Estimating the Kinematic Viscosity of Petroleum Fractions

Kinematic viscosity correlation has been developed for liquid petroleum fractions at 37.78\(\,^{\circ }\hbox {C}\) and \(98.89\,^{\circ }\hbox {C}\) (100 and \(210^{\circ }\hbox {F})\) standard temperatures using a large variety of experimental data. The only required inputs are the specific gravity and the average boiling point temperature. The accuracy of the correlation was compared with several other correlations available in the literature. The proposed correlations proved to be more accurate in predicting the viscosity at 37.78\(\,^{\circ }\hbox {C}\) and \(98.89\,^{\circ }\hbox {C}\) with average absolute deviations of 0.39 and \(0.72\hbox { mm}^{2}/\hbox {s}\), respectively. Another objective was to develop a relation for the variation of viscosity with temperature to predict the viscosity of petroleum fraction at a certain temperature from the knowledge of the viscosity for the same liquid at two other temperatures. The newly developed correlation represents a wide array of temperatures from 20 \(^{\circ }\hbox {C}\) to 150 \(^{\circ }\hbox {C}\) and viscosities from 0.14\(\hbox { mm}^{2}/\hbox {s}\) to 343.64\(\hbox { mm}^{2}/\hbox {s}\). The results have been validated with experimental data consisting of 9558 data points, yielding an overall deviation of \(0.248\hbox { mm}^{2}/\hbox {s}\) and \(\hbox {R}^{2}\) of 0.998. In addition, new formulas were developed to interconvert the viscosity of petroleum fractions from one unit of measure to another based on finding the best fit for a set of experimental data from the literature with \(R^{2}\) as high as 1.0 for many cases. Detailed analysis showed good agreement between the predicted values and the experimental data.     

The Russian National Standard of Gases Humidity and Traceability System of Humidity Measurements

The Russian national humidity standard of gases has been modernized in order to increase the number of reproducible quantities of humidity (relative humidity, dew/frost-point temperature, mole fraction) and to extend the humidity and operating temperature ranges. The basis of the standard comprises two humidity generators with operating temperature ranges from \(5\,^{\circ }\hbox {C}\) to \(90\,^{\circ }\hbox {C}\) and from \(-60\,^{\circ }\hbox {C}\) to \(15\,^{\circ }\hbox {C}\). The common working range (from \(5\,^{\circ }\hbox {C}\) to \(15\,^{\circ }\hbox {C}\)) allows comparison of the generators. The generators use the two-pressure method to generate humid gas defined in terms of the relative humidity (from 5 %rh to 98 %rh at temperatures from \(90\,^{\circ }\hbox {C}\) to \(-60\,^{\circ }\hbox {C}\)) and the one-pressure (or phase equilibrium) method to generate humid gas defined in terms of the vapor mole fraction (from 0.6 ppm to \(700\times 10^{3}\) ppm) and dew/frost-point temperature (from \(-79\,^{\circ }\hbox {C}\) to \(90\,^{\circ }\hbox {C}\)). The expanded uncertainty in the relative humidity is no more than 0.2 %rh, no more than 1.2 % in the vapor mole fraction, and no more than \(0.12\,^{\circ }\hbox {C}\) in the dew/frost-point temperature. The ordinary hygrometers are traceable to the national primary standard in accordance with the state hierarchical chain for measuring means of gas humidity. The state hierarchical chain consists of three branches for means of measurements: (a) mole fraction, (b) dew/frost-point temperature, and (c) relative humidity with each branch represented as the scheme: primary standard–secondary standard–working standard–ordinary hygrometer. Calibration and verification of working standards and ordinary hygrometers, and their traceability to the primary standard use methods of (i) direct measurements, (ii) direct comparison, or (iii) comparison with a comparator.     

