Time-resolved ultra-small-angle X-ray scattering beamline(BL10U1)at SSRF

The construction of a new beamline,BL10U1,was completed at the Shanghai synchrotron radiation facility in 2020.This multipurpose beamline was designed to provide X-ray scattering techniques such as ultra-small-angle X-ray scattering(USAXS),small-angle X-ray scattering(SAXS),wide-angle X-ray scattering,and microfocus SAXS(μSAXS)for a broad user community.To realize fast time-resolved USAXS experiments,the beamline adopted an in-vacuum undulator with a total length of 1.6 m as the photon source.An in-house cryogenic-cooled double multilayer monochromator was installed to deliver a photon flux of approximately 10^(13) photons/s at a photon energy of 10 keV.The three-year successful operation of this beamline demonstrated that the monochromator operated smoothly,as expected.BL10U1 has three end stations in succession:USAXS end station,μSAXS end station,and end station for industrial applications.The minimum scattering vector q~0.0042 nm^(-1) at 10 keV can be achieved at the USAXS end station equipped with a 28 m-long and 1.8 m-diameter vacuum flight tube.At theμSAXS end station,a beam spot of less than 10×8μm was achieved for micro-SAXS experiments.In contrast,in situ experimental instruments up to 5 m high and 8 m wide can be mounted at the industrial application end station,which offers industrial scientists the opportunity to use their large industrial equipment.BL10U1 opens up a new capability to investigate phenomena such as non-equilibrium and dynamic processes of materials with a wide length scale from angstroms to micrometers with millisecond time resolution.In this paper,we also report beamline design considerations and commissioning results.

Time-resolved fluoroimmunoassay of zearalenone in cereals with a europium chelate as label

A competitive indirect time-resolved fluoroimmunoassay(TRFIA) was developed for detection of zearalenone(ZEN) in cereals,in which ZEN conjugated to bovine serum albumin(BSA) is used as solid-phase antigen.A competitive indirect TRFIA was conducted by simultaneously incubating ZEN in standard or extracted samples with anti-ZEN monoclonal antibody over ZEN-BSA coated plates,and then determining the bound ZEN monoclonal antibody with goat anti-mouse europium conjugate.Samples were extracted with methanol/water...

Eu-Chelate Construct Ultrasensitive Time-Resolved Fluoroimmunoassay-Assay of Pepsinogen I

Eu-chelate were used to construct a two-site sandwich-type assay for pepsinogen Ⅰ （PGI） with time-resolved fluoroimmunoassay （TRFIA） as a detection technique. On the noncompetitive assay, captured monoclonal antibodies （McAbs） coated on wells were directed against a specific antigenic site on the PGI. Another McAbs, called as labeling McAbs, were prepared with the Eu-chelate of N-（p-isothiocyanatobenzyl）-diethylenetriamine-N, N, N, N-tetraacetic acid and directed against a different antigenic site on the PGI. The fluorescence counts of bound Eu^3＋ -McAbs were measured with the auto DELFIA1235 system. The PGI in sera from healthy volunteers were determined by PGI-TRFIA. The within-run and between-run CVs of the PGI-TRFIA were 1.9% and 4.7%, respectively, and the recovery rate was 102.65%. The assay had a detection limit of 0.05 μg· L^-1. The PGI-TRFIA provided a linear response from 3.5 to 328 μg· L^-1. The cross-reacting rate with pepsinogen Ⅱ was negligible. The linear correlation of PGI-TRFIA and radioimmunassay measurements resulted in a correlation coefficient of 0.977. The means of healthy volunteers were 154 ±43 μg·L^-1 for serum PGI. The availability of a highly sensitive, reliable, and convenient method for quantifying PGI will allow investigations into the possible diagnostic value of this analyte in various clinical conditions, including gastric carcinoma, duodenal ulcer, gastritis and severe atrophic gastritis.

