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DOE OSTI2025

Open Specy 1.0: Automated (Hyper)spectroscopy for Microplastics

Microplastic spectral analysis is one of the most time-consuming processes in studying microplastic pollution, often requiring days per sample. Researchers are transitioning to automated batch and hyperspectral image analysis techniques to enhance efficiency. Open Specy, initially aimed at manual single-spectrum analysis, has now integrated automated methods. This updated version, Open Specy 1.0, introduces several new features, including two algorithms for automated processing (smoothing and particle compression), an extensive library containing over 40,000 open-source Raman and FTIR spectra, and two machine learning classifiers (logistic regression and k medoids) developed from this library. Furthermore, it includes a revamped user interface, an R package, and a benchmark data set for testing future advancements in automated techniques. Researchers evaluated various configurations for hyperspectral smoothing, particle identification, compression, and splitting, to achieve combined recovery rates between 50 and 150% particle counts, identities, and sizes with a coefficient of variation (CV) of less than 40% (the accredited standard). Mean absorbance times the standard deviation provided a consistent particle identification. Hyperspectral smoothing led to a 96% combined recovery rate and reduced variability (CV = 38%) compared to the 86% recovery (CV = 83%) of nonsmoothed controls. Additionally, compressing spectra for particles was significantly faster (>3x) and showed similar accuracy but with reduced variability than processing each pixel individually. Key challenges persist in automating spectral analysis, particularly in refining particle splitting algorithms, and improving identification routines to minimize false positives and negatives. In conclusion, new methods in sample preparation for better stabilization and dispersion of particles could overcome some of these issues.

13 HYDRO ENERGY↗

NASA NTRS1974

Remote measurement of atmospheric temperatures by Raman lidar

The Raman shifted return of a lidar system has been utilized to make atmospheric temperature measurements. The measurements were made along a horizontal path at temperatures ranging from -30 C to +30 C and at ranges of about 100 meters. The temperature data were acquired by recording the intensity ratio of two portions of the rotational Raman spectrum which were simultaneously sampled from a preset range. A temperature measurement accuracy of plus or minus 4 C and a temporal resolution of one minute were realized with this system. The combined results of the theoretical analysis and the experimentation indicate that system improvements will significantly increase both accuracy and range.

Coney, T. A.↗

NASA NTRS2003

Raman-atomic force microscopy of the ommatidial surfaces of Dipteran compound eyes

The ommatidial lens surfaces of the compound eyes in several species of files (Insecta: Diptera) and a related order (Mecoptera) were analyzed using a recently developed Raman-atomic force microscope. We demonstrate in this work that the atomic force microscope (AFM) is a potentially useful instrument for gathering phylogenetic data and that the newly developed Raman-AFM may extend this application by revealing nanometer-scale surface chemistry. This is the first demonstration of apertureless near-field Raman spectroscopy on an intact biological surface. For Chrysopilus testaceipes Bigot (Rhagionidae), this reveals unique cerebral cortex-like surface ridges with periodic variation in height and surface chemistry. Most other Brachyceran flies, and the "Nematoceran" Sylvicola fenestralis (Scopoli) (Anisopodidae), displayed the same morphology, while other taxa displayed various other characteristics, such as a nodule-like (Tipula (Triplicitipula) sp. (Tipulidae)) or coalescing nodule-like (Tabanus punctifer Osten Sacken (Tabanidae)) morphology, a smooth morphology with distinct pits and grooves (Dilophus orbatus (Say) (Bibionidae)), or an entirely smooth surface (Bittacus chlorostigma MacLachlan (Mecoptera: Bittacidae)). The variation in submicrometer structure and surface chemistry provides a new information source of potential phylogenetic importance, suggesting the Raman-atomic force microscope could provide a new tool useful to systematic and evolutionary inquiry.