Hysteresis and Instability in Some IPRT Sensors Within Temperature Ranges Extending from $$-196\,^{\circ }\hbox {C}$$ to $$150\,^{\circ }\hbox {C}$$150∘C

Industrial platinum resistance thermometer (IPRT) sensors or probes suffer from some instability on cycling over significant ranges of temperature and, specifically, from hysteresis in which the resistance tends to follow different paths for increasing temperatures compared with decreasing temperatures. The effect is well known, and cases of quite large hysteresis have been reported in the literature. Therefore, in establishing calibration and measurement capabilities for IPRT calibrations it is important to include an assessment of the performance which can be expected of a ‘typical good’ IPRT and to include this in the overall uncertainty which the laboratory can expect to achieve in such calibrations, even though the effect itself is outside the laboratory’s control. This paper presents results which have been obtained in cycling IPRT probes from four sources within various temperature ranges of current interest at NPL, between \(-196\,^{\circ }\hbox {C}\) and \(150\,^{\circ }\hbox {C}\), to see what levels of hysteresis may be expected. The cycles were carried out quite quickly in order to detect the hysteresis before it was mitigated by relaxation effects, but the time dependence was not itself studied. In most cases, hysteresis was \({<}0.0025\,^{\circ }\hbox {C}\) between \(0\,^{\circ }\hbox {C}\) and \(100\,^{\circ }\hbox {C}\), and \({<}0.0035\,^{\circ }\hbox {C}\) when the range extended down to \(-80\,^{\circ }\hbox {C}\) or up to \(150\,^{\circ }\hbox {C}\). Greater instability occurred when the sensors were cooled to \(-196\,^{\circ }\hbox {C}\).     

Influence of Thermal Annealings in Argon on the Structural and Thermochromic Properties of $$\mathrm{MoO}_{3}$$ Thin Films

The effect of thermal annealing in an inert atmosphere (argon) on the structural and thermochromic properties of \(\hbox {MoO}_{3}\) thin films was investigated. \(\hbox {MoO}_{3}\) thin films were deposited by thermal evaporation in vacuum of \(\hbox {MoO}_{3}\) powders. X-ray diffraction patterns of the films showed the presence of the monoclinic Magneli phase \(\hbox {Mo}_{9}\hbox {O}_{26}\) for annealing temperatures above \(250\,{^{\circ }}\hbox {C}\). Absorbance spectra of the films annealed in argon indicated that their thermochromic response increases with the annealing temperature in the analyzed range (23 \({^{\circ }}\hbox {C}\)–300 \({^{\circ }}\hbox {C}\)), a result opposite to the case of thermal annealings in air, for which case the thermochromic response shows a maximum value around 200 \({^{\circ }}\)C–225 \({^{\circ }}\)C and decreases for higher temperatures. These results are explained in terms of a higher density of oxygen vacancies formed upon thermal treatments in inert atmospheres.     

Small Multiple Fixed-Point Cell as Calibration Reference for a Dry Block Calibrator

A small multiple fixed-point cell (SMFPC) was designed to be used as in situ calibration reference of the internal temperature sensor of a dry block calibrator, which would allow its traceable calibration to the International Temperature Scale of 1990 (ITS-90) in the operating range of the block calibrator from \(70\,^{\circ }\hbox {C}\) to \(430\,^{\circ }\hbox {C}\). The ITS-90 knows in this temperature range, three fixed-point materials (FPM) indium, tin and zinc, with their respective fixed-point temperatures (\(\vartheta _\mathrm {FP}\)), In (\(\vartheta _\mathrm {FP}\,{=}\,156.5985\,^{\circ }\hbox {C}\)), Sn (\(\vartheta _\mathrm {FP}\,{=}\,231.928\,^{\circ }\hbox {C}\)) and Zn (\(\vartheta _\mathrm {FP}\,{=}\,419.527\,^{\circ }\hbox {C}\)). All of these FPM are contained in the SMFPC in a separate chamber, respectively. This paper shows the result of temperature measurements carried out in the cell within a period of 16 months. The test setup used here has thermal properties similar to the dry block calibrator. The aim was to verify the metrological properties and functionality of the SMFPC for the proposed application.     

