CN103207129B - Sample chamber for testing adsorption isotherm of material - Google Patents
Sample chamber for testing adsorption isotherm of material Download PDFInfo
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- CN103207129B CN103207129B CN201310159603.1A CN201310159603A CN103207129B CN 103207129 B CN103207129 B CN 103207129B CN 201310159603 A CN201310159603 A CN 201310159603A CN 103207129 B CN103207129 B CN 103207129B
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- pressure head
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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
Technical field
The present invention relates to material property detection sample chamber, particularly a kind of sample chamber for the test of materials adsorption isotherm.
Background technology
Adsorption isothermal is the key property curve of the multiple performance of research material.Absorption platform pressure can be directly obtained, berm width and slope, lag coefficient, the parameters such as reversible adsorption amount by it, and then according to the absorption platform pressure under different temperatures, and Van ' tHoff formulary regression goes out adsorption enthalpies and reaction entropy.These parameters have extremely important theory and actual directive significance to the research of material, development and utilization.Current people generally adopt volumetric method test macro to carry out the isothermal test of materials adsorption.The principle of volumetric method test is the gaseous tension by changing in sample chamber and air storage chamber, extrapolates the change of adsorption capacities of materials according to the equation of gas state and law of conservation of mass.In test process, require whole system, comprise sample chamber that all there is good sealing, otherwise test data distortion do not have practical significance.Material require is placed in sample chamber, then sample chamber is connected to the test that volumetric method test macro carries out adsorption isothermal.
Materials adsorption isotherm test sample room is in the past substantially all simple steel vessel, is then threadedly attached to test macro.The shortcoming of current material adsorption isothermal test sample room is that a lot of material is understood efflorescence and produced a large amount of micron-sized particle after multiple adsorb, or material virgin state is exactly powdered form, and test isothermal adsorption process and relate to system and vacuumize, particle is so inevitably made to flee in internal system, destroy the sealing property of valve, or some sample chambers have installed filtrator additional, but filtrator can not carry out good disassembly, cleaning or replacing, cause through using after-filter one end to have accumulated a lot of powder particle for a long time, and these powder particles itself can adsorbed gas, therefore the correctness of test data can all finally be had influence on.And sample chamber is threadedly attached to test macro, or less number of times uses rear sealing to be easily deteriorated, or needs to change gasket seal before each test, and testing expense significantly improves.And the reliability be threaded in reality neither be fine, often easily cause test gas to external leakage, after sample test is simultaneously complete, easily causes outside air to contact with the direct of sample when disconnecting from test macro, be unfavorable for carrying out subsequent analysis to sample.In addition, the dead volume of existing steel vessel sample chamber is comparatively large, easily causes larger test error.Finally, temperature thermocouple is separated the outer wall being placed on sample chamber with sample chamber, institute's measured reaction temperature error can be caused so bigger than normal, finally also can affect the accuracy of test data.
Summary of the invention
Technical matters: in order to overcome the above-mentioned various shortcoming of materials adsorption isotherm test sample room in the past, the object of the present invention is to provide one can connecting test system fast, dead volume is little, cleaned and changed convenience, vacuumize resistance little, simple and easy to do, the materials adsorption isotherm test sample room of measured material and temperature thermocouple close contact.
Technical scheme: a kind of sample chamber for the test of materials adsorption isotherm of the present invention is made up of sample hose, temperature thermocouple, pressure head nut, pressure head, screen pack or silica wool, four snorkels, joint steel pipe, rapid-acting coupling, sealing gasket or O-ring seal; Wherein, there is cylindrical cavity sample hose inside, placing measured material bottom cylindrical cavity, upper end open, remains silent and is welded with temperature thermocouple in lower end, when ensureing test, temperature thermocouple contacts with the direct of measured material, and openend outer wall has screw thread, and openend has seal groove, for placing sealing gasket or O-ring seal, there are two parallel planes the outside lower end of sample hose or are hexagon shape; Pressure head nut sleeve is on pressure head, inwall has screw thread, and outer wall has two parallel planes or in hexagon shape, pressure head nut is connected with sample hose by screw thread, extrude pressure head simultaneously and then extrude sealing gasket or O-ring seal, making it to deform obtains sample chamber sealing effectiveness; Pressure head one end and joint steel pipe are welded to connect, then be connected with rapid-acting coupling, and have threaded hole in the middle of the pressure head other end, screen pack or silica wool is put in threaded hole, then four snorkels are connected with pressure head by screw thread, ensure that four snorkels can have extruding to screen pack or silica wool simultaneously; There is screw thread four snorkel one end, and the other end is solid pole, have center, screw thread one end to have the tracheae of a section shorter, and what be connected with this tracheae is that four sections of uniform tracheaes export.Turn on four snorkels can realize cleaning screen pack or silica wool or changing.After whole sample chamber assembles, be connected with test macro by the rapid-acting coupling of steel pipe front end.
