CN103207129A - Sample chamber for testing adsorption isotherm of material - Google Patents

Sample chamber for testing adsorption isotherm of material Download PDF

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Publication number
CN103207129A
CN103207129A CN2013101596031A CN201310159603A CN103207129A CN 103207129 A CN103207129 A CN 103207129A CN 2013101596031 A CN2013101596031 A CN 2013101596031A CN 201310159603 A CN201310159603 A CN 201310159603A CN 103207129 A CN103207129 A CN 103207129A
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pressure head
sample chamber
tracheae
test
sample
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CN103207129B (en
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程宏辉
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Yangzhou University
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Yangzhou University
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Abstract

The invention relates to a sample chamber for detecting the property of a material, in particular relates to a sample chamber for testing an adsorption isotherm of a material, and solves the problems of large dead size, high gas resistance and difficulty in dismounting and cleaning of the conventional steel container sample chamber and the problem that the tested material cannot be in direct contact with a temperature measurement thermocouple. The sample chamber consists of a sample pipe (8), the temperature measurement thermocouple (9), a pressure head nut (4), a pressure head (3), a filter net or quartz cotton (5), a four-way gas pipe (7), a connection steel pipe (2), a quick joint (1) and a sealing pad or sealing ring (5), wherein the quick joint is connected with one end of the pressure head through the connection steel pipe; the pressure head nut is sleeved on the pressure head; the filter net or quartz cotton is placed in a threaded hole in the other end of the pressure head and is connected with the four-way gas pipe; the pressure head nut is in threaded connection with the sample pipe; the temperature measurement thermocouple is welded at the bottom of the sample pipe; and the sealing pad or the sealing ring is arranged between the pressure head and the sample pipe.

