CN107884437B - Calorimeter sample cell convenient to replace and good in sealing performance - Google Patents

Calorimeter sample cell convenient to replace and good in sealing performance Download PDF

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Publication number
CN107884437B
CN107884437B CN201711327071.2A CN201711327071A CN107884437B CN 107884437 B CN107884437 B CN 107884437B CN 201711327071 A CN201711327071 A CN 201711327071A CN 107884437 B CN107884437 B CN 107884437B
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sample cell
main body
thickness
sample
hollow
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CN107884437A (en
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史全
罗积鹏
尹楠
刘忻
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/20Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity

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Abstract

The invention discloses a calorimeter sample cell with convenient sample changing and good sealing performance, which has the highest working temperature of 600K and can be conveniently and firmly fixed in a calorimeter. The sample cell specifically comprises: a metal gasket having a set dimension and hardness (mechanical strength); the sample cell comprises a sample cell main body, a cylindrical barrel, a sealing receiving module and a sealing receiving module, wherein a cylindrical well penetrating into the barrel is arranged at the center of the bottom of the cylindrical barrel so as to accommodate a thermometer-heating unit; thermowell symmetrically welded on the side surface of the sample cell; the hollow hexagonal nut is provided with an inward annular clamping groove in the upper hole; the upper part of the solid cylinder is provided with a hanging hole for hanging the sample cell, and the lower part of the solid cylinder is provided with an annular extension buckled with the annular clamping groove. The seal receiving module is a hollow cylinder with a hexagonal rectangular lower part, a threaded main body and a knife edge on the top. The sample cell has the advantages of compact structure, novel design, tight sealing, convenient sample changing and flexible use.

