WO2017109246A1 - Device for maintaining constant the temperature of a sample-holder and use of the device in sorption analysers - Google Patents

Device for maintaining constant the temperature of a sample-holder and use of the device in sorption analysers Download PDF

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Publication number
WO2017109246A1
WO2017109246A1 PCT/ES2016/070878 ES2016070878W WO2017109246A1 WO 2017109246 A1 WO2017109246 A1 WO 2017109246A1 ES 2016070878 W ES2016070878 W ES 2016070878W WO 2017109246 A1 WO2017109246 A1 WO 2017109246A1
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Prior art keywords
cryogenic liquid
vessel
level
thermal
container
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PCT/ES2016/070878
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Spanish (es)
French (fr)
Inventor
Enrique Gadea Ramos
Diego CAZORLA AMORÓS
Francisco RODRÍGUEZ REINOSO
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Universidad De Alicante
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Publication of WO2017109246A1 publication Critical patent/WO2017109246A1/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L7/00Heating or cooling apparatus; Heat insulating devices
    • B01L7/04Heat insulating devices, e.g. jackets for flasks
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25DREFRIGERATORS; COLD ROOMS; ICE-BOXES; COOLING OR FREEZING APPARATUS NOT OTHERWISE PROVIDED FOR
    • F25D3/00Devices using other cold materials; Devices using cold-storage bodies
    • F25D3/10Devices using other cold materials; Devices using cold-storage bodies using liquefied gases, e.g. liquid air
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
    • G01N15/08Investigating permeability, pore-volume, or surface area of porous materials

Definitions

  • 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.
  • Sorption analyzers have been widely used for surface area measurement, pore size distribution and solids adsorption capacity.
  • 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.
  • 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.
  • 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.
  • 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 the average temperature of the gas contained in the partially submerged container varies with the variation of the level of the cryogenic fluid
  • 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.
  • 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.
  • 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:
  • cryogenic liquid configured to continuously pump cryogenic liquid into the vessel.
  • cryogenic liquid pumping means are located inside the thermal container.
  • cryogenic liquid pumping means are discharge pumps.
  • 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.
  • 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.
  • 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.
  • the lower level of cryogenic liquid control of the thermal vessel is below the pumping means.
  • 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.
  • 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.
  • the upper level of cryogenic liquid control of the thermal vessel is below the level of overflow of the vessel.
  • the device of the present invention comprises automatic control means for the level of cryogenic liquid in the thermal vessel.
  • 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 cryogenic liquid replacement system.
  • the thermal vessel houses more than one vessel, said vessels may in turn be connected to each other with pumping means of cryogenic liquid.
  • each of the vessels houses more than one sample holder.
  • 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.
  • the present invention relates to the use of the device of the present invention in sorption analyzers.
  • 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, lower control level and higher level of control
  • the device for keeping the temperature (1) of a sample holder (2) of the present invention constant comprises:
  • 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 vessel (3) when the edge of the vessel (5) is overflowed by the cryogenic liquid (4).
  • 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) falls back into the thermal container (3) maintaining a stable level 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.
  • the system works correctly until the level of the cryogenic liquid (4) contained in the thermal container (3) falls below the intake of the pumping means (6) which is where the level of lower control (31) of the cryogenic liquid.

Abstract

The invention relates to a device (1) for maintaining constant the temperature of a sample-holder (2), which device has: a thermal recipient (3) containing a cryogenic liquid (4); a vessel (5) through which the cryogenic liquid (4) flows; a sample-holder (2) housed inside the vessel (5); pumping equipment (6) for the cryogenic liquid (4), to continuously pump cryogenic liquid (4) towards the vessel (5). The vessel (5) is placed so that the cryogenic liquid (4) falls into the thermal recipient (3) when the cryogenic liquid (4) flows over the edge of the vessel (5).