Description

A kind of sample chamber for the test of material adsorption isothermal
Technical field
The present invention relates to the material property detection and use the sample chamber, particularly a kind of sample chamber for the test of material adsorption isothermal.
Background technology
Adsorption isothermal is the key property curve of the multiple performance of research material.Can directly obtain to adsorb platform by it and press, berm width and slope, lag coefficient, parameters such as reversible adsorption amount, and then according to the pressure of the absorption platform under the different temperatures, and Van ' t Hoff formula returns out adsorption reaction enthalpy and reaction entropy.These parameters have extremely important theory and actual directive significance to research, the development and utilization of material.People generally adopt the volumetric method test macro to carry out the test of material adsorption isothermal at present.The volumetric method testing principle is by changing the gaseous tension in sample chamber and the air storage chamber, extrapolating the variation of material adsorbance according to the equation of gas state and law of conservation of mass.In test process, require total system, comprise the sample chamber, all have good sealing property, otherwise the test data distortion there is not practical significance.Material require is placed in the sample chamber, then the sample chamber is connected to the test that the volumetric method test macro carries out adsorption isothermal.
Material adsorption isothermal test sample chamber in the past substantially all is simple steel vessel, then by being threaded onto test macro.The shortcoming of current material adsorption isothermal test sample chamber is that a lot of materials understand efflorescence later on through multiple adsorb and produce a large amount of micron-sized particles, perhaps the material virgin state is exactly powdered form, and test isothermal adsorption process relates to system and vacuumizes, particle is fled in internal system, destroy the sealing property of valve, the sample chamber that perhaps has has installed filtrator additional, but filtrator can not carry out good disassembly, cleaning or replacing, cause having accumulated a lot of powder particles through long-time use after-filter one end, and these powder particles itself can adsorbed gas, therefore all can finally have influence on the correctness of test data.And the sample chamber is by being threaded onto test macro, or less number of times uses the easy variation of back sealing, or needs to change gasket seal before each test, and testing expense obviously improves.And the reliability that is threaded in the reality neither be fine, often cause easily test gas to external leakage, after sample test simultaneously is intact, when test macro disconnects, cause outside air to contact with the direct of sample easily, be unfavorable for sample is carried out subsequent analysis.In addition, the dead volume of existing steel vessel sample chamber is bigger, causes bigger test error easily.At last, temperature thermocouple separates the outer wall that is placed on the sample chamber with the sample chamber, can cause institute's measured reaction temperature error bigger than normal like this, finally also can influence the accuracy of test data.
Summary of the invention
Technical matters: in order to overcome the above-mentioned various shortcomings of material adsorption isothermal test sample chamber in the past, the object of the present invention is to provide and a kind ofly can connect test macro fast, dead volume is little, cleaned and changed convenience, it is little to vacuumize resistance, the material adsorption isothermal test sample chamber simple and easy to do, that measured material and temperature thermocouple closely contact.
Technical scheme: a kind of sample chamber for the test of material adsorption isothermal of the present invention is made up of sample hose, temperature thermocouple, pressure head nut, pressure head, screen pack or silica wool, four-way tracheae, connection steel pipe, rapid-acting coupling, sealing gasket or O-ring seal; Wherein, there is the column type cavity sample hose inside, the column type cavity bottom is placed measured material, upper end open, and remain silent and be welded with temperature thermocouple in the lower end, when guaranteeing test, temperature thermocouple contacts with the direct of measured material, and the openend outer wall has screw thread, and openend has seal groove, be used for placing sealing gasket or O-ring seal, there are two parallel planes the outside lower end of sample hose or are the hexagon shape; The pressure head nut sleeve is on pressure head, inwall has screw thread, and outer wall has two parallel planes or is the hexagon shape, and the pressure head nut is connected with sample hose by screw thread, simultaneously pressure head is pushed then sealing gasket or O-ring seal are pushed, acquisition sample chamber sealing effectiveness makes it to deform; Pressure head one end be connected steel pipe and be welded to connect, be connected with rapid-acting coupling then, and there is threaded hole pressure head other end centre, in threaded hole, put into screen pack or silica wool, then the four-way tracheae is connected with pressure head by screw thread, guarantees that simultaneously the four-way tracheae can have extruding to screen pack or silica wool; Four-way tracheae one end has screw thread, and the other end is solid pole, has screw thread one end center that one section short tracheae is arranged, and what link to each other with this tracheae is four sections uniform tracheae outlets.Turning on the four-way tracheae can realize screen pack or silica wool are cleaned or change.After the whole sample chamber assembled, the rapid-acting coupling by the steel pipe front end was connected with test macro.
Described four-way tracheae adopts 2 to 12 sections uniform tracheae export structure forms.
The non-threaded end of described four-way tracheae comprises one section solid pole.
Described quick tieing adopts and has the rapid-acting coupling of stopping device voluntarily, and when preventing that the sample chamber is connected with the test macro disconnection, air enters the sample chamber.
The filter that the porous disk that described screen pack or silica wool be stainless (steel) wire, formed by stainless powder or ceramic powders sintering or quartz fibre compacting form.
Described sealing gasket or O-ring seal are teflon pad, red copper pad, silicagel pad, nitrile rubber O-ring seal or polytetrafluoro rubber seal.
Beneficial effect:
(1) adopts rapid-acting coupling to connect, can be connected fast with test macro, can prevent that air from entering the sample chamber simultaneously;
(2) has less dead volume;
(3) the test process air resistance is little, can realize higher system vacuum tightness;
(4) when guaranteeing the filtering material particulate, can be easy to realize dismounting again, clean or change;
(5) measured material directly contacts with the test thermopair, and institute's measured reaction temperature is more accurate.
