Application of EBSD technique to ultrafine grained and nanostructured materials processed by severe plastic deformation:Sample preparation, parameters optimization and analysis

With the help of FESEM, high resolution electron backscatter diffraction can investigate the grains/subgrains as small as a few tens of nanometers with a good angular resolution （~0.5°）. Fast development of EBSD speed （up to 1100 patterns per second） contributes that the number of published articles related to EBSD has been increasing sharply year by year. This paper reviews the sample preparation, parameters optimization and analysis of EBSD technique, emphasizing on the investigation of ultrafine grained and nanostructured materials processed by severe plastic deformation （SPD）. Detailed and practical parameters of the electropolishing, silica polishing and ion milling have been summarized. It is shown that ion milling is a real universal and promising polishing method for EBSD preparation of almost all materials. There exists a maximum value of indexed points as a function of step size. The optimum step size depends on the magnification and the board resolution/electronic step size. Grains/subgrains and texture, and grain boundary structure are readily obtained by EBSD. Strain and stored energy may be analyzed by EBSD.

Characterization, preparation, and reuse of metallic powders for laser powder bed fusion: a review

Laser powder bed fusion(L-PBF) has attracted significant attention in both the industry and academic fields since its inception, providing unprecedented advantages to fabricate complex-shaped metallic components. The printing quality and performance of L-PBF alloys are infuenced by numerous variables consisting of feedstock powders, manufacturing process,and post-treatment. As the starting materials, metallic powders play a critical role in infuencing the fabrication cost, printing consistency, and properties. Given their deterministic roles, the present review aims to retrospect the recent progress on metallic powders for L-PBF including characterization, preparation, and reuse. The powder characterization mainly serves for printing consistency while powder preparation and reuse are introduced to reduce the fabrication costs.Various powder characterization and preparation methods are presented in the beginning by analyzing the measurement principles, advantages, and limitations. Subsequently, the effect of powder reuse on the powder characteristics and mechanical performance of L-PBF parts is analyzed, focusing on steels, nickel-based superalloys, titanium and titanium alloys, and aluminum alloys. The evolution trends of powders and L-PBF parts vary depending on specific alloy systems, which makes the proposal of a unified reuse protocol infeasible. Finally,perspectives are presented to cater to the increased applications of L-PBF technologies for future investigations. The present state-of-the-art work can pave the way for the broad industrial applications of L-PBF by enhancing printing consistency and reducing the total costs from the perspective of powders.

Gold Characterization by MLA and Technological Tests-Discussion of Sample Preparation and Results

Gold has been present throughout the history of mankind and used to make jewelry and coins, and recently, acquired several industrial uses. The price of gold in international market had a significant increasing, surpassing 100% in the last five years. Thereby, deposits with low levels of gold content, gold with complex associations or in a very fine particle size became exploitable again, allowing new projects and expansion of existing ones. However, for maximum process efficiency is indispensable a deep knowledge of the characteristics of these minerals and their behavior in face of beneficiation processes. Consequently, an accurate routine for mineralogical and technological characterization is essential.

Quantitative Analysis of Heavy Metals in Water Based on LIBS with an Automatic Device for Sample Preparation

Abstract Heavy metals in water can be deposited on graphite flakes, which can be used as an enrichment method for laser-induced breakdown spectroscopy （LIBS） and is studied in this paper. The graphite samples were prepared with an automatic device, which was composed of a loading and unloading module, a quantitatively adding solution module, a rapid heating and drying module and a precise rotating module. The experimental results showed that the sample preparation methods had no significant effect on sample distribution and the LIBS signal accumulated in 20 pulses was stable and repeatable. With an increasing amount of the sample solution on the graphite flake, the peak intensity at Cu I 324.75 nm accorded with the exponential function with a correlation coefficient of 0.9963 and the background intensity remained unchanged. The limit of detection （LOD） was calculated through linear fitting of the peak intensity versus the concentration. The LOD decreased rapidly with an increasing amount of sample solution until the amount exceeded 20 mL and the correlation coefficient of exponential function fitting was 0.991. The LOD of Pb, Ni, Cd, Cr and Zn after evaporating different amounts of sample solution on the graphite flakes was measured and the variation tendency of their LOD with sample solution amounts was similar to the tendency for Cu. The experimental data and conclusions could provide a reference for automatic sample preparation and heavy metal in situ detection.

