Enhancing chemical analysis with signal derivatization using simple available software packages

Derivative techniques for analytical signal processing are useful for solving some noise and signal resolution problems in various fields of study such as titrimetry, spectrophotometry, chromatography and electrochemistry. The broad use of these techniques, however, is often limited by costly inflexible built-in software packages in commercial analytical instruments. We propose here the application of commercial simple software packages such as Microsoft® Excel and Microcal Origin for signal smoothing and fitting, and for obtaining derivative analytical signals in batch and flow-based analyses, including potentiometric titration, spectrophotometry, chromatography, voltammetry and sequential injection analysis (SIA). The worldwide (especially Excel) software packages are easy-to-use for less experienced users and have also capabilities for advanced users, and therefore employing such packages can result in expansion of useful derivative techniques. We demonstrate application of the available package-aided derivative capabilities for enhancing some chemical analyses, including potentiometric acid–base titration, Bradford assay of protein, chromatographic separation of ajmaline and reserpine and anodic stripping voltammetry of copper. The derivative signals from smoothed and fitted curves offer better accuracy and precision, even for non-resolving peaks and tailing peaks. In some cases, the optimization of experimental conditions is not further required, which can lead to fast method development.     

Flow Injection/Sequential Injection Chromatography: A Review of Recent Developments in Low Pressure with High Performance Chemical Separation

This review focuses on the developments of the various parts of instrumentation and the operation of low to medium pressure flow injection and sequential injection chromatography (FIC and SIC) systems. The report and discussion include solution delivery system, separation column, flow cell and detector, mobile phase management, and online sample pretreatment. Applications of FIC and SIC and their differences as compared to HPLC are also presented.     

Pd nanoparticle-modified Bi2WO6 nanoplates used for visible-light-driven photocatalyst

Pd nanoparticles supported on Bi₂WO₆ nanoplates used for visible-light-driven photocatalyst were successfully synthesized by photoreduction deposition method under visible-light irradiation. Different analytical techniques including X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy and photoluminescence spectroscopy revealed that face-centered cubic metallic Pd nanoparticles were uniformly loaded on top of orthorhombic Bi₂WO₆ nanoplates to form heterostructure Pd/Bi₂WO₆ nanocomposites. Photocatalytic activities of pure Bi₂WO₆ sample and heterostructure Pd/Bi₂WO₆ nanocomposites were studied through the photodegradation of rhodamine B (RhB) under visible-light irradiation. The photocatalytic efficiency of Bi₂WO₆ was increased to the highest by being loaded with 5 wt% Pd and then decreased by being loaded with 10 wt% Pd. The improved photocatalytic efficiency caused by high-efficiency diffusion and separation of photo-generated charge carriers was explained and can lead to superior photodegradation of RhB under visible-light irradiation.

     

Thermal conductivity modeling of MgO/EG nanofluids using experimental data and artificial neural network

The application of nanofluids in energy systems is developing day by day. Before using a nanofluid in an energy system, it is necessary to measure the properties of nanofluids. In this paper, first the results of experiments on the thermal conductivity of MgO/ethylene glycol (EG) nanofluids in a temperature range of 25–55 °C and volume concentrations up to 5 % are presented. Different sizes of MgO nanoparticles are selected to disperse in EG, including 20, 40, 50, and 60 nm. Based on the results, an empirical correlation is presented as a function of temperature, volume fraction, and nanoparticle size. Next, the model of thermal conductivity enhancement in terms of volume fraction, particle size, and temperature was developed via neural network based on the measured data. It is observed that neural network can be used as a powerful tool to predict the thermal conductivity of nanofluids.     

The effects of channel diameter on flow pattern,void fraction and pressure drop of two-phase air–water flow in circular micro-channels

Two-phase air–water flow characteristics are experimentally investigated in horizontal circular micro-channels. Test sections are made of fused silica. The experiments are conducted based on three different inner diameters of 0.53, 0.22 and 0.15 mm with the corresponding lengths of 320, 120 and 104 mm, respectively. The test runs are done at superficial velocities of gas and liquid ranging between 0.37–42.36 and 0.005–3.04 m/s, respectively. The flow visualisation is facilitated by systems mainly including stereozoom microscope and high-speed camera. The flow regime maps developed from the observed flow patterns are presented. The void fractions are determined based on image analysis. New correlation for two-phase frictional multiplier is also proposed for practical applications.     