Description

Calorimeter sample cell convenient to replace and good in sealing performance
Technical Field
The invention belongs to a heat measuring device in calorimetric heat, in particular to a sample cell of a heat insulating heat measuring device which is convenient to change samples and good in sealing performance, and has the characteristics of excellent sealing performance, convenience in sample replacement, capability of normally working at a high temperature of 600K, and convenience and firmness in sample cell fixation.
Background
The heat capacity is the sum of energy contributions of movement forms such as crystal lattice, electrons and the like in a substance system, and is one basic thermophysical parameter of a substance. Basic thermodynamic data such as enthalpy, entropy and Gibbs free energy of a substance can be obtained through accurate measurement of heat capacity, and the method for knowing the structure and phase change of the substance is also a method for obtaining lattice vibration and electron energy level transition of a microstructure of the substance and understanding superconducting phenomena, magnetic action mechanisms and structural distortion. Therefore, the acquisition of accurate data of the heat capacity of the substance has important significance for the development and design of new materials, the optimization of the preparation process of the materials and the promotion of the understanding and development of the science of the substance.
The adiabatic heat is one of the most accurate and reliable methods for measuring the heat capacity of a substance, however, the defects of time consumption, troublesome sample changing, low and narrow working temperature area, certain expertise required by operators and the like limit the development and the use of the adiabatic heat, so the adiabatic heat measuring device is particularly important in developing and controlling the adiabatic heat measuring device, along with convenient sample changing, stable performance, high and wide working temperature area and high accuracy. The most critical link is the optimization of the structure of the sample cell, so that the sample cell not only has reliable sealing performance, but also can realize the rapid and convenient replacement of the sample, and simultaneously ensures that the calorimeter has high accuracy and precision in a high and wide temperature area.
Representative calorimetric systems currently internationally in the field of adiabatic calorimetric studies include 13-530K temperature zone devices (M.Sorai, K.Kaji, Y.Kaneko.An automated adiabatic calorimeter for the temperature range 13K to 530K The heat capacities of benzoic acid from 15K to 305K and of synthetic sapphire from 60to 505K.J.Chem.Thermodyn..1992,24,167-180.); 50-310K warm zone apparatus (T.Tanaka, T.Atake, H.Nakayama, T.Eguchi, K.Saito, I.Ikemoto.Heat capacity and an incommensurate phase transition of crystalline bis (4-chlorophenyl) sulfone.j. Chem. Thermodyn. 1994,26,1231-1239.) established by Atake, university of tokyo industrial, japan; 10-350K temperature zone device established by Van Miltenburg, university of the Netherlands Wu Dele (J.C.Van Miltenburg, G.J.K.Van Den Berg, M.J.Van Bommel. Construction of an adiabatic calorimeter measurements of the molar heat capacity of synthetic sapphire and of n-heptane.J.chem. Thermosyn., 1987,19,1129-1137.). However, the sample cells of the first two adiabatic calorimeters are sealed by pinching off the capillary tube, and the method has complex operation and poor repeatability and reliability; wu Dele university's instrument trades appearance troublesome, and sample cell and heat insulation screen zonulae occludens, is unfavorable for controlling the heat leak, influences the instrument precision. Meanwhile, the highest temperature of the three heat measuring devices does not exceed 550K, and the application of the three heat measuring devices is seriously influenced.
Therefore, there is an urgent need to develop a sample cell for an adiabatic calorimeter with compact structure, excellent performance, novel design and high temperature area, so as to meet the urgent need of research on heat capacity properties of the current condensed substances.
Disclosure of Invention
Aiming at the defects of the existing heat insulation heat measurement device, the invention provides a calorimeter sample cell with convenient sample changing and good sealing property, which has excellent sealing property, can realize quick and convenient sample changing, can work at 600K high temperature at most, does not damage the accuracy and precision of the heat insulation heat measurement device, and can be conveniently fixed in the heat measurement device.
The technical scheme of the invention is as follows: a calorimeter sample cell with convenient sample exchange and good sealing performance, comprising:
the device comprises a metal gasket 1, a sample cell main body 2, a cylindrical well 3, a seal bearing module 4, a thermowell 5, a hollow hexagonal nut 6 and a solid cylinder 7;
the sample cell main body 2 is a cylindrical barrel and comprises an upper cover 15 and a bottom cover 14, a cylindrical well 3 penetrating into the barrel is arranged in the center of the bottom of the sample cell main body 2 so as to accommodate a thermometer-heating unit, and a seal bearing module 4 is arranged at the upper part of the sample cell main body 2;
the number of the thermowells 5 is two, and the thermowells are symmetrically welded on the side surface of the sample cell main body 2;
an inward annular clamping groove 12 is formed in the upper hole of the hollow hexagonal nut 6;
the upper part of the solid cylinder 7 is provided with a hanging hole 8 for hanging the sample cell, and the lower part of the solid cylinder 7 is provided with an annular extension 13 buckled with the annular clamping groove 12;
the seal bearing module 4 is a hollow cylinder with a regular hexagon 9 in the lower section, a main body 10 with threads on the outer surface in the middle and a knife edge 11 at the top; the seal bearing module 4 is matched with the metal gasket 1 to be in threaded connection with the hollow hexagonal nut 6.