Electrical and Thermal Characteristics of the Insulator–Metal Transition in Crystalline $$\hbox {V}_{2}\hbox {O}_{5}$$ Films

The electrical and thermal properties with respect to the crystallization in \(\hbox {V}_{2}\hbox {O}_{5}\) thin films were investigated by measuring the resistance at different temperatures and applied voltages. The changes in the crystal structure of the films at different temperatures were also explored using Raman measurements. The thermal diffusivity of the crystalline \(\hbox {V}_{2}\hbox {O}_{5}\) film was measured by the nanosecond thermoreflectance method. The microstructures of amorphous and crystalline \(\hbox {V}_{2}\hbox {O}_{5}\) were observed by SEM and XRD measurements. The temperature-dependent Raman spectra revealed that a structural phase transition does not occur in the crystalline film. The resistance measurements of an amorphous film indicated semiconducting behavior, whereas the resistance of the crystalline film revealed a substantial change near \(250\,{^{\circ }}\hbox {C}\), and Ohmic behavior was observed above \(380\,{^{\circ }}\hbox {C}\). This result was due to the metal–insulator transition induced by lattice distortion in the crystalline film, for which \(T_{\mathrm{c}}\) was \(260\,{^{\circ }}\hbox {C}\). \(T_{\mathrm{c}}\) of the film decreased from 260 \({^{\circ }}\hbox {C}\) to \(230\,{^{\circ }}\hbox {C}\) with increasing applied voltage from 0 V to 10 V. Furthermore, the thermal diffusivity of the crystalline film was \(1.67\times 10^{-7}\,\hbox {m}^{2}\cdot \hbox {s}^{-1}\) according to the nanosecond thermoreflectance measurements.     

Measurement of the Water Relaxation Time of $${\upvarepsilon }$$-Polylysine Aqueous Solutions

\({\upvarepsilon }\)-Polylysine is an effective food preservative. In this paper, the \({\upbeta }\)-relaxation time of \({\upvarepsilon }\)-polylysine aqueous solutions, which represents the rotational speed of a single water molecule, was measured by broadband dielectric spectroscopy at various temperatures and concentrations. The broadband dielectric spectrum of each sample containing water ranging from 35 wt% to 75 wt% at temperatures ranging from \(0\,^{\circ }\hbox {C}\) to \(25\,^{\circ }\hbox {C}\) was measured using a co-axial semirigid cable probe. The measured dielectric spectra of the samples were composed of several Debye relaxation peaks, including a shortest single molecular rotational relaxation time of water, the \({\upbeta }\)-relaxation time, longer than that of pure water. This result represents that \({\upvarepsilon }\)-polylysine suppresses the molecular kinetics of water. It is also found that the \({\upbeta }\)-relaxation time of an \({\upvarepsilon }\)-polylysine solution that contained more than 35 wt% water showed a typical Arrhenius plot in the temperature range from \(0\,^{\circ }\hbox {C}\) to \(25\,^{\circ }\hbox {C}\). The activation energy of each sample depends on the water content ratio of the sample. As indicated by its long \({\upbeta }\)-relaxation time, \({\upvarepsilon }\)-polylysine is expected to possess high abilities of suppressing freezing and ice coarsening.     

Dry Block Calibrator with Improved Temperature Field and Integrated Fixed-Point Cells

To reduce uncertainty of calibrations of contact thermometers using dry block calibrators, a concept was developed at Institute for Process Measurement and Sensor Technology of Technische Universität Ilmenau. This concept uses a multi-zone heating, heat flux sensors and a multiple fixed-point cell. The paper shows the concept and its validation on the basis of a dry block calibrator with a working temperature range of \(70\,^{\circ }\hbox {C}\) to \(430\,^{\circ }\hbox {C}\). The experimental results show a stability of \({\pm } 4\,\hbox {mK}\) for the reference temperature and axial temperature differences in the normalization block less than \({\pm }55\,\hbox {mK}\).     

