G. Lawrence Carr

Imaging the Material Properties of Bone Specimens Using Reflection-Based Infrared Microspectroscopy

Fourier transform infrared microspectroscopy (FTIRM) is a widely used method for mapping the material properties of bone and other mineralized tissues, including mineralization, crystallinity, carbonate substitution, and collagen cross-linking. This technique is traditionally performed in a transmission-based geometry, which requires the preparation of plastic-embedded thin sections, limiting its functionality. Here, we theoretically and empirically demonstrate the development of reflection-based FTIRM as an alternative to the widely adopted transmission-based FTIRM, which reduces specimen preparation time and broadens the range of specimens that can be imaged. In this study, mature mouse femurs were plastic-embedded and longitudinal sections were cut at a thickness of 4 μm for transmission-based FTIRM measurements. The remaining bone blocks were polished for specular reflectance-based FTIRM measurements on regions immediately adjacent to the transmission sections. Kramers-Kronig analysis of the reflectance data yielded the dielectric response from which the absorption coefficients were directly determined. The reflectance-derived absorbance was validated empirically using the transmission spectra from the thin sections. The spectral assignments for mineralization, carbonate substitution, and collagen cross-linking were indistinguishable in transmission and reflection geometries, while the stoichiometric/nonstoichiometric apatite crystallinity parameter shifted from 1032/1021 cm(-1) in transmission-based to 1035/1025 cm(-1) in reflection-based data. This theoretical demonstration and empirical validation of reflection-based FTIRM eliminates the need for thin sections of bone and more readily facilitates direct correlations with other methods such as nanoindentation and quantitative backscatter electron imaging (qBSE) from the same specimen. It provides a unique framework for correlating bones material and mechanical properties.

Silicon beam splitter for far-infrared and terahertz spectroscopy

Silicon beam splitters several millimeters thick offer numerous advantages over thin freestanding dielectric beam splitters. For routine spectroscopy for which resolutions of better than 1 cm(-1) are not required, a silicon beam splitter can replace several Mylar beam splitters to span the entire far-infrared region. In addition to superior long-wavelength performance that extends well into the terahertz region, the silicon beam splitter has the additional advantage that its efficiency displays little polarization dependence.

Gemini Planet Imager Coronagraph Testbed Results

The Gemini Planet Imager (GPI) is an extreme AO coronagraphic integral field unit YJHK spectrograph destined for first light on the 8m Gemini South telescope in 2011. GPI fields a 1500 channel AO system feeding an apodized pupil Lyot coronagraph, and a nIR non-common-path slow wavefront sensor. It targets detection and characterizion of relatively young (<2GYr), self luminous planets up to 10 million times as faint as their primary star. We present the coronagraph subsystems in-lab performance, and describe the studies required to specify and fabricate the coronagraph. Coronagraphic pupil apodization is implemented with metallic half-tone screens on glass, and the focal plane occulters are deep reactive ion etched holes in optically polished silicon mirrors. Our JH testbed achieves H-band contrast below a million at separations above 5 resolution elements, without using an AO system. We present an overview of the coronagraphic masks and our testbed coronagraphic data. We also demonstrate the performance of an astrometric and photometric grid that enables coronagraphic astrometry relative to the primary star in every exposure, a proven technique that has yielded on-sky precision of the order of a milliarsecond.

Infrared microspectroscopy with synchrotron radiation

Infrared microspectroscopy with a high brightness synchrotron source can achieve a spatial resolution approaching the diffraction limit. However, in order to realize this intrinsic source brightness at the specimen location, some care must be taken in designing the optical system. Also, when operating in diffraction limited conditions, the effective spatial resolution is no longer controlled by the apertures typically used for a conventional (geometrically defined) measurement. Instead, the spatial resolution depends on the wavelength of light and the effective apertures of the microscopes Schwarzchild objectives. We have modeled the optical system from the synchrotron source up to the sample location and determined the diffraction-limited spatial distribution of light. Effects due to the dependence of the synchrotron sources numerical aperture on wavelength, as well as the difference between transmission and reflection measurement modes, are also addressed. Lastly, we examine the benefits (when using a high brightness source) of an extrinsic germanium photoconductive detector with cone optics as a replacement for the standard MCT detector.

