A small-angle scattering chamber for x-ray photon correlation spectroscopy at low temperatures

A low temperature sample environment for x-ray photon correlation spectroscopy measurements in small-angle scattering geometry is presented. The chamber has been designed to allow investigations of dynamical phenomena in supercooled liquids and the typical working temperature range is 110-330 K with a thermal stability ΔT/T down to 10(-4). A variable external magnetic field up to 0.12 T can be applied, which is of interest in studies of, e.g., ferrofluids and liquid crystalline materials. Here, technical details about the sample environment are given together with examples of recent applications.     

Gold nanorods as probes in two‐photon fluorescence correlation spectroscopy: Emerging applications and potential artifacts

Owing to the highly efficient two‐photon fluorescence of gold nanorods and very short fluorescence lifetime compared with the rotational correlation time, the rotation and diffusion of a single gold nanorod can be easily observed by two‐photon fluorescence correlation spectroscopy (TP‐FCS). This property, along with the previous successful use as a contrast agent in two‐photon fluorescence imaging, suggests a potential application in TP‐FCS as well. Although the FCS measurement becomes highly efficient with gold nanorods as probes, the amplitude and temporal decay of the measured correlation functions depend critically on excitation power. Here, we investigate various photophysical processes of gold nanorods to determine the cause of such a sensitive power dependency. This understanding provides a basis for choosing appropriate FCS models to recover reasonable physical parameters. Although the correlation function amplitude G(0) is 32 times lower when the excitation power increases from 20 µW to 1.12 mW, the application of a saturation‐modified FCS model yields very good fit to each data set and the fitted concentration of 0.64 nM is comparable to the 0.7 nM given by the inductively coupled plasma mass spectrometry measurement. The FCS assay appears to be an efficient method for the quantification of gold nanorods when correctly interpreted. However, even with the saturation considered in the fitting model, the fitted rotational and translational diffusion rates are getting faster as the power increases. This indicates that other effects such as photothermal effects may raise the local temperature, and thus increasing the rotational and translational diffusion rate. Microsc. Res. Tech. 76:882–889, 2013. © 2013 Wiley Periodicals, Inc.     

Continuous flow time-resolved small-angle x-ray scattering and X-ray absorption spectroscopy

A continuous flow device to characterize the growth of nanometer particles was assembled. In-situ millisecond or second-order time-resolved small angle x-ray scattering and x-ray absorption spectroscopy was performed using this device at the Beijing Synchrotron Radiation Facility. The time resolution was adjusted from 10 ms to 1.0 s by changing the flow rate of the solution. The temperature was variable from 5–95°C. Custom-designed pulse eliminators were employed to eliminate adverse pump fluctuations and improve the quality of measurements. The system was used to characterize zinc sulfide nanoparticles by small angle x-ray scattering and x-ray absorption spectroscopy.     

A wavelet transform algorithm for peak detection and application to powder x-ray diffraction data

Peak detection is ubiquitous in the analysis of spectral data. While many noise-filtering algorithms and peak identification algorithms have been developed, recent work [P. Du, W. Kibbe, and S. Lin, Bioinformatics 22, 2059 (2006); A. Wee, D. Grayden, Y. Zhu, K. Petkovic-Duran, and D. Smith, Electrophoresis 29, 4215 (2008)] has demonstrated that both of these tasks are efficiently performed through analysis of the wavelet transform of the data. In this paper, we present a wavelet-based peak detection algorithm with user-defined parameters that can be readily applied to the application of any spectral data. Particular attention is given to the algorithm's resolution of overlapping peaks. The algorithm is implemented for the analysis of powder diffraction data, and successful detection of Bragg peaks is demonstrated for both low signal-to-noise data from theta-theta diffraction of nanoparticles and combinatorial x-ray diffraction data from a composition spread thin film. These datasets have different types of background signals which are effectively removed in the wavelet-based method, and the results demonstrate that the algorithm provides a robust method for automated peak detection.     

Image compression and data integrity in confocal microscopy

To manage large volumes of image data generated routinely using real-time confocal microscopy, compressing image data using a lossy algorithm prior to sustained video rate transferring and/or storing is proposed. Test criteria for determining the acceptability of uncompressed data, both qualitatively and quantitatively, are described, and an empirical demonstration of the use of lossy compression in data management is provided. It is found that, if appropriately used, the lossy compression scheme could retain all the useful information in the data while providing better compression ratios (memory for the original/ memory for the compressed) when compared with a lossless scheme.     

