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At least 577 records · Page 32

Doppler lidar wind measurement with the edge technique

The edge technique is a new and powerful method for measuring small frequency shifts. Range resolved lidar measurements of winds can be made with high accuracy and high vertical resolution using the edge technique to measure the Doppler shift of an atmospheric backscattered signal from a pulsed laser. The edge technique can be used at near-infrared or visible wavelengths using well developed solid state lasers and detectors with various edge filters. In the edge technique, the laser frequency is located on the steep slope of the spectral response function of a high resolution optical filter. Due to the steep slope of the edge, very small frequency shifts cause large changes in measured signal. The frequency of the outgoing laser pulse is determined by measuring its location on the edge of the filter. This is accomplished by sending a small portion of the beam to the edge detection setup where the incoming light is split into two channels - an edge filter and an energy monitor channel. The energy monitor signal is used to normalize the edge filter signal for magnitude. The laser return backscattered from the atmosphere is collected by a telescope and directed through the edge detection setup to determine its frequency (location on the edge) in a similar manner for each range element. The Doppler shift, and thus the wind, is determined from a differential measurement of the frequency of the outgoing laser pulse and the frequency of the laser return backscattered from the atmosphere. We have conducted simulations of the performance of an edge lidar system using an injection seeded pulsed Nd:YAG laser at 1.06 microns. The central fringe of a Fabry-Perot etalon is used as a high resolution edge filter to measure the shift of the aerosol return.

Korb, C. Laurence↗

Synchrotron infrared nano-spectroscopy and -imaging

Infrared (IR) spectroscopy has evolved into a powerful analytical technique to probe molecular and lattice vibrations, low-energy electronic excitations and correlations, and related collective surface plasmon, phonon, or other polaritonic resonances. In combination with scanning probe microscopy, near-field infrared nano-spectroscopy and -imaging techniques have recently emerged as a frontier in imaging science, enabling the study of complex heterogeneous materials with simultaneous nanoscale spatial resolution and chemical and quantum state spectroscopic specificity. Here, we describe synchrotron infrared nano-spectroscopy (SINS), which takes advantage of the low-noise, broadband, high spectral irradiance, and coherence of synchrotron infrared radiation for near-field infrared measurements across the mid- to far-infrared with nanometer spatial resolution. This powerful combination provides a qualitatively new form of broadband spatio-spectral analysis of nanoscale, mesoscale, and surface phenomena that were previously difficult to study with IR techniques, or even any form of micro-spectroscopy in general. We review the development of SINS, describe its technical implementations, and highlight selected examples representative of the rapidly growing range of applications in physics, chemistry, biology, materials science, geology, and atmospheric and space sciences.

47 OTHER INSTRUMENTATION↗

Demonstration of the Wide-Field Imaging Interferometer Testbed Using a Calibrated Hyperspectral Image Projector

The Wide-field Imaging Interferometer testbed (WIIT) at NASA's Goddard Space Flight Center uses a dual-Michelson interferometric technique. The WIIT combines stellar interferometry with Fourier-transform interferometry to produce high-resolution spatial-spectral data over a large field-of-view. This combined technique could be employed on future NASA missions such as the Space Infrared Interferometric Telescope (SPIRIT) and the Sub-millimeter Probe of the Evolution of Cosmic Structure (SPECS). While both SPIRIT and SPECS would operate at far-infrared wavelengths, the WIIT demonstrates the dual-interferometry technique at visible wavelengths. The WIIT will produce hyperspectral image data, so a true hyperspectral object is necessary. A calibrated hyperspectral image projector (CHIP) has been constructed to provide such an object. The CHIP uses Digital Light Processing (DLP) technology to produce customized, spectrally-diverse scenes. CHIP scenes will have approximately 1.6-micron spatial resolution and the capability of . producing arbitrary spectra in the band between 380 nm and 1.6 microns, with approximately 5-nm spectral resolution. Each pixel in the scene can take on a unique spectrum. Spectral calibration is achieved with an onboard fiber-coupled spectrometer. In this paper we describe the operation of the CHIP. Results from the WIIT observations of CHIP scenes will also be presented.

