Backscatter Mode Research Articles

Temporal and Spatial Resolution in Transmission Raman Spectroscopy

Picosecond time-resolved transmission Raman data were acquired for 1 mm thick powder samples of trans-stilbene, and a Monte Carlo model was developed that can successfully model the laser and Raman pulse profiles. Photon migration broadened the incident (approximately 1 ps) probe pulse by two orders of magnitude. As expected from previous studies of Raman photon migration in backscattering mode, the transmitted Raman pulse was broader than the transmitted laser pulse and took longer to propagate through the sample. The late-arriving photons followed tortuous flight paths in excess of 50 mm on traversing the 1 mm sample. The Monte Carlo code was also used to study the spatial resolution (lateral and depth) of steady-state transmission Raman spectroscopy in the diffusion regime by examining the distribution of Raman generation positions as a function of incident beam size, sample thickness, and transport length. It was predicted that the lateral resolution should worsen linearly with sample thickness (typically the resolution was about 50% of the sample thickness), and this is an inevitable consequence of operating in the diffusion regime. The lateral resolution was better at the sample surface (essentially determined by the probe beam diameter or the collection aperture) than for buried objects, but transmission sampling was shown to be biased towards the mid-point of thick samples. Time-resolved transmission experiments should improve the lateral resolution by preferentially detecting snake photons, subject to constraints of signal-to-noise ratio.

Transmission Raman spectroscopy as a tool for quantifying polymorphic content of pharmaceutical formulations

We present the first quantitative study of polymorphic content in a model pharmaceutical formulation using transmission Raman spectroscopy (TRS), and compare the results obtained with those from traditional backscattering geometry. The transmission method is shown to provide a true bulk measurement of the composition, being unaffected by systematic or stochastic sub-sampling issues that can plague traditional backscattering geometries. The accuracy of the quantification of the polymorphs using TRS was shown to surpass considerably that achieved using conventional backscattering mode. For a model-free fit, the TRS method yielded R(2) of 0.996 compared to the backscattering value of 0.802; for a partial least squares fit with a single component the TRS method accounted for 98.09% of the variance in the data and yielded an R(2) of 0.985, compared to 89.65% of the variance and R(2) of 0.804 for the backscattering method.

Mössbauer spectroscopy characterization of automotive brake disc and polymer matrix composite (PMC) pad surfaces

In the last few years tribology researchers have attempted to characterize the braking film (third body) formed dynamically between disc and pad during frictional load. In automotive braking systems this friction layer is formed by the wear of two complex matrices and several analytical techniques are necessary for a comprehensive characterization. In this work Mössbauer Spectroscopy (MS) in transmission and backscattering modes, and X-ray Diffraction (XRD) were used to investigate the contact surfaces of polymer matrix composite (PMC) pads and cast iron discs, after they were tested in an Inertia Dynamometer Test Procedure (SAE J2784). Iron containing phases on the surfaces of disc and pad were identified, revealing the formation of magnetite and significant amounts of pyrite.

Nanoscale optical tomography using volume-scanning near-field microscopy

The relationship between sample structure and data in volume-scanning backscattering mode near-field optical microscopy is investigated. It is shown that the three-dimensional structure of a dielectric sample is encoded in the phase and amplitude of the scattered field and that an approximate reconstruction of the sample structure may be obtained.

In vitro degradation of resin–dentin bonds with one‐bottle self‐etching adhesives

The purpose of this study was to evaluate the durability of one-bottle self-etching adhesive during long-term water-storage testing. Resin-dentin bonded specimens were prepared using four commercially available one-bottle self-etching adhesives. The specimens were sectioned perpendicular to the adhesive interface to produce beam-shaped specimens that were stored in water for 24 h (control group) and 100, 200, and 300 d (experimental groups). After each storage period, the beams were subjected to a microtensile bond test. After the bond test, fractured surfaces were examined using a scanning electron microscope. In addition, interfacial observations of the silver tracer were performed using the secondary and back-scatter modes of the scanning electron microscope. The bond strength of all tested adhesives decreased significantly after 100 or more days in water. The interfacial observations showed an oxygen-inhibition zone as electron lucent in the adhesive-composite border in control specimens, displaying silver impregnation with breakage after aging. The deterioration of the oxygen-inhibition zone in the adhesive-resin composite junction resulted in a decrease in bond strength after 100 d in water for one-bottle self-etching adhesives.