Implementation of a Water Heat Pipe at CETIAT

CETIAT’s calibration laboratory, accredited by COFRAC, is a secondary thermometry laboratory. It uses overflow and stirred calibration baths \((\hbox {from} -\,80\,{^{\circ }}\hbox {C} \hbox { up } \hbox { to } +\,215\,{^{\circ }}\hbox {C})\), dry blocks and furnaces \((\hbox {from } +\,100\,{^{\circ }}\hbox {C} \hbox { up } \hbox { to } +\,1050\,{^{\circ }}\hbox {C})\) and thermostatic chambers \((\hbox {from } -\,30\,{^{\circ }}\hbox {C} \hbox { up } \hbox { to } +\,160\,{^{\circ }}\hbox {C})\). Typical calibration uncertainties that can be reached for platinum resistance thermometers in a thermostatic bath are between \(0.03\,{^{\circ }}\hbox {C}\) and \(0.06\,{^{\circ }}\hbox {C}\). In order to improve its calibration capabilities, CETIAT is working on the implementation of a gas-controlled heat pipe (GCHP) temperature generator, used for industrial sensor calibrations. This article presents the results obtained during the characterization of water GCHP for industrial applications. This is a new approach to the use of a heat pipe as a temperature generator for industrial sensor calibrations. The objective of this work is to improve measurement uncertainties and daily productivity. Indeed, as has been shown in many studies (Dunn and Reay in Heat Pipes, Pergamon Press, Oxford, 1976; Merlone et al. 2012), the temperature of the system is pressure dependent and the response time, in temperature, follows the pressure accordingly. Thanks to this generator, it is possible to perform faster calibrations with smaller uncertainties. In collaboration with INRiM, the GCHP developed at CETIAT works with water and covers a temperature range from \(+\,30\,{^{\circ }}\hbox {C}\) up to \(+\,150\,{^{\circ }}\hbox {C}\). This device includes some improvements such as a removable cover, which allows us to have different sets of thermometric wells adjustable according to the probe to be calibrated, and a pressure controller based on a temperature sensor. This article presents the metrological characterization in terms of homogeneity and stability in temperature. A rough investigation of the response time of the system is also presented in order to evaluate the time for reaching thermal equilibrium. The results obtained in this study concern stability and thermal homogeneity. The homogeneity on 200 mm is better than 5 mK and with a calibration uncertainty reduced by a factor of three.     

Measurement of the Inhomogeneity in Type B and Land–Jewell Noble-Metal Thermocouples

Inhomogeneity is the largest contributor to uncertainty in temperature measurements made with thermocouples, and the knowledge of inhomogeneity is essential if low-uncertainty measurements are required. Inhomogeneity is a particular problem for long-term applications at temperatures near or above 1500 \(^{\circ }\hbox {C}\), where pairs of alloyed noble-metal thermocouples must be used and the alloy components and potential contaminants become very mobile and cause large deviations in the Seebeck coefficient. While changes in inhomogeneity are a known and well-studied problem in noble-metal alloys at temperatures below 1100 \(^{\circ }\hbox {C}\), the effects are not well quantified at higher temperatures. This paper reports the first detailed measurements of inhomogeneity in a number of Type B and Land–Jewell thermocouples exposed to either short-term calibration up to 1600 \(^{\circ }\hbox {C}\) or long-term in situ measurements for a period of approximately 3000 h at 1600 \(^{\circ }\hbox {C}\). The inhomogeneity is measured in a high-resolution scanner operating over the range from 600 \(^{\circ }\hbox {C}\) to 900 \(^{\circ }\hbox {C}\). The results show that drifts of between 0.2 % and 0.6 % can be expected for reversible crystallographic and oxidation effects, whereas drift caused by irreversible contamination effects can be expected to be between 0.6 % and 1.1 %. It is also shown that the deviations in emfs caused by irreversible homogeneities in these thermocouples scale approximately linearly with temperature. This scalability allows uncertainties assessed at one temperature, to be extrapolated to other temperatures. Additionally it is shown that a preconditioning anneal at 1100 \(^{\circ }\hbox {C}\) should be applied both before and after calibration to remove undesirable crystallographic and rhodium-oxidation effects.     