Characterization of the new NSLS infrared microspectroscopy beamline U10B

The first of several new infrared beamlines, built on a modified bending magnet port of the NSLS VUV ring, is now operational for mid-infrared microspectroscopy. The port simultaneously delivers 40 mrad by 40 mrad to two separate beamlines and spectrometer endstations designated U10A and U10B. The latter is equipped with a scanning infrared microspectrometer. The combination of this instrument and high brightness synchrotron radiation makes diffraction- limited microspectroscopy practical. This paper describes the beamlines performance and presents quantitative information on the diffraction-limited resolution.

Two-color experiments combining the UV storage ring free-electron laser and the SA5 IR beamline at Super-ACO

The UV-storage ring Free Electron Laser (FEL) operating at Super-ACO is a tunable, coherent and intense (up to 300 mW) photon source in the near-UV range (300 - 350 nm). Besides, it has the unique feature to be synchronized in a one-to-one shot ratio with the Synchrotron Radiation (SR) at the high repetition rate of 8.32 MHz. This FEL + SR combination appears to be very powerful for the performance of pump- probe time-resolved and/or frequency-resolved experiments on the sub-ns and ns time-scales. In particular, there is a strong scientific case for the combination of the recently- commissioned SA5 Infra-Red Synchrotron Radiation beamline with the UV-FEL, for the performance of transient IR- absorption spectroscopy on FEL-excited samples with a Fourier-transform spectrometer coupled with a microscope allowing high spectral and spatial resolution. The principle and interest of the two-color combination altogether with the description of both the FEL and the SA5 IR beamline are presented. The first synchronization signal between the IR and the UV beams is shown. The correct spatial overlap between the UV (FEL) and the IR (SR) photon beams is demonstrated by monitoring via IR-spectro-microscopy the time evolution of a single mineral particulate (kaolinite) under UV-FEL irradiation.

Industrial applications of accelerator-based infrared sources Analysis using infrared microspectroscopy

Infrared Microspectroscopy, using a globar source, is now widely employed in the industrial environment, for the analysis of various materials. Since synchrotron radiation is a much brighter source, an enhancement of an order of magnitude in lateral resolution can be achieved. Thus, the combination of IR microspectroscopy, and synchrotron radiation provides a powerful tool enabling sample regions only few microns size to be studied. This opens up the potential for analyzing small particles. Some examples for hair, bitumen and polymer are presented.

Synchrotron infrared microspectroscopy as a means of studying the chemical composition of bone: Applications to osteoarthritis

Infrared microspectroscopy combines microscopy and spectroscopy for the purpose of chemical microanalysis. Light microscopy provides a way to generate and record magnified images and visibly resolve microstructural detail. Infrared spectroscopy provides a means for analyzing the chemical makeup of materials. Combining light microscopy and infrared spectroscopy permits the correlation of microstructure with chemical composition. Inherently, the long wavelengths of infrared radiation limit the spatial resolution of the technique. However, synchrotron infrared radiation significantly improves both the spectral and spatial resolution of an infrared microspectrometer, such that data can be obtained with high signal-to-noise at the diffraction limit, which is 3 - 5 micrometers in the mid-infrared region.

Synchrotron powered FT-IR microspectroscopy permits small spot ATR sampling of fiber finish and other materials

The absence of thermal noise, the nondivergence, and brightness of synchrotron radiation for FT-IR microspectroscopy permit aperturing the beam entering the ATR objective to less than the 100 μm diameter pattern usually used. With a ZnSe crystal, the 100 μm aperture produces a 42 μm spot of optical contact with the specimen. With synchrotron radiation, excellent S/N with smaller apertures permits spatially resolved probing of adjacent small spots along a specimen to reveal heterogeneity in the surface chemistry.

Technical Report: The Diversity of Infrared Programs at the NSLS

For about 20 years, synchrotron radiation (SR) has benefited the field of infrared (IR) spectroscopy in a wide range of disciplines from condensed matter physics to medicine. While a synchrotron infrared source does not typically produce more power than a conventional thermal (globar) source, its brightness (defined as the photon flux or power emitted per source area and solid angle) is 100–1000 times greater [1]. This advantage, arising from the small effective source size and narrow angular range of emission, has enabled a wide spectrum of throughput-limited experiments that were not possible with a conventional IR source.