Eye/ultrastructure↗

NASA NTRS2005

Chirality Characterization of Dispersed Single Wall Carbon Nanotubes

Raman scattering and optical absorption spectroscopy are used for the chirality characterization of HiPco single wall carbon nanotubes (SWNTs) dispersed in aqueous solution with the surfactant sodium dodecylbenzene sulfonate. Radial breathing mode (RBM) Raman peaks for semiconducting and metallic SWNTs are identified by directly comparing the Raman spectra with the Kataura plot. The SWNT diameters are calculated from these resonant peak positions. Next, a list of (n, m) pairs, yielding the SWNT diameters within a few percent of that obtained from each resonant peak position, is established. The interband transition energies for the list of SWNT (n, m) pairs are calculated based on the tight binding energy expression for each list of the (n, m) pairs, and the pairs yielding the closest values to the corresponding experimental optical absorption peaks are selected. The results reveal that (1, 11), (4, 11), and (0, 11) as the most probable chiralities of the semiconducting nanotubes. The results also reveal that (4, 16), (6, 12) and (8, 8) are the most probable chiralities for the metallic nanotubes. Directly relating the Raman scattering data to the optical absorption spectra, the present method is considered the simplest technique currently available. Another advantage of this technique is the use of the E(sup 8)(sub 11) peaks in the optical absorption spectrum in the analysis to enhance the accuracy in the results.

Namkung, Min↗

DOE OSTI2026

Exploring Local Vibrational Structure in Protein-Bound Chlorophyll a: Isotope-Enrichment Experiments and Electrostatic Analysis

Local chlorophyll (Chl) vibrations play an essential role in biological photosynthesis by facilitating rapid energy transfer between pigments. In research studies, they also provide a useful spectroscopic probe of the local protein environment that surrounds each pigment. However, measuring the complete vibrational absorption spectrum of a protein-bound Chl molecule is much more difficult than, for example, Chl in neat solvent due to overlap with protein vibrations that typically drown out Chl vibrational features. Resonance Raman and fluorescence spectroscopies provide a way around this problem for Franck–Condon active vibrations, but these often rely on cryogenic measurement conditions and fail to capture vibrational signatures from, e.g., ester-group vibrations that lack coupling to a convenient electronic transition. In the present contribution, we use 13 C-enrichment of the protein backbone to shift protein background signals to lower frequency, providing a largely clean spectral window in which to study local Chl a C═O stretch modes. A room-temperature absorption spectrum for Chl a in the water-soluble chlorophyll protein (WSCP) of Lepidium virginicum is thus extracted as a difference between protein-plus-pigment and protein-only vibrational spectra. Excellent agreement in the molecular fingerprint region with the vibrational spectrum of Chl a in organic solvents confirms that the resulting spectrum represents the response of the protein-bound Chl a molecule. Furthermore, the ester group resonance is observed to shift in response to the S53P mutation that eliminates a 17 3 ester group hydrogen bond from the protein environment. Finally, we analyze these experimental results using MD-based electrostatic analysis, finding that electric-field mapping at the C atom of the ester group provides a satisfactory explanation for the observed frequency shifts between organic solvent and protein environment. MD analysis further suggests that a red-shifted ester peak observed experimentally for the S53P mutant results from solvation of the 17 3 Chl ester group due increase water penetration into the Chl-binding pocket relative to wild-type WSCP. Here, we anticipate that these results will prove useful both for benchmarking future simulation work and as a reference for interpreting Chl vibrational spectra as a probe of pigment–protein interactions.

14 SOLAR ENERGY↗

DOE OSTI2026

Reactions of U(DMSO) 8 (ClO 4 ) 4 with Terpyridine Yield Dimeric Hydrolysis Products and Induce C–C Coupling

Reactions have been carried out using UIV(DMSO) 8 (ClO 4 ) 4 with 2,2′:6′,2″-terpyridine (terpy) under nonaqueous conditions. At room temperature in acetonitrile, the combination of the U(IV) starting material with terpy resulted in a mixture containing [UO 2 (DMSO) 2 terpy][ClO 4 ] 2 ·MeCN, while increasing the water content led to the hydrolysis products [(UO 2 (DMSO)terpy) 2 (μ 2 –O)][ClO 4 ] 2 and [(UO 2 terpy) 2 (μ 2 –OH) 2 ][ClO 4 ] 2 ·MeCN·H 2 O. Performing the reaction at slightly elevated temperature with no added water led to the formation of [UO 2 sexipyridine][ClO 4 ] 2 ·MeCN. This new uranyl complex contains the hexadentate ligand 2,2′:6′,2″:6″,2″:6‴,2⁗:6⁗,2⁗′-sexipyridine, which formed in situ from the tetravalent uranium starting material, where photoexcited uranyl or in situ generated peroxide could have induced C–C coupling. Analysis of bonding in the dimeric uranyl species via quantum chemical methods revealed a small increase in covalency of the bridging oxo unit and a slightly greater stability compared to the bridging hydroxo compound, which causes a significant shift in the uranyl symmetric stretch in the Raman spectrum. Structural, spectroscopic, and computational comparisons are made across the series of compounds, providing insight into the bonding and reactivity of uranium in nonaqueous media.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2021

