Design of an ultrahigh‐energy‐resolution and wide‐energy‐range soft X‐ray beamline

A new ultrahigh‐energy‐resolution and wide‐energy‐range soft X‐ray beamline has been designed and is under construction at the Shanghai Synchrotron Radiation Facility. The beamline has two branches: one dedicated to angle‐resolved photoemission spectroscopy (ARPES) and the other to photoelectron emission microscopy (PEEM). The two branches share the same plane‐grating monochromator, which is equipped with four variable‐line‐spacing gratings and covers the 20–2000 eV energy range. Two elliptically polarized undulators are employed to provide photons with variable polarization, linear in every inclination and circular. The expected energy resolution is approximately 10 meV at 1000 eV with a flux of more than 3 × 10¹⁰ photons s^?1 at the ARPES sample positions. The refocusing of both branches is based on Kirkpatrick–Baez pairs. The expected spot sizes when using a 10 µm exit slit are 15 µm × 5 µm (horizontal × vertical FWHM) at the ARPES station and 10 µm × 5 µm (horizontal × vertical FWHM) at the PEEM station. The use of plane optical elements upstream of the exit slit, a variable‐line‐spacing grating and a pre‐mirror in the monochromator that allows the influence of the thermal deformation to be eliminated are essential for achieving the ultrahigh‐energy resolution.     

Design and analysis of miniature high-resolution omnidirectional gaze optical imaging system

A miniature high-resolution omnidirectional gaze optical imaging system comprising one optical low-pass filter and 5 lens elements with just one aspheric surface was successfully designed. The total tracking length of the system is 14.7 mm and fit on a 5MPx 2/3in CCD with 2448?×?2050 pixel of 3.45 μm for the full 360°?×?200° imaging. We introduced the difficulties in the design of ultrawide field of view system and proposed specific computations to overcome them by aberration theories, furthermore making a simulated analysis and performance evaluation using ZEMAX optical design software. The result shows that an admirable corrected field curvature along with a low F-theta distortion, and a perfect lateral and longitudinal color aberration correction were achieved; relative illumination of all field is over 68%; when the ambient temperature changes from ?40 to 70 ℃, the modulation transfer function performs in a steady range at 75 lp/mm; all of these will promote the wide-field lens application in medical, automotive, and stereo vision.     

Polycapillary‐optics‐based micro‐XANES and micro‐EXAFS at a third‐generation bending‐magnet beamline

A focusing system based on a polycapillary half‐lens optic has been successfully tested for transmission and fluorescence µ‐X‐ray absorption spectroscopy at a third‐generation bending‐magnet beamline equipped with a non‐fixed‐exit Si(111) monochromator. The vertical positional variations of the X‐ray beam owing to the use of a non‐fixed‐exit monochromator were shown to pose only a limited problem by using the polycapillary optic. The expected height variation for an EXAFS scan around the Fe K‐edge is approximately 200 µm on the lens input side and this was reduced to ～1 µm for the focused beam. Beam sizes (FWHM) of 12–16 µm, transmission efficiencies of 25–45% and intensity gain factors, compared with the non‐focused beam, of about 2000 were obtained in the 7–14 keV energy range for an incoming beam of 0.5 × 2 mm (vertical × horizontal). As a practical application, an As K‐edge µ‐XANES study of cucumber root and hypocotyl was performed to determine the As oxidation state in the different plant parts and to identify a possible metabolic conversion by the plant.     

Cavity-enhanced optical feedback-assisted photo-acoustic spectroscopy with a 10.4 μm external cavity quantum cascade laser

An ultra-sensitive photo-acoustic spectrometer using a 10.4 μm broadly tunable mid-IR external cavity quantum cascade laser (EC-QCL) coupled with optical feedback to an optical power buildup cavity with high reflectivity mirrors was developed and tested. A laser optical power buildup factor of 181 was achieved, which corresponds to an intra-cavity power of 9.6 W at a wavelength of 10.4 μm. With a photo-acoustic resonance cell placed inside the cavity this resulted in the noise-equivalent absorption coefficient of 1.9 × 10^?10 cm^?1 Hz^?1/2, and a normalized noise-equivalent absorption of 1.1 × 10^?11 cm^?1 W Hz^?1/2. A novel photo-acoustic signal normalization technique makes the photo-acoustic spectrometer’s response immune to changes and drifts in the EC-QCL excitation power, EC-QCL to cavity coupling efficiency and cavity mirrors aging and contamination. An automatic lock of the EC-QCL to the cavity and optical feedback phase optimization permitted long wavelength scans within the entire EC-QCL spectral tuning range.     

