Direct tensile tests on particulate agglomerates for the determination of tensile strength and interparticle bond forces

The importance of direct tensile tests on solid and capillary bonded particulate agglomerates is investigated and compared to compression test measurements. The properties of wet agglomerates are varied by changing the contact angle by means of functionalization of the particle surface. Process conditions are considered by variation of ambient humidity. A qualitative evaluation of the results is performed by analyzing the measured force distance curves of different tensile tests. The results are quantitatively evaluated by calculating the breakage strength, mass related breakage energy and breakage probability showing that the ratio between tensile and compressive tests is highly dependent on the adjusted parameters. Next to the process parameter effect, also the influence of agglomerate size is considered. Tensile strength data are used to estimate the single bond forces between the primary particles of the agglomerates. Tensile and compressive test results are compared to numerical results (DEM) of agglomerate breakage using an elastic stiff bond model.     

Development and validation of a rapid HPLC method for the determination of ketotifen in pharmaceuticals

In the present study, a simple, sensitive, rapid, and stability-indicating high performance liquid chromatographic (HPLC) method with ultraviolet detection for the analysis of ketotifen was developed and validated. The method was applied to the determination of ketotifen in pharmaceutical formulations (tablets and syrups). The HPLC method utilized isocratic elution technique with a reversed phase C8 column, detection at 297 nm and a mixture of methanol, triethylamine phosphate buffer (pH 2.8; 0.04 M), and tetrahydrofuran (43: 55: 2, v/v/v) as mobile phase at a flow rate of 1.2 mL/min. Total analysis time was about 7 min with typical retention time of ketotifen of about 5 min. The method was validated for selectivity, linearity, accuracy, and precision following International Conference of Harmonization, 1996 (ICH) recommendations. Due to its simplicity and accuracy, the method can be used for routine quality control analysis.     

Generation and validation of failure assessment diagram for notched strength prediction of solid propellant tensile specimens

Abstract

Failure assessment diagrams are generated utilising the well known inherent flaw model and stress fracture models for accurate prediction of notched tensile strength of different cracked configurations of a solid propellant material. The notched strength estimates from the fracture models are found to be close to the test results. This study indicates that any one of the above fracture models may be used for the generation of a failure assessment diagram used to predict the notched strength of cracked configurations made of solid propellant materials.     

Mathematical modelling of an experimental‐analytical method for friction coefficient determination in deep drawing

The main aim of this paper is to determine the friction coefficient μ and maximum drawing force in deep drawing process of aluminum alloy EN AW 1050 utilizing strip drawing method. Influence and interaction between lubrication condition, blank holder force and strip surface roughness on maximum drawing force and friction coefficient are investigated. Response surface methodology and D‐Optimal design are utilized in order to create an experimental plan. According to the design, 23 strip drawings experiments are performed and statistical analysis was done. The regression and variance analysis results with 18 significant mathematical models which are derived in order to describe influence of mentioned parameters on friction coefficient and maximum drawing force. Results are discussed according to previous research. Finally, the optimization of processing parameters is performed aiming for lower friction coefficient and maximal drawing force.     

A simple method for measuring tensile and shear bond strength of ceramic-ceramic and metal-ceramic joining

A simple method for measuring the ceramic-ceramic and metal-ceramic bond strength was presented, by which uniaxial tensile stress normal to the interface or shear stress in the interface can be produced using uniaxial compression load on a cross-bonded sample. Both tensile and shear bond strength were obtained by this testing technique for Ti₃SiC₂–TiO₂ and Ti₃SiC₂–Al₂O₃ composite as well as for glued steel samples, respectively. The novel method provided a solution for determining bond strength in solid (especially brittle) materials, and it is also demonstrated as a useful method for evaluating the tensile and shear strength of various glues. Electronic Publication     

Development of particle size and shape measuring system for machine-made sand

Abstract

In recent years, the use of machine-made sand has gradually increased. Simultaneous monitoring of the particle size and shape of machine-made sand during its production is vital. Here, a machine-made sand size measuring methods were developed using vibration dispersion and high-speed video imaging and subsequently evaluated. Moreover, a software system for particle size and shape identification of machine-made sand was also developed using image processing algorithms. Experiment studies on this system were conducted, and the results show that the measurement results of particle size between the vibration screening method and imaging method are different. The measurement results of particle size obtained from the imaging method were affected by the degree of dispersion and particle shape of the machine-made sand. The particle shape parameter of the machine-made sand was modified to compensate for the measurement results of particle size. After compensation for measurement results of the sand size by the imaging method, the cumulative curve of the particle size distribution was in agreement with that obtained from the vibratory sieve method; the measurement error of sand size is less than 3%. Based on sphericity characterization of the particles, the particle shape measurement using the imaging method was accurate. Thus, the particle size and shape measuring system based on imaging method met the monitoring requirements for machine-made sand.     