Described four snorkels employings have 2 to 12 sections of uniform tracheae export structure forms.
The non-threaded end of described four snorkels comprises one section of solid pole.
Described quick tieing adopts the rapid-acting coupling with stopping device voluntarily, and when disconnecting to prevent sample chamber and test macro, air enters sample chamber.
The filter that described screen pack or silica wool are stainless (steel) wires, the porous disk sintered by stainless powder or ceramic powders or quartz fibre are suppressed.
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) adopt rapid-acting coupling to connect, can be connected fast with test macro, can prevent air from entering sample chamber simultaneously;
(2) there is less dead volume;
(3) test process air resistance is little, can realize higher system vacuum;
(4) while guarantee filtering material particulate, can be easy to again realize dismounting, cleaning or replacing;
(5) measured material directly contacts with test thermopair, and institute's measured reaction temperature is more accurate.
Accompanying drawing explanation
Fig. 1 is materials adsorption isotherm test sample cell structure simplified schematic diagram.
Fig. 2 is the sectional view of four snorkels.
Fig. 3 is the vertical view of four snorkels.
Comprising: rapid-acting coupling 1, joint steel pipe 2, pressure head 3, pressure head nut 4, screen pack or silica wool 5, sealing gasket or O-ring seal 6, four snorkel 7, sample hose 8, thermometric galvanic couple 9.
Embodiment
Materials adsorption isotherm test sample room of the present invention is made up of following structure: sample hose, thermometric galvanic couple, pressure head nut, pressure head, screen pack or silica wool, four snorkels, joint steel pipe, rapid-acting coupling, sealing gasket or O-ring seal; Wherein, there is cylindrical cavity sample hose inside, measured material is placed bottom cylindrical cavity, upper end open, remain silent and be welded with temperature thermocouple in lower end, when ensureing test, temperature thermocouple contacts with the direct of measured material, thus reduce thermal conduction resistance to the impact of real reaction temperature test, have screw thread at openend outer wall, openend has seal groove, for placing sealing gasket or O-ring seal, there are two parallel planes the outside lower end of sample hose or in hexagon shape, carry out dismounting to facilitate sample chamber by bench vice or spanner; Pressure head nut sleeve is on pressure head, inwall has screw thread, outer wall has two parallel planes or is hexagon, dismounting is carried out by bench vice or spanner to facilitate sample chamber, pressure head nut is connected with sample hose by screw thread, extrude pressure head simultaneously and then extrude sealing gasket or O-ring seal, making it to deform realizes obtaining sample chamber sealing effectiveness; Pressure head one end and joint steel pipe are welded to connect, then be connected with rapid-acting coupling, and have threaded hole in the middle of the pressure head other end, screen pack or silica wool is put in threaded hole, then four snorkels are connected with pressure head by screw thread, ensure that four snorkels can have extruding to a certain degree to screen pack or silica wool simultaneously, prevent from producing gap in test process, cause material granule to flee from gap; There is screw thread four snorkel one end, the other end does not have screw thread to be solid pole, center, screw thread one end is had to have the tracheae of a section shorter, what be connected with this tracheae is that four sections of uniform tracheaes export, in sample chamber gas inflow and flow out through this tracheae realize, realize less vacuumizing resistance by four snorkels, ensure that again the dead volume of whole sample chamber drops to minimum simultaneously.Turn on four snorkels can realize cleaning screen pack or silica wool or changing at any time.After whole sample chamber assembles, be connected with test macro by the rapid-acting coupling of steel pipe front end, very succinctly facilitate.
Four sections of uniform tracheae export structure forms preferentially selected by described four snorkels, but do not get rid of the tracheae egress form selecting other to arrange yet, as single outlet, two sections uniform, three sections uniform, five sections uniform, six sections uniform ... the form that 20 sections uniform is adopted until the highest.
Described quick tieing prioritizing selection is with the rapid-acting coupling of stopping device voluntarily, and when disconnecting to prevent sample chamber and test macro, air enters sample chamber, but sometimes also can select the rapid-acting coupling not with stopping device voluntarily.
Described screen pack or silica wool can be stainless (steel) wires, the porous disk sintered by stainless powder or ceramic powders, or the filter of quartz fibre compacting.