Simultaneous determination of captopril and hydrochlorothiazide by time-resolved chemiluminescence with artificial neural network calibration

The combined use of chemometrics and chemiluminescence（CL）measurements,with the aid of the stopped-flow mixing technique,developed a simple time-resolved CL method for the simultaneous determination of captopril（CPL）and hydrochlorothiazide（HCT）.The stopped-flow technique in a continuous-flow system was employed in this work in order to emphasize the kinetic differences between the two analytes in cerium（IV）-rhodamine 6G CL system.After the flow was stopped,an initial rise of CL signal was observed for HCT standards,while a direct decay of CL signal was obtained for CPL standards.The mixed CL signal was monitored and recorded on the whole process of continuous-flow/stopped-flow,and the obtained data were processed by the chemometric approach of artificial neural network.The relative prediction error（RPE）of CPL and HCT was 5.9% and 8.7%,respectively.The recoveries of CPL and HCT in tablets were found to fall in the range between 95% and 106%.The proposed method was successfully applied to the simultaneous determination of CPL and HCT in a compound pharmaceutical formulation.

Analysis of Turbulence Structure in the Stirred Tank with a Deep Hollow Blade Disc Turbine by Time-resolved PIV

The turbulence structure in the stirred tank with a deep hollow blade(semi-ellispe) disc turbine(HEDT) was investigated by using time-resolved particle image velocimetry(TRPIV) and traditional PIV.In the stirred tank,the turbulence generated by blade passage includes the periodic components and the random turbulent ones.Traditional PIV with angle-resolved measurement and TRPIV with wavelet analysis were both used to obtain the random turbulent kinetic energy as a comparison.The wavelet analysis method was successfully used in this work to separate the random turbulent kinetic energy.The distributions of the periodic kinetic energy and the random turbulent kinetic energy were obtained.In the impeller region,the averaged random turbulent kinetic energy was about 2.6 times of the averaged periodic one.The kinetic energies at different wavelet scales from a6 to d1 were also calculated and compared.TRPIV was used to record the sequence of instantaneous velocity in the impeller stream.The evolution of the impeller stream was observed clearly and the sequence of the vorticity field was also obtained for the identification of vortices.The slope of the energy spectrum was approximately-5/3 in high frequency representing the existence of inertial subrange and some isotropic properties in stirred tank.From the power spectral density(PSD) ,one peak existed evidently,which was located at f0(blade passage frequency) generated by the blade passage.

Time-resolved shadowgraphs and morphology analyses of aluminum ablation with multiple femtosecond laser pulses

Aluminum ablation by multiple femtosecond laser pulses is investigated via time-resolved shadowgraphs and scanning electron microscope （SEM） images of the ablation spot. The spatial distribution of the ejected material and the radius of the shock wave generated during the ablation are found to vary with the increase in the number of pulses. In the initial two pulses, nearly concentric and semicircular stripes within the shock wave front are observed, unlike in subsequent pulses. Ablation by multiple femtosecond pulses exhibits different characteristics compared with the case induced by single femtosecond pulse because of the changes to the aluminum target surface induced by the preceding pulses.

Time Sequential and Phase-resolved Measurement and Analysis of Corona Discharge in Air and Streamer Discharge in Insulating Liquid

Insulation is one of the most important parts in a high voltage equipment.There are gaseous,liquid and solid insulations which are commonly used.In a high voltage transformer for example the insulating materials are all used.During operation of a high voltage equipment high electric stress may occur.Under extreme condition failure of the insulation may take place.Excessive electric field in air may cause corona discharges while in liquid insulation discharges may take place in the form of streamer.This paper reports experimental results on the corona and streamer discharges in air and silicone oil.The discharges were artificially generated around a needle tip in a needle-plane electrode system with gap length of 4 mm under sinusoidal and triangular voltages.The needle was made of steel with tip radius of 3 μm and curvature angle of 30°.The needle was made by Ogura Jewelry.The discharge pulses were measured using personal-computer based partial discharge(PD)measurement system with sensitivity of better than 0.5 pC.The system is able to measure discharge in time sequential.Phase-resolved analysis of the discharges was done to interpret the physical processes behind the discharges.The experimental results showed that corona discharges took place at negative half cycles.The discharges were concentrated around 270° of phase angle of applied voltage.The discharge magnitude and discharge number of corona clearly dependent on the instantaneous of applied voltage.These were strongly supported by the application of triangular voltage.Streamer discharges occurred at both positive and negative half cycles.The discharges pulses concentrated around the peak of applied voltage at phase angle of 90° and 270°.Experimental results under sinusoidal and triangular voltages revealed that streamer discharge magnitude as well as probability of occurrence was strongly dependent on the instantaneous applied voltage.