人工耳蜗非实时研究平台开发与验证

人工耳蜗帮助超过40万人恢复了部分听力,但其性能仍有较大提升空间,且电听觉机理仍有待进一步揭示。针对诺尔康人工耳蜗系统开发了非实时研究平台。为了验证平台的有效性,对成年植入者开展了电听觉基础心理物理实验(位置音高和包络音高)和噪声中的言语接受阈测量实验。心理物理结果显示,被试者可以按照电极位置从蜗尖到蜗底或按照幅度调制频率从50~200 Hz,产生音高上升的感觉。言语测试显示,基于该平台实现的策略,能提供与临床处理器相当水平的噪声中言语接受阈。该平台可以帮助研究者快速开展电听觉心理物理和信号处理策略方面的研究。     

Development of specimen and test method for strength analysis of MEMS micromirror

Specimens and fracture test methods for strength analysis of MEMS micromirrors were proposed. Bending and combined loading tests were performed, and torsion strength was estimated from those results. Two-parameter Weibull distribution was used to evaluate the fracture stresses estimated from the FEM model. The resulting scale and shape parameters were 787 MPa and 7.77 for the bending test and 517 MPa and 5.28 for the combined loading test. There was a difference in strength between the results of the bending and combined loading tests. From the load factor analysis, it was found that both geometry and stress distribution have to be considered to estimate the strength of MEMS since flaws are non-uniformly distributed. It was also found that torsional strength can be estimated on the safe side using the results of the combined loading test.     

Electrostatic Effects on Dispersion,Transport, and Deposition of Fine Pharmaceutical Powders: Development of an Experimental Method for Quantitative Analysis

Currently, there is no standard method for testing the electrostatic properties of pharmaceutical powders. The objective of this study was to develop a method of characterizing the dispersion, charging, and transport properties of fine powder flowing through tubes of different materials. Powders of known composition and size distribution were dispersed pneumatically and transported through a short section of tubing containing spiral baffle inserts of the same material to simulate powder flow in long sections of horizontal and vertical tubes with bends. The test powder was dispersed using ring jet suction and passed through the baffled tube to a sampling chamber, from which the powder cloud was sampled for particle size and electrostatic charge distribution measurement using an Electrical Single Particle Aerodynamic Relaxation Time (E-SPART) analyzer. Experimental data on the tribocharging and transport properties of different powders are presented along with an explanation of the charging mechanisms. Analyses of particle size and electrostatic charge distributions in real time and on a single particle basis using the E-SPART analyzer coupled with surface structure analyses with XPS and UPS showed that: (1) most powders are charged bipolarly with relatively high charge-to-mass ratio (Q/M) values that would have a strong effect on transport and deposition of powders; and (2) surface structures, particularly adsorbates, influence the work function and tribocharging of powder. Different methods, including plasma treatment, with minimal changes or contamination of the bulk properties of the powders are also suggested. pharmaceutical powders tribocharging dispersion work function charge distributions charge decay plasma treatment     

Development and evaluation of an isotope dilution LC/MS method for the determination of total homocysteine in human plasma