Description

DESCRIPCIÓN  DESCRIPTION
DISPOSITIVO PARA MANTENER CONSTANTE LA TEMPERATURA DE UN PORTA- MUESTRAS Y USO DEL DISPOSITIVO EN ANALIZADORES DE SORCIÓN DEVICE TO KEEP THE TEMPERATURE OF A SAMPLE HOLDER AND USE OF THE DEVICE IN SORTION ANALYZERS CONSTANT
Campo de la invención Field of the Invention
La presente invención se refiere a un dispositivo para mantener constante la temperatura media de un recipiente porta-muestras parcialmente sumergido en un líquido criogénico, cuya tasa de evaporación es alta, durante un largo periodo de tiempo. La invención también se refiere a un uso del dispositivo de la presente invención en analizadores de sorción.  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.
Estado de la técnica anterior  Prior art
Los analizadores de sorción vienen siendo ampliamente utilizados para la medida del área superficial, distribución de tamaño de poro y capacidad adsorbente de sólidos.  Sorption analyzers have been widely used for surface area measurement, pore size distribution and solids adsorption capacity.
Para realizar estas medidas, se adiciona una cantidad conocida de un gas en un recipiente cerrado en el que se encuentra la muestra a analizar y en el que se mide la presión. Al menos una parte de este recipiente, donde se encuentra la muestra a analizar, se encuentra a la temperatura de análisis. Conociendo la cantidad de gas que se ha adicionado, la presión final que se alcanza en el recipiente, el volumen del recipiente y la temperatura media del recipiente, se puede obtener la cantidad de gas sorbido por la muestra.  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.
Para que el análisis sea preciso, la temperatura media del recipiente no debe variar durante toda la duración del análisis o, si ésta varía, se debe conocer exactamente su variación a lo largo del análisis. En muchas de estas medidas, la temperatura de trabajo es una temperatura criogénica. 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.
Una forma muy habitual de mantener la muestra a analizar a la temperatura criogénica de análisis es sumergir la parte del recipiente donde se encuentra la muestra a analizar en un líquido criogénico, quedando otra parte del recipiente fuera de él. Para que la temperatura media del recipiente donde se encuentra la muestra sea constante durante todo el análisis, el nivel del líquido criogénico con respecto al recipiente donde se encuentra la muestra debe mantenerse constante, lo cual es un problema debido a que la tasa de evaporación de los líquidos criogénicos es muy elevada y los análisis pueden durar desde varios minutos hasta varios días, con lo que la temperatura media del gas contenido en el recipiente parcialmente sumergido varía con la variación del nivel del fluido criogénico Los fabricantes de equipos de sorción tratan de solucionar este efecto mediante diferentes sistemas de control basados en mantener un nivel lo más constante posible de fluido criogénico alrededor del recipiente donde se aloja la muestra a estudiar. Algunos de estos sistemas implementados en la actualidad están descritos en las patentes US4693124, US5646335, USRE33567 y CN202330371. 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 the average temperature of the gas contained in the partially submerged container varies with the variation of the level of the cryogenic fluid 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.
En otros casos, en vez de tratar de controlar el nivel constante de fluido criogénico, se han propuesto soluciones para poder conocer cómo afecta la variación del nivel de éste a la temperatura media del recipiente, de modo que se pueda aplicar correcciones a la medida de la presión interna del recipiente, como la descrita en la patente US6387704.  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.
Existe pues la necesidad de proporcionar un dispositivo mediante el cual se asegure el control y la constancia de la temperatura media de un recipiente donde se aloje una muestra a estudiar mediante el aseguramiento de un nivel constante de líquido criogénico con respecto a este recipiente por un largo tiempo, incluso pudiendo llegar a ser indefinido. .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. .
Breve descripción de la invención Brief Description of the Invention
La presente invención soluciona los problemas descritos en el estado de la técnica ya que se refiere a un dispositivo para mantener constante la temperatura media de un porta- muestras cerrado, parcialmentesumergido en un líquido criogénico mediante el mantenimiento de un nivel constante del líquido criogénico en el que está sumergido este porta-muestras. 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.
Así pues, en un primer aspecto, la presente invención se refiere a un dispositivo para mantener constante la temperatura de un porta-muestras que contiene una muestra (de aquí en adelante, dispositivo de la presente invención), que comprende: 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:
- un recipiente térmico que contiene un líquido criogénico,  - a thermal container containing a cryogenic liquid,
- al menos un vaso por el que fluye el líquido criogénico  - at least one vessel through which the cryogenic liquid flows
- al menos un porta- muestras, alojado en el interior del vaso  - at least one sample holder, housed inside the vessel
- medios de bombeo del líquido criogénico configurados para bombear de forma continua líquido criogénico hacia el vaso.  - means for pumping the cryogenic liquid configured to continuously pump cryogenic liquid into the vessel.
donde el vaso está configurado para que el líquido criogénico caiga en el interior del recipiente térmico cuando el borde del vaso es rebosado por el líquido criogénico. En una realización en particular de la presente invención, los medios de bombeo del líquido criogénico se encuentran en el interior del recipiente térmico. En una realización en particular de la presente invención, los medios de bombeo del líquido criogénico son bombas de impulsión. 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 cryogenic liquid pumping means are located inside the thermal container. In a particular embodiment of the present invention, the cryogenic liquid pumping means are discharge pumps.
En una realización particular de la presente invención, el nivel de líquido criogénico en el recipiente térmico está, como máximo, al mismo nivel que la parte superior del vaso donde se aloja el porta-muestras cuya temperatura se quiere controlar.  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.
En una realización en particular de la presente invención, el recipiente térmico comprende un nivel de control inferior, indicativo de un nivel insuficiente de líquido criogénico en el recipiente térmico. El nivel de control inferior está configurado de tal forma que, cuando el líquido criogénico desciende por debajo de dicho nivel, se puede realizar un aporte externo de líquido criogénico al recipiente térmico.  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.