Microstructural and surface characterization of thin gold films on n-Ge (111)

Abstract Thin gold films were fabricated by vacuum resistive deposition on the n-Ge (1 1 1) wafers. The films were annealed between 300 and 600 °C. These resulting thin films were then characterised using scanning electron microscopy (field emission and back-scattering modes), Rutherford back scattering spectroscopy and time of flight secondary ion mass spectroscopy (TOF-SIMS). For temperatures below the eutectic temperature the distribution of both the gold and the germanium on the surface are uniform. Above the eutectic temperature, the formation of gold rich islands on the surface of the Germanium were observed. These changes in the microstructure were found to correspond to changes in the electrical characteristics of the diodes.

Exfoliative epitheliopathy of bullous keratopathy with breaches in the MUC16 Glycocalyx.

Expression of cellular adhesion molecules is altered in bullous keratopathy. The hypothesis that epithelial alterations in bullous keratopathy compromise the surface of the cornea and its glycocalyx was tested. Studies were performed on eight cases each of pseudophakic bullous keratopathy and healthy corneas. The number of epithelial cell layers was determined with a stereological method of point counting. The minimum distance between points was established by estimates of cell size with variable pressure scanning electron microscopy performed in backscatter mode. The mean number of cell layers with mucin expression was identified by immunohistochemistry with mouse monoclonal antibodies for MUC1 and MUC16. Data were analyzed by Student's t-test if values showed a normal distribution or, alternatively, by the Wilcoxon rank-sum test. Mean numbers of wing cell and superficial cell layers were lower in bullous keratopathy specimens (1.6 vs. 2.0; P < 0.0001) than in controls (1.1 vs. 1.8; P < 0.000001). The number of exfoliated cell layers evident in sections was increased in the bullous keratopathy specimens compared with controls (0.36 vs. 0.03; P < 0.0001). The number of cell layers decorated with antibodies to MUC16 was lower in bullous keratopathy specimens than in controls (0.5 vs. 1.2; P < 0.025). The reduction of layers expressing MUC1 in bullous keratopathy was not statistically significant. Pseudophakic bullous keratopathy manifests an abnormal corneal ocular surface in which superficial cell layers are exfoliated, leaving breaches in the protective MUC16 glycocalyx. The results provide a morphologic correlate for the surface epithelial abnormalities noted clinically in these patients.

Depth range of primary electrons, electron beam broadening, and spatial resolution in electron-beam studies

A comparative analysis of the electron range in solids as a function of the initial electron energy (in the range 1–50 keV) and parameters of matter is performed. A relationship between the full length range of electrons and the depth of their penetration into the target material is established using simple empirical relations. The broadening of an electron beam upon its penetration into a material is considered and the spatial resolution of electron-beam instruments (in particular, in the backscattering mode) is determined.

Effects of ethylenediaminetetraacetic, etidronic and peracetic acid irrigation on human root dentine and the smear layer

To evaluate the effects of ethylenediaminetetraacetic (EDTA), etidronic (EA) and peracetic acid (PA) when used in conjunction with sodium hypochlorite (NaOCl) as root canal irrigants on calcium eluted from canals, smear layer, and root dentine demineralization after instrumentation/irrigation. Single-rooted human premolars were irrigated as follows (n = 12 per group): (1) 1% NaOCl during instrumentation, deionized water after instrumentation, (2) 1% NaOCl during, 17% EDTA after instrumentation, (3) a 1 : 1-mixture of 2% NaOCl and 18% EA during and after instrumentation, and (4) 1% NaOCl during, 2.25% PA after instrumentation. Irrigant volumes and contact times were 10 mL/15 min during and 5 mL/3 min after instrumentation. The evaluated outcomes were eluted calcium by atomic absorption spectroscopy, smear-covered areas by scanning electron microscopy in secondary electron mode and apparent canal wall decalcifications on root transsections in backscatter mode. For the smear layer analysis, sclerotic dentine was taken into consideration. Results were compared using appropriate parametric and nonparametric tests, alpha = 0.05. The statistical comparison of the protocols regarding calcium elution revealed that protocol (1) yielded less calcium than (3), which yielded less than protocols (2) and (4). Most of the instrumented canal walls treated with one of the decalcifying agents were free of smear layer. Protocols (1) and (3) caused no decalcification of root dentine, whilst (2) and (4) showed substance typical demineralization patterns. The decalcifying agents under investigation were all able to remove or prevent a smear layer. However, they eroded the dentine wall differently.

