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At least 775 records · Page 43

Update on Development of the Potassium-Argon Laser Experiment (KArLE) Instrument for In Situ Geochronology

Absolute dating of planetary samples is an essential tool to establish the chronology of geological events, including crystallization history, magmatic evolution, and alteration. We are addressing this challenge by developing the Potassium (K) -- Argon Laser Experiment (KArLE), building on previous work to develop a K-Ar in situ instrument. KArLE ablates a rock sample, determines the K in the plasma state using laser-induced breakdown spectroscopy (LIBS), measures the liberated Ar using quadrupole mass spectrometry (QMS), and relates the two by the volume of the ablated pit using laser confocal microscopy (LCM). Our goal is for the KArLE instrument to be capable of determining the age of several kinds of planetary samples to address a wide range of geochronolgy problems in planetary science.

Cohen, Barbara A.↗

Volume Measurements of Laser-generated Pits for in Situ Geochronology Using KArLE (Potassium-Argon Laser Experiment)

KArLE (Potassium-­‐Argon Laser Experiment) has been developed for in situ planetary geochronology using the K - Ar (potassium-­‐argon) isotope system, where material ablated by LIBS (Laser-­‐Induced Breakdown Spectroscopy) is used to calculate isotope abundances. We are determining the accuracy and precision of volume measurements of these pits using stereo and laser microscope data to better understand the ablation process for isotope abundance calculations. If a characteristic volume can be determined with sufficient accuracy and precision for specific rock types, KArLE will prove to be a useful instrument for future planetary rover missions.

French, R. A.↗

Machine learning in analytical spectroscopy for nuclear diagnostics [Invited]

Analytical spectroscopy methods have shown many possible uses for nuclear material diagnostics and measurements in recent studies. In particular, the application potential for various atomic spectroscopy techniques is uniquely diverse and generates interest across a wide range of nuclear science areas. Over the last decade, techniques such as laser-induced breakdown spectroscopy, Raman spectroscopy, and x-ray fluorescence spectroscopy have yielded considerable improvements in the diagnostic analysis of nuclear materials, especially with machine learning implementations. These techniques have been applied for analytical solutions to problems concerning nuclear forensics, nuclear fuel manufacturing, nuclear fuel quality control, and general diagnostic analysis of nuclear materials. The data yielded from atomic spectroscopy methods provide innovative solutions to problems surrounding the characterization of nuclear materials, particularly for compounds with complex chemistry. Implementing these optical spectroscopy techniques can provide comprehensive new insights into the chemical analysis of nuclear materials. In particular, recent advances coupling machine learning methods to the processing of atomic emission spectra have yielded novel, robust solutions for nuclear material characterization. This review paper will provide a summation of several of these recent advances and will discuss key experimental studies that have advanced the use of analytical atomic spectroscopy techniques as active tools for nuclear diagnostic measurements.

Rao, Ashwin P. (ORCID:0000000319312568)↗

Accurate determination of the fine-structure intervals in the 3P ground states of C-13 and C-12 by far-infrared laser magnetic resonance

Accurate values are presented for the fine-structure intervals in the 3P ground state of neutral atomic C-12 and C-13 as obtained from laser magnetic resonance spectroscopy. The rigorous analysis of C-13 hyperfine structure, the measurement of resonant fields for C-12 transitions at several additional far-infrared laser frequencies, and the increased precision of the C-12 measurements, permit significant improvement in the evaluation of these energies relative to earlier work. These results will expedite the direct and precise measurement of these transitions in interstellar sources and should assist in the determination of the interstellar C-12/C-13 abundance ratio.