Preferably, the metal gasket 1 is made of metal or alloy with the Mohs hardness of 2-3, and has the properties of high and low temperature resistance, high heat conductivity, chemical inertness, high mechanical strength and the like.
Preferably, the metal gasket 1 is round, has a thickness of 0.1-2 mm and a diameter of 4-10 mm.
Preferably, the sample cell main body 2 is a cylindrical cylinder made of a metal or alloy with high temperature resistance, low temperature resistance, high pressure resistance, high thermal conductivity, stable chemical property and high mechanical strength, and the inner surface and the outer surface of the cylindrical cylinder are plated with a layer of metal or alloy with high temperature resistance, low temperature resistance, high thermal conductivity and stable chemical property.
Preferably, the length of the sample cell main body 2 is 40-80 mm, the outer diameter is 10-40 mm, and the thickness is 0.5-5 mm; the bottom cover 14 is a circular ring with the outer diameter of 10-40 mm, the inner diameter of 3-15 mm and the thickness of 0.5-5 mm; the upper cover 15 is a regular hexagonal ring with the outer diameter of 10-40 mm and the inner hole section of 2-10 mm and the thickness of 0.5-5 mm; the thickness of the inner plating layer and the outer plating layer of the sample cell main body 2 is 0.1-1 mm.
Preferably, the cylindrical well 3 is made of the same material as the sample cell body 2, and is closed at the top and open at the bottom; the diameter of the cylindrical well is 3-15 mm, and the length is 20-50 mm.
Preferably, the thermowell 5 is a cylinder made of metal or alloy with high thermal conductivity and high mechanical strength and is resistant to high and low temperatures, and symmetrically welded on the side surface of the sample cell main body 2; the length of the thermowell 5 is 5-25 mm, the outer diameter is 0.5-3 mm, and the thickness is 0.05-0.5 mm.
Preferably, the hollow hexagonal nut 6 is made of metal or alloy with high temperature resistance, low temperature resistance, high thermal conductivity and high mechanical strength; the thickness of the hollow hexagonal nut 6 is 2-10 mm, the side length is 2-10 mm, the inner diameter of the nut is 4-10 mm, the screw pitch is 1-2.5 mm, the thickness of the annular clamping groove 12 is 0.5-3 mm, and the inner diameter is 3-8 mm.
Preferably, the solid cylinder 7 and the hollow hexagonal nut 6 are made of the same material; the length of the solid cylinder 7 is 5-15 mm, the diameter of the solid cylinder is 3-8 mm, the diameter of the hanging hole 8 is 1-3 mm, the thickness of the annular extension 13 is 0.5-3 mm, and the outer diameter of the annular extension 13 is 4-10 mm.
Preferably, the seal receiving module 4 is a hollow cylinder made of the same material as the sample cell main body 2, and is hollow to fill or replace the sample.
Preferably, the hollow inner diameter of the seal bearing module 4 is 3-8 mm; the side length of the regular hexagon 9 is 2-10 mm, and the thickness is 2-8 mm; the outer diameter of the main body 10 is 4-10 mm, the screw pitch is 1-2.5 mm, and the length is 5-15 mm; the length of the knife edge 11 is 0.5-3 mm, and the inclination angle is 30-60 degrees.
The invention has the following beneficial effects:
(1) The sample tank has a compact structure and fine design, so that the sample in the sample tank is not leaked under the internal and external pressure difference of 100MPa, and the sample tank has excellent tightness;
(2) Through the assembly and disassembly of the hollow nut and the metal gasket, an operator can conveniently replace a sample;
(3) Because each part is closely contacted, the whole sample cell can keep good heat conduction, the temperature difference of each part is not more than 0.05K, and heat capacity data with high accuracy and precision can be obtained;
(4) The sample cell can normally work at 600K high temperature;
(5) The sample cell is fixed in the whole heat measuring device by using the hanging rope penetrating through the hanging hole;
(6) In addition, the whole sample cell can be conveniently assembled and disassembled, and direct contact between the sample cell and other parts of the heat measuring device is avoided.
Drawings
FIG. 1 is a schematic diagram of a sample cell according to the present invention.
FIG. 2 is a schematic diagram of the structure of the upper cover and the seal receiving module of the sample cell of the present invention.
Fig. 3 is a schematic structural view of the hollow hexagonal nut of the present invention.
In the figure: 1. a metal gasket; 2. a sample cell body; 3. a cylindrical well; 4. a seal receiving module; 5. a thermowell; 6. a hollow hexagonal nut; 7. a solid cylinder; 8. a hanging hole; 9. a regular hexagon; 10. a thread; 11. a knife edge; 12. an annular clamping groove; 13. annular epitaxy; 14. a bottom cover; 15. and (5) an upper cover.
Detailed Description
The invention is described in detail below with reference to the drawings and examples.
The heat insulation device achieves the heat insulation requirement by eliminating the heat exchange between the sample cell and the environment, so that accurate and reliable heat capacity data is obtained, and the sample cell structure is the important part of the design of the heat insulation device.
The calorimeter sample cell with convenient sample replacement and good sealing performance can meet the requirements of intrinsic heat insulation, high accuracy, high precision, good repeatability and the like of a heat insulation calorimeter, can realize quick and convenient replacement of a measurement sample, and still has good sealing performance at 600K high temperature.
As shown in fig. 1-3, a calorimeter sample cell with convenient sample exchange and good sealing performance comprises:
the device comprises a metal gasket 1, a sample cell main body 2, a cylindrical well 3, a seal bearing module 4, a thermowell 5, a hollow hexagonal nut 6 and a solid cylinder 7;
