• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Device for maintaining constant the temperature of a sample holder and use of the device in sorption analyzers. Device (1) to keep the temperature of a sample holder (2) constant, which has: - a thermal vessel (3) containing a cryogenic liquid (4); - a vessel (5), through which cryogenic liquid flows (4); - a sample holder (2), housed inside the vessel (5); - a pumping device (6) of the cryogenic liquid (4) for continuously pumping cryogenic liquid (4) into the vessel (5). The vessel (5) is positioned so that the cryogenic liquid (4) falls inside the thermal vessel (3) when the rim of the vessel (5) is overflowed by the cryogenic liquid (4). (Machine-translation by Google Translate, not legally binding)
    公开号:ES2561707A1
    申请号:ES201531857
    申请日:2015-12-21
    公开日:2016-02-29
    发明作者:Enrique Gadea Ramos；Diego CAZORLA AMORÓS；Francisco RODRÍGUEZ REINOSO
    申请人:Universidad de Alicante；
    IPC主号:
    专利说明:

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    DEVICE TO KEEP THE TEMPERATURE OF A SAMPLE HOLDER AND USE OF THE DEVICE IN SORTION ANALYZERS CONSTANT
    Field of the Invention
    The present invention relates to a device for maintaining the average temperature of a sample holder partially submerged in a cryogenic liquid, whose evaporation rate is high, for a long period of time. The invention also relates to a use of the device of the present invention in sorption analyzers.
    Prior art
    Sorption analyzers have been widely used for surface area measurement, pore size distribution and solids adsorption capacity.
    To perform these measurements, a known amount of a gas is added in a closed container in which the sample to be analyzed is located and in which the pressure is measured. At least a part of this container, where the sample to be analyzed is located, is at the analysis temperature. By knowing the amount of gas that has been added, the final pressure reached in the container, the volume of the container and the average temperature of the container, the amount of gas absorbed by the sample can be obtained.
    For the analysis to be precise, the average temperature of the container must not vary during the entire duration of the analysis or, if this varies, its variation must be known exactly throughout the analysis. In many of these measures, the working temperature is a cryogenic temperature.
    A very common way to keep the sample to be analyzed at the cryogenic temperature of analysis is to submerge the part of the container where the sample to be analyzed is in a cryogenic liquid, leaving another part of the container out of it. For the average temperature of the container where the sample is to be constant throughout the analysis, the level of the cryogenic liquid with respect to the container where the sample is located must be kept constant, which is a problem because the evaporation rate of The cryogenic liquids are very high and the analyzes can last from several minutes to several days, so that the average temperature of the gas contained in the container partially
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    submerged varies with the variation of the cryogenic fluid level
    Sorption equipment manufacturers try to solve this effect through different control systems based on maintaining as constant a level as possible of cryogenic fluid around the container where the sample to be studied is housed. Some of these systems currently implemented are described in patents US4693124, US5646335, USRE33567 and CN202330371.
    In other cases, instead of trying to control the constant level of cryogenic fluid, solutions have been proposed to know how the variation of the level of the latter affects the average temperature of the container, so that corrections can be applied to the extent of the internal pressure of the vessel, as described in US6387704.
    There is therefore a need to provide a device by which the control and constancy of the average temperature of a container where a sample to be studied is ensured by ensuring a constant level of cryogenic liquid with respect to this container for a long time, even being able to become undefined. .
    Brief Description of the Invention
    The present invention solves the problems described in the state of the art as it relates to a device for keeping the average temperature of a closed sample holder constant, partially submerged in a cryogenic liquid by maintaining a constant level of the cryogenic liquid in the that this sample holder is submerged.
    Thus, in a first aspect, the present invention relates to a device for maintaining constant the temperature of a sample holder containing a sample (hereinafter, device of the present invention), comprising:
    - a thermal container containing a cryogenic liquid,
    - at least one vessel through which the cryogenic liquid flows
    - at least one sample holder, housed inside the vessel
    - means for pumping the cryogenic liquid configured to continuously pump cryogenic liquid into the vessel.
    where the vessel is configured so that the cryogenic liquid falls inside the thermal vessel when the edge of the vessel is overflowed by the cryogenic liquid.