Cooksy, A. L.↗

Surface Monitoring of CFRP Structures for Adhesive Bonding

Adhesive bonding of composite materials requires reliable monitoring and detection of surface contaminants to assure robust and durable bonded structures. Surface treatment and effective monitoring prior to bonding is essential in order to obtain a surface free from contaminants that may degrade structural performance. Two techniques which monitor the effectiveness of the laser surface treatment of carbon fiber reinforced polymer (CFRP) materials are being investigated: laser induced breakdown spectroscopy (LIBS) and optically stimulated electron emission (OSEE). The applicability of LIBS to detect silicone contaminants on CFRP composites is studied using ~35 ns Nd:YAG laser pulses at 355 nm with a pulse energy of 45 mJ. The LIBS regime in which pulse energies are < 100 mJ is referred to as mLIBS. CFRP surfaces were contaminated with polydimethylsiloxane (PDMS), a major component of silicone based mold release agents. The presence of PDMS is found by inspecting the Si I emission line at 288.2 nm. Untreated CFRP samples and CFRP contaminated with PDMS were tested. The PDMS areal density ranged from 0.36 Â+/- 0.04 to 0.51 Â+/- 0.16 mg/cm2. The results demonstrate the successful detection of PDMS on CFRP using mLIBS. In addition, OSEE was used to measure CFRP surface cleanliness pre- and post-treatment by laser ablation on specimens contaminated with PDMS coatings from 8 nm to 1311 nm in thickness. The results showed a significant increase in the OSEE photocurrent after laser surface treatment.

Ledesma, Rodolfo↗

Excitation of optically trapped single particles using femtosecond pulses

Excitation from optically trapped particles is examined through laser-induced breakdown spectroscopy following interactions with mJ-level fs pulses. Optical emissions from sub-ng ablation of precisely positioned cupric oxide microparticles are used as a method to spatially resolve laser–particle interactions resulting in excitation. External focusing lenses are often used to change the dynamics of nonlinear self-focusing of fs pulses to form laser filaments or, alternatively, to form very intense air plasmas. Given the significant implications external focusing has on laser propagation and plasma conditions, single-particle emissions are studied with focusing lenses ranging from 50 to 300 mm. It is shown that, while single particles are less excited at longer focal lengths due to limited energy transfer through laser–particle interactions, the cooler plasma results in a lower thermal background to reveal resolved single-shot emission peaks. Furthermore, by developing an understanding in the fundamental interaction that occurs between single particles and fs pulses and filaments, practical improvements can be made for atmospheric remote sensing of low-concentration aerosols.

42 ENGINEERING↗

Oceanic Lidar

Instrument concepts which measure ocean temperature, chlorophyll, sediment and Gelbstoffe concentrations in three dimensions on a quantitative, quasi-synoptic basis were considered. Coastal zone color scanner chlorophyll imagery, laser stimulated Raman temperaure and fluorescence spectroscopy, existing airborne Lidar and laser fluorosensing instruments, and their accuracies in quantifying concentrations of chlorophyll, suspended sediments and Gelbstoffe are presented. Lidar applications to phytoplankton dynamics and photochemistry, Lidar radiative transfer and signal interpretation, and Lidar technology are discussed.

Carder, K. L.↗

High power actively Q-switched downhole LIBS analysis systems

An actively Q-switched laser induced breakdown spectroscopy (LIBS) probe, utilizing an optical fiber, a pump beam transmitted through the optical fiber, a coupler, and a lens for collimating the pump beam. The actively Q-switched laser, coupled to a sensor which provides information to a computer that controls a high voltage pulser providing a pulse to a Pockels cell located within the laser which can selectively cause the laser to pulse, resulting in high energy pulses and a second lens for focusing the output pulse such that it creates a plasma or spark. The light from the spark is captured and directed back through an optical system to remote equipment for elemental and/or molecular analysis.