Elevated plasma homocysteine has been identified as a strong and independent risk factor for cardiovascular diseases, and recently, it has been associated with the development of dementia in older adults. Selected ion-monitoring isotope-dilution LC/MS (electrospray) has been developed and evaluated as a reference method for the accurate determination of total homocysteine in human plasma. Homocysteine is quantitatively isolated from plasma via the use of anion-exchange resins and then detected and quantified in stabilized plasma extracts with selected ion-monitoring LC/MS. This method is shown to be highly comparable to LC/MS/MS determinations in terms of its analytical accuracy and precision, yet this alternative measurement approach does not necessitate the enhanced instrumentation or added expense required of tandem MS/MS determinations. LC/MS detection of homocysteine was linear (standard error of the estimate for the regression line was 0.0323) over 3 orders of magnitude, and the calculated limits of detection and quantification were 0.06 micromol/L (0.12 ng on column) and 0.6 micromol/L (1.2 ng on column), respectively. Independent calibration curves showed excellent linearity (r2 > or = 0.996) between 0 and 25 micromol/L homocysteine over a 3-day period. The accuracy and precision of total homocysteine measurements for patient samples and quality control pools using LC/MS were compared to total homocysteine measurements using LC/MS/MS, GC/MS, FPIA, and LC-FD. LC/MS performed well in relation to the other homocysteine methods in terms of its capability to accurately quantify plasma homocysteine over the normal range (5-15 micromol/L).     

Generalized model for the simulation of food refrigeration. Development and validation of the predictive numerical method

A generalized mathematical model was developed to simulate food refrigeration in air. The model takes into account surface water evaporation. It allows food physical properties to be considered as functions of temperature and/or composition, while providing means for including internal heat generation, composite materials (for instance, flesh and skin) and time-varying external temperature and humidity. Wetted surfaces and packaging can also be accounted for by the model, which can be used for spheres, infinite or finite cylinders, slabs. The numerical method was developed using the Crank-Nicolson scheme, and compared with exact analytical solutions as well as with experimental data on the refrigeration of various foods.     

A study of the effect of filler metal thickness on tensile strength for a stainless steel plate-fin structure by experiment and finite element method

This paper presents a study of the effect of filler metal thickness on tensile strength for a stainless steel plate-fin structure by finite element method and experiment. The results show that the filler metal thickness has a great effect on tensile strength. The tensile strength is increased with the filler metal thickness increase, then it keeps stable when the filler metal thickness is 105–140 μm. But it decreases rapidly when the filler metal thickness is larger than 140 μm. The fracture location is shown at the end of vertical fin when the filler metal thickness is 105–140 μm. Specimens with filler metal thickness smaller or larger than 105–140 μm rupture in the brazed filler metal. The optimal filler metal thickness is 105 μm, using which can get higher strength for 304 stainless steel plate-fin structures.     

A unified and integrated numerical‐analytical approach for evaluation of Jk‐integrals of an interfacial crack in orthotropic and isotropic bimaterials

A new unified and integrated method for the numerical‐analytical calculation of J_k‐integrals of an in‐plane traction free interfacial crack in homogeneous orthotropic and isotropic bimaterials is presented. The numerical algorithm, based on the boundary element crack shape sensitivities, is generic and flexible. It applies to both straight and curved interfacial cracks in anisotropic and/or isotropic bimaterials. The shape functions of semidiscontinuous quadratic quarter point crack tip elements are correctly scaled to adapt the singular oscillatory near tip field of tractions. The length of crack is designated as the design variable to compute the strain energy release rate precisely. Although an analytical equation relating J₁ and stress intensity factors (SIFs) exists, a similar relation for J₂ in debonded anisotropic solids for decoupling SIFs is not available. An analytical expression was recently derived by this author for J₂ in aligned orthotropic/orthotropic bimaterials with a straight interface crack. Using this new relation and the present computed J_k values, the SIFs can be decoupled without the need for an auxiliary equation. Here, the aforementioned analytical relation is reconstructed for cubic symmetry/isotropic bimaterials and used with the present numerical algorithm. An example with known analytical SIFs is presented. The numerical and analytical magnitudes of J_k for an interface crack in orthotropic/orthotropic and cubic symmetry/isotropic bimaterials show an excellent agreement.     

Development and validation of spectrophotometric and HPTLC methods for simultaneous determination of rosiglitazone maleate and metformin hydrochloride in the presence of interfering matrix excipients