Simultaneous measurements of global vibrational spectra and dephasing times of molecular vibrational modes by broadband time-resolved coherent anti-Stokes Raman scattering spectrography

In broadband coherent anti-Stokes Raman scattering （CARS） spectroscopy with supercontinuum （SC）, the simultaneously detectable spectral coverage is limited by the spectral continuity and the simultaneity of various spectral components of SC in an enough bandwidth. By numerical simulations, the optimal experimental conditions for improving the SC are obtained. The broadband time-resolved CARS spectrography based on the SC with required temporal and spectral distributions is realised. The global molecular vibrational spectrum with well suppressed nonresonant background noise can be obtained in a single measurement. At the same time, the measurements of dephasing times of various molecular vibrational modes can be conveniently achieved from intensities of a sequence of time-resolved CARS signals. It will be more helpful to provide a complete picture of molecular vibrations, and to exhibit a potential to understand not only both the solvent dynamics and the solute-solvent interactions, but also the mechanisms of chemical reactions in the fields of biology, chemistry and material science.

Space-time Resolved Spectroscopic System Based on a Rotating Hexahedral Mirror for Measurement of Visible and Ultraviolet Spectral Line Emissions

By using a rotating hexahedral mirror placed in front of the objective lens and two sets of visible and ultraviolet monochromators coupled with a branchy quartz fiber bundle, a space-time resolved spectroscopic system has been developed on the HT-7 superconducting tokamak. A center monitoring system has been used including a Helium-Neon laser and a photodiode detector to indicate the absolute position of the measurement in order to reduce the error caused by the uncertain emissive position of the plasma. By using the asymmetric Abel inversion, the space-time resolved local emission coefficients of the spectroscopic line emissions have been obtained. Presented in this article are simultaneous measurements of two spectral line emissions such as CV-227.1 nm and OV-278.1 nm during a single plasma discharge on the HT-7. Experimental results indicate that the time resolution is better than 3 ms, the space resolution is better than 1.5cm, the ratio of signal to background is better than 10：1, and the relative error of chord-integrated emission profile is less than 10%. Compared to traditional multichannel detecting systems, this system has considerably improved measurement efficiency, reduced uncertainty, and is therefore suitable for transport studies of global particles and impurities.

Study on local topology model of low/high streak structures in wall-bounded turbulence by tomographic time-resolved particle image velocimetry

The relationship between the in the logarithmic law （log-law） region of bursting event and the low/high-speed streak a turbulent boundary layer is investigated. A tomographic time-resolved particle image velocimetry （TRPIV） system is used to measure the instantaneous three-dimensional-three-component （3D-3C） velocity field. The momentum thickness based Reynolds number is about 2 460. The topological information in the log-law region is obtained experimentally. It is found that the existence of the quadrupole topological structure implies a three-pair hairpin-like vortex packet, which is in connection with the low/high-speed streak. An idealized 3D topological model is then proposed to characterize the observed hairpin vortex packet and low/high-speed streak.

Time-resolved measurement of atomic emission enhancement by fs-ns dual-pulsed laser-induced breakdown spectroscopy

Time-resolved measurement of atomic emission enhancement is performed by using a 500-fs KrF laser pulse incident upon a high density supersonic O2 gas jet, synchronized with an orthogonal ns frequency-doubled Nd：YAG laser pulse. The ultra-short pulse serves as an igniter of the gas jet, and the subsequent ns-laser pulse significantly enhances the atomic emission. Analysis shows that the contributions to the enhancement effect are made mainly by the bremsstrahlung radiation and cascade ionization.

