSTI2020

Bismuth Subcarbonate Decorated Reduced Graphene Oxide Nanocomposite for the Sensitive Stripping Voltammetry Analysis of Pb(II) and Cd(II) in Water

In this paper, bismuth subcarbonate (BiO)2CO3-reduced graphene oxide nanocomposite incorporated in Nafion matrix ((BiO)2CO3-rGO-Nafion) was synthesized and further applied, for the first time, in the sensitive detection of Pb(II) and Cd(II) by square-wave anodic stripping voltammetry (SWASV). The as-synthesized nanocomposites were characterized by energy-dispersive spectroscopy (EDS), Raman spectroscopy, scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). (BiO)2CO3 composite plays a key role in the improvement of the detection sensitivity, which can form multicomponent alloy with cadmium and lead. Additionally, the unique structure of rGO can enlarge the surface area and provide abundant active sites. Moreover, Nafion incorporation in the nanocomposite can effectively increase the adhesion and mechanical strength of the film, and further improve the preconcetration ability due to the cation-exchange capacity of its abundant sulfonate groups. As expected, the (BiO)2CO3-rGO/Nafion nanocomposite-modified glassy carbon electrode ((BiO)2CO3-rGO-Nafion/GCE) achieved low detection limits of 0.24 μg/L for Pb(II) and 0.16 μg/L for Cd(II), in the linear range of 1.0–60 μg/L, and showed some excellent performance, such as high stability, good selectivity, and sensitivity. Finally, synthetic water samples were prepared and further used to verify the practicability of the (BiO)2CO3-rGO-Nafion/GCE with satisfactory results.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2019

Initial Trade Study for In-line Silver Sensor for Spacecraft Potable Water Systems

Ionic silver is currently baselined as the biocide for microbial control in potable water systems for future space exploration missions. In-line monitoring of silver ion concentration is desired for system feedback control to introduce and maintain sufficient and safe levels of biocide in the water. To date, NASA testing of silver biocide system prototypes has made use of an Ion-Selective Electrode (ISE) for in-line silver concentration measurements. However, known issues with ISE technology have continued to motivate a search for alternate sensor systems. Although devices capable of detecting silver are available for terrestrial applications, these systems are generally not well-suited for the unique demands of spaceflight. Desired attributes include: low weight, volume, and power consumption; stable, autonomous, and in-line measurement capability; long calibration lifetime; and limited maintenance requirements. This paper provides the results from a preliminary trade study conducted on three candidate silver sensor technologies: ISEs, Anodic Stripping Voltammetry (ASV), and Fiber Optic Chemical Sensors (FOCS). The review of these technologies includes the rationale for their selection, an overview of the principles of their operation, and a detailed assessment of their strengths and weaknesses relative to the anticipated requirements of future spacecraft applications. The study concluded that none of the currently-available versions of these technologies is suitable for immediate application to spacecraft systems; further technology development should be considered. To that end, recommendations for forward development work have been proposed and provided herein.

Potable Water↗
DOE OSTI2021

Linker-Free Magnetite-Decorated Gold Nanoparticles (Fe3O4-Au): Synthesis, Characterization, and Application for Electrochemical Detection of Arsenic (III)

Linker-free magnetite nanoparticles (Fe3O4NPs)-decorated gold nanoparticles (AuNPs) were grown using a new protocol that can be used as a new platform for synthesis of other intact metal–metal oxide nanocomposites without the need for linkers. This minimizes the distance between the metal and metal oxide nanoparticles and ensures the optimum combined effects between the two material interfaces. X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy confirmed the successful synthesis of the Fe3O4-Au nanocomposite, without any change in the magnetite phase. Characterization, using transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy, revealed the composite to consist of AuNPs of 70 ± 10 nm diameter decorated with tiny 10 ± 3 nm diameter Fe3O4NPs in Au:Fe mass ratio of 5:1. The prepared Fe3O4-Au nanocomposite was embedded in ionic liquid (IL) and applied for the modification of glassy carbon electrode (GCE) for the electrochemical detection of As(III) in water. By combining the excellent catalytic properties of the AuNPs with the high adsorption capacity of the tiny Fe3O4NPs towards As(III), as well as the good conductivity of IL, the Fe3O4-Au-IL nanocomposite showed excellent performance in the square wave anodic stripping voltammetry detection of As(III). Under the optimized conditions, a linear range of 1 to 100 μg/L was achieved with a detection limit of 0.22 μg/L (S/N = 3), and no interference from 100-fold higher concentrations of a wide variety of cations and anions found in water. A very low residual standard deviation of 1.16% confirmed the high precision/reproducibility of As(III) analysis and the reliability of the Fe3O4-Au-IL sensing interface. Finally, this proposed sensing interface was successfully applied to analyzing synthetic river and wastewater samples with a 95–101% recovery, demonstrating excellent accuracy, even in complex synthetic river and wastewater samples containing high concentrations of humic acid without any sample pretreatments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