En la presente invención, el nivel de control inferior del líquido criogénico se refiere a la altura o medida mínima que debe alcanzar el líquido criogénico en el recipiente térmico por debajo de la cual debe haber un aporte externo del líquido criogénico.  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.
En una realización en particular de la presente invención, el nivel de control inferior de líquido criogénico del recipiente térmico se encuentra por debajo de los medios de bombeo. In a particular embodiment of the present invention, the lower level of cryogenic liquid control of the thermal vessel is below the pumping means.
En una realización en particular de la presente invención, el recipiente térmico comprende un nivel de control superior de líquido criogénico indicativo de un nivel excesivo de líquido criogénico (4) en el recipiente térmico (3). El nivel de control superior está configurado de tal forma que, cuando el líquido criogénico que se repone supera dicho nivel, se puede detener el aporte externo de líquido criogénico. 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.
En la presente invención el nivel de control superior del líquido criogénico se refiere a la altura o medida máxima que debe alcanzar el líquido criogénico en el recipiente térmico por encima de la cual debe detenerse el aporte externo del líquido criogénico.  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.
En una realización en particular de la presente invención, el nivel de control superior de líquido criogénico del recipiente térmico se encuentra por debajo del nivel de rebose del vaso.  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.
En una realización en particular, el dispositivo de la presente invención comprende medios de control automático para el nivel de líquido criogénico en el recipiente térmico. En una realización en particular, los medios de control automático para el nivel del líquido criogénico, están conectados a un sistema de aviso al usuario para que éste haga la reposición manual y/o conectados a un sistema automático de reposición de líquido criogénico. Con este dispositivo y teniendo en cuenta las tasas de evaporación de los fluidos criogénicos y los volúmenes habituales de los termos utilizados en los equipos de sorción (entre 1 y 5 litros), se consigue mantener el nivel de líquido criogénico constante alrededor del porta-muestras durante un periodo de tiempo que puede ser de hasta varios días sin necesidad de reponer líquido criogénico. 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 cryogenic liquid replacement system. 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 the sample holder over a period of time that can be up to several days without the need to replace cryogenic liquid.
En una realización en particular, el recipiente térmico alberga más de un vaso, dichos vasos pueden estar a su vez conectados cada uno de ellos con medios de bombeo de líquido criogénico. En una realización más en particular, cada uno de los vasos alberga más de un porta-muestras.  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 one sample holder.
Los medios de bombeo utilizados en la presente invención están configurados de tal forma que aportan al menos un caudal equivalente a la tasa de evaporación del líquido criogénico en el área transversal expuesta del vaso o de los vasos. 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.
En un segundo aspecto, la presente invención se refiere al uso del dispositivo de la presente invención en analizadores de sorción.  In a second aspect, the present invention relates to the use of the device of the present invention in sorption analyzers.
Descripción de los dibujos Description of the drawings
La figura 1 muestra una realización particular de la invención en la que el dispositivo para mantener constante la temperatura comprende un recipiente térmico, con al menos un vaso, al menos un porta-muestras, medios de bombeo del líquido criogénico, nivel de control inferior y nivel de control superior.  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, lower control level and higher level of control
Referencias: References:
- Dispositivo para mantener constante la temperatura (1)  - Device to keep the temperature constant (1)
- Porta-muestras (2) - Sample holder (2)
- Recipiente térmico (3)  - Thermal container (3)
- Nivel de control inferior del recipiente térmico (31)  - Lower control level of the thermal vessel (31)
- Nivel de control superior del recipiente térmico (32)  - Upper control level of the thermal vessel (32)
- Líquido criogénico (4)  - Cryogenic liquid (4)
- Vaso (5)  - Glass (5)
- Medios de bombeo (6)  - Pumping means (6)
Descripción detallada de la invención El dispositivo para mantener constante la temperatura (1) de un porta-muestras (2) de la presente invención comprende: Detailed description of the invention The device for keeping the temperature (1) of a sample holder (2) of the present invention constant comprises:
- un recipiente térmico (3) que contiene un líquido criogénico (4),  - a thermal container (3) containing a cryogenic liquid (4),
- al menos un vaso (5), por el que fluye líquido criogénico (4) - at least one vessel (5), through which cryogenic liquid flows (4)
- al menos un porta-muestras (2), alojado en el interior del vaso (5)  - at least one sample holder (2), housed inside the vessel (5)
- medios de bombeo (6) del líquido criogénico (4) configurados para bombear de forma continua líquido criogénico (4) hacia el vaso (5).  - pumping means (6) of the cryogenic liquid (4) configured to continuously pump cryogenic liquid (4) into the vessel (5).
El vaso (5) está configurado para que el líquido criogénico (4) caiga en el interior del recipiente térmico (3) cuando el borde del vaso (5) es rebosado por el líquido criogénico (4). En un ejemplo de realización de la presente invención, que se observa en la figura 1 , se parte de un estado inicial en el que el nivel del líquido criogénico (4) no supera el nivel de rebose del vaso (5), una vez se conecta los medios de bombeo (6) del líquido criogénico (4), éste rebosa por la parte superior del vaso (5) de tal forma que el líquido criogénico (4) vuelve a caer en el recipiente térmico (3) manteniendo un nivel estable de líquido criogénico (4) alrededor del porta-muestras (2) parcialmente sumergido en el líquido criogénico (4), cuya temperatura se quiere controlar independientemente de la evaporación del líquido criogénico. En este ejemplo de realización, el sistema funciona correctamente hasta que el nivel del líquido criogénico (4) contenido en el recipiente térmico (3) caiga por debajo de la toma de los medios de bombeo (6) que es donde se encuentra el nivel de control inferior (31) del líquido criogénico.  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). 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) falls back into the thermal container (3) maintaining a stable level 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 intake of the pumping means (6) which is where the level of lower control (31) of the cryogenic liquid.