Description of drawings
Fig. 1 is material adsorption isothermal test sample cell structure simplified schematic diagram.
Fig. 2 is the sectional view of four-way tracheae.
Fig. 3 is the vertical view of four-way tracheae.
Comprising: rapid-acting coupling 1, connection steel pipe 2, pressure head 3, pressure head nut 4, screen pack or silica wool 5, sealing gasket or O-ring seal 6, four-way tracheae 7, sample hose 8, thermometric galvanic couple 9.
Embodiment
Material adsorption isothermal test sample of the present invention chamber is made up of following structure: sample hose, thermometric galvanic couple, pressure head nut, pressure head, screen pack or silica wool, four-way tracheae, connection steel pipe, rapid-acting coupling, sealing gasket or O-ring seal; Wherein, there is the column type cavity sample hose inside, the column type cavity bottom is placed measured material, upper end open, remain silent and be welded with temperature thermocouple in the lower end, when guaranteeing test, temperature thermocouple contacts with the direct of measured material, thereby reduce thermal conduction resistance to the influence of real reaction temperature test, at the openend outer wall screw thread is arranged, openend has seal groove, is used for placing sealing gasket or O-ring seal, there are two parallel planes the outside lower end of sample hose or are the hexagon shape, carries out dismounting to make things convenient for the sample chamber by bench vice or spanner; The pressure head nut sleeve is on pressure head, inwall has screw thread, outer wall has two parallel planes or is hexagon, carry out dismounting to make things convenient for the sample chamber by bench vice or spanner, the pressure head nut is connected with sample hose by screw thread, simultaneously pressure head is pushed then sealing gasket or O-ring seal are pushed, make it to deform and realize obtaining the sample chamber sealing effectiveness; Pressure head one end be connected steel pipe and be welded to connect, be connected with rapid-acting coupling then, and there is threaded hole pressure head other end centre, in threaded hole, put into screen pack or silica wool, then the four-way tracheae is connected with pressure head by screw thread, guarantee that simultaneously the four-way tracheae can have to a certain degree extruding to screen pack or silica wool, prevent from producing the slit in the test process, cause material granule from the slit, to flee; Four-way tracheae one end has screw thread, it is solid pole that the other end does not have screw thread, there is screw thread one end center that one section short tracheae is arranged, what link to each other with this tracheae is four sections uniform tracheae outlets, the inflow of gas and outflow realize by this tracheae in the sample chamber, realize the less resistance that vacuumizes by the four-way tracheae, guarantee that again the dead volume of whole sample chamber drops to minimum simultaneously.Turning on the four-way tracheae can realize at any time screen pack or silica wool being cleaned or changing.After the whole sample chamber assembled, the rapid-acting coupling by the steel pipe front end was connected with test macro, and is very succinctly convenient.
Described four-way tracheae is preferentially selected four sections uniform tracheae export structure forms for use, but also do not get rid of the tracheae outlet form of selecting other layouts for use, uniform as single outlet, two sections, three sections uniform, five sections uniform, six sections uniform ... adopt 20 sections uniform forms up to the highest.
Described quick tieing is preferential selects to have the rapid-acting coupling of stopping device voluntarily, and when preventing that the sample chamber is connected with the test macro disconnection, air enters the sample chamber, is not with the rapid-acting coupling of stopping device voluntarily but also can select for use sometimes.
Described screen pack or silica wool can be stainless (steel) wires, the porous disk that is formed by stainless powder or ceramic powders sintering, or the filter that forms of quartz fibre compacting.
Described sealing gasket or O-ring seal can be the teflon pads, red copper pad, silicagel pad, nitrile rubber O-ring seal, polytetrafluoro rubber seal.
Embodiment 1
As shown in Figure 1 and Figure 2, sample chamber of the present invention is made of rapid-acting coupling 1, connection steel pipe 2, pressure head 3, pressure head nut 4, screen pack or silica wool 5, sealing gasket or O-ring seal 6, four-way tracheae 7, sample hose 8, thermometric galvanic couple 9.Wherein, rapid-acting coupling 1 top has A.C.D., and when preventing from dismantling from test macro, air enters the sample chamber; Pressure head nut 4 is enclosed within on the pressure head 3, and an end of pressure head 3 is welded to connect with being connected steel pipe 2, is connected with rapid-acting coupling 1 then; Threaded hole is arranged in the middle of the other end of pressure head 3, in threaded hole, put into screen pack or silica wool 5, then four-way tracheae 7 is connected with pressure head 3 by screw thread, guarantee that simultaneously four-way tracheae 7 can have to a certain degree extruding to screen pack or silica wool 5, prevent from producing the slit in the test process, cause material granule from the slit, to flee; There is the column type cavity sample hose 8 inside, the column type cavity bottom is placed measured material, upper end open, remain silent and be welded with temperature thermocouple 9 in the lower end, when guaranteeing test, temperature thermocouple 9 contacts with the direct of measured material, thereby reduce thermal conduction resistance to the influence of real reaction temperature test, at the openend outer wall screw thread is arranged, openend has seal groove, be used for placing sealing gasket or O-ring seal 6, there are two parallel planes sample hose 8 outside lower ends or are the hexagon shape, carry out dismounting to make things convenient for the sample chamber by bench vice or spanner; Pressure head nut 4 inwalls have screw thread, outer wall has two parallel planes or is hexagon, carry out dismounting to make things convenient for the sample chamber by bench vice or spanner, pressure head nut 4 is connected with sample hose 8 by screw thread, simultaneously pressure head 3 is pushed then sealing gasket or O-ring seal are pushed, make it to deform and realize the effect of sample chamber sealing; There is one section short tracheae at four-way tracheae 7 thread end centers, what link to each other with this tracheae is four sections uniform tracheae outlets, the inflow of gas and outflow realize by this tracheae in the sample chamber, the other end is solid pole, can realize the less resistance that vacuumizes by the four-way tracheae, make the dead volume of whole sample chamber drop to minimum again simultaneously.Turning on four-way tracheae 7 can realize at any time screen pack or silica wool being cleaned or changing.After the whole sample chamber assembles, be connected with test macro by the rapid-acting coupling 1 that connects steel pipe 2 front ends, very succinctly convenient.