Focusing,collimation and flux throughput at the IMCA‐CAT bending‐magnet beamline at the Advanced Photon Source

The IMCA‐CAT bending‐magnet beamline was upgraded with a collimating mirror in order to achieve the energy resolution required to conduct high‐quality multi‐ and single‐wavelength anomalous diffraction (MAD/SAD) experiments without sacrificing beamline flux throughput. Following the upgrade, the bending‐magnet beamline achieves a flux of 8 × 10¹¹ photons s^?1 at 1 Å wavelength, at a beamline aperture of 1.5 mrad (horizontal) × 86 µrad (vertical), with energy resolution (limited mostly by the intrinsic resolution of the monochromator optics) δE/E = 1.5 × 10^?4 (at 10 kV). The beamline operates in a dynamic range of 7.5–17.5 keV and delivers to the sample focused beam of size (FWHM) 240 µm (horizontally) × 160 µm (vertically). The performance of the 17‐BM beamline optics and its deviation from ideally shaped optics is evaluated in the context of the requirements imposed by the needs of protein crystallography experiments. An assessment of flux losses is given in relation to the (geometric) properties of major beamline components.     

Changes in Dentin Collagen After Sample Grinding and Heating

ABSTRACT

Changes to the structure of the organic matrix of the dentin tissue were determined after sample grinding and heating. Powder dentin measuring 25–38 µm and slices with a thickness of about 50 µm were employed. Spectra acquisition was conducted with a Fourier-transform infrared spectrometer. The thermal treatment was performed between 100°C and 300°C, with steps of 25°C. After grinding, two bands (1283.5 ± 0.5 cm^?1 and 1240.7 ± 0.5 cm^?1) shifted to higher wavenumbers, while three bands (1339.5 ± 0.5 cm^?1, 1283.5 ± 0.5 cm^?1, and 1202.7 ± 0.5 cm^?1) shifted to lower wavenumbers after thermal treatment in the range 100–300°C; the band at 1283.5 ± 0.5 cm^?1 shifted only 2 cm^?1. Thermal treatment produced a wavenumber shift in the opposite direction compared with the shift produced after grinding. The observed changes in the vibration modes of the structure indicate that sample preparation or sterilization involving grinding and heating must be carefully evaluated in order to preserve the natural characteristic of the collagen structure.     

Dispersive liquid–liquid microextraction based on solidification of floating organic drop for separation and preconcentration of malachite green before its determination by flow injection spectrophotometry

ABSTRACT

A simple and fast dispersive liquid–liquid microextraction based on solidification of floating organic drop has been developed for the separation and preconcentration of malachite green in water samples prior to its determination by flow injection spectrophotometry. Sodium lauryl sulfate, an anionic surfactant, was used for the ion-pair formation with malachite green. The factors affecting the ion-pair formation and extraction were optimized. Under the optimized conditions (volume of 1-undecanol as the extraction solvent, 40 μL; the volume of ethanol as the disperser solvent, 100 μL; sodium lauryl sulfate concentration, 7.5 × 10^?7 mol L^?1, and the pH of the sample, ～3.0), the calibration graph was linear over the range of 0.8–25 µg L^?1 with the detection limit of 0.3 µg L^?1 and the preconcentration factor of 750. The relative standard deviation at 7 µg L^?1 (n = 6) was found to be 2.1%. The developed method was successfully applied to the determination of malachite green in river water and fish farming water samples.     

Lensless high-resolution photoacoustic imaging scanner for in vivo skin imaging

We previously launched a high-resolution photoacoustic (PA) imaging scanner based on a unique lensless design for in vivo skin imaging. The design, imaging algorithm and characteristics of the system are described in this paper. Neither an optical lens nor an acoustic lens is used in the system. In the imaging head, four sensor elements are arranged quadrilaterally, and by checking the phase differences for PA waves detected with these four sensors, a set of PA signals only originating from a chromophore located on the sensor center axis is extracted for constructing an image. A phantom study using a carbon fiber showed a depth-independent horizontal resolution of 84.0 ± 3.5 µm, and the scan direction-dependent variation of PA signals was about ± 20%. We then performed imaging of vasculature phantoms: patterns of red ink lines with widths of 100 or 200 μm formed in an acrylic block co-polymer. The patterns were visualized with high contrast, showing the capability for imaging arterioles and venues in the skin. Vasculatures in rat burn models and healthy human skin were also clearly visualized in vivo.     