McIntyre, Dustin Langdon↗

Design, construction, and validation of an in-situ groundwater trace element analyzer with applications in carbon storage

Abstract It is estimated that carbon emissions should reach net-zero by 2050 to meet important climate targets. Carbon capture is likely necessary to reach these targets, requiring a long-term storage solution such as geological carbon sequestration. However, as with any subsurface activity, leakage can occur, potentially impacting groundwater quality near the storage site. Rapid detection is essential to mitigate damage to this resource. Since CO 2 will acidify groundwater, the concentrations of acid soluble minerals and associated cations will increase. Thus, an in-situ, real-time element analysis system based on laser-induced breakdown spectroscopy (LIBS) is under development to monitor these elements. The system splits the traditional LIBS system into a miniature, all-optical sensor head built around a passively Q-switch laser fiber coupled to a control unit. Previous work has validated the LIBS technique for use at high pressure as well as the split system design. In this work, a fieldable prototype sensor is developed and tested in an onsite monitoring well where trace elements concentrations (approx. 0–3 ppm) were tracked over 20 days. These concentrations varied in response to local rainfall, diluting with increased rain, demonstrating the ability of a LIBS-based sensor to track trace elements under real-world conditions.

54 ENVIRONMENTAL SCIENCES↗

Frame-Transfer Gating Raman Spectroscopy for Time-Resolved Multiscalar Combustion Diagnostics

Accurate experimental measurement of spatially and temporally resolved variations in chemical composition (species concentrations) and temperature in turbulent flames is vital for characterizing the complex phenomena occurring in most practical combustion systems. These diagnostic measurements are called multiscalar because they are capable of acquiring multiple scalar quantities simultaneously. Multiscalar diagnostics also play a critical role in the area of computational code validation. In order to improve the design of combustion devices, computational codes for modeling turbulent combustion are often used to speed up and optimize the development process. The experimental validation of these codes is a critical step in accepting their predictions for engine performance in the absence of cost-prohibitive testing. One of the most critical aspects of setting up a time-resolved stimulated Raman scattering (SRS) diagnostic system is the temporal optical gating scheme. A short optical gate is necessary in order for weak SRS signals to be detected with a good signal- to-noise ratio (SNR) in the presence of strong background optical emissions. This time-synchronized optical gating is a classical problem even to other spectroscopic techniques such as laser-induced fluorescence (LIF) or laser-induced breakdown spectroscopy (LIBS). Traditionally, experimenters have had basically two options for gating: (1) an electronic means of gating using an image intensifier before the charge-coupled-device (CCD), or (2) a mechanical optical shutter (a rotary chopper/mechanical shutter combination). A new diagnostic technology has been developed at the NASA Glenn Research Center that utilizes a frame-transfer CCD sensor, in conjunction with a pulsed laser and multiplex optical fiber collection, to realize time-resolved Raman spectroscopy of turbulent flames that is free from optical background noise (interference). The technology permits not only shorter temporal optical gating (down to <1 s, in principle), but also higher optical throughput, thus resulting in a substantial increase in measurement SNR.

Nguyen, Quang-Viet↗

Meteorological lidar developments

A research program on remote optical measurements of humidity and temperature is summarized, and new results are given of such measurements as well as new data on the near IR absorption spectrum of H2O. The basic atmospheric technique is differential absorption lidar (DIAL) using narrow band, tunable dye lasers. Approximate wavelengths are 720, 820, 940 nm (H2O) and 690, 760 nm (O2; temperature). The requisite absorption line strengths and widths are measured in a controlled environment by means of grating spectroscopy and tunable lasers. Prospects for routine lidar meteorology, even from airplane and satellite platforms, appear excellent in several important applications; the conditions and the optical properties of the atmosphere can be obtained remotely by these means.

Wilkerson, T. D.↗

Application of Raman Spectroscopy for Nondestructive Evaluation of Composite Materials

This paper will present an overview of efforts to investigate the application of Raman spectroscopy for the characterization of Kevlar materials. Raman spectroscopy is a laser technique that is sensitive to molecular interactions in materials such as Kevlar, graphite and carbon used in composite materials. The overall goal of this research reported here is to evaluate Raman spectroscopy as a potential nondestructive evaluation (NDE) tool for the detection of stress rupture in Kevlar composite over-wrapped pressure vessels (COPVs). Characterization of the Raman spectra of Kevlar yarn and strands will be presented and compared with analytical models provided in the literature. Results of testing to investigate the effects of creep and high-temperature aging on the Raman spectra will be presented.