Classification of fixed urological cells using Raman tweezers

In this paper we report on preliminary investigations into using Raman tweezers to classify urological cell lines. This builds on earlier work within the group, whereby Raman tweezer methodologies were developed, and the application of this technique to differentiate between live prostate cancer (CaP) and bladder cells lines (PC-3 and MGH-U1 respectively) was demonstrated.In this present study we analysed chemically fixed cells using two different fixative methods; SurePath (a commercial available liquid based cytology media) and 4% v/v formalin/PBS fixatives. The study has been expanded from our previous live cell study to include the androgen sensitive CaP cell line LNCaP, primary benign prostate hyperplasia (BPH) cells as well as primary urethral cells. Raman light from the cells was collected using a 514.5 nm Ar-ion laser excitation source in back-scattering configuration mode.Principal component-linear discriminate analysis (PC-LDA) models of resulting cell spectra were generated and these were validated using a blind comparison. Sensitivities and specificities of > 72% and 90% respectively, for SurePath fixed cells, and > 93% and 98% respectively for 4% v/v formalin/PBS fixed cells was achieved. The higher prediction results for the formalin fixed cells can be attributed to a better signal-to-noise ratio for spectra obtained from these cells.Following on from this work, urological cell lines were exposed to urine for up to 12 hours to determine the effect of urine on the ability to classify these cells. Results indicate that urine has no detrimental effect on prediction results.

Relationships of Bone Density with Quantitative Ultrasound Parameter in Bovine Cancellous Bone

The present study aims to investigate the relationships of bone density with quantitative ultrasound (QUS) parameters measured in transmission and backscatter modes in bovine cancellous bone. The speed of sound (SOS), the normalized broadband ultrasound attenuation (nBUA), the broadband ultrasound backscatter (BUB) and the integrated re ection coe cient (IRC) were measured for 35 specimens obtained from proximal ends of seven bovine tibiae. The highest correlation coe cient was observed for SOS (r = 0.75, p < 0.001). Similarly, nBUA was signi cantly correlated with density (r = 0.71, p < 0.001). In contrast, BUB and IRC were less correlated with density than transmission QUS parameters, but still signi cantly (r = 0.63 and 0.65, respectively, all p < 0.01). A multiple regression analysis was used to nd optimal models for the prediction of apparent bone density by using linear combinations of SOS, nBUA, BUB and IRC, with density as an independent variable and 2, 3 and 4 QUS parameters as dependent variables (r = 0.77 0.88, all p < 0.001). The results suggest that the analysis of multiple QUS parameters can contribute to improving the e cacy of QUS procedures in the diagnosis of osteoporosis beyond the established value of SOS and nBUA.

High-frequency wave propagation in suspensions of elastic particles: Experimental validation of a time domain numerical simulation.

Sound propagation in suspensions of elastic particles immersed in a fluid is a difficult problem due to (i) the random distribution of the particles and (ii) possible multiple scattering and mode conversion effects. The ultrasonic propagation in suspensions has mostly been studied in the frequency domain and time domain approaches may also be of interest. Here, two‐dimensional finite difference time domain numerical simulations of ultrasonic propagation in suspensions of polystyrene 6‐μm‐diameter microspheres immersed in water were performed around 50 MHz. The numerical results were compared with the Faran analytical model, leading to a maximum difference of 15%, which constitutes a validation of the numerical approach. Experiments were carried out in transmission and backscattering modes. The attenuation coefficient 50 MHz [α(50)], the ultrasonic velocity (V) and the relative backscattered intensity (IB) were measured for different concentrations (from 2 to 25 mg/ml). Each experimental ultrasonic paramet...