Determination of Protoporphyrin IX Disodium Salt Based on Fluorescence Quenching of Glutathione-Capped Cadmium/Tellurium Quantum Dots

ABSTRACT

Aqueous glutathione-capped cadmium/tellurium quantum dots with a diameter of about 3 nm were synthesized. The fluorescence was quenched in the presence of protoporphyrin IX disodium salt, with the excitation wavelength at 320 nm. Under the optimal conditions, the quenched fluorescence intensity was linear in the range of 0.096–16 µg · mL^?1 with a concentration of protoporphyrin IX disodium salt, and the detection limit (3σ) was 2.8 × 10^?2 µg · mL^?1. The proposed method has been applied to the determination of protoporphyrin in serum samples with satisfactory results. The interaction mechanism was investigated.     

Fourier Transform Mid-Infrared Photoacoustic Spectroscopy for Presymptomatic Detection of Powdery Mildew Infection in Rubus corchorifolius L.

A powdery mildew fungi-induced disease appearing on leaves of Rubus corchorifolius L. has been observed in China, which resulted in seriously influencing the yield and quality of the fruit, and a presymptomatic detection of powdery mildew infection is needed to guarantee the yield and quality through removing the fungi in an early stage. Depth-profiling Fourier transform mid-infrared photoacoustic spectroscopy was applied to characterize both the healthy leaves and powdery mildew-infected leaves of Rubus corchorifolius L. The profiled surface could be divided into out layer (depth of about 1.32 µm) and deep layer (depth of about 1.87 µm). There were numerous differences in the total spectral range (500–4000 cm^?1) between healthy leaves and infected leaves, especially the intensity of absorption bands of 2800–3000 cm^?1 (aliphatic C–H vibration) and 2250–2350 cm^?1 (CO₂) significantly decreased when the leaf was infected by powdery mildew. For the out layer the standard spectral variance between healthy leaf and infected leaf was 7.33 × 10², whereas it was 1.86 × 10⁴ for the deep layer; the standard spectral variance between out layer and deep layer for healthy leaf was 3.38 × 10³, whereas it was 1.84 × 10⁴ for infected leaf, which implied that both out layer and deep layer responded to powdery mildew infection. Combining spectral differences between healthy leaf and infected leaf and variances between out layer and deep layer, a presymptomatic detection of powdery mildew infection was successfully made, which provided an alternative option and noninvasive method for the fast diagnosis of powdery mildew infection on Rubus corchorifolius L.     

Thermal lens spectrometry under excitation of a divergent pump beam

Thermal lens spectrometry (TLS) under excitation of a divergent pump beam is discussed in both conventional and microscopic TLS instruments. A refined thermal lens (TL) model was proposed for calculating the TL signal of a “finite TL element.” Experiments as well as comparison with numerical simulations demonstrated that the effective sample length for a certain pump beam profile was about six times the confocal distance of the pump beam for laser-excited case and 1.5 mm for incoherent light source-excited case. For laser-excited conventional TLS instrument or thermal lens microscope (TLM), an empirical formula of the optimum pump beam waist radius for maximum detection sensitivity was obtained at a given sample length. At larger pump beam waist radius of 7 μm, the TL signal was found 2.5 times lower compared to the diffraction limit; however, the resulting two orders of magnitude lower power density in the sample could be quite desirable for the detection of photolabile analytes. By investigating the influence of a finite TL element on the TL signal, we found that an optimal distance between the probe beam waist and the sample was needed to assure the maximum detection sensitivity and good response linearity. Under the optimal detection scheme, limit of detection of the laser-excited TLM at 4 mW power was evaluated to be 8.6 × 10^?9 M for 100-μm-thick ferroin solution, corresponding to an absorbance of 9.5 × 10^?7 absorbance units.     

Near-Infrared Methane Detection Device Using Wavelength-Modulated Distributed Feedback Diode Laser around 1.654 µm

By using a wavelength-modulated distributed feedback laser centered at 1.654 µm, a stand-alone near-infrared methane detection device was experimentally proposed based on the tunable diode laser absorption spectroscopy technique. An intelligent temperature controller, a scan and modulation module, and a cost-effective lock-in amplifier were developed to drive the distributed feedback laser and extract the second harmonic signal. Experimental results show that the relative detection error is less than 7% within the detection range of 0–10⁶ ppm, and the limit of detection is about 11 ppm with an absorption length of 0.2 m. Long-term monitoring on two gas samples (10³ ppm and 2 × 10⁵ ppm) suggests good stability with the maximum detection errors smaller than 7% and 2.5%, respectively. Due to careful design and integration, the developed near-infrared sensor reveals competitive performances compared with our previously reported sensing devices at the mid-infrared region.     