Applied Study on Magnetic Nanometer Beads in Preparation of Genechip Samples

A protocol for enrichment and adsorption of karyocyte from whole blood by using magnetic nanometer beads as solid phase absorbents was presented. The PCR amplification could be accomplished by using the nanobeads with karyocyte as template directly and the PCR products were applied on an oligonucleotide array to do gene typing. The HLA A PCR amplification system and a small HLA A oligonucleotide microarray were applied as the platform and an experiment protocol of separating karyocyte from whole blood using the magnetic nanometer beads (Fe 2O 3) were set up. The experimental conditions were also discussed. It showed that pH level of PBS eluent, Taq enzyme quantity and fragment length of products could influent the amplification results, and the magnetic nano beads could succeed in sample preparation in microarray to provide a promising way in automatic detection and lab on a chip.

Sample preparation for isotopic determination of boron in clay sediments

The procedures of sample preparation for isotopic determination of boron in clay sediments is very cumbersome, by far, there haven't been relevant reports on that. In order to establish an effective method for sample preparation, a series of experiments were carried out. In this paper, boron in clay sediments was extracted with HCl solution and purified by two-step ion exchange method. Extracted HCl solution should be adjusted to alkalescency before passing through the Amberlite IRA 743 resin column due to the fact that Amberlite IRA 743 resin absorbs boron only from alkalescent solution. However, a mass of hydroxides of Al and Fe will be precipitated when the extracted HCl solution becomes alkalescent. Hydroxides of Al and Fe have a strong adsorption capacity for boron, which can cause boron isotope fractionation. To treat precipitated hydroxides of Al and Fe, four procedures, namely direct ion exchange (DRIE), decationizing ion exchange (DCIE), once sedimentation ion exchange (OSIE) and repeated sedimentation ion exchange (RSIE) were used and assessed. The influences of the four procedures on separation and extraction and isotopic composition of boron in experimental solutions and clay sediments were also discussed. According to the results, the DRIE, DCIE and OSIE are improper. The result of sample determination indicates that when extracting boron via RSIE, with the increase of precipitation times, there's an obvious decrease in boron content in the precipitated hydroxides while a sharp increase in recovery of boron and it is favorable for weakening the influence of boron isotope fractionation. But the process of RSIE is time consuming and it may introduce boron. It needs further research to establish a more effective sample preparation method for isotopic deter- mination of boron in clay sediments.

Analytical quality-by-design approach for sample treatment of BSA-containing solutions

The sample preparation of samples conlaining bovine serum albumin（BSA）,e.g..as used in transdermal Franz diffusion cell（FDC） solutions,was evaluated using an analytical qualily-by-design（QbD）approach.Traditional precipitation of BSA by adding an equal volume of organic solvent,often successfully used with conventional HPLC-PDA,was found insufficiently robust when novel fused-core HPLC and/or UPLC-MS methods were used.In this study,three factors（acetonitrile（%）.formic acid（%） and boiling time（min）） were included in the experimental design to determine an optimal and more suitable sample treatment of BSAcontaining FDC solutions.Using a QbD and Derringer desirability（D） approach,combining BSA loss,dilution factor and variability,we constructed an optimal working space with the edge of failure defined as D〈0.9.The design space is modelled and is confirmed to have an ACN range of 83 ± 3% and FA content of 1 ±0.25%.

Sample Preparation for Monolithic Refractories Part 1:Refractory Castables

1 Scope This standard specifies the definition and test methods of flowability of dense and insulating refractory castables, and moulding equipment, moulding methods, curing and drying conditions of castables samples.

Prediction to the Efficiency of Soft Clay Sample Preparation with Vacuum Loading

Vacuum loading has been examined as a way of preparing uniformly consolidated soft clay samples. The facility and loading procedure are described in this paper. An analytical solution to the three dimensional consolidation equation is derived for estimating the degree of consolidation of the soil sample with vacuum loading. The given example shows that the predicted degree of consolidation of a soft clay bulk with vacuum loading is close to that measured in the consolidation process.

Evaluation of HemogloBind^TMtreatment for preparation of samples for cholinesterase analysis

Acetylcholine is an essential neurotransmitter found throughout the nervous system. Its action on postsynaptic receptors is regulated through hydrolysis by various carboxylesterases, especially cholinesterases (ChEs). The acute toxicity of organophosphate (OP) compounds is directly linked to their action as inhibitors of ChE. One widely used assay for evaluating ChE activity is a spectrophotometric method developed by Ellman et al. When the enzyme source is from tissues or, in particular, blood, hemoglobin displays a spectrophotometric peak at the same wave-length used to analyze cholinergic activity. This creates a substantial background that interferes with the Ellman’s assay and must be overcome in order to accurately monitor cholinesterase activity. Herein, we directly compare blood processing methods: classical method (1.67 ± 0.30 U/mL) and HemogloBindTM treatment (1.51 ± 0.17 U/mL), and clearly demonstrate that pretreatment of blood samples with HemoglobindTM is both a sufficient and rapid sample preparation method for the assessment of ChE activity using the Ellman’s method.