Bolcar, Matthew R.↗

Infrared nanoimaging and nanospectroscopy of electrochemical energy storage materials and interfaces

Electrochemical interfaces are central to the function and performance of energy storage devices. Thus, the development of new methods to characterize these interfaces, in conjunction with electrochemical performance, is essential for bridging the existing knowledge gaps and accelerating the development of energy storage technologies. Of particular need is the ability to characterize surfaces or interfaces in a non-destructive way with adequate resolution to discern individual structural and chemical building blocks. To this end, sub-diffraction-limit low-energy infrared optical probes that exploit near-field interactions within atomic force microscopy platforms, such as pseudoheterodyne nanoimaging, photothermal nanoimaging and nanospectroscopy, and nanoscale Fourier transform infrared spectroscopy, are all powerful emerging techniques. These are capable of non-destructive surface probing and imaging at nanometer resolution. This review outlines recent efforts to characterize ex situ, in situ, and operando electrode materials and electrochemical interfaces in rechargeable batteries with these advanced infrared near-field probes.

25 ENERGY STORAGE↗

Spectroscopic features of dissolved iodine in pristine and gamma-irradiated nitric acid solutions

While iodine speciation is important for a wide range of nuclear activities, understanding the mechanisms of the transformations of iodine between chemical forms and the sensitivity of these transitions to solution conditions and exposure to radiation remains an active area of research. This work curates spectroscopic data from several experimental techniques and establishes their sensitivity and limitations in detecting changes in iodine speciation in both neutral and acidic regimes. The techniques include Raman spectroscopy, Fourier Transform Infrared (FTIR) spectroscopy, 127 I NMR spectroscopy, and ultraviolet-visible (UV-Vis) spectroscopy. Analysis of these data indicates that these commonly accessible spectroscopies often have dynamic ranges of measurable concentrations that do not always overlap between all techniques. The experimental techniques are disparately sensitive to iodide (I - ), molecular iodine (I 2 ), iodate (IO 3 - ), and periodate (IO 4 - ) species. Raman, FTIR, and NMR spectra were subsequentially analyzed using two-dimensional correlation analyses to generate high-resolution autocorrelation spectra. Here, the use of these spectroscopies is then extended to tracking acidification-induced and gamma irradiation-induced transformations of dissolved sodium iodate in deionized water and concentrated nitric acid. Both dissolution into nitric acid and irradiation with a gamma source are demonstrated to perturb the iodine speciation promoting their assembly into molecular iodine (I 2 ) and/or triiodide (I 3 - ). While I 2 and I 3 - species are undetectable with FTIR spectroscopy and 127 I NMR spectroscopy, the species can be detected with UV-Vis spectroscopy, and in some instances, I 3 - can be detected with Raman spectroscopy in the low wavenumber region. Ultimately, the results of this work provide a path to designing optimal combinations of techniques to detect forms of iodine across a wide range of concentrations and conditions.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

An Intercomparison Between Radar Reflectivity and the IR Cloud Classification Technique for the TOGA-COARE Area

Satellite infrared (IR) and visible (VIS) images from the Tropical Ocean Global Atmosphere - Coupled Ocean Atmosphere Response Experiment (TOGA-COARE) experiment are investigated through the use of Clustering Analysis. The clusters are obtained from the values of IR and VIS counts and the local variance for both channels. The clustering procedure is based on the standardized histogram of each variable obtained from 179 pairs of images. A new approach to classify high clouds using only IR and the clustering technique is proposed. This method allows the separation of the enhanced convection in two main classes: convective tops, more closely related to the most active core of the storm, and convective systems, which produce regions of merged, thick anvil clouds. The resulting classification of different portions of cloudiness is compared to the radar reflectivity field for intensive events. Convective Systems and Convective Tops are followed during their life cycle using the IR clustering method. The areal coverage of precipitation and features related to convective and stratiform rain is obtained from the radar for each stage of the evolving Mesoscale Convective Systems (MCS). In order to compare the IR clustering method with a simple threshold technique, two IR thresholds (Tir) were used to identify different portions of cloudiness, Tir=240K which roughly defines the extent of all cloudiness associated with the MCS, and Tir=220K which indicates the presence of deep convection. It is shown that the IR clustering technique can be used as a simple alternative to identify the actual portion of convective and stratiform rainfall.

Carvalho, L. M. V.↗

Spectroscopic pressure investigation of a novel high energy system

This work here combines a novel multimodal spectroscopic technique, O–PTIR and Raman spectroscopy, which allows for the simultaneous collection of infrared and Raman spectra, with traditional diamond anvil cell techniques to explore pressure induced phase transitions in a high energy material. Two phase transitions are revealed, with the first transition emerging below 0.23 GPa, to a higher order phase, followed by a broad transition to a lower order phase. Aside from the pressure studies, hyperspectral imaging was performed, confirming the homogeneous nature of the system.

