Experimental Measurement Methods Research Articles

The crystal structure and Gibbs free energy of formation of chukanovite as an oxidation product of carbon steel in human liver

Chukanovite has been identified as an oxidation product of carbon steel in a human liver through powder X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Steel oxidation products include siderite, chukanovite, vivianite, magnetite, goethite, 2-line ferrihydrite. Hydroxylapatite and amorphous silica surrounding the oxidized steel are precipitated from body fluid. The Rietveld refinement of the chukanovite structure shows it is as expected monoclinic, space group of P21/a, with a = 12.402(2), b = 9.414(1), c = 3.216(1) Å, β = 97.73(3)°. The standard Gibbs free energy of formation of chukanovite is estimated at −1167.2 ± 1.2 kJ mol−1 from the equilibrium between siderite and chukanovite. By using linear free energy relationship, the Gibbs free energy of formation for other isostructural phases of pokrovskite, parádsasvárite, and nullaginite are predicted. The results of this study could improve the mineralogical and geochemical properties of chukanovite which is an oxidation product of carbon steel relevant also in radioactive waste containers and oil/gas pipes. Furthermore, the combined method of experimental measurements and geochemical modeling could be a useful tool to study the formation of inorganic solid precipitates and bio-materials in biofluids, and is especially important in medical mineralogy field.

(Invited) Analytical Methods for Understanding Multiscale Thermal Transport in Li-Ion Batteries Towards Improved Safety and Performance

Li-ion cells are widely used for electrochemical energy storage and conversion in applications such as consumer electronics, transportation, grid storage, etc. Multiple transport processes such as ionic, electronic and thermal transport occur simultaneously in a Li-ion cell, and interact with each other through a number of mechanisms at multiple length scales. This considerable complexity makes it imperative to carry out a careful, analytical investigation of these transport processes for optimizing performance and ensuring safety. This presentation will summarize ongoing research on analytical modeling of heat transfer in Li-ion cells with the overarching of improving safety and performance of electrochemical devices and systems. The governing energy conservation equation in a Li-ion cell is solved in a variety of scenarios to help better understand the nature of heat transfer in the cell. Specifically the effect of temperature-dependent, exothermic decomposition processes is examined. It is shown that such processes can lead to a thermal runaway situation wherein the cell temperature becomes unbounded. It is shown whether thermal runaway occurs or not depends on the value of a specific non-dimensional parameter called the thermal runaway number which captures the contributions of three different thermal processes that combine to determine the thermal fate of the cell. This treatment offers a potential mechanism to monitor the health of a cell and proactively take measures to prevent thermal runaway before it is too late. Further, analytical modeling of temperature distribution with a cell is carried out in order to develop a method for non-invasively determining the core temperature of a cell. This is important because a direct measurement of the core temperature is not possible in most cases due to lack of physical access to the cell core. An analytical model for the temperature distribution in the cell is developed using the method of undetermined parameters. This shows that the core temperature of a cell undergoing any arbitrary process can be determined through appropriate time and space integrals of the outside temperature of the cell, combined with certain other thermal parameters. This has enabled an experimental method for non-invasive core temperature measurement of a Li-ion cell based on infrared thermography of its outside surface. These results indicate, for example, that the core temperature of the cell may be hundreds of degrees Celsius greater than the measured outside temperature during a thermal runaway event. Given that the thermal fate of the cell is ultimately governed by its peak temperature, which occurs at its core, this is an important insight into the thermal state of a cell undergoing, or close to thermal runaway. In addition to improving the understanding of fundamental heat transfer processes in a Li-ion cell, the analytical modeling work described here also forms the basis for novel techniques for measurement of critical processes and properties, thereby contributing towards improved overall safety and performance of the cell.

Membrane stabilization activity as anti-inflammatory mechanisms of Vernonia amygdalina leaves extracts

Inflammation is a normal process in the human body as a response to injury from healing process. Meanwhile, chronic inflammation will cause new health problems to patients. Anti-inflammatory agents generally used for those conditions, have several side effects to patients. The aim of this research was to find alternative anti-inflammatory agents, especially from natural sources. Vernonia amygdalina knew locally as “daun afrika” belong to family Apiaceae is one of those potential natural sources for alternative anti-inflammatory agents. This plant is known astraditionalmedicine from East Kalimantanfor health problems caused by the muscle stiffness and used as material in this research. The experimental method of anti-inflammatory measurement using membrane stabilization activity for V. amygdalina leaves extracts. The results showed that significant differences of EC50(p<0.05)achieved between indomethacin as the positive control (26.39 ± 2.91 µg/mL) with V. amygdalina leaves extracts for concentration 1% (131.81 ± 2.95 µg/mL) and 10% (62.54 ± 2.05 µg/mL). EC50 of V.amygdalina leaves extracts showed the potential anti-inflammatory activities. It could be concluded that V. amygdalina leaves extracts to have anti-inflammatory activities, which could be further developed as a new natural source of the anti-inflammatory agents.

