WO2019172794A1 - Instrument de mesure de la conductivité thermique d'un liquide à l'aide d'un capteur en forme d'aiguille - Google Patents

Instrument de mesure de la conductivité thermique d'un liquide à l'aide d'un capteur en forme d'aiguille Download PDF

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Publication number
WO2019172794A1
WO2019172794A1 PCT/RS2018/000017 RS2018000017W WO2019172794A1 WO 2019172794 A1 WO2019172794 A1 WO 2019172794A1 RS 2018000017 W RS2018000017 W RS 2018000017W WO 2019172794 A1 WO2019172794 A1 WO 2019172794A1
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WO
WIPO (PCT)
Prior art keywords
heating element
thermal conductivity
liquid
measuring
needle
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Application number
PCT/RS2018/000017
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English (en)
Inventor
Emila ZIVKOVIC
Andrej STANIMIROVIC
Divna MAJSTOROVIC
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Univerzitet U Beogradu
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Application filed by Univerzitet U Beogradu filed Critical Univerzitet U Beogradu
Publication of WO2019172794A1 publication Critical patent/WO2019172794A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00—Investigating or analyzing materials by the use of thermal means
    • G01N25/18—Investigating or analyzing materials by the use of thermal means by investigating thermal conductivity

Definitions

  • the present invention relates to an instrument for measuring the thermal conductivity of pure liquids and multicomponent liquid mixtures whose use is based on the transient hot wire method with the specific needle-shaped sensor and the appropriate control system for controlling the running of the instrument.
  • the present invention belongs to the field of measuring the thermophysical properties of materials, specifically, measuring the thermal conductivity of liquids.
  • the thermal conductivity of a material depends to a large extent on the physical structure, chemical composition and condition of the material itself (US 9182364). Therefore, measurement of heat conductivity of liquids is in a metrological sense a bigger challenge than measuring heat conductivity of solid substances. Measuring the thermal conductivity of substances is only possible when the temperature field is nonhomogeneous, as it causes the heat transport. However, due to the relatively free motion of molecules in substances in the liquid aggregate state and dependence of the density of the substances themselves on temperature, there are spontaneous flows in liquids, i.e. natural convection, changing the shape of the temperature field and very quickly impairing and eventually practically disabling measurement. This is not the case with solid materials.
  • the measuring techniques described so far have numerous disadvantages since they are slow, uneconomical and complicated for use. They are slow since they do not allow the examination of multiple samples simultaneously, but only one by one, they are uneconomical due to the relatively large volume of the sample needed for the measuring, and expensive, as high- purity chemicals are often used in the preparation of the samples. They are complicated because the sensor which is in the form of a thin wire, is mechanically sensitive and susceptible to damage, making cleaning difficult and often requiring the reconstruction of the sensor.
  • the technical problem solved by the present invention is how to construct a device based on the transient hot wire method allowing simultaneous measurement of the thermal conductivity of single or multiple liquid samples.
  • a needle-shaped sensor construction according to the present invention enables efficient and reliable measuring with a simple measuring procedure and maintenance of the sensors. It also allows measuring of the thermal conductivity of a small volume sample (approximately 25 ml) in comparison with the volumes required in the procedures described so far: Gosala et al., Sensors & Transducers Journal, 129 (2011) 42-56, Holeschovsky et al., Intt. J.
  • the instrument according to the present invention makes determination of the thermal conductivity and optimization of multicomponent liquid mixture compositions significantly more effective compared to the devices and methods that are so far disclosed (Buongiorno et al., Journal of Applied Physics 106 (2009) 094312, J. M. P. Franfa et al. J. Chem Eng. Data 58 (2013) 467-476).
  • Measuring methods adapted for measuring the thermal conductivity of substances in a liquid aggregate state can, in principle, be classified into stationary and nonstationary.
  • the device described in this patent application is based on the nonstationary - transient hot wire method, which is a reliable and precise technique for measuring the thermal conductivity of liquid.
  • US 9182364 describes a device for measuring the thermal conductivity implying the use of a needle-shaped sensor.
  • the field of use is the measurement of the thermal conductivity of nuclear materials in a solid state, within a nuclear reactor, i.e. in the field of strong radioactive radiation and at high temperature.
  • This device comprises the needle-shaped sensor and the control system.
  • the sensor described in this patent comprises a thermometer which is surrounded by a heating element within a sheath, as well as an electrical insulator which completely isolates the sheath, the heating element and the thermometer from each other.
  • US 4861167 describes an apparatus for measuring the thermal conductivity of melted polymers.
  • the apparatus comprises a needle-shaped portion, wherein the heating element and temperature sensor are located.