Calibration of the SHERLOC Deep Ultraviolet Fluorescence–Raman Spectrometer on the Perseverance Rover

We describe the wavelength calibration of the spectrometer for the scanning of habitable environments with Raman and luminescence for organics and chemicals (SHERLOC) instrument onboard NASA’s Perseverance Rover. SHERLOC utilizes deep ultraviolet Raman and fluorescence (DUV R/F) spectroscopy to enable analysis of samples from the Martian surface. SHERLOC employs a 248.6 nm deep ultraviolet laser to generate Raman-scattered photons and native fluorescence emission photons from near-surface material to detect and classify chemical and mineralogical compositions. The collected photons are focused on a charge-coupled device and the data are returned to Earth for analysis. The compact DUV R/F spectrometer has a spectral range from 249.9 nm to 353.6 nm (200 cm1 to 12, 000 cm1) (with a spectral resolution of 0.296 nm (40 cm1)). The compact spectrometer uses a custom design to project a high-resolution Raman spectrum and a low-resolution fluorescence spectrum on a single charge-coupled device. The natural spectral separation enabled by deep ultraviolet excitation enables wavelength separation of the Raman/fluorescence spectra. The SHERLOC spectrometer was designed to optimize the resolution of the Raman spectral region and the wavelength range of the fluorescence region. The resulting illumination on the charge-coupled device is curved, requiring a segmented, nonlinear wavelength calibration in order to understand the mineralogy and chemistry of Martian materials.

Kyle Uckert↗

NASA NTRS2003

Infrared Spectroscopy as a Chemical Fingerprinting Tool

Infrared (IR) spectroscopy is a powerful analytical tool in the chemical fingerprinting of materials. Any sample material that will interact with infrared light produces a spectrum and, although normally associated with organic materials, inorganic compounds may also be infrared active. The technique is rapid, reproducible and usually non-invasive to the sample. That it is non-invasive allows for additional characterization of the original material using other analytical techniques including thermal analysis and RAMAN spectroscopic techniques. With the appropriate accessories, the technique can be used to examine samples in liquid, solid or gas phase. Both aqueous and non-aqueous free-flowing solutions can be analyzed, as can viscous liquids such as heavy oils and greases. Solid samples of varying sizes and shapes may also be examined and with the addition of microscopic IR (microspectroscopy) capabilities, minute materials such as single fibers and threads may be analyzed. With the addition of appropriate software, microspectroscopy can be used for automated discrete point or compositional surface area mapping, with the latter providing a means to record changes in the chemical composition of a material surface over a defined area. Due to the ability to characterize gaseous samples, IR spectroscopy can also be coupled with thermal processes such as thermogravimetric (TG) analyses to provide both thermal and chemical data in a single run. In this configuration, solids (or liquids) heated in a TG analyzer undergo decomposition, with the evolving gases directed into the IR spectrometer. Thus, information is provided on the thermal properties of a material and the order in which its chemical constituents are broken down during incremental heating. Specific examples of these varied applications will be cited, with data interpretation and method limitations further discussed.

Huff, Timothy L.↗

NASA NTRS1986

Infrared absorption and emission characteristics of interstellar PAHs

The mid-infrared interstellar emission spectrum with features at 3.28, 6.2, 7.7, 8.7 and 11.3 microns is discussed in terms of the Polycyclic Aromatic Hydrocarbon (PAH) hypothesis, which is based on the suggestive, but inconclusive comparison between the interstellar emission spectrum with the infrared absorption and Raman spectra of a few PAHs. The fundamental vibrations of PAHs and PAH-like species which determine the IR and Raman properties are discussed. Interstellar IR band emission is due to relaxation from highly vibrationally excited PAHs excited by ultraviolet photons. The excitation/emission process is described and the IR fluorescence from one PAH, chrysene, is traced. Generally, there is sufficient energy to populate several vibrational levels in each mode. Molecular vibrational potentials are anharmonic and emission from these higher levels will fall at lower frequencies and produce weak features to the red of the stronger fundamentals. This process is also described and can account for some spectroscopic details of the interstellar emission spectra previously unexplained. Analysis of the interstellar spectrum shows that PAHs contain between 20 and 30 carbon atoms are responsible for the emission.