the sample cell main body 2 is a cylindrical barrel and comprises an upper cover 15 and a bottom cover 14, a cylindrical well 3 penetrating into the barrel is arranged in the center of the bottom of the sample cell main body 2 so as to accommodate a thermometer-heating unit, and a seal bearing module 4 is arranged at the upper part of the sample cell main body 2;
the number of the thermowells 5 is two, and the thermowells are symmetrically welded on the side surface of the sample cell main body 2;
an inward annular clamping groove 12 is formed in the upper hole of the hollow hexagonal nut 6;
the upper part of the solid cylinder 7 is provided with a hanging hole 8 for hanging the sample cell, and the lower part of the solid cylinder 7 is provided with an annular extension 13 buckled with the annular clamping groove 12;
the seal bearing module 4 is a hollow cylinder with a hexagonal 9 lower section, a main body 10 with threads on the outer surface in the middle and a knife edge 11 at the top; the seal bearing module 4 is matched with the metal gasket 1 to be in threaded connection with the hollow hexagonal nut 6.
Wherein, the metal gasket 1 is made of metal or alloy with Mohs hardness of 2-3, and has the properties of high and low temperature resistance, high heat conductivity, chemical inertness, high mechanical strength and the like.
The metal gasket 1 is round, has the thickness of 0.1-2 mm and the diameter of 4-10 mm.
The sample cell main body 2 is a cylindrical cylinder body made of metal or alloy with high temperature resistance, low temperature resistance, high pressure resistance, high heat conductivity, stable chemical property and high mechanical strength, and the inner surface and the outer surface of the cylindrical cylinder body are plated with a layer of metal or alloy with high temperature resistance, low temperature resistance, high heat conductivity and stable chemical property.
The length of the sample cell main body 2 is 40-80 mm, the outer diameter is 10-40 mm, and the thickness is 0.5-5 mm; the bottom cover 14 is a circular ring with the outer diameter of 10-40 mm, the inner diameter of 3-15 mm and the thickness of 0.5-5 mm; the upper cover 15 is a regular hexagonal ring with the outer diameter of 10-40 mm and the inner hole section of 2-10 mm and the thickness of 0.5-5 mm; the thickness of the inner and outer plating layers of the sample cell main body 2 is 0.1-1 mm.
The cylindrical well 3 is made of the same material as the sample cell main body 2, and is closed at the top and open at the bottom; the diameter of the cylindrical well is 3-15 mm, and the length is 20-50 mm.
The thermowell 5 is a cylinder made of metal or alloy with high heat conductivity and high mechanical strength and is resistant to high and low temperatures and symmetrically welded on the side surface of the sample cell main body 2; the length of the thermowell 5 is 5-25 mm, the outer diameter is 0.5-3 mm, and the thickness is 0.05-0.5 mm.
The hollow hexagonal nut 6 is made of metal or alloy with high temperature resistance, high heat conductivity and high mechanical strength; the thickness of the hollow hexagonal nut 6 is 2-10 mm, the side length is 2-10 mm, the inner diameter of the nut is 4-10 mm, the screw pitch is 1-2.5 mm, the thickness of the annular clamping groove 12 is 0.5-3 mm, and the inner diameter is 3-8 mm.
The solid cylinder 7 and the hollow hexagonal nut 6 are made of the same material; the length of the solid cylinder 7 is 5-15 mm, the diameter is 3-8 mm, the diameter of the hanging hole 8 is 1-3 mm, the thickness of the annular extension 13 is 0.5-3 mm, and the outer diameter is 4-10 mm.
The seal receiving module 4 is a hollow cylinder made of the same material as the sample cell main body 2, and is hollow to fill or replace the sample.
The hollow inner diameter of the seal bearing module 4 is 3-8 mm; the side length of the regular hexagon 9 is 2-10 mm, and the thickness is 2-8 mm; the outer diameter of the main body 10 is 4-10 mm, the screw pitch is 1-2.5 mm, and the length is 5-15 mm; the length of the knife edge 11 is 0.5-3 mm, and the inclination angle is 30-60 degrees.
The method of using the sample cell of the present invention is described below:
the following procedure was used to load and unload samples to measure the heat capacity of substances, particularly liquids:
(1) Washing each part of the sample cell with absolute ethyl alcohol for three times, and washing with deionized water for three times;
(2) Drying and baking each part of the sample cell, cooling to room temperature, weighing for three times, and taking an average value;
(3) Placing all parts and samples of the sample cell into a glove box filled with helium;
(4) Adding a sample from the hollow cylinder of the seal receiving module 4 to the sample cell body 2 until 3/4 of the sample cell volume is reached;
(5) Tightly buckling the hollow hexagon nut 6 with the solid cylinder 7 through the annular clamping groove 12 and the annular extension 13;
(6) The whole sample cell is sealed through the metal gasket 1, the seal bearing module 4 and the hollow hexagonal nut 6, and a spanner is used for applying 20N force so as to ensure equivalent tightness;
(7) Taking out the whole sample cell, weighing for three times again, taking an average value, and subtracting the average values of the former and later two times to obtain the sample mass;
(8) Fixing the thermometer-heating unit to the cylindrical well 3, the thermocouple junction to the thermowell 5;
(9) Fixing the sample cell into the heat measuring device by using a rope passing through the hanging hole 8;
(10) After other wiring or plug wires of the heat measuring device are connected, starting a heat capacity test;
(11) After the experiment is finished, the sample cell is taken down, and then the thermometer-heating unit and the thermocouple are taken down;
(12) The cell was opened and the sample was removed, and the various parts of the cell were rinsed with absolute ethanol and deionized water for the next measurement.
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.