Evaluation of residual stress development in FRP-metal hybrids using fiber Bragg grating sensors

This paper presents experimental measurement methods for the determination and evaluation of process related thermal residual stresses in fiber metal laminates. A cure monitoring system with fiber Bragg grating (FBG) sensors is used to measure the in-plane strains during processing of carbon fiber reinforced plastic (CFRP)-steel laminates. The simultaneous measurement captures the thermal expansion during the heating stages, the cure shrinkage, and the cooling thermal shrinkage. The results enable the characterization of the co-cure bonding process and the stress transfer between the metal and FRP-layers during the creation process. The residual strains, which are used for calculation of the residual stresses, are recorded at room temperature after manufacturing. In addition, an advanced method using FBG-sensors and the deflection of asymmetric hybrid specimens is developed to validate the gained residual stress data. Asymmetrical specimens are created by removing selected layers after cure. Quantitative evaluation is achieved by determination of their curvature and measuring the strain changes with the embedded FBG-sensors. For validation, the methods were successfully demonstrated on two different curing cycles with different resulting residual stress levels. The simultaneous strain measurement enables the investigation of stress development and delivers more in-depth process knowledge for further optimization of the manufacturing process.

ANALYSIS OF RESILIENT DESIGN BY THERMOACOUSTIC ADAPTATION OF TROPICAL URBAN MODEL

Climate and urban environment changes lead to tropical building adaptation and resilient strategy. They focus especially on thermal comfort and noise propagation variation as the result of global warming and urban growth. This study analyzes a conceptual design of tropical urban model on integrated design of thermal and acoustic (thermoacoustic) issues. By experimental measurement and simulation method using Computational Fluid Dynamics, the findings are directed to meet the standards and to recommend the new guidelines for sustainable urban building. The research location is in Surabaya as the urban tropical lowland area and Eco-House of ITS, a tropical building model in an urban environment, was built as experiment model. The results highlighted that the noise barrier should consider 5.24% of the maximum window to wall ratio (WWR) in tree dimensionally analysis, horizontally and vertically. Providing vertical ventilation is the best solution for urban density, but the orientation and its flanking noise affect the passive cooling. In general, there are some factors having a high contribution in addition to WWR, such as wind acceleration, the distance, and building material.

Experimental method for simultaneous and continuous measurement of absorption rate, viscosity and heat of reaction of carbon dioxide capture solvents

When screening solvents for carbon capture, a large amount of property data for each solvent in the CO2-loaded state is required. In this paper, a novel experimental method is proposed that involves modifying a wetted wall column in order to simultaneously measure the absorption rate, viscosity, pH, and heat of reaction of carbon capture solvents while the CO2 loading is increased continuously. The proposed method was applied to 30wt% aqueous monoethanolamine and 30wt% aqueous piperazine as solvents and found to produce measurement results that matched well with literature data.

Non-contact measurement of eyeblink by using Doppler sensor

In this report, we introduce an experimental method for eyeblink measurement by utilizing Doppler effect phenomena. In the cognitive science literature, eyeblink has been proposed as a complex phenomenon and acts as a representative of higher nervous processes. We developed an experimental setup in which the measurement of the eyeblink was conducted using a Doppler sensor accompanied by an accelerometer and an EOG (electrooculography) recording. From our experimental results, we found that the Doppler frequency related to blinking contains a dominant frequency at 2 Hz. Finally, we showed that when blinking is accompanied with head and body movements, eyeblink signal is separable by deploying the principal component analysis (PCA).

A new moving model test method for the measurement of aerodynamic drag coefficient of high-speed trains based on machine vision

A moving model test method has been proposed to measure the aerodynamic drag coefficient of a high-speed train based on machine vision technology. The total resistance can be expressed as the track friction resistance and the aerodynamic drag according to Davis equation. Cameras are set on one side of the track to capture the pictures of the train, from which the line marks on the side surface of the train are extracted and analyzed to calculate the speed and acceleration of the train. According to Newton’s second law, the aerodynamic drag coefficient can be resolved through multiple tests at different train speeds. Comparisons are carried out with the full-scale coasting test, wind tunnel test, and numerical simulation; good agreement is obtained between the moving model test and the full-scale field coasting test with difference within 1.51%, which verifies that the method proposed in this paper is feasible and reliable. This method can accurately simulate the relative movement between the train, air, and ground. The non-contact measurement characteristic will increase the test accuracy, providing a new experimental method for the aerodynamic measurement.