Barker, J. R.↗

NASA NTRS1987

Infrared absorption and emission characteristics of interstellar PAHs

Allamandola, L. J.↗

NASA NTRS1991

High-energy transients

The observational characteristics of X-ray bursts are reviewed and the thermonuclear-flash model is examined to assess the suitability of the model and the sources of X- and gamma-ray bursts. The profiles of X-ray bursts from five different sources are delineated, and the global analysis of nuclear burning is discussed to review th range possible X-ray burst behavior. The analysis by Fushiki and Lamb (1987) is noted for the description of regions which lie away from the steady-state cut. The discussion of cyclotron lines in gamma-ray bursts emphasizes the source GB880205, and it is shown that Raman and cyclotron resonant scattering can explain the observed positions, strengths, and widths of the dips in the spectrum. X-ray bursts are theorized to emanate from weakly magnetic neutron stars, and gamma-ray bursts are shown to be the products of strongly magnetic neutron stars.

Lamb, D. Q.↗

NASA NTRS2005

Extracting Olivine (Fo-Fa) Compositions from Raman Spectral Peak Positions

Olivine and pyroxene are two major basaltic minerals that have been identified at Gusev Crater and Meridiani Planum by the Mars Exploration Rovers. Full petrologic characterization of a sample (rock or soil), however, requires determining the range of mineral compositions, extent of zoning, range of grain sizes, mineral associations, presence of xenocrysts, etc. Information of this sort will aid the interpretation of sample crystallization and differentiation histories and help discriminate between lithologies. In Raman spectroscopic experiments, minerals are identified by their spectral patterns and mineral compositions can be inferred from the peak positions. Instruments currently in use or slated for impending surface exploration missions provide only average elemental compositions for relatively large rock or soil targets or bulk mineral analysis. No techniques currently in use or scheduled for flight can characterize both structure and composition of individual mineral grains, in-situ, like the Mars Microbeam Raman Spectrometer (MMRS). The MMRS is designed to take 100 spectra along a 1 cm linear traverse on the surface of a sample, with contributions from one or a few mineral phases per spectrum. We presented a method to extract structural and compositional information from the Raman spectra of quadrilateral pyroxenes. The pyroxene calibration was applied to a Raman spectroscopic study of Martian meteorite EETA79001 along with a preliminary olivine calibration, where we demonstrated the capability to discriminate related lithologies using Raman point counts. This paper presents an improved olivine calibration that will further aid sample characterization and the study of alteration processes.

Kuebler, K.↗

NASA NTRS2002

Outbursts In Symbiotic Binaries (FUSE 2000)