Two simple methods have been developed and validated for the simultaneous determination of rosiglitazone maleate (ROS) and metformin hydrochloride (MET) in synthetic mixtures and coated tablets in a ratio of 1:250 (ROS:MET). The first method was a spectrophotometric one. The minor component, ROS was determined by measuring the values of absorbance at λ_max 312?nm and the D₁ amplitudes at 331?nm where MET shows no absorption contribution. However, absorbance interferences from tablet excipients were successfully corrected by D₁ at 331?nm zero-crossing technique. Study of spectral interference from tablet excipients was included in the text. Standard curves for A_max and D₁ methods were in the concentration range 20.0–80.0?μg?mL^?1. The major component, MET was determined both in binary mixtures and tablets by measuring its A_max at 236?nm. Extensive dilution eliminated any absorption contribution from the coexisting ROS or tablet matrix. Standard curves showed linearity in the concentration range 4.0–12.8?μg?mL^?1. The second method was based on high performance thin layer chromatography (HPTLC) separation of the two drugs followed by densitometric measurements of their spots at 230?nm. The separation was carried out on Merck HPTLC aluminium sheets of silica gel 60 F254 using methanol:water:NH₄Cl 1% w/v (5:4:1 v/v/v) as the mobile phase. Linear calibration graphs of peak area values were obtained versus concentrations in the range of 0.4–2.0?μg?band^?1 and 20.0–100.0?μg?band^?1 for ROS and MET, respectively. According to International Conference on Harmonisation (ICH) guidelines, different validation parameters were verified for the two methods and presented.     

Development of an automated method for simultaneous determination of low molecular weight aliphatic amines and ammonia in ambient air by diffusion scrubber coupled to ion chromatography

A method has been developed for the simultaneous determination of low molecular weight aliphatic amines and ammonia in the atmosphere. Analyte gases are collected quantitatively in high-purity deionized water of a planar diffusion scrubber, and the resultant solution is analyzed by ion chromatography. A 1-h cycle analysis could be continuously repeated. The calibrations for the amines are linear between 5 and 500 pptv. The detection limits are a few pptv with RSD of less than 3%. The calibration for ammonia shows severe curvature at high concentrations so that second-order fitting is required for accurate determination. This method was successfully applied to the environmental air analyses. The major amines in the atmosphere were trimethylamine, dimethylamine, and methylamine, and the temporal variations were closely correlated with that of ammonia, implying their identical emission sources.     

Development and validation of a versatile HPLC-DAD method for simultaneous determination of the antiviral drugs daclatasvir,ledipasvir, sofosbuvir and ribavirin in presence of seven potential impurities. Application to assay of dosage forms and dissolution studies

This study describes a simple, sensitive, specific and generic HPLC-DAD method for simultaneous determination of four drugs prescribed for treatment of Hepatitis C Virus (HCV) infection. Investigated drugs include daclatasvir (DAC), ledipasvir (LED), sofosbuvir (SOF) and ribavirin (RIB). Successful separation was accomplished using Thermohypersil BDS-C8 column (4.6?×?250?mm, 5?µm) with gradient elution of the mobile phase consisted of mixed phosphate buffer pH 7.5 and methanol. Gradient elution started with 25% methanol, ramped up linearly to 80% in 15?min then kept constant till the end of the run. Flow rate was 1.5?mL/min. Peak areas were measured at 235, 260, 315, and 332?nm for RIB, SOF, DAC, and LED, respectively. Peaks of the analytes were perfectly resolved with retention times 2.0, 12.1, 14.7, and 17.2?min for RIB, SOF, DAC, and LED, respectively. The developed method was validated according to ICH guidelines with respect to system suitability, linearity, ranges, accuracy, precision, specificity, robustness, and limits of detection and quantification. The proposed method showed good linearity in the ranges 5–500, 2–300, 0.5–75, and 0.5–75?µg/mL for RIB, SOF, DAC, and LED respectively. Limits of detection were 0.10–0.66?μg/mL for the analyzed drugs. Specificity was established by separation of target drugs from 7 process-related impurities for SOF including its major metabolite (GS-331007). Applicability of the proposed method to real life situations was assessed through the analysis of four different pharmaceutical formulations and satisfactory results were obtained. Additionally, dissolution profiles of the 4 drugs were studied using the developed method.     

Development of a cloud point extraction-spectrofluorimetric method for trace copper(II) determination in water samples and parenteral solutions

A simple and efficient cloud point extraction-spectrofluorimetric method for the determination of copper(II) in different samples has been proposed. The procedure is based on the oxidation of thiamine with copper(II) to form highly fluorescent thiochrome, its extraction to Triton X-114 micelles and spectrofluorimetric determination. The variables affecting the analytical performance were studied and optimized. The calibration graphs using the preconcentration system for copper were linear over the range 1.0-250 ng ml-1 with limit of detection of 0.29 ng ml-1. Relative standard deviation for five replicate determinations of copper at 100 ng ml-1 concentration level was 2.12%. Average recoveries between 94 and 105% were obtained for spiked samples. The method has been applied to water samples and parenteral solutions and the amounts of copper found are very similar to those obtained by a standard method.     