Picosecond Raman spectroscopy with a fast intensified CCD camera for depth analysis of diffusely scattering media

A spectroscopic depth profiling approach is demonstrated for layers of non-transparent, diffusely scattering materials. The technique is based on the temporal discrimination between Raman photons emitted from the surface and Raman photons originating from a deeper layer. Excitation was carried out with a frequency-doubled, 3 ps Ti:sapphire laser system (398 nm; 76 MHz repetition rate). Time-resolved detection was carried out with an intensified CCD camera that can be gated with a 250 ps gate width. The performance of the system was assessed using 1 mm and 2 mm pathlength cuvettes with powdered PMMA and trans-stilbene (TS) crystals, respectively, or solid white polymer blocks: Arnite (polyethylene terephthalate), Delrin (polyoxymethylene), polythene (polyethylene) and Teflon (polytetrafluoroethylene). These samples were pressed together in different configurations and Raman photons were collected in backscatter mode in order to study the time difference in such media corresponding with several mm of extra net photon migration distance. We also studied the lateral contrast between two different second layers. The results demonstrate that by means of a picosecond laser system and the time discrimination of a gated intensified CCD camera, molecular spectroscopic information can be obtained through a turbid surface layer. In the case of the PMMA/TS two-layer system, time-resolved detection with a 400 ps delay improved the relative intensity of the Raman bands of the second layer with a factor of 124 in comparison with the spectrum recorded with a 100 ps delay (which is more selective for the first layer) and with a factor of 14 in comparison with a non-gated setup. Possible applications will be discussed, as well as advantages/disadvantages over other Raman techniques for diffusely scattering media.

Interest of the attenuation coefficient in multiparametric high frequency ultrasound investigation of whole blood coagulation process

Previous studies [R. Libgot, F. Ossant, Y. Gruel, P. Lermusiaux, and F. Patat, Proc.-IEEE Utrason. Symp. 4, 2259-2262 (2005); R. Libgot-Calle, F. Ossant, Y. Gruel, P. Lermusiaux, and F. Patat, Ultrasound Med. Biol. 34, 252-264 (2008); F. Ossant, R. Libgot, P. Coupe, P. Lermusiaux, and F. Patat, Proc.-IEEE Ultrason. Symp. 2, 846-849 (2004)] showed the potential of an in vitro high frequency ultrasound (beyond 20 MHz) device to describe the blood clotting process. The parameters were simultaneously estimated in double transmission (DT) with the calculation of the velocity of longitudinal waves and in backscattering (BS) modes with the estimation of the integrated BS coefficient and the effective scatterer size. The aim of the present study was to show how the integrated attenuation coefficient (IAC) assessed in DT mode could provide additional information on this process, especially regarding the fibrin polymerization which is an important part of the coagulation process. A characteristic time t(a) of the variations in IAC that could be linked to fibrin formation was identified.

Equatorial Spread F structures and associated airglow intensity variations observed over Gadanki

Abstract. Co-ordinated campaigns have been conducted from Gadanki (13.5° N, 79.2° E, dip lat 6.4° N) by operating simultaneously the Indian MST radar in ionospheric coherent backscatter mode and by monitoring thermosphere airglow line emissions (630.0 nm and 777.4 nm) using a narrow band multi-wavelength scanning photometer during January-March for the past five years (2003–2007) and also during April 2006, as a special campaign. Simultaneous radar and optical observations reveal optical signatures corresponding to a variety of equatorial spread F (ESF) structures. The optical signatures corresponding to ESF structures with wave-like bottomside modulations with plasma plumes, confined bottomside flat and wavelike structures, vertically extended plume structure in the absence of bottomside structure apart from the classical plasma depletions and enhancements are obtained during these campaigns. The plasma depletions and enhancements were identified using optical measurements. In addition, estimations of zonal wavelength of the bottomside structures and the inference of shears in the zonal plasma drift in the presence of confined structures, were carried out using bi-directional airglow measurements. Furthermore, it is found that the vertical columnar intensity of OI 630.0 nm airglow exceeded the slanted columnar intensity in the presence of large bottomside structure. The need for the appropriate physical mechanisms for some of the ESF structures and their characterizations with optical observations are discussed.