    In a particular embodiment of the present invention, the liquid pumping means
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    Cryogenic are found inside the thermal vessel.
    In a particular embodiment of the present invention, the cryogenic liquid pumping means are discharge pumps.
    In a particular embodiment of the present invention, the level of cryogenic liquid in the thermal vessel is, at most, at the same level as the top of the vessel where the sample holder is housed whose temperature is to be controlled.
    In a particular embodiment of the present invention, the thermal container comprises a lower level of control, indicative of an insufficient level of cryogenic liquid in the thermal container. The lower control level is configured in such a way that, when the cryogenic liquid drops below said level, an external supply of cryogenic liquid can be made to the thermal vessel.
    In the present invention, the lower level of cryogenic liquid control refers to the minimum height or measure that the cryogenic liquid must reach in the thermal vessel below which there must be an external input of the cryogenic liquid.
    In a particular embodiment of the present invention, the lower level of cryogenic liquid control of the thermal vessel is below the pumping means.
    In a particular embodiment of the present invention, the thermal container comprises a higher level of cryogenic liquid control indicative of an excessive level of cryogenic liquid (4) in the thermal container (3). The upper control level is configured in such a way that when the cryogenic liquid that is replaced exceeds that level, the external supply of cryogenic liquid can be stopped.
    In the present invention, the upper control level of the cryogenic liquid refers to the maximum height or measure that the cryogenic liquid must reach in the thermal vessel above which the external contribution of the cryogenic liquid must be stopped.
    In a particular embodiment of the present invention, the upper level of cryogenic liquid control of the thermal vessel is below the level of overflow of the vessel.
    In a particular embodiment, the device of the present invention comprises automatic control means for the level of cryogenic liquid in the thermal vessel. In a particular embodiment, the automatic control means for the level of the cryogenic liquid are connected to a user warning system for the latter to make the manual replacement and / or connected to an automatic liquid replacement system.
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    cryogenic
    With this device and taking into account the evaporation rates of cryogenic fluids and the usual volumes of the thermos used in the sorption equipment (between 1 and 5 liters), it is possible to keep the level of cryogenic liquid constant around 5 of the carrier. samples over a period of time that can be up to several days without the need to replenish cryogenic liquid.
    In a particular embodiment, the thermal vessel houses more than one vessel, said vessels may in turn be connected to each other with pumping means of cryogenic liquid. In a more particular embodiment, each of the vessels houses more than 10 sample holders.
    The pumping means used in the present invention are configured in such a way that they provide at least a flow rate equivalent to the evaporation rate of the cryogenic liquid in the exposed cross-sectional area of the vessel or vessels.
    In a second aspect, the present invention relates to the use of the device of the present invention in sorption analyzers.
    Description of the drawings
    Figure 1 shows a particular embodiment of the invention in which the device for maintaining the temperature constant comprises a thermal vessel, with at least one vessel, at least one sample holder, cryogenic liquid pumping means, control level 2 0 Lower and upper control level.
    References:
    - Device to keep the temperature constant (1)
    - Sample holder (2)
    - Thermal container (3)
    2 5 - Lower control level of the thermal vessel (31)
    - Upper control level of the thermal vessel (32)
    - Cryogenic liquid (4)
    - Glass (5)
    - Pumping means (6)
    Detailed description of the invention
    The device for keeping the temperature (1) of a sample holder (2) of the present invention constant comprises:
    - a thermal container (3) containing a cryogenic liquid (4),
    5 - at least one glass (5), through which cryogenic liquid flows (4)
    - at least one sample holder (2), housed inside the vessel (5)
    - pumping means (6) of the cryogenic liquid (4) configured to continuously pump cryogenic liquid (4) into the vessel (5).
    The vessel (5) is configured so that the cryogenic liquid (4) falls inside the thermal container (3) when the edge of the vessel (5) is overflowed by the cryogenic liquid (4).