During the past year, we made good progress on analysis of FUSE observations of the symbiotic binary Z And. For background, Z And is a binary system composed of a red giant and a hot component of unknown status. The orbital period is roughly 750 days. The hot component undergoes large-scale eruptions every 10-20 yr. An outburst began several years ago, triggering this FUSE opportunity. First, we obtained an excellent set of ground-based optical data in support, of the FUSE observations. We used FAST, a high throughput low resolution spectrograph on the 1.5-m telescope at Mt. Hopkins, Arizona. A 300 g/ mm grating blazed at 4750 A, a 3 in. slit, and a thinned Loral 512 x 2688 CCD gave us spectra covering 3800-7500 A at a resolution of 6 A. The wavelength solution for each spectrum has a probable error of +/- 0.5 A or better. Most of the resulting spectra have moderate signal-to-noise, S/.N approx. greater than 30 per pixel. The time coverage for these spectra is excellent. Typically, we acquired spectra every 1-2 nights during dark runs at Mt. Hopkins. These data cover most of the rise and all of the decline of the recent outburst. The spectra show a wealth of emission lines, including H I, He I, He II, [Fe V11], and the Raman scattering bands at 6830 A and 7088 A. The Raman bands and other high ionization features vary considerably throughout the outburst. These features will enable us to correlate variations in the FUSE spectra with variations in the optical spectra. Second, we began an analysis of FUSE spectra of Z And. We have carefully examined the spectra, identifying real features and defects. We have identified and measured fluxes for all strong emission lines, including the O VI doublet at 1032 A and 1038 A. These and several other strong emission lines display pronounced P Cygni absorption components indicative of outgrowing gas. We will attempt to correlate these velocities with similar profiles observed on optical spectra. The line velocities - together with line variations - will yield physical parameters for the expanding shell of gas in the outer atmosphere of the hot component. We also worked on several diagnostic tools, including upgrades to photoionization programs developed by the PI and others. We plan to use these tools to derive electron densities and temperatures front intercombination and forbidden lines observed on optical and FUSE spectra. Preliminary results indicate a large electron density, n(sub e) is greater than or = 10(exp 10)/cc and a modest electron temperature, T(sub e) approx. 20,000 K. We see no evidence for shocked gas as observed in some other symbiotics. However, we have yet to include several important lines of [Fe VII] and [Ne V] in the analysis. Inclusion of these lines will yield an improved estimate of the electron temperature in the gas. Finally, we have one additional FUSE spectrum planned for acquisition during this cycle. These data will provide important information concerning the state of the system farther along in its decline. Once we have this spectrum in hand, we plan to complete our analysis and publish our results.

Kenyon, Scott J.↗

DOE OSTI2024

The Raman gap and collisional absorption

One of the long-standing puzzles observed in many laser-plasma experiments is the gap in the Raman backscattering spectrum. This gap is characterized by the absence of backscattered light between some critical wavelength and twice the incident laser wavelength. The latter is associated with the absolute Raman instability from the quarter-critical density surface. Supported by particle-in-cell (PIC) simulations, it is suggested that the gap can result from the collisional damping of the backscattered light. A linear analysis of the competition between the Raman growth rate and the damping rate in a non-homogenous plasma predicts the gap's existence and width as a function of the system's parameters. The theory is compared with the PIC simulations and past experiments.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2020

Structure Analysis of Natural Wangdaodeite—LiNbO3-Type FeTiO3

This paper reports the first structure refinement of natural wangdaodeite, LiNbO3-type FeTiO3 from the Ries impact structure. Wangdaodeite occurs together with recrystallized ilmenite clasts in shock melt veins which have experienced peak shock pressures of between 17 and 22 GPa. Comparison of natural and synthetic wangdaodeite points toward a correlation between the distortion of ferrate- and titanate-polyhedra and the c/a ratio of the unit cell. The Raman spectrum of wangdaodeite is calculated based on the refined structure. Comparison to the reported spectrum of the type-material shows that the Raman peak at 738–740 cm−1 is indicative for this phase, whereas other features in type-wangdaodeite are tentatively assigned to disordered ilmenite.

58 GEOSCIENCES↗

NASA NTRS2020

Use of an Internal Mercury-Argon Lamp for the Calibration of Raman Frequency in Large Raman Images of Astromaterials

Raman imaging is an emerging tool for the analysis of meteorites, as it is capable of describing mineralogy, carbon composition/speciation, and crystal orientation all within a petrographic context. Adequately examining the heterogeneous composition of a meteorite, while maintaining low laser powers needed to prevent damage to meteorite mineralogy and organics, often requires the collection of large Raman images with long collection times on the timescale of days. However, the frequency calibration of the Raman instrument/spectrometer drifts on long timescales resulting in low frequency precision for the Raman spectra comprising a large Raman image. This decrease in frequency precision can compromise the analysis of geological markers that can provide important information on a meteorite sample. We examine, in detail, the change in bandwidth and frequency of the Raman bands and Hg-Ar emission lines in our Raman images as a function of time and laboratory temperature. To overcome the drift in calibration, we utilize a commercial WITec Raman instrument with an internal Hg-Ar calibration lamp to individually calibrate each spectrum in the Raman image. Our instrument, known as “Ratatoskr”, uses a beam splitter in place of the customary mirror to facilitate collection of Hg-Ar calibration lines concurrent with Raman spectra. We show that using the internal calibration we can improve the frequency precision for the spectra in our Raman images from ~±0.15 cm(exp -1) to ~±0.05 cm(exp -1) for Raman spectra collected over multiple days. This is important as it improves measurements of mineral chemistry, latent strain, and other features that are dependent upon accurate peak position determination. We also examine the spectral signal-to-noise ratio needed to minimize the frequency error when fitting bands to Gaussian/Lorentzian profiles. We then use our results to suggest a general method for calibrating the frequency of Raman spectra in large Raman images.