Claims (10)

1. Calorimeter sample cell that trades appearance is convenient and leakproofness is good, a serial communication port includes:
the device comprises a metal gasket (1), a sample cell main body (2), a cylindrical well (3), a seal bearing module (4), a thermowell (5), a hollow hexagonal nut (6) and a solid cylinder (7);
the sample cell main body (2) is a cylindrical barrel and comprises an upper cover (15) and a bottom cover (14), a cylindrical well (3) penetrating into the barrel is arranged in the center of the bottom of the sample cell main body (2), and a seal bearing module (4) is arranged at the upper part of the sample cell main body (2);
the number of the thermowells (5) is two, and the thermowells are symmetrically welded on the side surface of the sample cell main body (2);
an inward annular clamping groove (12) is formed in the upper hole of the hollow hexagonal nut (6);
the upper part of the solid cylinder (7) is provided with a hanging hole (8) for hanging the sample cell, and the lower part of the solid cylinder (7) is provided with an annular extension (13) buckled with the annular clamping groove (12);
the sealing receiving module (4) is a hollow cylinder with a hexagonal section (9) at the lower part, a main body (10) with threads on the outer surface at the middle part and a knife edge (11) at the top; the seal bearing module (4) is matched with the metal gasket (1) to be in threaded connection with the hollow hexagonal nut (6).
2. A sample cell according to claim 1, characterized in that the metal gasket (1) material is a metal or alloy of 2-3 mohs hardness.
3. The cuvette according to claim 1, characterized in that the metal gasket (1) is circular, with a thickness of 0.1-2 mm and a diameter of 4-10 mm.
4. The sample cell according to claim 1, wherein the sample cell body (2) has a length of 40-80 mm, an outer diameter of 10-40 mm, and a thickness of 0.5-5 mm; the bottom cover (14) is a circular ring with the outer diameter of 10-40 mm, the inner diameter of 3-15 mm and the thickness of 0.5-5 mm; the upper cover (15) is a regular hexagonal circular ring with the outer diameter of 10-40 mm and the inner hole section of 2-10 mm and the thickness of 0.5-5 mm; the thickness of the inner plating layer and the outer plating layer of the sample pool main body (2) is 0.1-1 mm.
5. A cuvette according to claim 1, characterized in that the cylindrical well (3) is made of the same material as the cuvette body (2), closed at the top and open at the bottom; the diameter of the cylindrical well is 3-15 mm, and the length is 20-50 mm.
6. The sample cell according to claim 1, characterized in that the thermowell (5) is a cylinder, symmetrically welded to the side of the sample cell body (2); the length of the thermocouple well (5) is 5-25 mm, the outer diameter is 0.5-3 mm, and the thickness is 0.05-0.5 mm.
7. The sample cell according to claim 1, wherein the hollow hexagonal nut (6) has a thickness of 2-10 mm, a side length of 2-10 mm, an inner diameter of 4-10 mm, a thread pitch of 1-2.5 mm, and the annular clamping groove (12) has a thickness of 0.5-3 mm and an inner diameter of 3-8 mm.
8. The sample cell according to claim 1, characterized in that the solid cylinder (7) and the hollow hexagonal nut (6) are made of the same material; the length of the solid cylinder (7) is 5-15 mm, the diameter of the solid cylinder is 3-8 mm, the diameter of the hanging hole (8) is 1-3 mm, the thickness of the annular extension (13) is 0.5-3 mm, and the outer diameter of the annular extension is 4-10 mm.
9. The cuvette according to claim 1, characterized in that the seal receiving module (4) is a hollow cylinder made of the same material as the cuvette body (2).
10. The sample cell according to claim 1, wherein the hollow inner diameter of the seal receiving module (4) is 3-8 mm; the side length of the regular hexagon (9) is 2-10 mm, and the thickness is 2-8 mm; the outer diameter of the main body (10) is 4-10 mm, the screw pitch is 1-2.5 mm, and the length is 5-15 mm; the length of the knife edge (11) is 0.5-3 mm, and the inclination angle is 30-60 degrees.
CN201711327071.2A 2017-12-13 2017-12-13 Calorimeter sample cell convenient to replace and good in sealing performance Active CN107884437B (en)

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CN110871982B (en) * 2018-09-03 2021-01-26 中国科学院大连化学物理研究所 High temperature calorimeter sample deposits and remove device
CN114062413A (en) * 2020-08-04 2022-02-18 中国科学院大连化学物理研究所 Sample packaging mode for measuring heat capacity

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CN101354365A (en) * 2008-04-02 2009-01-28 中国科学院大连化学物理研究所 Adiabatic calorimeter and heat measuring system
CN104535612A (en) * 2015-01-16 2015-04-22 中国计量科学研究院 Sample container for solid specific heat capacity measurement standard device
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