Mesoscale evolution of non-graphitizing pyrolytic carbon in aligned carbon nanotube carbon matrix nanocomposites

Polymer-derived pyrolytic carbons (PyCs) are highly desirable building blocks for high-strength low-density ceramic meta-materials, and reinforcement with nanofibers is of interest to address brittleness and tailor multi-functional properties. The properties of carbon nanotubes (CNTs) make them leading candidates for nanocomposite reinforcement, but how CNT confinement influences the structural evolution of the PyC matrix is unknown. Here, the influence of aligned CNT proximity interactions on nano- and mesoscale structural evolution of phenol-formaldehyde-derived PyCs is established as a function of pyrolysis temperature (\(T_{\mathrm {p}}\)) using X-ray diffraction, Raman spectroscopy, and Fourier transform infrared spectroscopy. Aligned CNT PyC matrix nanocomposites are found to evolve faster at the mesoscale by plateauing in crystallite size at \(T_{\mathrm {p}}\) \(\sim\)800 \(^{\circ }\hbox {C}\), which is more than \(200\,\,^{\circ }\hbox {C}\) below that of unconfined PyCs. Since the aligned CNTs used here exhibit \(\sim\)80 nm average separations and \(\sim\)8 nm diameters, confinement effects are surprisingly not found to influence PyC structure on the atomic-scale at \(T_{\mathrm {p}}\) \(\le \)1400 \(^{\circ }\hbox {C}\). Since CNT confinement could lead to anisotropic crystallite growth in PyCs synthesized below \(\sim\)1000 \(^{\circ }\hbox {C}\), and recent modeling indicates that more slender crystallites increase PyC hardness, these results inform fabrication of PyC-based meta-materials with unrivaled specific mechanical properties.     

Synthesis,structural and dielectric properties of 0.8PMN–0.2PT relaxor ferroelectric ceramic

A 0.8PMN–0.2PT solid-solution ceramic was synthesized by columbite processing technique. The effects of sintering temperature on the density, structure and microstructure and in turn on the dielectric properties were investigated. The ceramics sintered at and above 1050\(^{\circ }\hbox {C}\) resulted in single-phase perovskite formation. However, high density >90% is achieved only after 1170\(^{\circ }\hbox {C}\). Microstructural analysis revealed that grain size increases with increase in sintering temperature. A significant increase in the peak of dielectric permittivity only after 1150\(^{\circ }\hbox {C}\) owing to increase in density is noted in this study. The quadratic law applied to this ceramic demonstrates that the transition is diffused. The broadness in phase transition and lower dielectric relaxation obtained for the composition demonstrate that the ceramic exhibits characteristics of both relaxor and normal ferroelectrics. The ceramic of composition 0.8PMN–0.2PT exhibits excellent dielectric properties \(\varepsilon _{\mathrm{r}\text {-}\mathrm{max}} =\) 20294?27338 at 100 Hz with \(T_{\mathrm{c}} = 100\)–\(96^{\circ }\hbox {C}\) at low sintering temperature 1170–1180\(^{\circ }\hbox {C}\), respectively.     

Effect of Solar Radiation on Viscoelastic Properties of Bovine Leather: Temperature and Frequency Scans