New Time-resolved-Tween 80 Chemiluminescent System for Simultaneous Determination of Trace Gold and Osmium

A time resolved chemiluminescent analysis for simultaneous determination of trace Au(Ⅲ) and Os(Ⅳ) was proposed. The method is based on the kinetic distinction of Au(Ⅲ) and Os(Ⅳ) in Tween 80 KOH chemilumescent system. The detection limits were 1.1×10 -9 g/ml for Au(Ⅲ) and 1.0×10 -8 g/ml for Os(Ⅳ), with the linear ranges of 1.0×10 -8 ～1.0×10 -5 g/ml for Au(Ⅲ) and 1.0×10 -7 ～1.0×10 -6 g/ml for Os(Ⅳ). The method was applied to the determination of Au(Ⅲ) and Os(Ⅳ) in the sample of metallurgical materials of noble metals with satisfactory results.

Development of time-resolved immunofluorometric assays for the detection of house dust mite-allergic IgE in human sera

Dermatophagoides farinae and D. pteronyssinus are the prevalent house dust mites (HDM) in tropical countries and are associated with allergic diseases. This investigation developed a time- resolved immunofluorometric assay (TR-IFMA) for the first time to detect specific IgE antibody in patients with skin prick test positive to HDM but no detectable IgE by other means. Levels of IgE to natural and recombinant HDM allergens were measured by TR-IFMA in 50 HDM-allergic patients and 19 healthy participants compared to sandwich enzyme-linked immunosorbent assay (ELISA). A recombinant allergen, rDerf2, showed a 14 kDa band corresponding to broad range proteins of natural HDM.TR-IFMA showed sensitivity lower than 0.35 kUA/l. TR-IFMA employing three HDM antigens showed good correlations with sandwich ELISA at R2 0.93-0.96. TR-IFMA detected HDM IgE in 62, 62, 25 percent of allergic patient serum sample compared to 28, 32, and 22 percent detected by ELISA result using three HDM allergen. TR-IFMA also detected 26.3, 31.6, and 5.3 percent positive samples from 19 healthy participants while ELISA showed 0, 5.3, and 0 percents IgE positive samples. The use of rDerf2 as an HDM allergen for the assay was verified with no statistically different from other HDM allergens. TR-IFMA showed lower detection limit than ELISA and yielded higher sensitivity for serum of people with allergic symptoms with no detectable HDM IgE. It is anticipated that TR-IFMA for HDM-specific IgE detection will play an important role in future diagnosis of HDM allergy in clinical laboratories and for different research purposes.

Coherent coupling between vibrational modes of C-H bonds at different positions studied by femtosecond time-resolved coherent anti-Stokes Raman scattering

We performed femtosecond time-resolved coherent anti-Stokes Raman scattering （fs-CARS） measurements on liquid toluene and PVK film. For both samples, we selectively excited the CH stretching vibrational modes and observed the expected quantum beat signals. The frequency of the well-defined beats is in good agreement with the energy difference between the two simultaneously excited modes, which demonstrates that a coherent coupling between the vibrational modes of the C H chemical bonds exists at the different positions of the molecules. The dephasing times of the excited modes are obtained simultaneously.

USING TWO-DIMENSIONAL TIME RESOLVED LIGHT SCATTERING TO STUDY THE CURE REACTION INDUCED PHASE SEPARATION PROCESS OF EPOXY-AMINE-POLYETHERSULFONE BLEND WITH SECONDARY PHASE SEPARATION

The generalized two-dimensional correlation analysis based on time-resolved light scattering patterns （2D TRLS） has been employed to study the phase separation process of an epoxy-amine-polyethersulfone blend in which the secondary phase separation takes place. The results of the 2D TRLS provided more detailed information that was not readily observed in the 1D TRLS patterns. （i） During the first process of phase separation, the sequential order of coarsening in size of the domains among the larger and smaller ones has been reversed between the diffusion regime and the hydrodynamic regime. （ii） The change of the larger domains in size, due to the hydrodynamic flow in the late stage of the first phase separation process, keeps on taking place earlier than that of the new domains appeared in the secondary phase separation process. （iii） During the secondary phase separation process the size growth of the smaller domains takes place earlier than that of the larger ones, probably due to the assumption that the coarsening mode could decrease the interface tension more quickly.

