Multipass capillary cell for enhanced Raman measurements of gases

A simple Raman multipass capillary cell (MCC) is described that gives 12- to 30-fold signal enhancements for non-absorbing gases. The cell is made by coating the inside of 2-mm inner diameter silica capillary tubes with silver. The device is very small and suitable for remote and in situ Raman measurements with optical fibers. Application of the MCC is similar to previously described liquid core waveguides but, unlike the latter devices, the MCC is generally more applicable to a wide range of non-absorbing gases.     

Microcalorimeter design for fast-neutron spectroscopy

We are developing microcalorimeters for fast-neutron spectroscopy. The goal is to develop a detector with an energy resolution of 0.1% for 1–20 MeV neutrons with an efficiency of 1%. We discuss the design of such a detector and present the first results of a transition edge sensor based microcalorimeter with a small TiB₂ absorber. The best energy resolution obtained was 5.5 keV FWHM for a total energy deposition of 2.792 MeV by thermal neutrons.     

Multipass acoustically open photoacoustic detector for trace gas measurements

What we believe to be a novel multipass, acoustically open photoacoustic detector designed for fast-response, high-sensitivity detection of trace gases and pollutants in the atmosphere is demonstrated. The acoustic pulses generated by the absorption of the light pulses of a tunable optical parametric oscillator by target molecules are detected by an ultrasonic sensor at 40 kHz. The photoacoustic signal is enhanced by an optical multipass arrangement and by concentration of the acoustic energy to the surface of the ultrasonic sensor. The detection sensitivity, estimated from CO2 measurements around a 2 microm wavelength, is approximately 3.3 x 10(-9) W cm(-1).     

Multiple-fiber probe design for fluorescence spectroscopy in tissue

The fiber-optic probe is an essential component of many quantitative fluorescence spectroscopy systems, enabling delivery of excitation light and collection of remitted fluorescence in a wide variety of clinical and laboratory situations. However, there is little information available on the role of illumination--collection geometry to guide the design of these components. Therefore we used a Monte Carlo model to investigate the effect of multifiber probe design parameters--numerical aperture, fiber diameter, source--collection fiber separation distance, and fiber-tissue spacer thickness--on light propagation and the origin of detected fluorescence. An excitation wavelength of 400 nm and an emission wavelength of 630 nm were simulated. Noteworthy effects included an increase in axial selectivity with decreasing fiber size and a transition with increasing fiber-tissue spacer size from a subsurface peak in fluorophore sensitivity to a nearly monotonic decrease typical of single-fiber probes. We provide theoretical evidence that probe design strongly affects tissue interrogation. Therefore application-specific customization of probe design may lead to improvements in the efficacy of fluorescence-based diagnostic devices.     

Top notch design for fiber-loop cavity ring-down spectroscopy

Fiber-loop cavity ring-down spectroscopy (CRDS) is a highly sensitive spectroscopic absorption technique which has shown considerable promise for the analysis of small-volume liquid samples. We have developed a new light coupling method for fiber-loop CRDS, which overcomes two disadvantages of the technique: low efficiency light coupling into the cavity and high loss per pass. The coupler is based on a 45° reflective notch polished between 10 and 30 μm into the core of a large-core-diameter (365 μm) optical fiber, and allows for nearly 100% light coupling into the cavity, with a low loss per pass (<4%). The coupler has the additional advantage that the input and output light is spatially separated on opposite sides of the fiber. The detection sensitivity of a fiber-loop CRD spectrometer employing the new coupling method is established from ring-down measurements on aqueous rhodamine 6G (Rh6G) at 532 nm. The results are compared with data obtained using the same light source and detector, but a conventional bend-coupled small-core-diameter (50 μm) optical fiber loop. With our new coupler, a detection limit of 0.11 cm(-1) is found, which corresponds to detection of 0.93 μM Rh6G in a volume of only 19 nL. This is an improvement of over an order of magnitude on our bend-coupled small-core optical fiber results, in which a detection limit of 5.3 cm(-1) was found, corresponding to a detection of 43 μM Rh6G in a volume of 20 pL.     

Multipass optical absorption spectroscopy: a fast-scanning laser spectrometer for the in situ determination of atmospheric trace-gas components, in particular OH

The optical design of an absorption spectrometer for in situ measurements of atmospheric trace gases is reported. The light source is a rapidly tuned and power-stabilized dye-ring laser, which is frequency doubled by an intracavity BBO crystal. The second harmonic and the fundamental are used simultaneously for measurement of OH, SO(2), CH(2)O, and naphthalene in the UV and of NO(2) in the visible. The 1.2-km absorption path is folded within a 6-m White-cell-type multiple-reflection system with an open-path setup. The absorption sensitivity of the spectrometer is better than 1 part in 10(-5) under tropospheric conditions (integration time 1 min., signal-to-noise ratio 1).     