Appearance potential spectroscopy with a photon counting detector and multiple scattering spectral interpretation

We describe a soft x-ray appearance potential spectroscopy apparatus, which uses a windowless hyperpure Ge detector operated in the photon counting mode. Direct comparisons of recorded spectra with the self-convolution of x-ray absorption spectra and with ab initio simulations in the multiple scattering framework are reported and discussed.     

遥测数据实时压缩技术的设计与实现

本文在分析了目前常用的几种数据压缩的原理、算法和功效后,提出了一个新的改进压缩算法,并从理论上阐述了该算法的优点及较好的压缩性能.     

Comparison and accuracy of methods to determine the confocal volume for quantitative fluorescence correlation spectroscopy

Single molecule detection based on fluorescent labels offers the possibility to gain not only qualitative but also quantitative insight into specific functions of complex biological systems. Fluorescence correlation spectroscopy is one of the favourite techniques to determine concentrations and diffusion constants as well as molecular brightness of molecules in the pico‐ to nano‐molar concentration range, with broad applications in biology and chemistry. Although fluorescence correlation spectroscopy in principle has the potential to measure absolute concentrations and diffusion coefficients, the necessity to know the exact size and shape of the confocal volume very often hampers the possibility to obtain quantitative results and restricts fluorescence correlation spectroscopy to relative measurements mainly. The determination of the confocal volume in situ is difficult because it is sensitive to optical alignment and aberrations, optical saturation and variations of the index of refraction as observed in biological specimen. In the present contribution, we compare different techniques to characterize the confocal volume and to obtain the confocal parameters by fluorescence correlation spectroscopy curve fitting, a fluorescence correlation spectroscopy dilution series and confocal scanning of fluorescent beads. The results are compared in the view of quantitative fluorescence correlation spectroscopy measurement and analysis. We investigate how unavoidable artefacts caused by a non‐ideal confocal volume can be experimentally determined and validated.     

Comparison between beryllium and diamond-backing plates in diamond-anvil cells: application to single-crystal x-ray diffraction high-pressure data

A direct comparison between two complete intensity datasets, collected on the same sample loaded in two identical diamond-anvil pressure cells equipped, respectively, with beryllium and diamond-backing plates was performed. The results clearly demonstrate that the use of diamond-backing plates significantly improves the quality of crystal structure data. There is a decrease in the internal R factor for averaging, structure refinement agreement factors, and in the errors and uncertainties of the atomic coordinates, atomic displacement parameters, and individual bond lengths.     

Improved correlation analysis and visualization of industrial alarm data

The problem of multivariate alarm analysis and rationalization is complex and important in the area of smart alarm management due to the interrelationships between variables. The technique of capturing and visualizing the correlation information, especially from historical alarm data directly, is beneficial for further analysis. In this paper, the Gaussian kernel method is applied to generate pseudo continuous time series from the original binary alarm data. This can reduce the influence of missed, false, and chattering alarms. By taking into account time lags between alarm variables, a correlation color map of the transformed or pseudo data is used to show clusters of correlated variables with the alarm tags reordered to better group the correlated alarms. Thereafter correlation and redundancy information can be easily found and used to improve the alarm settings; and statistical methods such as singular value decomposition techniques can be applied within each cluster to help design multivariate alarm strategies. Industrial case studies are given to illustrate the practicality and efficacy of the proposed method. This improved method is shown to be better than the alarm similarity color map when applied in the analysis of industrial alarm data.     

Spectroscopically pure metal vapor source for highly charged ion spectroscopy and capillary discharge soft x-ray lasers

We describe a compact, pulsed metal vapor source used for the production of dense plasma columns of interest for both soft x-ray laser research and spectroscopy of highly ionized plasmas. The source generates spectroscopically pure cadmium vapor jets in a room-temperature environment by rapidly heating an electrode with a capacitive discharge. In the configuration described herein, the metal vapor jet produced by the source is axially injected into a fast (up to 15 kA/ ns), high current (up to 200 kA peak) capillary discharge to generate highly ionized cadmium plasma columns. Spectroscopic analysis of the discharge emission in the 12-25 nm spectral range evidences the dominance of Cu-like (CdXX) and Ni-like (CdXXI) lines and shows strong line emission at 13.2 nm from the 4d (1)S(0)-4p (1)P(1) laser transition of Ni-like Cd. Hydrodynamic/atomic physics simulations performed to describe the dynamics of the plasma column and compute the optimum discharge conditions for laser amplification are discussed.     