A Comparison of Weighing Methods Prior to Fusion Preparing Iron Samples for XRF Analysis

Sample preparation by fusion for XRF analysis is all about knowing the exact weights of the sample and the flux (sample-to-flux ratio). The whole analytical chain, including the weighing step in sample preparation prior to fusion, is of crucial importance to get precise and accurate x-ray fluorescence (XRF) results. Consequently, the weighing method will affect the quality of the analytical results given by the spectrometer. In this study, the effects of different weighing methods on the precision (RSD) of the obtained XRF results are compared to determine the best weighing method for sample preparation by fusion in terms of comparable precisions in the XRF results.

Sample Preparation of Urine Samples Prior to CE-MS in Toxicological Analysis

Capillary electrophoresis （CE） coupled with mass spectrometry （MS） with a sheath liquid interface is nowadays recognized as a powerful separation technique for drugs and metabolites analysis in human urine and can be applied in numerous fields such as clinical toxicology, drug substitution monitoring, forensic sciences and antidoping. With an acidic background electrolyte containing 15 mM ammonium formate at pH 2.5 and a sheath liquid consisting in a mixture of isopropanol/water （50：50, v/v） with 0.5% formic acid, CE-ESI-MS in positive mode demonstrated excellent performance for simultaneous analysis of basic drugs of abuse and metabolites in urine （e.g. cocaine, amphetamine, morphine and phase II metabolites）. To achieve the desired level of sensitivity, two injection modes and three sample pre-treatments were evaluated. The detection of basic drugs and phase Ⅱ metabolites in diluted urine was achieved at concentrations above 1μg/mL. In order to enhance sensitivity, a sample preparation was required. A liquid-liquid extraction （LLE） was compared with solid-phase extraction. LLE was performed at alkaline pH and samples were electrokinetically injected. A chemometric approach （Doehlert design） was carried out in order to determine optimized injection parameters. Limits of detection （LOD） down to 10 ng/mL were reached with field-amplified sample injection but phase II metabolites were not extracted. Therefore, instead of LLE a SPE was performed on C 18 sorbent, and elution fraction after washing step containing phase Ⅱ metabolites was loaded on mixed-mode anion exchanger cartridges. After electrokinetic injection, this two-step SPE allowed LOD ca. 10 ng/mL for drugs and phase Ⅱ metabolites.

Variations of trace elements and rare earth elements(REEs)treated by two different methods for snow-pit samples on the Qinghai-Tibetan Plateau and their implications

Although previous investigations of the trace elements in snow and ice from the Qinghai-Tibetan Plateau obtained interesting information about pollution from human activities on the plateau, most were based on traditional acidification methods.To emphasize the influence of the different sample-preparation methods on the records of trace elements and rare earth elements, snow samples were collected from glaciers on the Qinghai-Tibetan Plateau in China and prepared using two methods: traditional acidification and total digestion. Concentrations of 18 trace elements(Al, Ti, Fe, Rb, Sr, Ba, V, Cr, Mn, Li,Cu, Co, Mo, Cs, Sb, Pb, Tl, and U), along with 14 rare earth elements(REEs: La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er,Tm, Yb, and Lu), Y, and Th in the snow samples, were measured using inductively coupled plasma-sector field mass spectrometry(ICP-SFMS). The results showed that the mass fraction of the trace elements(defined as ratio of concentration in the acid-leachable fraction to that in the digested sample) such as Mo, Ti, Al, Rb, and V, varied from 0.06 to 0.5. The mass fraction of other trace elements varied from about 0.6 to more than 0.9; those of the REEs, Y, and Th varied from 0.34 to0.75. Lower mass fractions will lead to an overestimated contribution of other sources, especially human activities, and the underestimated fluxes of these trace elements(especially REEs, Y, and Th, as well as dust) if the REEs are used as the proxy for the crust dust. The two sample-preparation methods exhibited different REE normalized distribution patterns,REE ratios, and provenance-tracing results. The REE normalized distribution patterns and proxies in the digested samples are more reliable and integrated than those found in traditional acidification method for dust-provenance tracing.