Described sealing gasket or O-ring seal can be 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 up of rapid-acting coupling 1, joint steel pipe 2, pressure head 3, pressure head nut 4, screen pack or silica wool 5, sealing gasket or O-ring seal 6, four snorkel 7, sample hose 8, thermometric galvanic couple 9.Wherein, with A.C.D. above rapid-acting coupling 1, during to prevent from dismantling from test macro, air enters sample chamber; Pressure head nut 4 is enclosed within pressure head 3, and one end and the joint steel pipe 2 of pressure head 3 are welded to connect, and are then connected with rapid-acting coupling 1; Threaded hole is had in the middle of the other end of pressure head 3, screen pack or silica wool 5 is put in threaded hole, then four snorkels 7 are connected with pressure head 3 by screw thread, ensure that four snorkels 7 can have extruding to a certain degree to screen pack or silica wool 5 simultaneously, prevent from producing gap in test process, cause material granule to flee from gap; There is cylindrical cavity sample hose 8 inside, measured material is placed bottom cylindrical cavity, upper end open, remain silent and be welded with temperature thermocouple 9 in lower end, when ensureing test, temperature thermocouple 9 contacts with the direct of measured material, thus reduce thermal conduction resistance to the impact of real reaction temperature test, screw thread is had at openend outer wall, openend has seal groove, for placing sealing gasket or O-ring seal 6, there are two parallel planes the outside lower end of sample hose 8 or in hexagon shape, carry out dismounting to facilitate sample chamber by bench vice or spanner; Pressure head nut 4 inwall has screw thread, outer wall has two parallel planes or is hexagon, dismounting is carried out by bench vice or spanner to facilitate sample chamber, pressure head nut 4 is connected with sample hose 8 by screw thread, extrude pressure head 3 simultaneously and then extrude sealing gasket or O-ring seal, making it to deform realizes the effect of sample chamber sealing; There is the tracheae of a section shorter at four snorkel 7 thread end centers, what be connected with this tracheae is that four sections of uniform tracheaes export, in sample chamber gas inflow and flow out through this tracheae realize, the other end is solid pole, can realize less vacuumizing resistance by four snorkels, make again the dead volume of whole sample chamber drop to minimum simultaneously.Turn on four snorkels 7 can realize cleaning screen pack or silica wool or changing at any time.After whole sample chamber assembles, be connected with test macro by the rapid-acting coupling 1 of joint steel pipe 2 front end, very succinctly facilitate.
Claims (1)
1., for a sample chamber for materials adsorption isotherm test, it is characterized in that this sample chamber is made up of sample hose (8), temperature thermocouple (9), pressure head nut (4), pressure head (3), screen pack or silica wool (5), four snorkels (7), joint steel pipe (2), rapid-acting coupling (1), sealing gasket or O-ring seal (6); Wherein, there is cylindrical cavity sample hose (8) inside, placing measured material bottom cylindrical cavity, upper end open, remains silent and is welded with temperature thermocouple (9) in lower end, when ensureing test, temperature thermocouple (9) contacts with the direct of measured material, and openend outer wall has screw thread, and openend has seal groove, for placing sealing gasket or O-ring seal (6), there are two parallel planes sample hose (8) outside lower end or are hexagon shape; Pressure head nut (4) is enclosed within pressure head, inwall has screw thread, outer wall has two parallel planes or is hexagon shape, pressure head nut (4) is connected with sample hose (8) by screw thread, extrude pressure head (3) simultaneously and then extrude sealing gasket or O-ring seal (6), making it to deform obtains sample chamber sealing effectiveness; Pressure head (3) one end and joint steel pipe (2) are welded to connect, then be connected with rapid-acting coupling (1), and have threaded hole in the middle of pressure head (3) other end, screen pack or silica wool (5) is put in threaded hole, then four snorkels (7) are connected with pressure head (3) by screw thread, ensure that four snorkels can have extruding to screen pack or silica wool simultaneously; There is screw thread four snorkel one end, the other end is solid pole, center, screw thread one end is had to have the tracheae of a section shorter, what be connected with this tracheae is that four sections of uniform tracheaes export, turn on four snorkels can realize cleaning screen pack or silica wool or changing, after whole sample chamber assembles, be connected with test macro by the rapid-acting coupling of steel pipe front end;
The employing of described four snorkels (7) has 2 to 12 sections of uniform tracheae export structure forms;
The non-threaded end of described four snorkels (7) comprises one section of solid pole;
Described quick tieing (1) adopts the rapid-acting coupling with stopping device voluntarily, and when disconnecting to prevent sample chamber and test macro, air enters sample chamber;
The filter that described screen pack or silica wool (5) are stainless (steel) wires, the porous disk sintered by stainless powder or ceramic powders or quartz fibre are suppressed;
Described sealing gasket or O-ring seal (6) are teflon pad, red copper pad, silicagel pad, nitrile rubber O-ring seal or polytetrafluoro rubber seal.
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CN201310159603.1A CN103207129B (en) | 2013-04-28 | 2013-04-28 | Sample chamber for testing adsorption isotherm of material |
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CN201310159603.1A CN103207129B (en) | 2013-04-28 | 2013-04-28 | Sample chamber for testing adsorption isotherm of material |
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CN103207129B true CN103207129B (en) | 2015-04-01 |
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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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