  • the needle-shaped sensor is introduced into the melted material, and when the temperature between the sensor and sample is equalized, the heating element is activated.
  • the temperature change of the material is measured using a thermocouple. Measuring is repeated in cycles, in order to determine the sample temperature change due to the activation of the heating element. Transient sample temperature change is used for calculating the thermal conductivity of the melted polymer.
  • the present invention relates to a needle-shaped sensor and instrument with one or more such sensors, intended for measuring the thermal conductivity of single and multiple liquids, simultaneously.
  • the instrument consists of one or more needle-shaped sensors, the same number of the liquid sample containers and the control system.
  • the needle-shaped sensor comprises a heating element which is at the same time a temperature change detector, current lines and voltage lines, an electrical insulator, a smaller cross section sheath, and a larger cross section sheath.
  • the heating element is heated by the electric current flow (Joule effect).
  • the rate of heating of the sensor depends on current intensity that generates heat and on the dissipation of heat into the surrounding medium - the sample of the liquid whose thermal conductivity is measured. Higher thermal conductivity of the liquid results in the greater dissipation of heat into the environment, and consequently, slower heating of the sensor. Conversely, lower thermal conductivity of the liquid results in lesser dissipation of heat and faster heating of the sensor.
  • the liquid sample container is filled with a certain amount of the liquid whose thermal conductivity is to be determined, and the needle-shaped sensor is immersed in it.
  • the control system has an electrical power supply and a multi-channel voltmeter.
  • the control system has a programmed algorithm for calculating the thermal conductivity of the liquid, based on the temperature change of the sensor while being heated by electric current from the electrical power supply.
  • the present invention relates to the needle-shaped sensor 24, as shown in Fig. 1, and the instrument 25, intended for measuring the thermal conductivity of the liquid, as well as measuring the thermal conductivity of multiple liquid samples, simultaneously, whereby the said instrument 25 comprises one or more said sensors 24.
  • the functioning of the instrument 25 and needle-shaped sensor 24 is based on the transient hot wire method for measuring thermal conductivity of the liquid.
  • the needle-shaped sensor 24 (Fig. 1) comprises a heating element 4, which is concurrently a temperature change detector, current lines 7, 8, and voltage lines 3, 9, 10, an electrical insulator 5, and a sheath consisting of a smaller cross section sheath 2 and a larger cross section sheath 11.
  • the melting temperatures of insulator 5 and the sheaths 2, 11 must be higher than the operating temperature of the heating element 4.
  • Electrical power supply 19 is connected to the heating element 4 via the current lines 7, 8, which enables the electric current to flow through the heating element 4.
  • the multi-channel voltmeter 23 is a part of the data acquisition system 20, and it is connected to the heating element 4 via voltage lines 3, 9, 10, which allows the measurement of the voltage at the ends of the heating element 4.
  • the heating element 4 is an electrical conductor, and it is placed within the sheaths 2, 11.
  • the heating element 4 may be a metal wire of a small cross-section, which is heated by the Joule effect when an electric current flows through it.
  • Electrical insulator 5 isolates the heating element 4, as well as the current lines 7, 8, and the voltage lines 3, 9, 10, from each other and from the sheaths 2, 11, except at the position of junction 6 which resulted from the spot welding of the voltage line 3, the smaller cross section sheath 2 and the heating element 4.
  • the thermal conductivity of electrical insulator 5 is high enough to prevent the accumulation of heat in the sensor 24, which could impair measuring the thermal conductivity of the sample of the liquid 1.
  • the heating element 4 represents at the same time the temperature change detector of the sensor 24, which is determined via the electrical resistance change of the heating element 4.
  • the sheath of the needle-shaped sensor 24, shown in Fig. 1, consists of two sections, whereby one section is sheath 2, with the smaller cross section and wherein the heating element 4 and one voltage line 3 are located. Another section, the sheath 11, is with the larger cross section, and wherein the current lines 7, 8, and the voltage lines 9, 10 are located. Electrical power supply 19 is electrically connected to the heating element 4 via current lines 7, 8.
  • the multi-channel voltmeter 23 registers the changes in the voltage drop at the heating element 4 through the voltage lines 3, 9, 10.
  • the current lines 7, 8 must have a larger cross section than the heating element 4.
  • the voltage line 9 and the voltage line 3 are connected by the junction 22 within the larger cross section sheath 11.
  • the instrument 25 shown in Fig. 2 may comprise one or multiple described needle-shaped sensors 24, one or multiple containers for the sample of liquid 1 and the control system 12.
  • the container for the sample of liquid 1 is filled with a certain amount of liquid 1 whose thermal conductivity is being determined, and the needle-shaped sensor 24 is immersed in it.
  • the container for the sample of liquid 1 is a vertically oriented cylinder, with a cross section that allows spreading the heat emitted by the sensor 24 in the form of a cylindrical temperature wave through the liquid sample.