PDM与ERP的数据集成方案应用研究

BOM是PDM、CAPP和ERP系统集成的核心.对PDM与ERP的两种接口集成方案作了详细的阐述,较好的实现了从EBOM到MBOM的数据转换和集成.指出了两种PDM与ERP集成方案的优缺点,为企业PDM与ERP的集成选型提供了依据.     

Automated alignment and pattern recognition of single-molecule force spectroscopy data

Recently, direct measurements of forces stabilizing single proteins or individual receptor–ligand bonds became possible with ultra-sensitive force probe methods like the atomic force microscope (AFM). In force spectroscopy experiments using AFM, a single molecule or receptor–ligand pair is tethered between the tip of a micromachined cantilever and a supporting surface. While the molecule is stretched, forces are measured by the deflection of the cantilever and plotted against extension, yielding a force spectrum characteristic for each biomolecular system. In order to obtain statistically relevant results, several hundred to thousand single-molecule experiments have to be performed, each resulting in a unique force spectrum. We developed software and algorithms to analyse large numbers of force spectra. Our algorithms include the fitting polymer extension models to force peaks as well as the automatic alignment of spectra. The aligned spectra allowed recognition of patterns of peaks across different spectra. We demonstrate the capabilities of our software by analysing force spectra that were recorded by unfolding single transmembrane proteins such as bacteriorhodopsin and NhaA. Different unfolding pathways were detected by classifying peak patterns. Deviant spectra, e.g. those with no attachment or erratic peaks, can be easily identified. The software is based on the programming language C++, the GNU Scientific Library (GSL), the software WaveMetrics IGOR Pro and available open-source at http://bioinformatics.org/fskit/ .     

A high resolution and large solid angle x-ray Raman spectroscopy end-station at the Stanford Synchrotron Radiation Lightsource

We present a new x-ray Raman spectroscopy end-station recently developed, installed, and operated at the Stanford Synchrotron Radiation Lightsource. The end-station is located at wiggler beamline 6-2 equipped with two monochromators-Si(111) and Si(311) as well as collimating and focusing optics. It consists of two multi-crystal Johann type spectrometers arranged on intersecting Rowland circles of 1 m diameter. The first one, positioned at the forward scattering angles (low-q), consists of 40 spherically bent and diced Si(110) crystals with 100 mm diameters providing about 1.9% of 4π sr solid angle of detection. When operated in the (440) order in combination with the Si (311) monochromator, an overall energy resolution of 270 meV is obtained at 6462.20 eV. The second spectrometer, consisting of 14 spherically bent Si(110) crystal analyzers (not diced), is positioned at the backward scattering angles (high-q) enabling the study of non-dipole transitions. The solid angle of this spectrometer is about 0.9% of 4π sr, with a combined energy resolution of 600 meV using the Si (311) monochromator. These features exceed the specifications of currently existing relevant instrumentation, opening new opportunities for the routine application of this photon-in/photon-out hard x-ray technique to emerging research in multidisciplinary scientific fields, such as energy-related sciences, material sciences, physical chemistry, etc.     

High resolution absorption spectroscopy of exploding wire plasmas using an x-pinch x-ray source and spherically bent crystal

We present here the use of absorption spectroscopy of the continuum radiation from x-pinch-produced point x-ray sources as a diagnostic to investigate the properties of aluminum plasmas created by pulsed power machines. This technique is being developed to determine the charge state, temperature, and density as a function of time and space under conditions that are inaccessible to x-ray emission spectroscopic diagnostics. The apparatus and its characterization are described, and the spectrometer dispersion, magnification, and resolution are calculated and compared with experimental results. Spectral resolution of about 5000 and spatial resolution of about 20 μm are demonstrated. This spectral resolution is the highest available to date in an absorption experiment. The beneficial properties of the x-pinch x-ray source as the backlighter for this diagnostic are the small source size (<5 μm), smooth continuum radiation, and short pulse duration (<0.1 ns). Results from a closely spaced (1 mm) exploding wire pair are shown and the general features are discussed.     