Impact of Dynamics on the Accuracies of Different Experimental Data-Processing Methods for Steady-State Heat Transfer Rate Measurement

It is becoming often to measure steady-state heat transfer rate from thermal systems with variable speed and volume equipment and hence with fluctuating properties and mass flow rates. However, it is unclear if the conventional heat transfer rate measurement based on averages of temperature and pressure measurement is representative enough to represent the effect of system dynamics and measure their heat transfer rates accurately. This paper studied the issue by comparing its accuracy and uncertainty to that of alternative data-processing methods with theoretically less systematic bias. The comparison was conducted with steady-state data from a variable-speed ductless heat pump (DHP) system with occasional fluctuation of refrigerant flow and properties. The results show that the accuracy improvement brought by one alternative method is statistically significant albeit small in magnitude, and the other method may reduce uncertainty of the heat transfer rate measurement in tests with large periodic changes of measured variables. Nonetheless, both alternative methods are about 100 times more computationally expensive than the conventional averaging method, and averages of temperature and pressure measurement are still appropriate when computational resources are limited.

Solubility of carbon dioxide and hydrogen sulfide in the ionic liquid 1-butyl-3-methylimidazolium trifluoromethanesulfonate

Solubility of the single gases CO2 and H2S in the ionic liquid 1-butyl-3-methylimidazolium trifluoromethanesulfonate ([C4mim][OTf]) was measured at temperatures from (303.15–343.15) K and pressures up to about 3.2 MPa for CO2 and 1.6 MPa for H2S. A modified isochoric saturation technique was developed in this study to determine the volume of the gas saturated liquid phase in the solubility measurements. The reliability of the experimental setup and measurement method was assessed through detailed comparison of generated data for CO2 + [C6mim][Tf2N] binary mixture with the most reliable data reported in the literature. The average of percent absolute relative deviation (AARD%) of pTx and specific volume data (in cm3·kg−1) measured in this work from the corresponding data in the literature is 3.7% and 0.23%, respectively. Comparison of the obtained solubility data shows that H2S is more than 4 times as soluble as CO2 in [C4mim][OTf]. The solubility of both gases in [C4mim][OTf] is higher than in the lower homologue [C2mim][OTf]. Furthermore, [C4mim][OTf] shows the highest absorption capacity for H2S and high H2S over CO2 selectivity relative to other [C4mim]/[C2mim] – based ionic liquids with different anions. The experimental data were correlated by using the extended Henry's law combined with a simplified Pitzer's model. The values of AARD% of correlated molalities from experimental data are 1.1% for CO2 + [C4mim][OTf] and H2S + [C4mim][OTf] binary mixtures. The Henry's law constants, partial molar volume at infinite dilution and thermodynamic functions for dissolution of CO2 and H2S gases in [C4mim][OTf], as a function of temperature, were calculated from the experimental data.

A critical review of preparation design and workability measurement of concrete material for largescale 3D printing

In recent few years, significant improvement has been made in developing largescale 3D printers to accommodate the need of industrial-scale 3D printing. It is of great feasibility to construct structural components and buildings by means of 3D concrete printing. The major issues of this innovative technique focus on the preparation and optimization of concrete materials which possess favourable printable properties as well as the measurement and evaluation methods of their workability. This paper firstly introduces three largescale 3D printing systems that have been successfully applied in construction industry. It then summarizes the commonly used raw materials in concrete manufacturing. Critical factors that should be particularly controlled in material preparation are specified. Easy-extrusive, easy-flowing, well-buildable, proper setting time and low shrinkage are significant for concrete mixture to meet the critical requirements of a freeform construction process. Thereafter, measuring methods that can be employed to assess the fresh and hardened properties of concrete at early stages are suggested. Finally, a few of evaluation methods are presented which may offer certain assistance for optimizing material preparation. The objective of this work is to review current design methodologies and experimental measurement and evaluation methods for 3D printable concrete materials and promote its responsible use with largescale 3D printing technology.