Flow injection in-valve-mini-column pretreatment combined with ion chromatography for cadmium, lead and zinc determination

A flow injection (FI) in-valve-mini-column packed with Chelex-100 resin is proposed for on-line sample pretreatment for some metal ions, namely, Cd(II), Pb(II) and Zn(II), prior to simultaneous determination using ion chromatography (IC). A solution containing a mixture of the cations was first passed through the in-valve-mini-column, followed by on-line elution. The eluate was then flowed further to an injection valve and was injected into an ion chromatograph. Conditions of the system were optimized. A single standard calibration was possible. The recoveries of cations were found to be in the range of 95–105%. The developed method was applied to the accurate analysis of zinc ore samples.     

Measurement of temperature-dependent thermal conductivity and viscosity of TiO2-water nanofluids

Nanofluid is an innovative heat transfer fluid with superior potential for enhancing the heat transfer performance of conventional fluids. Many attempts have been made to investigate its thermal conductivity and viscosity, which are important thermophysical properties. No definitive agreements have emerged, however, about these properties. This article reports the thermal conductivity and dynamic viscosity of nanofluids experimentally. TiO₂ nanoparticles dispersed in water with volume concentration of 0.2–2 vol.% are used in the present study. A transient hot-wire apparatus is used for measuring the thermal conductivity of nanofluids whereas the Bohlin rotational rheometer (Malvern Instrument) is used to measure the viscosity of nanofluids. The data are collected for temperatures ranging from 15 °C to 35 °C. The results show that the measured viscosity and thermal conductivity of nanofluids increased as the particle concentrations increased and are higher than the values of the base liquids. Furthermore, thermal conductivity of nanofluids increased with increasing nanofluid temperatures and, conversely, the viscosity of nanofluids decreased with increasing temperature of nanofluids. Moreover, the measured thermal conductivity and viscosity of nanofluids are quite different from the predicted values from the existing correlations and the data reported by other researchers. Finally, new thermophysical correlations are proposed for predicting the thermal conductivity and viscosity of nanofluids.     

Characterization of Li1−x Ni1+x O2 prepared by the thermal-assisted precipitation process

Li_1−x Ni_1+x O₂ was prepared by the thermal-assisted precipitation process of LiOH · H₂O and Ni(CH₃COO)₂ · 4H₂O at a pH of 6–13 followed by the high temperature calcination for a variety of prolonged times. Phases, morphologies and constituents were characterized using an x-ray diffractometer (XRD), a scanning electron microscope (SEM), an energy dispersive x-ray (EDX) analyzer an atomic absorption spectrophotometer (AAS) and titration. Maximum [I₍₀₀₃₎/I₍₁₀₄₎] and minimum [I_(006+102)/I₍₁₀₁₎] intensity ratios were used to determine the preparation conditions. In addition, possible formation reactions of the precursors and calcined products were proposed. The article was submitted by the authors in English.     

Superparamagnetic and ferromagnetic behavior of ZnFe2O4 nanoparticles synthesized by microwave-assisted hydrothermal method

Zinc ferrite (ZnFe₂O₄) nanoparticles were successfully synthesized from Zn(NO₃)₂ · 6H₂O and Fe(NO₃)₃ · 9H₂O by microwave hydrothermal method at 150°C for 1 h. Cubic ZnFe₂O₄ with particle size below 7 nm was formed in the solution at pH ≥ 6. The crystallinity and particle size of ZnFe₂O₄ nanoparticles were increased after calcination. The effects of pH of the precursor solution and calcination on the particle size and crystallinity of the particles were studied. At room temperature the products show superparamagnetic and ferromagnetic properties, determined by their size. The formation mechanism of ZnFe₂O₄ was also discussed according to the experimental results.

     

Hydrothermal synthesis of hexagonal WO3 nanowires with high aspect ratio and their electrochemical properties for lithium-ion batteries

One dimensional WO₃ nanowires with high aspect ratio of >200 were synthesized by hydrothermal method. The effects of reaction temperature and time on phase and morphologies were studied and discussed. In this research, a suitable hydrothermal condition is at 200°C for 48 h. XRD, SEM, and TEM results show that the product is hexagonal WO₃ phase with diameter of 25 nm and several ten micrometers long with growth in the c direction. The electrochemical properties were tested for rechargeable lithium batteries. The WO₃ NWs electrode exhibits a stability trend over the 30 cycle testing. Some long-term activation process is attributed to the WO₃ NWs electrode during charge/discharge reaction.