岗梅与毛冬青的二维红外相关光谱鉴别研究

采用红外光谱法(FTIR)并结合二维相关光谱(Two-dimensionalInfrared CorrelationSpectrocopy)分析技术,对岗梅与毛冬青进行无损快速鉴别研究。岗梅与毛冬青皆为冬青属植物,其外形极其相似,加工成饮片后更易混淆,因此通过红外光谱对其进行无损快速鉴别研究。两种药材在一维谱上几乎没有显著差别,因此需要借助二阶导数谱和二维红外光谱对其进行进一步的研究。结果表明:通过岗梅与毛冬青的红外光谱并结合二维相关谱完全可以将其区别开来。该方法快速、准确,对中药的鉴别提供一种新的方法和手段。     

野葛与粉葛的二维红外相关光谱鉴别

采用傅立叶变换红外(FTIR)光谱法并结合二维红外相关光谱(Two-dimensional Infrared Correlation Spectroscopy)分析技术,对野葛与粉葛进行无损快速鉴别研究。野葛和粉葛均为葛藤属植物,其外形极其相似,加工成粉末后更易混淆,但两种葛根的疗效并不完全相同,因此通过红外光谱法可对其进行无损快速鉴别研究。两种药材在一维红外光谱上略有差别,因此需要借助二阶导数光谱和二维红外光谱对其进行进一步的研究。结果表明,通过野葛与粉葛的红外光谱并结合二维相关光谱完全可以将其区别开来。该方法快速、准确,对中药的鉴别提供了一种新的方法和手段。     

Near-field reflection backscattering apertureless optical microscopy: application to spectroscopy experiments on opaque samples, comparison between lock-in and digital photon counting detection techniques

An apertureless scanning near-field optical microscope (ASNOM) in reflection backscattering configuration is designed to conduct spectroscopic experiments on opaque samples constituted of latex beads. The ASNOM proposed takes advantage of the depth-discrimination properties of confocal microscopes to efficiently extract the near-field optical signal. Given their importance in a spectroscopic experiment, we systematically compare the lock-in and synchronous photon counting detection methods. Some results of Rayleigh's scattering in the near field of the test samples are used to illustrate the possibilities of this technique for reflection backscattering spectroscopy.     

Soft x-ray scattering facility at the Advanced Light Source with real-time data processing and analysis

We present the development and characterization of a dedicated resonant soft x-ray scattering facility. Capable of operation over a wide energy range, the beamline and endstation are primarily used for scattering from soft matter systems around the carbon K-edge (～285 eV). We describe the specialized design of the instrument and characteristics of the beamline. Operational characteristics of immediate interest to users such as polarization control, degree of higher harmonic spectral contamination, and detector noise are delineated. Of special interest is the development of a higher harmonic rejection system that improves the spectral purity of the x-ray beam. Special software and a user-friendly interface have been implemented to allow real-time data processing and preliminary data analysis simultaneous with data acquisition.     

High energy resolution five-crystal spectrometer for high quality fluorescence and absorption measurements on an x-ray absorption spectroscopy beamline

Fluorescence detection is classically achieved with a solid state detector (SSD) on x-ray absorption spectroscopy (XAS) beamlines. This kind of detection however presents some limitations related to the limited energy resolution and saturation. Crystal analyzer spectrometers (CAS) based on a Johann-type geometry have been developed to overcome these limitations. We have tested and installed such a system on the BM30B/CRG-FAME XAS beamline at the ESRF dedicated to the structural investigation of very dilute systems in environmental, material and biological sciences. The spectrometer has been designed to be a mobile device for easy integration in multi-purpose hard x-ray synchrotron beamlines or even with a laboratory x-ray source. The CAS allows to collect x-ray photons from a large solid angle with five spherically bent crystals. It will cover a large energy range allowing to probe fluorescence lines characteristic of all the elements from Ca (Z = 20) to U (Z = 92). It provides an energy resolution of 1-2 eV. XAS spectroscopy is the main application of this device even if other spectroscopic techniques (RIXS, XES, XRS, etc.) can be also achieved with it. The performances of the CAS are illustrated by two experiments that are difficult or impossible to perform with SSD and the complementarity of the CAS vs SSD detectors is discussed.