Claims (6)

1. sample chamber that is used for the test of material adsorption isothermal, it is characterized in that this sample chamber by sample hose (8), temperature thermocouple (9), pressure head nut (4), pressure head (3), screen pack or silica wool (5), four-way tracheae (7), connect steel pipe (2), rapid-acting coupling (1), sealing gasket or O-ring seal (5) and form; Wherein, there is the column type cavity sample hose (8) inside, the column type cavity bottom is placed measured material, upper end open, and remain silent and be welded with temperature thermocouple (9) in the lower end, when guaranteeing test, temperature thermocouple (9) contacts with the direct of measured material, and the openend outer wall has screw thread, and openend has seal groove, be used for placing sealing gasket or O-ring seal (6), there are two parallel planes the outside lower end of sample hose (8) or are the hexagon shape; Pressure head nut (4) is enclosed within on the pressure head, inwall has screw thread, outer wall has two parallel planes or is the hexagon shape, pressure head nut (4) is connected with sample hose (8) by screw thread, simultaneously pressure head (3) is pushed then sealing gasket or O-ring seal (5) are pushed, acquisition sample chamber sealing effectiveness makes it to deform; Pressure head (3) one ends be connected steel pipe (2) and be welded to connect, be connected with rapid-acting coupling (1) then, and there is threaded hole pressure head (3) other end centre, in threaded hole, put into screen pack or silica wool (5), then four-way tracheae (7) is connected with pressure head (3) by screw thread, guarantees that simultaneously the four-way tracheae can have extruding to screen pack or silica wool; Four-way tracheae one end has screw thread, and the other end is solid pole, has screw thread one end center that one section short tracheae is arranged, and what link to each other with this tracheae is four sections uniform tracheae outlets.Turning on the four-way tracheae can realize screen pack or silica wool are cleaned or change.After the whole sample chamber assembled, the rapid-acting coupling by the steel pipe front end was connected with test macro.
2. according to right 1 described sample chamber for the test of material adsorption isothermal, it is characterized in that described four-way tracheae (7) employing has 2 to 12 sections uniform tracheae export structure forms.
3. according to right 1 described sample chamber for the test of material adsorption isothermal, it is characterized in that the non-threaded end of described four-way tracheae (7) comprises one section solid pole.
4. according to the described sample chamber for the test of material adsorption isothermal of right 1, it is characterized in that described quick tieing (1) adopts and have the rapid-acting coupling of stopping device voluntarily that when preventing that the sample chamber is connected with the test macro disconnection, air enters the sample chamber.
5. according to the described sample chamber for the test of material adsorption isothermal of right 1, the filter that the porous disk that its feature is stainless (steel) wire described screen pack or silica wool (5), formed by stainless powder or ceramic powders sintering or quartz fibre compacting form.
6. according to right 1 described sample chamber for the test of material adsorption isothermal, it is characterized in that described sealing gasket or O-ring seal (5) are teflon pad, red copper pad, silicagel pad, nitrile rubber O-ring seal or polytetrafluoro rubber seal.
CN201310159603.1A 2013-04-28 2013-04-28 Sample chamber for testing adsorption isotherm of material Expired - Fee Related CN103207129B (en)

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CN104535454A (en) * 2015-02-01 2015-04-22 林志苹 Detection device of carbon dioxide concentration
CN104777240A (en) * 2015-04-22 2015-07-15 安徽工业大学 Sample room for hydrogen absorbing and desorbing experiment by nitrogen storage material
CN110231273A (en) * 2019-07-11 2019-09-13 贝士德仪器科技(北京)有限公司 A kind of physical adsorption appearance with concentrated type Multi-example tube sealing device
CN111443140A (en) * 2020-04-10 2020-07-24 苏州天蓝分析仪器有限公司 Enrichment detection analysis device for online measurement of ultralow-concentration VOC

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104535454A (en) * 2015-02-01 2015-04-22 林志苹 Detection device of carbon dioxide concentration
CN104535454B (en) * 2015-02-01 2016-10-05 林志苹 A kind of detection device of gas concentration lwevel
CN104777240A (en) * 2015-04-22 2015-07-15 安徽工业大学 Sample room for hydrogen absorbing and desorbing experiment by nitrogen storage material
CN110231273A (en) * 2019-07-11 2019-09-13 贝士德仪器科技(北京)有限公司 A kind of physical adsorption appearance with concentrated type Multi-example tube sealing device
CN111443140A (en) * 2020-04-10 2020-07-24 苏州天蓝分析仪器有限公司 Enrichment detection analysis device for online measurement of ultralow-concentration VOC

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