This work presents both analytical and experimental results of the effect of unfiltered natural solar radiation on the thermal and dynamic mechanical properties of Boran bovine leather at both pickling and tanning stages of preparation. Samples cut from both pickled and tanned pieces of leather of appropriate dimensions were exposed to unfiltered natural solar radiation for time intervals ranging from 0 h (non-irradiated) to 24 h. The temperature of the dynamic mechanical analyzer was equilibrated at \(30\, ^\circ \hbox {C}\) and increased to \(240\, ^\circ \hbox {C}\) at a heating rate of \(5\,^\circ \hbox {C}\cdot \hbox {Min}^{-1}\), while its oscillation frequency varied from 0.1 Hz to 100 Hz. With the help of thermal analysis (TA) control software which analyzes and generates parameter means/averages at temperature/frequency range, the graphs were created by Microsoft Excel 2013 from the means. The viscoelastic properties showed linear frequency dependence within 0.1 Hz to 30 Hz followed by negligible frequency dependence above 30 Hz. Storage modulus (\(E'\)) and shear stress (\(\sigma )\) increased with frequency, while loss modulus (\(E''\)), complex viscosity (\(\eta ^{*}\)) and dynamic shear viscosity (\(\upeta )\) decreased linearly with frequency. The effect of solar radiation was evident as the properties increased initially from 0 h to 6 h of irradiation followed by a steady decline to a minimum at 18 h before a drastic increase to a maximum at 24 h. Hence, tanning industry can consider the time duration of 24 h for sun-drying of leather to enhance the mechanical properties and hence the quality of the leather. At frequencies higher than 30 Hz, the dynamic mechanical properties are independent of the frequency. The frequency of 30 Hz was observed to be a critical value in the behavior in the mechanical properties of bovine hide.     

First Interlaboratory Comparison on Calibration of Temperature-Controlled Enclosures in Turkey

The number of accredited laboratories in the field of calibration of temperature-controlled enclosures has been increasing in Turkey. One of the main criteria demonstrating the competence of a calibration laboratory is successful participation in interlaboratory comparisons. Therefore, TUBITAK UME Temperature Laboratory organized the first interlaboratory comparison on “Calibration of Temperature-Controlled Enclosures” in Turkey as a pilot laboratory between January and November, 2013. Forty accredited laboratories which provide routine calibration services to the industry in this field participated in the comparison. The standards used during the comparison was a climatic chamber for the measurements at \(-40\, {^{\circ }}\hbox {C},\,-20\, {^{\circ }}\hbox {C}, 40\, {^{\circ }}\hbox {C}\) and \(100\, {^{\circ }}\hbox {C}\) and an oven for the measurements at \(200\, {^{\circ }}\hbox {C}\). The protocol of the comparison was prepared considering guide EURAMET cg-20 and BS EN/IEC standards 600068-3-5 and 600068-3-11. During the comparison measurements, each participant had the liberty to choose the most convenient calibration points in terms of their accreditation scope among the values mentioned above and carried out on-site measurements at UME. The details and the results of this comparison are given in the paper. Determination of the statistical consistency of the results with the uncertainties given by the participants can be assessed by the method of \(E_{n}\) value assessment for each laboratory. \(E_{n}\) values for all measurement results based on the results of pilot and participating laboratories were calculated.     

Identification and Characterization of New Materials for Construction of Heating Plates for High-Temperature Guarded Hot Plates

The selection of a material for making the hot and cold plates of high-temperature guarded hot plates (HTGHPs) working up to \(800\,{^\circ }\hbox {C}\) is still an issue. The material must be machinable, have a high mechanical stability to keep the high level of flatness of the plates and have a high thermal conductivity and a high resistance to oxidation when used in air. Nickel 201 alloy has been used in several instruments, but has shown, sometimes, problems of mechanical stability. The total hemispherical emissivity of the plates must be higher than 0.8 as recommended by the standards. Three ceramic materials, a silicon infiltrated silicon carbide (SiSiC), a machinable aluminum nitride and a sintered aluminum nitride (AlN) with high thermal conductivity claimed at ambient temperature, were selected for tests in thermal conductivity and opacity to thermal radiation. Three paints withstanding high temperatures were tested in total hemispherical emissivity and durability at high temperature. Above \(600\,{^\circ }\hbox {C}\), Nickel 201 alloy has a higher thermal conductivity than the three ceramics. Below \(600\, \,{^\circ }\hbox {C}\), the SiSiC and the sintered AlN have a thermal conductivity significantly higher than Nickel 201, but the sintered AlN shows a wide transparency spectral band at short wavelengths (below \(6.5\,\upmu \hbox {m}\)). Above \(300\,{^\circ }\hbox {C}\), the three paints have a total hemispherical emissivity above 0.8. One of the paints has polluted the specimens of an insulation material tested in thermal conductivity up to \(650\,{^\circ }\hbox {C}\). The other two can be recommended to coat the hot and cold plates of HTGHPs used up to \(800\,{^\circ }\hbox {C}\).     