  • the control system 12 consists of the electrical power supply 19 and the multi-channel voltmeter 23.
  • the control system 12 comprises programmed electrical power supply 19 which provides electric current flow through the heating element 4 over a predetermined time interval.
  • the control system 12 also comprises a programmed multi-channel voltmeter 23 that allows calculation of the temperature change based on the change of voltage at the temperature change detector.
  • the control system 12 includes a programmed algorithm for calculating the thermal conductivity of the liquid 1 based on the temperature change of the needle-shaped sensor 24.
  • the heating element 4 may be an electrical conductor, preferably in the form of a wire of a smaller cross-section, which is heated by the Joule effect.
  • the ends of the heating element 4 are electrically connected by at least two pairs of electrical conductors.
  • the first pair of conductors i.e. current lines 7, 8 of low electrical resistance, supply the heating element 4 with electric current, while the second pair of the conductors, i.e. the voltage lines 3, 9, 10, allow an accurate measurement of the voltage drop at the heating element 4.
  • the heating element 4 is at the same time the temperature change detector - a resistance thermometer whose electrical resistance changes with temperature change.
  • the temperature change detector detects the temperature change in the needle- shaped sensor 24 and allows this change to be measured.
  • the temperature change detector is a thermocouple or resistance thermometer that can withstand the operating temperature of the heating element 4.
  • the temperature change detector may be a thermocouple and in such case the temperature change is determined by measuring voltage at the thermocouple ends.
  • the temperature detector is a resistor, whose electrical resistance changes with temperature. In such case, the temperature change is determined by measuring the voltage drop at the ends of the resistor and the intensity of the current flowing through the resistor and by calculation of the electrical resistance of the resistor.
  • Electrical insulator 5 is a material whose electrical resistance prevents the flow of electric current between the elements of the needle-shaped sensor 24. Electrical insulator 5 may be selected from MgO powder, epoxy resin, etc.
  • the sheaths 2, 11 contain all the elements of the needle-shaped sensor 24.
  • the sheaths 2, 11 are made of a material that can protect the elements of the sensor 24 from external influences that could damage it.
  • the sheaths 2, 11 must be made of a material whose melting temperature is higher than the operating temperature of the heating element 4.
  • the sheaths 2, 11 may be made of steel.
  • Smaller cross section sheath 2 comprises the heating element 4 of the needle-shaped sensor 24, one voltage line 3 and the electrical insulator 5.
  • Junction 6, that resulted from the spot welding of the smaller cross section sheath 2, the heating element 4 and the voltage line 3, is placed at the end of the needle-shaped sensor 24 contacting the sample of liquid 1, whose thermal conductivity is being measured.
  • Larger cross section sheath 11 comprises and mechanically protects the current lines 7, 8 and the voltage lines 9, 10, as well as the electrical insulator 5.
  • the control system 12 is a device, or a set of devices, that controls, manages, directs and regulates the operation of the instrument 25.
  • the control system 12 is designed to control or measure the electrical voltage, electric current and temperature signals.
  • the control system 12 can measure the testing time and control the voltage supplied to the needle-shaped sensor 24.
  • the control system has a user display indicating the temperature of the needle-shaped sensor 24.
  • the control system 12 preferably has a user display indicating current intensities, voltages and other variables that are generated or measured.
  • the control system 12 must also be calibrated, in such a way that the measured values can be used for a precise calculation of the thermal conductivity of the liquid sample.
  • the control system 12 is an electronic circuit.
  • the control system 12 is a computer or a microcontroller, or a combination thereof.
  • the control system 12 comprises the multi-channel voltmeter 23. Preferably, it is a digital voltmeter (analog-to-digital converter), for measuring the voltage on the elements of the needle- shaped sensor 24 and other elements of the instrument 25.
  • the control system 12 determines a value that is functionally related to temperature change of the temperature change detector and calculates the value of the change based on the known characteristics of the sensor 24.
  • the temperature change detector is a thermocouple whose voltage is being measured, and the temperature change is calculated based on the temperature coefficient of the thermoelectric potential.
  • the temperature change detector is a resistance thermometer whose electrical resistance is measured and the temperature change is calculated based on the value of the temperature coefficient of electrical resistance.
  • the heating element 4 is at the same time a resistor whose electrical resistance change allows calculation of the change of temperature of the needle-shaped sensor 24.
  • the control system 12 comprises the electric power supply 19 that can provide voltage at the ends of the heating element 4.
  • control system 12 is programmable, so that it could control the measurement process, save the measured values, and perform mathematical calculations.