Determination of subpixel microdisplacements of speckle structure using the phase shift of spatial spectrum field

An experimental method for measurement of subpixel microdisplacements of speckle structure based on the parameters of the linear phase shift in the field of the complex spatial spectrum of the displaced structure is proposed and experimentally implemented. The phase shift is determined when a phase shift of spectrum is numerically added and the correlation analysis of the resulting linear phase shift in the spatial spectrum of specklegrams is performed. The method provides additional possibilities in the measurements using digital speckle photography when the period of interference fringes formed in the total spatial spectrum of specklegrams is significantly greater than the spectral width.

Characterizing the Spatially Dependent Sensitivity of Resonant Mass Sensors Using Inkjet Deposition

Micro- and millimeter-scale resonant mass sensors have received widespread attention due to their robust and sensitive performance in a wide range of detection applications. A key performance metric for such systems is the sensitivity of the resonant frequency of a device to changes in mass, which needs to be calibrated. This calibration is complicated by the fact that the position of the added mass on a sensor can have an effect on the measured sensitivity—therefore, a spatial sensitivity mapping is needed. To date, most approaches for experimental sensitivity characterization are based upon the controlled addition of small masses, e.g., the direct attachment of microbeads via atomic force microscopy or the selective microelectrodeposition of material, both of which are time consuming and require specialized equipment. This work proposes a method of experimental spatial sensitivity measurement that uses an inkjet system and standard sensor readout methodology to map the spatially dependent sensitivity of a resonant mass sensor—a significantly easier experimental approach. The methodology is described and demonstrated on a quartz resonator. In the specific case of a Kyocera CX3225 thickness-shear mode resonator, the location of the region of maximum mass sensitivity is experimentally identified.

Effects of heat input on welding buckling distortion by experimental measurement method

ABSTRACTAn experimental method based on digital image correlation technology is proposed to measure welding buckling distortion for bead-on-plane with tungsten inert gas welding. This study focuses on the effect of welding heat input for dynamic buckling and full-field distribution. The experimental results demonstrate that heat input has a great influence on welding buckling distortion. The longitudinal shrinkage of the weld bead is in direct proportion to the heat input. In the weld bead, the longitudinal plastic strain is small, while the transverse strain is large. The key points on the line, that is perpendicular to the bisector of the weld bead, experience a distorted trend of positive increase, constant displacement, negative increase and stable displacement, although the heat inputs are different.

Evaluating the accuracy of theoretical one-bond 13 C─13 C scalar couplings and their ability to predict structure in a natural product.

This study explores the feasibility of using a combination of experimental and theoretical 1-bond 13 C─13 C scalar couplings (1 JCC ) to establish structure in organic compounds, including unknowns. Historically, n JCC and n JCH studies have emphasized 2 and 3-bond couplings, yet 1 JCC couplings exhibit significantly larger variations. Moreover, recent improvements in experimental measurement and data processing methods have made 1 JCC data more available. Herein, an approach is evaluated in which a collection of theoretical structures is created from a partial nuclear magnetic resonance structural characterization. Computed 1 JCC values are compared to experimental data to identify candidates giving the best agreement. This process requires knowledge of the error in theoretical methods, thus the B3LYP, B3PW91, and PBE0 functionals are evaluated by comparing to 27 experimental values from INADEQUATE. Respective errors of ±1.2, ±3.8, and ±2.3Hz are observed. An initial test of this methodology involves the natural product 5-methylmellein. In this case, only a single candidate matches experimental data with high statistical confidence. This analysis establishes the intramolecular hydrogen-bonding arrangement, ring heteroatom identity, and conformation at one position. This approach is then extended to hydroheptelidic acid, a natural product not fully characterized in prior studies. The experimental/theoretical approach proposed herein identifies a single best-fit structure from among 26 candidates and establishes, for the first time, 1 configuration and 3 conformations to complete the characterization. These results suggest that accurate and complete structural characterizations of many moderately sized organic structures (<800Da) may be possible using only 1 JCC data.

Experimental and Measurement Methods for the Small-Scale Model Testing of Lateral and Torsional Stability

Tests of the lateral and torsional stability are quite sensitive to the experimental conditions, such as support conditions and loading system. Controlling all of these conditions in a full-size test is a very challenging task. Therefore, in this paper, an experimental measurement method that can control the experimental conditions using a small-scale model was proposed to evaluate the lateral and torsional stability of beams. For this, a loading system was provided to maintain the vertical direction of the load applied to the beam, and a support frame was produced to satisfy the in-plane and out-of-plane support conditions. The experimental method using a small-scale model was applied successively to the lateral and torsional behavior and stability of I-shaped beams. The proposed experimental methods, which effectively accommodate the changes in the geometry and length of the beam, could contribute to further experimental studies regarding the lateral and torsional stability of flexural members.