Photoacoustic Study on the Structural Variation of Titania Nanomaterials Using the Pr (III) Ion as a Spectral Probe

In this work, \(\hbox {Pr}^{3+}\)-doped titania nanomaterials were prepared by a sol–gel method. The structural variations of the samples during the phase transitions were studied by using the \(\hbox {Pr}^{3+}\) ion as a photoacoustic spectral probe. The result shows that for the gel sample heated at \(80\,^{\circ }\hbox {C}\), the coordination environment of \(\hbox {Pr}^{3+}\) is similar to that of its aqueous ion. The f–f transitions of \(\hbox {Pr}^{3+}\) exhibit a continuous red shift along with the gel-to-anatase transition, indicating an increase of the ‘degree of covalency’ for the \(\hbox {Pr}^{3+}\) bonding. For the sample calcined at \(1100\,^{\circ }\hbox {C}\), however, the f–f transitions of \(\hbox {Pr}^{3+}\) show obvious blue shift. This can be attributed to the segregation of \(\hbox {Pr}^{3+}\) ions to the external surface during the anatase-to-rutile transition, forming \(\hbox {Pr}_{4}\hbox {Ti}_{9}\hbox {O}_{24}\). The stabilization effect of the doped \(\hbox {Pr}^{3+ }\)ions on the anatase phase of the samples is also discussed.     

Synthesis and luminescence in sol–gel auto-combustion-synthesized $$\hbox {CaSnO}_{3}{:}\hbox {Eu}^{3+}$$ phosphor

Undoped and Eu-doped \(\hbox {CaSnO}_{3}\) nanopowders were prepared by a facile sol–gel auto-combustion method calcined at \(800{^{\circ }}\hbox {C}\) for 1 h. The samples are found to be well-crystallized pure orthorhombic \(\hbox {CaSnO}_{3}\) structure. Photoluminescence (PL) measurements indicated that the undoped sample exhibits a broad blue emission at about 420–440 nm, which can be recognized from an intrinsic centre or centres in \(\hbox {CaSnO}_{3}\). Eu-doped \(\hbox {CaSnO}_{3}\) showed broad blue emission centred about 434 nm, a weak peak at 465 nm and a sharp intense yellow emission line at 592 nm. The emission situated at 592 nm was assigned to the f–f transition of \(^{5}\hbox {D}_{0}\rightarrow ^{7}\hbox {F}_{1}\) in \(\hbox {Eu}^{3+}\) ions. The afterglow emission and PL decay results in Eu-doped \(\hbox {CaSnO}_{3}\) phosphor, which revealed that there are at least two different traps in this phosphor. From the obtained results, \(\hbox {Eu}^{3+}\)-doped \(\hbox {CaSnO}_{3}\) phosphor could be proposed as a potential white luminescent optical material.     