A calix[4]arene derivative-doped perchlorate-selective membrane electrodes with/without multi-walled carbon nanotubes

In this study, poly (vinyl chloride)(PVC) membrane electrodes with/without multi-walled carbon nanotubes (MWCNTs) based on a calix[4]arene derivative for perchlorate ion were described. The influence of membrane composition, pH, conditioning solution on the potentiometric response of the electrodes was investigated. Perchlorate-selective PVC membrane electrode exhibited a slope of 47.8 ± 0.6 mV/pClO₄ in the range of 1.0 × 10^?7–1.0 × 10^?1 mol L^?1at pH 4.0 while the coated Pt electrodes with MWCNT-OH, MWCNT-COOH and MWCNT displayed slopes of 46.1 ± 0.7 mV/pClO₄ (5.0 × 10^?6–1.0 × 10^?1 mol L^?1), 50.4 ± 1.9 mV/pClO₄ (1.0 × 10^?6–1.0 × 10^?1 mol L^?1) and 44.4 ± 0.3 mV/pClO₄ (1.0 × 10^?5–1.0 × 10^?1 mol L^?1), respectively. Other response characteristics of these electrodes such as response time, lifetime and detection limit were identified, and the selectivity coefficients towards various anions were calculated by separate solution method. Moreover, the perchlorate-selective electrodes described here were successfully used as an indicator electrode for the determination of perchlorate in real samples such as tap water, river water and human urine by direct calibration method.     

Rapid Fluorescent Detection of Escherichia coli K88 Based on DNA Aptamer Library as Direct and Specific Reporter Combined With Immuno-Magnetic Separation

Nucleic acid aptamers have long demonstrated the capacity to bind cells with high affinity so that they have been utilized to diagnose various important pathogens. In this study, a DNA aptamer library was on initial efforts developed to act as a specific reporter for rapid detection of enter toxigenic Escherichia coli (ETEC) K88 combined with immuno-magnetic separation (IMS). During a Whole-cell Systematic Evolution of Ligands by Exponential Enrichment (CELL-SELEX) procedure, the last selection pool against ETEC K88, which is named “DNA aptamer library” here, was selected and subsequently identified by flow cytometric analysis and confocal imaging. A K88 monoclonal antibody (mAb) with high affinity (K_aff: 1.616?±?0.033?×?10⁸ M^?1) against K88 fimbrial protein was prepared, biotinylated and conjugated to streptavidin-coated magnetic beads (MBs). After the bacteria were effectively captured and enriched from the complex sample by immuno-magnetic beads (IMBs), 5′-FITC modified aptamer library was directly bound to target cells as a specific reporter for its detection. The detection system showed clearly high specificity and sensitivity with the detection limit of 1.1?×?10³ CFU/ml in pure culture and 2.2?×?10³ CFU/g in artificially contaminated fecal sample. The results also indicated that fluorophore-lablled DNA aptamer library as specific reporter could generate more reliable signals than individual aptamer with best affinity against target cells and implied it would have great applied potential in directly reporting bacteria from complex samples combined with IMS technology.     

Silicon nano crystal filled ellipse core based quasi photonic crystal fiber with birefringence and very high nonlinearity

In this paper, we have proposed a new type of quasi photonic crystal fiber (PCF) with a silicon nano crystal core. This structure can be used to sense aqueous analysis over a wavelength range of 1.00?µm to 3.00?µm. The properties of this structure are simulated using the vector-finite element method (VFEM) employing a boundary condition. The proposed model provides a significant effect of birefringence and a very high nonlinear coefficient for two different fundamental modes, which are obtained by adjusting the size of the silicon nano crystal filled ellipse core. This provides a high nonlinearity of 4.2?×?10⁵ W^?1Km^?1 and a birefringence of ? 3.2?×?10^?1 at the wavelengths 1.00?µm and 3.00?µm, respectively. Some others properties, such as the effective area, scattering loss, confinement loss, numerical aperture (NA)and power fraction are also analyzed to measure the performance of this structure. The proposed model is useful for sensing and biomedical imaging applications. The proposed structure may also find extensive applications in optical communication and sensor systems.     

Voltammetric determination of hydroxylamine in water samples using a 1-benzyl-4-ferrocenyl-1H-[1,2,3]-triazole/carbon nanotube-modified glassy carbon electrode

A modified glassy carbon electrode has been constructed using a 1-benzyl-4-ferrocenyl-1H-[1,2,3]-triazole along with multiwalled carbon nanotubes. The electrochemical behaviour of modified electrode has been investigated by cyclic voltammetry. Electrocatalytic activity of the modified electrode was investigated for the oxidation of hydroxylamine in 0.1 M phosphate-buffered solution of pH 8. The modified electrode showed electrocatalytic response to the oxidation of hydroxylamine at the potential of 330 mV. The linear range and detection limit for the detection of hydroxylamine in the optimum condition were found to be 4.0?×?10^?7 to 6.75?×?10^?4 M and 28.0?±?1.0 nM, respectively. Finally, the method was employed for the determination of hydroxylamine in water samples.     