Multipass System with Large Relative Aperture

Abstract

A six-pass system is proposed aimed at the problems of the high-temperature spectroscopy. As compared to the classical White system, the design under consideration provides twice increased relative aperture at the same transversal size of the cell and uses simple cylindric tubes instead of cells of more complicated shape. The proposed design is the unique multipass system with compensated astigmatism. The system could be recommended for gas analytical device of moderate sensitivity and also for the cells with the fixed path length in the various i.r. spectrometers in particular, in the Fourier-spectrometers.     

Multipass annular mirror system for spectroscopic studies in shock tubes

Abstract

A fundamentally new multipass reflecting mirror system for studies in shock tubes is designed. Conducting optical absorption measurements in shock tubes when modelling processes of controlled combustion is necessary. The results of these optical studies facilitate working out recommendations on efficient and non-polluting burning of natural fuels in industry. The basic component of the suggested multipass optical system is an annular reflector in the form of a spherical concave belt joined as a separate section to the shock tube. Radiation from a source directed inwards the annular reflector traverses the tube section many times reflecting from the mirror surface which thereby increases the thickness of the absorbing layer. Because of the absence of bulging edges inside the reflector, no perturbations appear in the flow. The system design allows simple control of the optical path length. Equations relating the angular aperture of an incident beam to the chosen parameters of the annular reflector are reported. A formula for the number of beam passes as a function of the incidence angle of the beam entering the reflector is derived.     

High-luminosity multipass cell for infrared imaging spectroscopy

An original imaging multipass cell for infrared spectroscopy has been designed and built. The cell design is aimed at overcoming intrinsic sensitivity limitations associated with the low specific spectral radiance power of blackbody sources. Owing to the implemented low f number, the detector collects a large amount of the energy emitted over a wide angle by a blackbody source. In addition, the adopted optical configuration allows maintenance of the same spatial distribution of the radiance pattern at the cell entrance and exit (imaging capability) within an aperture area of several square millimeters. This feature allows the use of uncollimated blackbody-type emitter arrays and infrared sensor arrays coupled with linear, spectrally variable filters, and performance of spectroscopic measurements of infrared absorption for low concentrated gases detection. In the present design the cell has an f number of about 2, and the optical path is ten times larger than the cell length.     

Multipass cold drawing of magnesium alloy minitubes for biodegradable vascular stents

Magnesium alloys possess highly limited room-temperature formabilities. This presents a technological barrier to the fabrication of minitubes for biodegradable vascular stents. The research was aimed at developing precision forming technology to fabricate ZM21 magnesium alloy minitubes with a refined microstructure. A multipass cold drawing process with a moving mandrel was successfully developed to convert seamless hollow billets through five passes of cold drawing and an interpass annealing treatment into minitubes with an outside diameter of 2.9 mm and a wall thickness of 0.217 mm, ready for laser cutting into vascular stents. It was found that a cumulative reduction in cross-section area as much as 32% could be applied to the material without causing fracture. However, a further reduction in cross-section area required annealing at 300 °C for 1 h to change a twinned microstructure into a recrystallized grain structure and to regain formability. The interpass annealing treatment after the fourth pass led to a reduction in drawing force by 22%, in comparison with the drawing force at the fourth pass of drawing. The variations in the outside diameter and wall thickness of the minitubes could be kept within 5 and 12 μm, respectively. Further research is directed toward improvements in dimensional precisions.     

Multipass open-path Fourier-transform infrared measurements for nonintrusive monitoring of gas turbine exhaust composition

The detection limits for NO and NO2 in turbine exhausts by nonintrusive monitoring have to be improved. Multipass mode Fourier-transform infrared (FTIR) absorption spectrometry and use of a White mirror system were found from a sensitivity study with spectra simulations in the mid-infrared to be essential for the retrieval of NO2 abundances. A new White mirror system with a parallel infrared beam was developed and tested successfully with a commercial FTIR spectrometer in different turbine test beds. The minimum detection limits for a typical turbine plume of 50 cm in diameter are approximately 6 parts per million (ppm) for NO and 9 ppm for NO2 (as well 100 ppm for CO2 and 4 ppm for CO).     

Rational design of fiber-optic probes for visible and pulsed-ultraviolet resonance Raman spectroscopy

We investigated the performance of fiber-optic resonance Raman probes with a series of experiments to determine the working curves of such probes using model analytes and to investigate the effects of absorbing media. A computer model designed to simulate these experiments is presented, and numerical results are found to be in agreement with the experimental data. Design considerations resulting from these studies are discussed, and novel designs for overcoming problems of coupling efficiency, damage threshold, and sensitivity in absorbing samples are presented. These findings are applied to the design of fiber-optic probes for ultraviolet resonance Raman spectroscopy involving nanosecond pulsed-ultraviolet excitation (225 and 266 nm). These probes have been used to collect what is, to our knowledge, the first reported fiber-optic-linked ultraviolet resonance Raman spectra of tryptophan and DNA.     

On the design of time-focused detector banks for pulsed neutron TOF spectroscopy

A study of the effects on the detected peak shapes of uncertainties in geometrical parameters is performed for time-focused detector banks used in neutron TOF spectroscopy. It is shown that it is convenient to put the detectors close to the sample with their axis on the scattering plane instead of perpendicular to it. A detector bank setting is proposed.     