Non-coherent contributions in charge-exchange reactions and $\eta$ η - $\eta{^\prime}$ η mixing

We analyse $K^- p \to (\eta, \eta',\pi^0) \Lambda$ on the basis of the fit of data in a wide region of energies, and $\pi^- p \to (\eta, \eta') n$ at the energies of GAMS-4$\pi$. We show that disagreements between the data and the predictions of Regge theory may be explained by the mode change of summation of intermediate contributions at increasing energy, from coherent to non-coherent. A method of experimental measurement of the non-coherent contributions is proposed. On the basis of available data on the charge-exchange reactions the $\eta$--$\eta'$ mixing is estimated.

Surface tension of liquid metal: role, mechanism and application

Surface tension plays a core role in dominating various surface and interface phenomena. For liquid metals with high melting temperature, a profound understanding of the behaviors of surface tension is crucial in industrial processes such as casting, welding, and solidification, etc. Recently, the room temperature liquid metal (RTLM) mainly composed of gallium-based alloys has caused widespread concerns due to its increasingly realized unique virtues. The surface properties of such materials are rather vital in nearly all applications involved from chip cooling, thermal energy harvesting, hydrogen generation, shape changeable soft machines, printed electronics to 3D fabrication, etc. owing to its pretty large surface tension of approximately 700 mN/m. In order to promote the research of surface tension of RTLM, this paper is dedicated to present an overview on the roles and mechanisms of surface tension of liquid metal and summarize the latest progresses on the understanding of the basic knowledge, theories, influencing factors and experimental measurement methods clarified so far. As a practical technique to regulate the surface tension of RTLM, the fundamental principles and applications of electrowetting are also interpreted. Moreover, the unique phenomena of RTLM surface tension issues such as surface tension driven selfactuation, modified wettability on various substrates and the functions of oxides are discussed to give an insight into the acting mechanism of surface tension. Furthermore, future directions worthy of pursuing are pointed out.

Correlation of sorption-induced swelling in polymeric films with reference to attenuated total reflectance Fourier-transform infrared spectroscopy data

The state of the art experimental method for measurement of polymeric film swelling is the Attenuated Total Reflectance Fourier-Transform Infrared spectroscopy (FTIR-ATR). However, the costs associated to the experimental data and set-up preparation still show the need of model development to reduce such costs. Therefore, here a model is developed for prediction of swelling behavior and data of three polymeric films and the model predictions are compared and correlated to the experimental data. For evaluation of model performance and calculations, the experimental data of dilation of polycarbonate, poly (vinyl acetate), and poly (ether urethane) induced by acetonitrile vapor sorption at 40°C were collected. Desirable agreement was found between model calculated data and the experimental data with an averaged R2 value of 0.95. The developed model provides a simple, straightforward, computationally feasible and easy to use method for accurate estimation of swelling data.

Dynamic contact strain measurement by time‐resolved stroboscopic energy dispersive synchrotron X‐ray diffraction

AbstractRecent developments of synchrotron X‐ray sources and dedicated high‐energy beamlines are now enabling strain measurements from large volumes of industrially relevant metallic materials. Such capability is allowing the validation of novel and alternative nondestructive experimental methods of strain measurement or computational models of complex deformation processes. This study describes the first dynamic contact strain measurement of a ball bearing using stroboscopic energy dispersive X‐ray diffraction. The experiment probed the dynamic contact strain in the outer raceway of a test bearing. The inner raceway of the bearing was attached to a shaft rotating at 150 revolutions per minute, and the outer raceway, where the measurements were made, was fixed in a stationary bearing housing. A triggering system was used to synchronise the data acquisition of the energy dispersive X‐ray diffraction detector with the bearing rotation. Specifically, diffraction data were acquired, stroboscopically, from the material volume within the raceway, in a known location, when the ball was positioned directly below it. A total of 20 s of accumulated diffraction signal was recorded, acquiring 2 ms of data per revolution, providing diffraction patterns of sufficient quality for the dynamic contact strain to be measured. Macromechanical stress field was calculated from the micromechanical strains measured from five lattice planes. This allowed a comparison of the experimentally measured stress field and that of finite element simulations. Good agreement was observed between the finite element results and experimental measurements indicating the applicability of this novel dynamic strain measurement technique for tribological systems.