  • the control system 12 calculates the value of the heat conductivity ( k ) of the liquid 1 by using the relation k - 1 1
  • dAT/dln(t) is the slope of the linear dependence of the temperature T on the natural logarithm of time t
  • q is the heating power per unit of the length of the heating element 4, calculated from the relation IwVw VsVw
  • the heating element 4 is electrically connected to the control system 12 via two pairs of conductors: current lines 7, 8, representing the conductors with larger cross section and low electrical resistance and through which the electric current for the heating of the heating element 4 by the Joule effect is flowing, and the voltage lines 3, 9, 10, representing the conductors that allow accurate measurement of the voltage at the ends of the heating element 4.
  • the intensity of the electric current flowing through the heating element 4 is determined by measuring the voltage drop at the standard resistor 16 (Fig. 3) connected in series to the heating element 4.
  • the needle-shaped sensor 24 can be manufactured using a coaxial thermocouple of type K (J, respectively), whose alumel (iron) line plays the role of the heating element 4 and temperature change detector.
  • Figure 1 is a detailed view of a lengthwise section of the needle-shaped sensor 24, which is immersed in the sample of liquid 1, and by voltage lines 3, 9, 10 and current lines 7, 8 is connected to the control system 12.
  • the sensor 24 consists of a smaller cross section sheath 2 and a larger cross section sheath 11, the heating element 4, electrical insulator 5, current lines 7, 8, and voltage lines 3, 9, 10, as previously described.
  • the sample of liquid 1 is in contact with the needle-shaped sensor 24, comprising the smaller cross section sheath 2 and the larger cross section sheath 11, the heating element 4, the electrical insulator 5, the current lines 7, 8, and the voltage lines 3, 9, 10.
  • the heating element 4 is connected by spot welding to the voltage line 3 and the smaller cross section sheath 2 at one of its ends, at the position of junction 6 contacting the sample of the liquid 1 whose thermal conductivity is being measured.
  • the control system 12 is connected to the needle-shaped sensor 24 via current lines 7, 8 and voltage lines 3, 9, 10.
  • the smaller cross section sheath 2 comprises the heating element 4 and one voltage line 3.
  • the larger cross section sheath 11 comprises the current lines 7, 8 and voltage lines 3, 9, 10 of the needle-shaped sensor 24.
  • Figure 2 depicts one possible embodiment of the needle-shaped sensor 24 with the container for the sample of the liquid 1.
  • the sheath 2 has a smaller cross section compared to the sheath 11 having the larger cross section.
  • the needle-shaped sensor 24 is conveniently attached to the coupling element 13, connected to the needle-shaped sensor 24.
  • the reservoir 14 of the sample of the liquid 1 is a test-tube.
  • a coupling element 15 which is connected to the reservoir 14 is conveniently attached to the reservoir 14. Assembly of the needle-shaped sensor 24 and the container for the sample of the liquid 1 is shown in Figure 2.
  • Figure 3 shows a principal scheme of the control system 12 and the connection of the control system 12 and the needle-shaped sensor 24.
  • the heating element 4 of the needle-shaped sensor 24 is supplied by the electric power supply 19 through the current line 8, connected in series to the standard resistor 16, and wherein the current line 7 is spot-welded to the smaller cross section sheath 2 of the needle-shaped sensor 24.
  • Digital commands for turning on and off the supplying of the electric power supply 19 travel along digital control lines 21 (or digital signals, Fig. 3).
  • the data acquisition system 20 via the voltage lines 9, 10, 17 and 18 collects and stores data on voltages at the ends of the heating element 4 and the standard resistor 16.
  • Instrument 25 may be equipped with a number of needle-shaped sensors 24 and reservoirs for the sample of liquid 1. It is necessary for the control system 12 to comprise the multi-channel digital voltmeter 23, which enables simultaneous measuring and recording of the voltage signals with multiple standard resistors 16 and heating elements 4. It is also necessary for the electric power supply 19 to have sufficient capacity for generating heat by the Joule effect in the required number of needle-shaped sensors 24.
  • the control system 12 has to be programmed in such way that it enables the collecting and processing of the data provided by the multiple needle-shaped sensors 24.
  • Thermal conductivity is, besides density, viscosity and specific thermal capacity, one of the basic thermophysical properties necessary for designing equipment and control of processes and products in petroleum refineries, petrochemical plants and the chemical industry.
  • a typical example is the production of cooling agents for internal combustion engines (antifreeze) where thermal conductivity represents the most important feature of the product.
  • the instrument represented by this invention is suitable for industrial application since it enables quick and simple determination of the thermal conductivity of a larger number of samples within the desired temperature range. Also, the device can be used in research and development of new heating and cooling fluids for use in thermal devices as well as new solvents (for different separation processes, flue gas purification, etc.), requiring complete thermophysical characterization including determination of thermal conductivity.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)