A simple and sensitive method for determination of vitamins D3 and K1 in rat plasma: application for an in vivo pharmacokinetic study

Purpose: To develop and to validate a simple but sensitive method for determination of vitamins D₃ and K₁ in rat plasma.

Methods: The sample treatment included protein precipitation by cold acetonitrile, evaporation, reconstitution with methanol and filtration. The chromatography conditions included Xterra RP18 3.5?µm 4.6?×?100?mm column at ambient temperature and mobile phase consisting of methanol/water (93/7, v/v) at 0.5?mL/min flow rate. Vitamin D₃ and probucol were detected at 265?nm and vitamin K₁ at 239?nm. Rats were administered intravenously by 0.1?mg/kg of vitamin D₃ or K₁ and the blood samples were withdrawn pre-administration and at pre-determined time points post-administration. The pharmacokinetic analysis was performed using a non-compartmental approach.

Results: The calibration curves in rat plasma were linear up to 5000?ng/mL for both vitamins. The limit of quantification (LOQ) was 20?ng/mL for vitamin D₃ and 40?ng/mL for K₁. Inter- and intra-day precision and accuracy were below 15%. The pharmacokinetic parameters of vitamin D₃ following intravenous administration were: AUC_0?∞?=?11323?±?1081?h?×?ng/mL, V_d?=?218?±?80?mL/kg, CL?=?8.9?±?0.8?mL/h/kg, t_1/2?=?16.8?±?5?h; and of vitamin K₁: AUC_0?∞?=?2495?±?297?h?×?ng/mL, V_d?=?60?±24?mL/kg, CL?=?40.5?±?5.1?mL/h/kg, t_1/2?=?1.1?±0.5?h.

Conclusion: The developed HPLC–UV assay is a simple and sensitive method for the determination of vitamins D₃ and K₁ in rat plasma. A higher dose of vitamin K₁ should be used in future studies for accurate estimation of pharmacokinetic parameters. The data show the suitability of the assay for pharmacokinetic studies in rats.     

Development of a selective and sensitive flotation method for determination of trace amounts of cobalt, nickel, copper and iron in environmental samples

A simple, selective and rapid flotation method for the separation-preconcentration of trace amounts of cobalt, nickel, iron and copper ions using phenyl 2-pyridyl ketone oxime (PPKO) has been developed prior to their flame atomic absorption spectrometric determinations. The influence of pH, amount of PPKO as collector, type and amount of eluting agent, type and amount of surfactant as floating agent and ionic strength was evaluated on the recoveries of analytes. The influences of the concomitant ions on the recoveries of the analyte ions were also examined. The enrichment factor was 93. The detection limits based on 3 sigma for Cu, Ni, Co and Fe were 0.7, 0.7, 0.8, and 0.7 ng mL(-1), respectively. The method has been successfully applied for determination of trace amounts of ions in various real samples.     

Application of finite element method for determination of stress intensity factor and plastic zone geometry in an aluminium alloy sheet under uniaxial tension

High strength materials have gained prominence in the fields of aero-structures, space missiles, ship-building, pressure vessels etc. However, high strength materials are often characterised by low values of crack resistance or fracture toughness. Knowledge of stress intensity factor (SIF) is essential to predict their fracture toughness. SIF values can be obtained both theoretically and experimentally. Theoretical methods include analytical techniques as well as the finite element method (FEM). The former is used for simpler geometries and the latter for complicated geometries of engineering structures. The SIF as a function of crack size in an aluminium alloy 2024-T₃ (Al-4·5% Cu, 1·5% Mg, 0·6% Mn) sheet was determined by a computer method. These values were obtained directly from the stresses as well as indirectly from strain energy release rateG andJ integral. The results agree well with the normalised values obtained from an ASTM formula. The size and shape of the plastic zone at the crack tip have been determined as a function of nominal stress for a fixed crack length. The plastic zone has the form of two ellipsoids with their maximum spreads oriented around 69° to the crack axis.