Detection of K in soil using time-resolved laser-induced breakdown spectroscopy based on convolutional neural networks

One of the technical bottlenecks of traditional laser-induced breakdown spectroscopy(LIBS) is the difficulty in quantitative detection caused by the matrix effect. To troubleshoot this problem,this paper investigated a combination of time-resolved LIBS and convolutional neural networks(CNNs) to improve K determination in soil. The time-resolved LIBS contained the information of both wavelength and time dimension. The spectra of wavelength dimension showed the characteristic emission lines of elements, and those of time dimension presented the plasma decay trend. The one-dimensional data of LIBS intensity from the emission line at 766.49 nm were extracted and correlated with the K concentration, showing a poor correlation of R_c^2?=?0.0967, which is caused by the matrix effect of heterogeneous soil. For the wavelength dimension, the two-dimensional data of traditional integrated LIBS were extracted and analyzed by an artificial neural network(ANN), showing R_v^2?=?0.6318 and the root mean square error of validation(RMSEV)?=?0.6234. For the time dimension, the two-dimensional data of time-decay LIBS were extracted and analyzed by ANN, showing R_v^2?=?0.7366 and RMSEV?=?0.7855.These higher determination coefficients reveal that both the non-K emission lines of wavelength dimension and the spectral decay of time dimension could assist in quantitative detection of K.However, due to limited calibration samples, the two-dimensional models presented over-fitting.The three-dimensional data of time-resolved LIBS were analyzed by CNNs, which extracted and integrated the information of both the wavelength and time dimension, showing the R_v^2?=?0.9968 and RMSEV?=?0.0785. CNN analysis of time-resolved LIBS is capable of improving the determination of K in soil.

TIME RESOLVED SPECTRA OF Eu(MBA)_3 PHEN COMPLEXES

Time-resolved fluorescence spectra of europium methylbenzoates (MBA)with 1,10-phenanthroline(phen)have been measured at room temperature.For each of the europium chelates,where the ligand triple states lie above the ~5D_1 level of Eu^(3-),the spectra providc evidence that the Eu^(3-) ~5D_0 state is populated by nonradiative energy transfer from the higher-lying ~5D_1,state.The relaxation time for energy decay from ~5D_1 state is measured in the microcrystals to bc of the order of a few microseconds.It is suggested that the ligand C=0 and C=C stretching vibrations and Eu-O vibrations,chclate ring and benzene ring vibrations make important contributions to the relaxation process.The ~5D\-1—~5D\-0 relaxation time of Eu- (p-MBA)_3phen is shorter than those of Eu(m-MBA)_3phen and Eu(o-MBA)_3phen since nonradiative degradation to ~5D_0 from ~5D_1 appears to be more strongly influenced by the E_u^(3+)sites in the former.

Enhancing redshift phenomenon in time-resolved photoluminescence spectra of AlGaN epilayer

AlGaN epitaxial layer has been studied by means of temperature-dependent time-integrated photoluminescence（PL）and time-resolved photoluminescence（TRPL）. An enhancing redshift phenomenon in TRPL spectra with increasing temperature was observed, and the localized excitons behaved like quasi two-dimensional excitons between 6 K and 90 K. We demonstrated that these behaviors are caused by a change in the carrier dynamics with increasing temperature due to the competition of carriers＇ localization and delocalization in the AlGaN alloy.

Time-Resolved Photoluminescence Spectra of Porous Si

he photoluminescence spectra of porous Si have been studied. Its timere-solved luminescence spectra show a red shift of luminescencc peak with increasingdelay time after exciting and a nonexponential decay. Several spectral bands withdifferent Gaussian center appear by means of the decomposition of a spetrum. Theresuits of our experiments show quantum confined characters in porous Si, and wespeculate that the short wavelength band at 465 nm is the direct band froni P_(15) toP_(25)