Tin dispersed in an oxide matrix as negative electrode material for Li-ion batteries

This paper deals with new tin-based composite β-Sn/(CaSiO 3) 0.4 negative electrode materials for Li-ion batteries. The nature of the oxide matrix and of dispersed tin particles has been investigated by X-ray diffraction (XRD), scanning electron microscope (SEM) coupled with energy dispersion spectroscopy (EDS) and Mössbauer spectroscopy by both transmission (TMS) and backscattering (CEMS) mode for bulk and interface characterizations. The electrochemical behaviour of the composite has been studied during Li-reaction processes. Electrochemical investigation and Mössbauer data analyses suggest the formation of Li 7Sn 2 during Li reaction. The reversible mechanism is based on cycling between β-Sn and Li 7Sn 2. An interface composed of CaSn IVSiO 5 and a Sn II species between tin particles dispersed in the CaSiO 3 matrix is responsible of the irreversible capacity observed in this composite during the first discharge.

A high-temperature furnace forin situsynchrotron X-ray spectroscopy under controlled atmospheric conditions

A high-temperature furnace with an induction heater coil has been designed and constructed for in situ X-ray spectroscopic experiments under controlled atmospheric conditions and temperatures up to 3275 K. The multi-purpose chamber design allows working in backscattering and normal fluorescence mode for synchrotron X-ray absorption and emission spectroscopy. The use of the furnace is demonstrated in a study of the in situ formation of Cr oxide between 1823 K and 2023 K at logPO(2) values between -10.0 and -11.3 using X-ray absorption near-edge spectroscopy. The set-up is of particular interest for studying liquid metals, alloys and other electrically conductive materials under extreme conditions.

Nondestructive Spectrometric Study on a Radioactive Particle Embedded in a Marine Sediment

A radioactive particle embedded in a sediment collected from the Irish Sea was examined with spectrometric methods to understand the potential bioavailability of its constituents. Images of the particle surface were acquired in the backscattering mode by scanning electron microscopy. The elemental composition of the particle surface layer was measured using energy dispersive (SEM-EDX) and wavelength dispersive (SEM-WDX) X-ray spectrometers. The investigation showed that the sample consists of a calcite matrix in which uranium is present in the form of separate inclusions. The diameter of U inclusions was less than 10 μm. Synchrotron radiation based X-ray fluorescence in confocal geometry (confocal μ-XRF) was used to determine the spatial distribution of elements in the particle. Three-dimensional reconstructions of the Ca, Cr, Mn, Fe, Zn, Sr, Ba, Pb, and U distributions were performed. The oxidation state of uranium in the different inclusions was determined by synchrotron radiation based X-ray absorption in confocal geometry (confocal μ-XANES). The isotopic composition of uranium was measured by secondary ion mass spectrometry. The results revealed that uranium was depleted in 235U. Pu and other actinides were not detected.

AFM Study of the Corrosion of Pipeline Steel in Organic Compounds Extracted from Soil

Aiming to simulate the external corrosion of pipelines, the first stages of the inclusion attack and nucleation of pits were studied by AFM on the API 5LX56 steel in pure 10mM Na2SO4 solution and with additions of HA or FA, both extracted from a Brazilian peat soil. For this, selected inclusions were first marked with micro indentations, viewed in the SEM in the backscattering mode and chemically mapped with EDS. Pit formation was then investigated by scanning Kelvin probe force microscopy (SKPFM). The SKPFM evidenced that HA added to sulfate solutions promotes the fast dissolution of the sulfides of complex inclusions, resulting in pit nucleation, while FA additions slow this attack, acting as a natural corrosion inhibitor.

Mineral phases and element composition of the copper hyperaccumulator lichen Lecanora polytropa

AbstractMineral phases and element localization were investigated in the vivid turquoise-coloured lichen, Lecanora polytropa, sampled from a psammite boulder in a wall supporting mine spoil at the abandoned copper mine, Riddarhyttan Kopparverke, southern Sweden. Normally pale yellowish (usnic acid), the lichen is turquoise coloured internally with bluish inclusions. X-ray mapping shows that Cu occurs on and within the lichen and does not coincide with P or S, suggesting that it is indeed associated with carbon or other elements not detected (or reported) using X-ray mapping. Scanning electron microscopy in back-scatter mode confirmed that the greatest Cu concentrations occur in the form of crystalline aggregates in coloured inclusions below the major internal turquoise layer with smaller Cu contents. X-ray diffraction with a position-sensitive detector (XRD-PSD) confirmed coloured crystalline aggregates consisted of the copper oxalate, moolooite. The study confirms the value of XRD-PSD as a non-destructive tool to characterize small (~50 μm) metal oxalate inclusions obtained from within lichen samples.