Washer, Glenn A.↗

Tunable diode laser measurements of HO2NO2 absorption coefficients near 12.5 microns

A tunable diode laser spectrometer has been used to measure absorption coefficients of peroxynitric acid (HO2NO2) near the 803/cm Q branch. HO2NO2 concentrations in a low-pressure flowing gas mixture were determined from chemical titration procedures and UV absorption spectroscopy. The diode laser measured absorption coefficients, at a spectral resolution of better than 0.001/cm, are about 10 percent larger than previous Fourier transform infrared measurements made at a spectral resolution of 0.06/cm.

May, R. D.↗

The SuperCam Instrument Suite on the NASA Mars 2020 Rover: Body Unit and Combined System Tests

The SuperCam instrument suite provides the Mars 2020 rover, Perseverance, with a number of versatile remote-sensing techniques that can be used at long distance as well as within the robotic-arm workspace. These include laser-induced breakdown spectroscopy (LIBS), remote time-resolved Raman and luminescence spectroscopies, and visible and infrared (VISIR; separately referred to as VIS and IR) reflectance spectroscopy. A remote micro-imager (RMI) provides high-resolution color context imaging, and a microphone can be used as a stand-alone tool for environmental studies or to determine physical properties of rocks and soils from shock waves of laser-produced plasmas. SuperCam is built in three parts: The mast unit (MU), consisting of the laser, telescope, RMI, IR spectrometer, and associated electronics, is described in a companion paper. The on-board calibration targets are described in another companion paper. Here we describe SuperCam’s body unit (BU) and testing of the integrated instrument. The BU, mounted inside the rover body, receives light from the MU via a 5.8 m optical fiber. The light is split into three wavelength bands by a demultiplexer, and is routed via fiber bundles to three optical spectrometers, two of which (UV and violet; 245–340 and 385–465 nm) are crossed Czerny-Turner reflection spectrometers, nearly identical to their counterparts on ChemCam. The third is a high-efficiency transmission spectrometer containing an optical intensifier capable of gating exposures to 100 ns or longer, with variable delay times relative to the laser pulse. This spectrometer covers 535–853 nm ( $105\text{--}7070~\text{cm}^{-1}$ Raman shift relative to the 532 nm green laser beam) with $12~\text{cm}^{-1}$ full-width at half-maximum peak resolution in the Raman fingerprint region. The BU electronics boards interface with the rover and control the instrument, returning data to the rover. Thermal systems maintain a warm temperature during cruise to Mars to avoid contamination on the optics, and cool the detectors during operations on Mars.Results obtained with the integrated instrument demonstrate its capabilities for LIBS, for which a library of 332 standards was developed. Examples of Raman and VISIR spectroscopy are shown, demonstrating clear mineral identification with both techniques. Luminescence spectra demonstrate the utility of having both spectral and temporal dimensions. Finally, RMI and microphone tests on the rover demonstrate the capabilities of these subsystems as well.

47 OTHER INSTRUMENTATION↗

Isolation, characterization, and primary structure of rubredoxin from the photosynthetic bacterium, Heliobacillus mobilis

Rubredoxin is a small nonheme iron protein that serves as an electron carrier in bacterial systems. Rubredoxin has now been isolated and characterized from the strictly anaerobic phototroph, Heliobacillus mobilis. THe molecular mass (5671.3 Da from the amino acid sequence) was confirmed and partial formylation of the N-terminal methionyl residue was established by matrix-assisted laser desorption mass spectroscopy. The complete 52-amino-acid sequence was determined by a combination of N-terminal sequencing by Edman degradation and C-terminal sequencing by a novel method using carboxypeptidase treatment in conjunction with amino acid analysis and laser desorption time of flight mass spectrometry. The molar absorption coefficient of Hc. mobilis rubredoxin at 490 nm is 6.9 mM-1 cm-1 and the midpoint redox potential at pH 8.0 is -46 mV. The EPR spectrum of the oxidized form shows resonances at g = 9.66 and 4.30 due to a high-spin ferric iron. The amino acid sequence is homologous to those of rubredoxins from other species, in particular, the gram-positive bacteria, and the phototrophic green sulfur bacteria, and the evolutionary implications of this are discussed.