Research on aiming methods for small sample size shooting tests of two-dimensional trajectory correction fuse

The longitudinal dispersion of the projectile in shooting tests of two-dimensional trajectory corrections fused with fixed canards is extremely large that it sometimes exceeds the correction ability of the correction fuse actuator.The impact point easily deviates from the target,and thus the correction result cannot be readily evaluated.However,the cost of shooting tests is considerably high to conduct many tests for data collection.To address this issue,this study proposes an aiming method for shooting tests based on small sample size.The proposed method uses the Bootstrap method to expand the test data;repeatedly iterates and corrects the position of the simulated theoretical impact points through an improved compatibility test method;and dynamically adjusts the weight of the prior distribution of simulation results based on Kullback-Leibler divergence,which to some extent avoids the real data being"submerged"by the simulation data and achieves the fusion Bayesian estimation of the dispersion center.The experimental results show that when the simulation accuracy is sufficiently high,the proposed method yields a smaller mean-square deviation in estimating the dispersion center and higher shooting accuracy than those of the three comparison methods,which is more conducive to reflecting the effect of the control algorithm and facilitating test personnel to iterate their proposed structures and algorithms.;in addition,this study provides a knowledge base for further comprehensive studies in the future.

Hierarchical hybrid testability modeling and evaluation method based on information fusion

In order to meet the demand of testability analysis and evaluation for complex equipment under a small sample test in the equipment life cycle, the hierarchical hybrid testability model- ing and evaluation method （HHTME）, which combines the testabi- lity structure model （TSM） with the testability Bayesian networks model （TBNM）, is presented. Firstly, the testability network topo- logy of complex equipment is built by using the hierarchical hybrid testability modeling method. Secondly, the prior conditional prob- ability distribution between network nodes is determined through expert experience. Then the Bayesian method is used to update the conditional probability distribution, according to history test information, virtual simulation information and similar product in- formation. Finally, the learned hierarchical hybrid testability model （HHTM） is used to estimate the testability of equipment. Compared with the results of other modeling methods, the relative deviation of the HHTM is only 0.52%, and the evaluation result is the most accu rate.

THE RESEARCH OF GRADATION FUSION ALGORITHM BASED ON MULTISENSOR ASYNCHRONOUS SAMPLING SYSTEM

This letter explores the distributed multisensor dynamic system, which has uniform sampling velocity and asynchronous sampling data for different sensors, and puts forward a new gradation fusion algorithm of multisensor dynamic system. As the total forecasted increment value between the two adjacent moments is the forecasted estimate value of the corresponding state increment in the fusion center, the new algorithm models the state and the forecasted estimate value of every moment. Kalman filter and all measurements arriving sequentially in the fusion period are employed to update the evaluation of target state step by step, on the condition that the system has obtained the target state evaluation that is based on the overall information in the previous fusion period. Accordingly, in the present period, the fusion evaluation of the target state at each sampling point on the basis of the overall information can be obtained. This letter elaborates the form of this new algorithm. Computer simulation demonstrates that this new algorithm owns greater precision in estimating target state than the present asynchronous fusion algorithm calibrated in time does.

Investigation of Image Fusion Between High-Resolution Image and Multi-spectral Image

On the basis of a thorough understanding of the physical characteristics of remote sensing image, this paper employs the theories of wavelet transform and signal sampling to develop a new image fusion algorithm. The algorithm has been successfully applied to the image fusion of SPOT PAN and TM of Guangdong province, China. The experimental results show that a perfect image fusion can be built up by using the image analytical solution and re-construction in the image frequency domain based on the physical characteristics of the image formation. The method has demonstrated that the results of the image fusion do not change spectral characteristics of the original image.

Mechanisms of antimicrobial peptides as characterized by solid-state NMR

Antimicrobial peptides(AMP)are small proteins that play critical roles in host defense against microbe invasion.Many AMPs disrupt the cellular membrane of microbe,while the mechanism of action of AMPs can be very sophisticated.Solid-state NMR(SSNMR)technique is powerful in characterizing the mechanism of AMPs in vivo and in vitro.This review summarizes the recent advance of SSNMR technique in AMP mechanisms characterization.We highlight the sample preparation approaches,the SSNMR spectroscopic methods,and a number of outstanding examples of AMP mechanisms elucidated via SSNMR spectroscopy.

PORCELAIN CRUCIBLE FUSION METHOD OF CERAMIC RAW MATERIALS HIGH IN ALUMINIUM AND ITS DETERMINATION

This paper introduces the ceramic materials fusion method to use porcelain crucible instead of platinum crucible. By this method, not only the funds can be saved, but also the operation becomes simple and the analysed results are accurate and reliable. On the other hand, the high fusion point materials, such as high aluminum ceramic raw ma- terials, can also be melted and their aluminum contents can be determined by this method. Thus, it can be widely used in the students laboratory and routine analysis of small and middle industrial enterprises.