    In an exemplary embodiment of the present invention, which can be seen in Figure 1, it starts from an initial state in which the level of the cryogenic liquid (4) does not exceed the level of overflow of the vessel (5), once it is connect the pumping means (6) of the cryogenic liquid (4), it overflows through the top of the vessel (5) so that the cryogenic liquid (4) 15 falls back into the thermal container (3) maintaining a level stable of cryogenic liquid (4) around the sample holder (2) partially submerged in the cryogenic liquid (4), whose temperature is to be controlled independently of the evaporation of the cryogenic liquid. In this exemplary embodiment, the system works correctly until the level of the cryogenic liquid (4) contained in the thermal container (3) falls below the 2 0 outlet of the pumping means (6) which is where the lower control level (31) of the cryogenic liquid.
    权利要求:
    Claims (10)
    [1]
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    1. Device for keeping the temperature (1) of a sample holder (2) constant, characterized in that it comprises:
    - a thermal container (3) containing a cryogenic liquid (4);
    - at least one vessel (5), through which cryogenic liquid (4) flows;
    - at least one sample holder (2), housed inside the vessel (5);
    - pumping means (6) of the cryogenic liquid (4) configured to continuously pump cryogenic liquid (4) into the vessel (5);
    where the vessel (5) is configured so that the cryogenic liquid (4) falls inside the thermal vessel (3) when the edge of the vessel (5) is overflowed by the cryogenic liquid (4).
    [2]
    2. Device according to claim 1, wherein the pumping means (6) of the cryogenic liquid (4) are inside the thermal container (3).
    [3]
    3. Device according to any of the preceding claims, wherein the pumping means (6) are discharge pumps.
    [4]
    Device according to any one of the preceding claims, wherein the thermal container (3) comprises a lower control level (31), indicative of an insufficient level of cryogenic liquid (4) in the thermal container (3).
    [5]
    5. Device according to claim 4, wherein the lower control level (31) is below the pumping means (6).
    [6]
    Device according to any of the preceding claims, wherein the thermal container (3) comprises a higher control level (32) indicative of an excessive level of cryogenic liquid (4) in the thermal container (3).
    [7]
    7. Device according to claim 6, wherein the upper control level (32) is below an overflow level of the vessel (5).
    [8]
    Device according to any one of the preceding claims, which comprises signaling means to show the level of cryogenic liquid (4) for possible manual replacement.
    [9]
    9. Device according to any of the preceding claims, comprising means for automatic control of the level of cryogenic liquid (4).
    7
    [10]
    10. Use of a device according to any of claims 1-9 in sorption analyzers.
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    同族专利:
    公开号 | 公开日
    ES2561707B1|2017-02-20|
    WO2017109246A1|2017-06-29|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    EP0239221A1|1986-02-25|1987-09-30|Micromeritics Instrument Corporation|A temperature controlling apparatus for use with pore volume and surface area analyzers and method for operating the same|
    USRE33567E|1986-02-25|1991-04-09|Micromeritics Instrument Corporation|Temperature controlling apparatus for use with pore volume and surface area analyzers|
    US5239482A|1990-03-09|1993-08-24|Institut Francais Du Petrole|Method of and an apparatus for measuring the adsorption and the desorption of a gas adsorbed by a solid sample and the use thereof|
    US6595036B1|2002-02-27|2003-07-22|Bel Japan, Inc.|Method and apparatus for measuring amount of gas adsorption|US10948461B2|2019-01-31|2021-03-16|Anton Paar Quantatec, Inc.|Inverted wick type temperature control system|
    法律状态:
    2017-02-20| FG2A| Definitive protection|Ref document number: 2561707 Country of ref document: ES Kind code of ref document: B1 Effective date: 20170220 |
    优先权:
    申请号 | 申请日 | 专利标题
    ES201531857A|ES2561707B1|2015-12-21|2015-12-21|Device to keep the temperature of a sample holder constant and use of the device in sorption analyzers|ES201531857A| ES2561707B1|2015-12-21|2015-12-21|Device to keep the temperature of a sample holder constant and use of the device in sorption analyzers|
    PCT/ES2016/070878| WO2017109246A1|2015-12-21|2016-12-12|Device for maintaining constant the temperature of a sample-holder and use of the device in sorption analysers|
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