NASA Discipline Number 52-30↗

Recent Advances in LIBS for Real-Time Detection of Silicone Contaminants on CFRP Surfaces

Laser induced breakdown spectroscopy (LIBS) is a materials characterization technique that has been advanced and refined to provide in situ, real-time quality control of carbon fiber reinforced polymer (CFRP) surfaces. As part of an effort to improve process control for adhesive bonding, aLIBS system was designed and assembled at the NASA Langley Research Center (LaRC) to enable detection of ultra low concentrations of silicone contamination on CFRP adherends. The LIBS instrument provides high sensitivity detection and quasi-nondestructive surface characterization ofCFRP adherends prior to adhesive bonding. This review focuses on the advancements at LaRC using LIBS as a quality control tool for the detection of silicone contaminants for improved adhesive bonding reliability of CFRP materials. This work describes how the LIBS technique was advanced by analyzing the laser parameters, studying the laser-matter interactions, and performing time-resolved measurements to determine the optimal plasma conditions for elemental detection. In addition, LIBS results were compared to X-ray photoelectron spectroscopy data to enable quantitative analysis from analytical calibration curves. Examples are shown of how to perform surface mapping of silicone contamination. Finally, a brief discussion is presented on LIBS instrumentation, recommendations for laser parameters and instrumentation components, and LIBS technique maturity

Rodolfo I. Ledesma↗

Recent Advances in LIBS for Real-Time Detection of Silicone Contaminants on CFRP Surfaces

Laser induced breakdown spectroscopy (LIBS) is a materials characterization technique that has been advanced and refined to provide in situ, real-time quality control of carbon fiber reinforced polymer (CFRP) surfaces. As part of an effort to improve process control for adhesive bonding, a LIBS system was designed and assembled at NASA Langley Research Center (LaRC) to enable detection of ultralow concentrations of silicone contamination on CFRP adherends. The LIBS instrument provides high sensitivity detection and quasi-nondestructive surface characterization of CFRP adherends prior to adhesive bonding. This review focuses on the advancements at LaRC using LIBS as a quality control tool for the detection of silicone contaminants for improved adhesive bonding reliability of CFRP materials. This work describes how the LIBS technique was advanced by analyzing the laser parameters, studying the laser-matter interactions, and performing time-resolved measurements to determine the optimal plasma conditions for elemental detection. In addition, LIBS results were compared to X-ray photoelectron spectroscopy data to enable quantitative analysis from analytical calibration curves. Examples are shown of how to perform surface mapping of silicone contamination. Finally, a brief discussion is also presented on LIBS instrumentation, recommendations for laser parameters and instrumentation components, and LIBS technique maturity.

Surface characterization, Carbon fiber reinforced ↗

A 10 micron heterodyne receiver for ultra high resolution astronomical spectroscopy

An improved CO2 laser heterodyne spectrometer is examined. The present system uses reflective optics to eliminate refocusing at different wavelengths, and the local oscillator is a line-center-stabilized isotopic CO2 laser. A tunable diffraction grating makes possible easy and rapid selection of over 50 transitions per isotope of CO2. The IF (0 to 1.6 GHz) from the HgCdTe photomizer is analyzed by a 128-channel filter bank, consisting of 64 tunable 5-MHz filters and 64 fixed 25-MHz RF filters. These filters provide resolving powers of about 1,000,000 to 10,000,000 and velocity resolution of 50 to 250 m/sec; their output is synchronously detected, integrated, multiplexed and stored in a buffer memory for the desired integration period. Kitt Peak observations show the wide spectral coverage, wide mixer and electronics bandwidth, and high sensitivity of the system.

Buhl, D.↗