36 MATERIALS SCIENCE↗

High resolution infrared spectroscopy from space: A preliminary report on the results of the Atmospheric Trace Molecule Spectroscopy (ATMOS) experiment on Spacelab 3

The ATMOS (Atmospheric Trace Molecule Spectroscopy) experiment has the broad purpose of investigating the physical structure, chemistry, and dynamics of the upper atmosphere through the study of the distributions of the neutral minor and trace constituents and their seasonal and long-term variations. The technique used is high-resolution infrared absorption spectroscopy using the Sun as the radiation source, observing the changes in the transmission of the atmosphere as the line-of-sight from the Sun to the spacecraft penetrates the atmosphere close to the Earth's limb at sunrise and sunset. During these periods, interferograms are generated at the rate of one each second which yield, when transformed, high resolution spectra covering the 2.2 to 16 micron region of the infrared. Twenty such occultations were recorded during the Spacelab 3 flight, which have produced concentration profiles for a large number of minor and trace upper atmospheric species in both the Northern and Southern Hemispheres. Several of these species have not previously been observed in spectroscopic data. The data reduction and analysis procedures used following the flight are discussed; a number of examples of the spectra obtained are shown, and a bar graph of the species detected thus far in the analysis is given which shows the altitude ranges for which concentration profiles were retrieved.

Farmer, Crofton B.↗

Thermal infrared remote sensing of crude oil slicks

Unambiguous detection of oil slicks by remote sensing techniques has proven an elusive goal. This article presents new thermal infrared spectra of oil slicks made from five different crude oil samples with a wide range of API gravities and compositions. After a brief outgassing phase, all oil slick spectra are quite similar and little affected by thickness, extended exposure to air or sunlight, and even by emulsification with seawater (mousse formation). Thus, oil slicks provide a remarkably unvarying spectral signature as remote sensing targets in the thermal infrared compared to other regions of the spectrum. This spectral signature in the 8-14 micron atmospheric window is flat, with an average reflectance of 4 percent. Seawater, on the other hand, has a spectrum that varies in reflectance with wavelength in the 8-14 micron window from 0.90 to 3.65 percent. In addition, we show that sea foam displays a reflectance spectrum quite similar to that of seawater in the 8-14 micron region. This results in a relatively uniform spectral background, against which oil slicks can be detected, based on their different spectral signature.

Salisbury, John W.↗

Thermal and Chemical Characterization of Non-Metallic Materials Using Coupled Thermogravimetric Analysis and Infrared Spectroscopy

Thermogravimetric analysis (TGA) is widely employed in the thermal characterization of non-metallic materials, yielding valuable information on decomposition characteristics of a sample over a wide temperature range. However, a potential wealth of chemical information is lost during the process, with the evolving gases generated during thermal decomposition escaping through the exhaust line. Fourier Transform-Infrared spectroscopy (FT-IR) is a powerful analytical technique for determining many chemical constituents while in any material state, in this application, the gas phase. By linking these two techniques, evolving gases generated during the TGA process are directed into an appropriately equipped infrared spectrometer for chemical speciation. Consequently, both thermal decomposition and chemical characterization of a material may be obtained in a single sample run. In practice, a heated transfer line is employed to connect the two instruments while a purge gas stream directs the evolving gases into the FT-IR. The purge gas can be either high purity air or an inert gas such as nitrogen to allow oxidative and pyrolytic processes to be examined, respectively. The FT-IR data is collected realtime, allowing continuous monitoring of chemical compositional changes over the course of thermal decomposition. Using this coupled technique, an array of diverse materials has been examined, including composites, plastics, rubber, fiberglass epoxy resins, polycarbonates, silicones, lubricants and fluorocarbon materials. The benefit of combining these two methodologies is of particular importance in the aerospace community, where newly developing materials have little available data with which to refer. By providing both thermal and chemical data simultaneously, a more definitive and comprehensive characterization of the material is possible. Additionally, this procedure has been found to be a viable screening technique for certain materials, with the generated data useful in the selection of other appropriate analytical procedures for further material characterization.