Abstract

L'invention concerne un instrument destiné à mesurer la conductivité thermique d'échantillons liquides à la pression atmosphérique, qui est basé sur la méthode du fil chaud transitoire. La spécificité de l'instrument est qu'au lieu d'un long fil mince constitué de platine (Pt) pour la détection de la variation de température de l'échantillon, un capteur en forme d'aiguille, plus résistant mécaniquement, est utilisé. Le capteur est nettement plus robuste, plus facile à nettoyer et à entretenir, et plus durable qu'un fil mince autoporteur. L'instrument est constitué d'une ou plusieurs cellules de mesure dotées d'un capteur en forme d'aiguille, qui permettent une mesure simultanée sur un échantillon ou de multiples échantillons et un accroissement significatif du rendement de travail, en particulier dans la caractérisation de mélanges à composants multiples. Une partie intégrante de l'instrument est le logiciel correspondant qui permet la régulation des paramètres de mesure, le recueil des données et le traitement des résultats de mesure. L'instrument peut être utilisé partout où il est nécessaire de déterminer la conductivité thermique d'échantillons liquides.
PCT/RS2018/000017 2018-03-06 2018-10-25 Instrument de mesure de la conductivité thermique d'un liquide à l'aide d'un capteur en forme d'aiguille WO2019172794A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
RS20180276A RS61920B1 (sr) 2018-03-06 2018-03-06 Uređaj za merenje toplotne provodljivosti tečnosti primenom senzora u obliku igle
RSP-2018/0276 2018-03-06

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WO2019172794A1 true WO2019172794A1 (fr) 2019-09-12

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115248231A (zh) * 2022-07-19 2022-10-28 北京工业大学 一种用于磁性液体导热性能的测量装置和系统

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4861167A (en) 1988-09-28 1989-08-29 Cornell Research Foundation, Inc. Line-heat-source thermal conductivity measuring system
CN103175862A (zh) * 2013-02-28 2013-06-26 江苏大学 基于瞬态双热线法测量液体导热系数的装置
US9182364B1 (en) 2012-10-10 2015-11-10 U.S. Department Of Energy Hot wire needle probe for thermal conductivity detection

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4861167A (en) 1988-09-28 1989-08-29 Cornell Research Foundation, Inc. Line-heat-source thermal conductivity measuring system
US9182364B1 (en) 2012-10-10 2015-11-10 U.S. Department Of Energy Hot wire needle probe for thermal conductivity detection
CN103175862A (zh) * 2013-02-28 2013-06-26 江苏大学 基于瞬态双热线法测量液体导热系数的装置

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
BUONGIORNO ET AL., JOURNAL OF APPLIED PHYSICS, vol. 106, 2009, pages 094312
GOSALA ET AL., SENSORS & TRANSDUCERS JOURNAL, vol. 129, 2011, pages 42 - 56
HOLESCHOVSKY ET AL., INLT. J. HEAT MASS TRANSFER, vol. 39, 1996, pages 1135 - 1140
J. M. P. FRANCA ET AL., J. CHEM ENG. DATA, vol. 58, 2013, pages 467 - 476

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115248231A (zh) * 2022-07-19 2022-10-28 北京工业大学 一种用于磁性液体导热性能的测量装置和系统
CN115248231B (zh) * 2022-07-19 2024-06-11 北京工业大学 一种用于磁性液体导热性能的测量装置和系统

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RS61920B1 (sr) 2021-06-30

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