Claims

REIVINDICACIONES
1. Dispositivo para mantener constante la temperatura (1) de un porta-muestras (2), caracterizado por que comprende:  1. Device for keeping the temperature (1) of a sample holder (2) constant, characterized in that it comprises:
- un recipiente térmico (3) que contiene un líquido criogénico (4);  - a thermal container (3) containing a cryogenic liquid (4);
- al menos un vaso (5), por el que fluye líquido criogénico (4)i  - at least one vessel (5), through which cryogenic liquid flows (4) i
- al menos un porta-muestras (2), alojado en el interior del vaso (5);  - at least one sample holder (2), housed inside the vessel (5);
- medios de bombeo (6) del líquido criogénico (4) configurados para bombear de forma continua líquido criogénico (4) hacia el vaso (5); - pumping means (6) of the cryogenic liquid (4) configured to continuously pump cryogenic liquid (4) into the vessel (5);
donde el vaso (5) está configurado para que el líquido criogénico (4) caiga en el interior del recipiente térmico (3) cuando el borde del vaso (5) es rebosado por el líquido criogénico (4).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. Dispositivo según la reivindicación 1 , donde los medios de bombeo (6) del líquido criogénico (4) están en el interior del recipiente térmico (3). 2. Device according to claim 1, wherein the pumping means (6) of the cryogenic liquid (4) are inside the thermal container (3).
3. Dispositivo según cualquiera de las reivindicaciones anteriores, donde los medios de bombeo (6) son bombas de impulsión.  3. Device according to any of the preceding claims, wherein the pumping means (6) are discharge pumps.
4. Dispositivo según cualquiera de las reivindicaciones anteriores, donde el recipiente térmico (3) comprende un nivel de control inferior (31), indicativo de un nivel insuficiente de líquido criogénico (4) en el recipiente térmico (3). 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. Dispositivo según la reivindicación 4, donde el nivel de control inferior (31) está por debajo de los medios de bombeo (6).  5. Device according to claim 4, wherein the lower control level (31) is below the pumping means (6).
6. Dispositivo según cualquiera de las reivindicaciones anteriores, donde el recipiente térmico (3) comprende un nivel de control superior (32) indicativo de un nivel excesivo de líquido criogénico (4) en el recipiente térmico (3). 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. Dispositivo según la reivindicación 6, donde el nivel de control superior (32) está por debajo de un nivel de rebose del vaso (5).  7. Device according to claim 6, wherein the upper control level (32) is below an overflow level of the vessel (5).
8. Dispositivo según cualquiera de las reivindicaciones anteriores, que comprende medios de señalización para mostrar el nivel de líquido criogénico (4) para su posible reposición manual. 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. Dispositivo según cualquiera de las reivindicaciones anteriores, que comprende medios de control automático del nivel de líquido criogénico (4).  9. Device according to any of the preceding claims, comprising means for automatic control of the level of cryogenic liquid (4).
10. Uso de un dispositivo según cualquiera de las reivindicaciones 1-9 en analizadores de sorción. 10. Use of a device according to any of claims 1-9 in sorption analyzers.
PCT/ES2016/070878 2015-12-21 2016-12-12 Device for maintaining constant the temperature of a sample-holder and use of the device in sorption analysers WO2017109246A1 (en)

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WO2020157646A1 (en) 2019-01-31 2020-08-06 Anton Paar Quantatec Inc. Inverted wick type temperature control system for sorption analysis
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