Micro-Raman spectroscopy for optical pathology of oral squamous cell carcinoma

Micro-Raman spectra of formalin-fixed oral squamous normal and carcinoma tissues, stored at room temperature for 2 months, have been recorded. Spectra were recorded both in the epithelial and subepithelial regions of the tissues. No noticeable spectral contamination due to formalin was observed. Very significant differences between spectra of normal epithelial and malignant epithelial samples were found. No such differences in spectra of subepithelial malignant and subepithelial normal samples could be observed. This study shows that spectra from the epithelial region changes drastically because of malignancy-induced biochemical changes in this region. Major differences between normal and malignant spectra seem to arise from the protein composition, conformational/structural changes, and possible increase in protein content in malignant epithelia. The differences between normal epithelial and subepithelial spectra, as expected, arise mainly from the collagen in subepithelial tissue. Principal component analysis of the combined sets of spectra-epithelial and subepithelial, normal and malignant- showed that very good discrimination can be achieved by Raman microspectroscopy. This study thus validates the suitability of formalin-fixed tissues for optical pathology in oral malignancy.     

High-temperature and high-pressure cubic zirconia anvil cell for Raman spectroscopy

A simple and inexpensive cubic zirconia anvil cell has been developed for the performance of in situ Raman spectroscopy up to the conditions of 500 degrees C and 30 kbar pressure. The design and construction of this cell are fully described, as well as its applications for Raman spectroscopy. Molybdenum heater wires wrapped around ceramic tubes encircling two cubic zirconia anvils are used to heat samples, and the temperatures are measured and controlled by a Pt-PtRh thermocouple adhered near the sample chamber and an intelligent digital control apparatus. With this cell, Raman spectroscopic measurements have been satisfactorily performed on water at 6000 bar pressure to 455 degrees C and on ice of room temperature to 24 kbar, in which the determinations of pressures make use of changes of the A1 Raman modes of quartz and the shift of the sharpline (R-line) luminescence of ruby, respectively.     

Graphene oxide windows for in situ environmental cell photoelectron spectroscopy

The performance of new materials and devices often depends on processes taking place at the interface between an active solid element and the environment (such as air, water or other fluids). Understanding and controlling such interfacial processes require surface-specific spectroscopic information acquired under real-world operating conditions, which can be challenging because standard approaches such as X-ray photoelectron spectroscopy generally require high-vacuum conditions. The state-of-the-art approach to this problem relies on unique and expensive apparatus including electron analysers coupled with sophisticated differentially pumped lenses. Here, we develop a simple environmental cell with graphene oxide windows that are transparent to low-energy electrons (down to 400 eV), and demonstrate the feasibility of X-ray photoelectron spectroscopy measurements on model samples such as gold nanoparticles and aqueous salt solution placed on the back side of a window. These proof-of-principle results show the potential of using graphene oxide, graphene and other emerging ultrathin membrane windows for the fabrication of low-cost, single-use environmental cells compatible with commercial X-ray and Auger microprobes as well as scanning or transmission electron microscopes.     

Cell design for picosecond time-resolved infrared spectroscopy in high-pressure liquids and supercritical fluids

The design of a new high-pressure infrared (IR) cell for carrying out picosecond time-resolved infrared (ps-TRIR) spectroscopy in supercritical fluids is described. We have employed thin (2 mm) MgF(2) windows in order to overcome possible undesirable nonlinear optical effects caused by the extremely high peak powers of ultrashort ultraviolet (UV)/visible pulses. The design of our cell allows for the study of systems at pressures of up to 5500 psi at temperatures of up to approximately 50 degrees C. The MgF(2) windows enable the excitation of samples with both UV and visible light pulses and these windows are transparent across much of the mid-infrared region. We have demonstrated the use of this cell by examining the photochemistry of Fe(CO)(5) in supercritical Kr (sc Kr).     

Multipass grating interferometer applied to line narrowing in excimer lasers

The line narrowing of excimer lasers is discussed. The theory for an optical two-effect intracavity line narrowing device, the multipass grating interferometer (MGI), is presented. An MGI contains a grating aligned in its second-order Littrow configuration and a mirror aligned parallel to the grating surface reflecting back the beam normal to the grating corresponding to the first-order diffraction. The Littrow grating is doing the coarse line narrowing, and the mirror aligned parallel to the grating has similar line narrowing properties as tilted intracavity Fabry-Perot etalons. An MGI is applied to a KrF laser cavity to achieve a linewidth of 0.03 cm(-1).     

Multipass Amplification Using Optical Phase Conjugation by Stimulated Brillouin Scattering

Abstract

We built up a multipass amplifier for multiplication of infrared nanosecond pulses based on stimulated Brillouin scattering in acetone. Starting with a Q-switched Nd-doped yttrium aluminium garnet oscillator emitting pulses with less than 5 ns duration, we were able to generate a train of up to five pulses with a pulse shortening. Because only phase-conjugating mirrors have been used, we expect the pulses to have a high transverse homogeneity.