Huff, Timothy L.↗

Thermal and Chemical Characterization of Non-metallic Materials Using Coupled Thermogravimetric Analysis and Infrared Spectroscopy

Thermogravimetric analysis (TGA) is widely employed in the thermal characterization of non-metallic materials, yielding valuable information on decomposition characteristics of a sample over a wide temperature range. However, a potential wealth of chemical information is lost during the process, with the evolving gases generated during thermal decomposition escaping through the exhaust line. Fourier Transform-Infrared spectroscopy (FT-IR) is a powerful analytical technique for determining many chemical constituents while in any material state, in this application, the gas phase. By linking these two techniques, evolving gases generated during the TGA process are directed into an appropriately equipped infrared spectrometer for chemical speciation. Consequently, both thermal decomposition and chemical characterization of a material may be obtained in a single sample run. In practice, a heated transfer line is employed to connect the two instruments while a purge gas stream directs the evolving gases into the FT-IR, The purge gas can be either high purity air or an inert gas such as nitrogen to allow oxidative and pyrolytic processes to be examined, respectively. The FT-IR data is collected real-time, allowing continuous monitoring of chemical compositional changes over the course of thermal decomposition. Using this coupled technique, an array of diverse materials has been examined, including composites, plastics, rubber, fiberglass epoxy resins, polycarbonates, silicones, lubricants and fluorocarbon materials. The benefit of combining these two methodologies is of particular importance in the aerospace community, where newly developing materials have little available data with which to refer. By providing both thermal and chemical data simultaneously, a more definitive and comprehensive characterization of the material is possible. Additionally, this procedure has been found to be a viable screening technique for certain materials, with the generated data useful in the selection of other appropriate analytical procedures for further material characterization.

Huff, Timothy L.↗

In Situ Analysis of Laser Powder Bed Fusion Using Simultaneous High-Speed Infrared and X-ray Imaging

Laser powder bed fusion is a metal additive manufacturing technique that has received significant scientific and industrial attention over the past decades. However, the quality and reproducibility of parts manufactured by this technique is still a problem. Overcoming this issue requires an understanding of multiple complex physical phenomena which occur simultaneously during the process. Here, we illustrate a powerful new technique which synchronizes high-speed x-ray imaging with high-speed infrared imaging to study laser powder bed fusion processes in real time. Using this technique, we demonstrate the simultaneous observation of multiple phenomena including three-dimensional melt pool visualization, vapor plume dynamics, spatter formation, thermal history, and point cooling rates. The paired observation of these dynamic phenomena is critical to understanding the fundamentals of laser powder bed fusion, and the overall impact of process parameters on print quality.

36 MATERIALS SCIENCE↗

High resolution spectroscopy in the microwave and far infrared

High resolution rotational spectroscopy has long been central to remote sensing techniques in atmospheric sciences and astronomy. As such, laboratory measurements must supply the required data to make direct interpretation of data for instruments which sense atmospheres using rotational spectra. Spectral measurements in the microwave and far infrared regions are also very powerful tools when combined with infrared measurements for characterizing the rotational structure of vibrational spectra. In the past decade new techniques were developed which have pushed high resolution spectroscopy into the wavelength region between 25 micrometers and 2 mm. Techniques to be described include: (1) harmonic generation of microwave sources, (2) infrared laser difference frequency generation, (3) laser sideband generation, and (4) ultrahigh resolution interferometers.

Pickett, Herbert M.↗

Analytical Tools to Assess Polymer Biodegradation: A Critical Review and Recommendations

Many petroleum-derived plastic materials are highly recalcitrant and persistent in the environment, posing significant threats to human and ecological receptors due to their accumulation in ecosystems. In recent years, research efforts have focused on advancing biological methods for polymer degradation. Enzymatic depolymerization has emerged as particularly relevant for biobased plastic recycling, potentially scalable for industrial use. Biodegradation involves adsorption to the plastic solid surface, followed by an interfacial reaction, resulting in cleavage of bonds of polymer chains exposed on the surface. Here, widely varying substrate-specific kinetics are observed, with the polymer’s properties possessing a significant impact on the rate of this interfacial catalysis. Thus, there is a critical need for sensitive and accurate characterization of the material surface during and after interfacial depolymerization to fully understand the reaction mechanisms. Here, we provide a critical review of a range of techniques used in the analysis of material surfaces to characterize the chemical, topological, and morphological features relevant to the study of enzymatic biocatalysis, including microscopy techniques, spectroscopic techniques (e.g., X-ray diffraction analysis, Fourier transform infrared attenuated total reflectance spectroscopy, and mass spectrometry detection of analytes associated with degradation). Techniques for evaluation of surface energy and topology in their relevancy for sensitive detection of biological surface modifications are also discussed. In addition, this paper provides an overview of the strengths of these techniques and compares their performance in both sensitivity and throughput, including emerging techniques, which can be useful, particularly for the rapid analysis of the surface properties of polymeric materials in high-throughput screening of candidate biocatalysts. This research serves as a starting point in selecting and applying appropriate methodologies that provide direct evidence to the ongoing biotic degradation of polymeric materials.

Colachis, Matthew↗