Jakubek, Ryan S.↗

DOE OSTI2025

Spectroscopic Properties of Americium(III) in Mineral Acid Media

We report the preparation and optical characterization of three solutions of Am(III) in common aqueous (aq.) mineral acids (HCl, HNO 3 and HBr), including absorption, emission, and Raman vibrational analyses. To our knowledge, this study provides the first detailed absorption spectra of Am(III) spanning the entire UV/Vis/NIR region in these mineral acids reported since the 1960s. Here, using this high-resolution absorption data, provided in an open access format for the broader field, we build on prior work by Carnall and others to provide detailed optical analysis including all transition assignments. This work also includes the first reported absorption spectrum of Am(III) in aq. HBr. Characteristic Am(III) luminescence could be detected from all three samples. These are the first reports of emission from Am(III) in these acid systems, which build on prior emission reports collected from aq. HClO 4 solutions. The acquired emission spectra display anion-dependent shifting of the visible-region transitions by up to 21 nm from their predicted positions, akin to the nephelauxetic effect. The shift magnitude trends linearly according to the acid p K a and more generally according to the transition metal spectrochemical series. These ligand field effects, coupled with luminescence lifetime experiments, indicate that weak Am-X interactions persist in solution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Analysis of picosecond coherent anti-Stokes Raman spectra for gas-phase diagnostics

We present a hybrid frequency- and time-domain solution, applicable to the case of picosecond coherent anti-Stokes Raman scattering (CARS), for gas-phase diagnostics. A solution has been derived based on both physical arguments and four-wave mixing equations for picosecond CARS, with pulse durations that are comparable to the dephasing time scale for gas-phase Raman coherence—a regime where commonly employed solutions for impulsive (femtosecond) or cw (nanosecond) pump/Stokes forcing are not strictly valid. We present the ps-CARS spectrum in the form of incoherent sums of CARS intensity spectra, calculated from the fundamental solution for impulsive pump/Stokes Raman preparation. The solution was examined for temperatures from 1000–3000 K, for four plausible experimental configurations, with laser pulse durations of 50–150 ps, and probe pulse delays from −20 to 240 ps. Approximations based on cw and impulsive pump/Stokes preparation to fit picosecond CARS spectra at atmospheric pressure were examined and the relative thermometric accuracy and computational cost of these approximations were quantified for the case of a zero nonresonant CARS contribution, and a nonresonant susceptibility equal to 10% of the Raman-resonant value at the N 2 bandhead. The nanosecond CARS approximation can result in large fitting errors when the probe pulse time delay is less than the probe pulse duration. Errors as large as 10–20% are observed in the fit temperatures for a zero picosecond probe pulse delay, when the nonresonant background is neglected, largely due to an inability of the time-independent cw model to capture transient frequency spread dephasing effects at the Q -branch bandhead. The inclusion of a nonresonant background results in 40–60% thermometry errors with a nanosecond model at a zero-probe delay. Time-dependent impulsive calculations used for femtosecond CARS better approximate the structure of the N 2 bandhead, reducing temperature fitting errors to 5–10% at a short probe pulse delay. The impulsive approximation results in errors up to 10% at intermediate probe pulse delays, where the coherence of the pump and probe pulses leads to multiple terms in the picosecond CARS solution. Both approximations improve as the probe pulse delay exceeds the probe duration. The nanosecond approximation results in a 2–3% error, while the impulsive model results in differences of less than 1% in some cases. Fits to experimental data obtained using short, ∼60ps pulses at a zero probe time delay and longer 100 ps pulses at a substantial 200 ps delay are presented with accuracies of 1–3% in the fit temperature.

Kearney, Sean P.↗