Cooling of High-Power LED Lamp Using a Commercial Paraffin Wax

Commercial paraffin wax used by Bolsius Nederland B.V. for manufacturing various kinds of candles was applied as a phase-change material (PCM) for cooling a 28 W high-power light emitting diode (LED) panel during its operation. The main problem arising during operation of an LED is thermal management. According to the manufacturer’s datasheet specifications (BioSolution Ltd. www.biosolution.pl), the operating temperature range for the LED street lamp UL28W is \((-30~{^{\circ }}\hbox {C})\) to \((+40~{^{\circ }}\hbox {C})\). The object of the present study was an LED panel containing 28 pieces of high-power 1W LEDs connected in series (4 LEDs in each of the 7 rows) mounted on an aluminum plate of dimensions 80 mm by 135 mm. The tested aluminum plate was placed in a block made of aluminum with a hollow compartment containing Bolsius paraffin wax of density \(914~\hbox {kg}\cdot \hbox {m}^{-3}\) at room temperature. Temperatures were recorded using K-type thermocouples at selected locations of the tested LED panel for several values of the power supplied to it, while utilizing PCM and without it. As the manufacturer of Bolsius wax candles does not provide any data on the thermal properties of the material used, it was necessary to carry out micro-calorimetric research. Thermophysical properties of the paraffin wax such as the apparent specific heat, enthalpy of phase transition and temperature of phase change transition during heating and cooling were determined using the Netzsch DSC 214 Polyma. The Netzsch TG 209F3 Tarsus was used for TG/DTG measurements. DSC investigations revealed the following thermal transitions taking place during the first heating: solid–solid transition (onset \(30.4~{^{\circ }}\hbox {C}\), peak at \(40.9~{^{\circ }}\hbox {C}\)), solid–liquid transition (onset \(47.7~{^{\circ }}\hbox {C}\), peak at \(54.9~{^{\circ }}\hbox {C}\), end at \(58.3~{^{\circ }}\hbox {C}\)), latent heat of energy storage \(201~\hbox {J}\cdot \hbox {g}^{-1}\), apparent specific heat corresponding to peak at \(41.5~{^{\circ }}\hbox {C}\) \((5.498~\hbox {J}\cdot \hbox {g}^{-1}\cdot \hbox {K}^{-1})\). DTG investigations revealed that the decomposition of paraffin wax is a two-step process. At \(283~{^{\circ }}\hbox {C}\) there was observed a slightly slower decomposition \((9.43\,\%\cdot \hbox {min}^{-1})\) than that at \(323~{^{\circ }}\hbox {C} (12.5\,\%\cdot \hbox {min}^{-1})\). The experimental results obtained upon cooling the high-power LED lamp during its operation can be applied to verify results of numerical modeling of the heat transfer problems with phase-change transitions. An attempt at modeling such a problem based on 1D fixed grid with variable time step approach was undertaken in this work.     

The Melting Point of Palladium Using Miniature Fixed Points of Different Ceramic Materials: Part II—Analysis of Melting Curves and Long-Term Investigation

Fifteen miniature fixed-point cells made of three different ceramic crucible materials (\(\hbox {Al}_{2}\hbox {O}_{3}\), \(\hbox {ZrO}_{2}\), and \(\hbox {Al}_{2}\hbox {O}_{3}(86\,\%)+\hbox {ZrO}_{2}\)(14 %)) were filled with pure palladium and used to calibrate type B thermocouples (Pt30 %Rh/Pt6 %Rh). A critical point by using miniature fixed points with small amounts of fixed-point material is the analysis of the melting curves, which are characterized by significant slopes during the melting process compared to flat melting plateaus obtainable using conventional fixed-point cells. The method of the extrapolated starting point temperature using straight line approximation of the melting plateau was applied to analyze the melting curves. This method allowed an unambiguous determination of an electromotive force (emf) assignable as melting temperature. The strict consideration of two constraints resulted in a unique, repeatable and objective method to determine the emf at the melting temperature within an uncertainty of about \(0.1\,\upmu \hbox {V}\). The lifetime and long-term stability of the miniature fixed points was investigated by performing more than 100 melt/freeze cycles for each crucible of the different ceramic materials. No failure of the crucibles occurred indicating an excellent mechanical stability of the investigated miniature cells. The consequent limitation of heating rates to values below \({\pm }3.5\,\hbox {K}\,\hbox {min}^{-1}\) above \(1100\,{^{\circ }}\hbox {C}\) and the carefully and completely filled crucibles (the liquid palladium occupies the whole volume of the crucible) are the reasons for successfully preventing the crucibles from breaking. The thermal stability of the melting temperature of palladium was excellent when using the crucibles made of \(\hbox {Al}_{2}\hbox {O}_{3}(86\,\%)+\hbox {ZrO}_{2}(14\,\%)\) and \(\hbox {ZrO}_{2}\). Emf drifts over the total duration of the long-term investigation were below a temperature equivalent of about 0.1 K–0.2 K.