Fixed-grid method for the modelling of unsteady partial oxidation of a spherical coal particle

The main goal of this work is the development of a fixed-grid method to model unsteady partial oxidation of a solid with implicit tracking of the interface. As a first step diffusive oxidation of a spherical coal particle is considered. The energy and species conservation equations formulated in spherical coordinates are discretised using the finite-volume approach. The boundary conditions for the temperature and species mass fractions at the solid–gas interface are modelled via special source terms activated in the interface cells. The numerical model was validated against analytic one- and two-film models for coal combustion in a dry-air atmosphere. Very good agreement was obtained. Based on the model developed a numerical study was carried out on the influence of water vapour on the partial oxidation of a spherical coal particle. Numerous numerical simulations were performed for particle diameters in the range 200×10^?6 m to 2×10^?2 m. The ambient temperature was varied in the range between 700 and 3000 K. The analysis of results showed that the addition of H₂O has an influence on the solution convergence due to the catalytic effect of water in the coal monoxide oxidation reaction making the whole system stiffer. However, at the same time, it was found that if the ambient mass fraction of water vapour is below 1×10^?3, its influence on combustion rates is minimal. The results of numerical simulations obtained for higher H₂O concentration (>1×10^?3) are discussed.     

Determination of Microamounts of Proteins by Resonance Light Scattering with Copper Phthalocyanine Tetrasulfonic Acid

Abstract

Based on the strong enhancement effect of proteins on the resonance light scattering of copper phthalocyanine tetrasulfonic acid, a method for the determination of microamounts of proteins has been developed. Under the experimental conditions (2.0×10^?6 mol/L copper phthalocyanine tetrasulfonic acid, pH 2.60, ionic strength 0.001 mol/L NaCl), the linear range of this assay is 0.06–4.0 µg/mL for bovine serum albumin (BSA), 0.1–2.0 µg/mL for human serum albumin (HSA), 0.0–2.0 µg/mL for human γ‐IgG, and 0.2–6.0 µg/mL for ovalbumin. The detection limits (3δ) are 16.8 ng/mL for BSA, 23.4 ng/mL for HSA, 37.6 ng/mL for human γ‐IgG, and 48.3 ng/mL for ovalbumin, respectively. This method has been applied to the analysis of total proteins in human serum samples collected from the hospital, and the results were in good agreement with those reported by the hospital.     

Simultaneous remote monitoring of atmospheric methane and water vapor using an integrated path DIAL instrument based on a widely tunable optical parametric source

We report on the remote sensing capability of an integrated path differential absorption lidar (IPDIAL) instrument, for multi-species gas detection and monitoring in the 3.3–3.7 µm range. This instrument is based on an optical parametric source composed of a master oscillator-power amplifier scheme—whose core building block is a nested cavity optical parametric oscillator—emitting up to 10 µJ at 3.3 µm. Optical pumping is realized with an innovative single-frequency, 2-kHz repetition rate, nanosecond microchip laser, amplified up to 200 µJ per pulse in a single-crystal fiber amplifier. Simultaneous monitoring of mean atmospheric water vapor and methane concentrations was performed over several days by use of a topographic target, and water vapor concentration measurements show good agreement compared with an in situ hygrometer measurement. Performances of the IPDIAL instrument are assessed in terms of concentration measurement uncertainties and maximum remote achievable range.     

Study on the Interaction Between Oxymatrine and Tungstosilicic Acid by Resonance Rayleigh Scattering and Its Analytical Applications

In the 0.1 mol · L^?1 hydrochloric acid solution, oxymatrine reacted with tungstosilicic acid to form a 2:1 ion-association complexes. This results in a great enhancement of resonance Rayleigh scattering. The maximum resonance Rayleigh scattering wavelength was located at 393 nm. Resonance Rayleigh scattering intensity was proportional to the concentration of oxymatrine in the range of 1.5–26.4 µg · mL^?1, and the detection limit (3σ) was 0.23 µg · mL^?1. The optimum conditions and the effects of coexisting substances on the reaction were investigated. The method shows a wide linear range and high sensitivity, and was applied to the determination of oxymatrine in marine capsules and human urine samples with satisfactory results. Therefore, a highly sensitive, simple, and quick method has been developed for the determination of oxymatrine.