• 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:
    The invention relates to a method and an ATR sensor for measuring the CO 2 content of fluids with an ATR sensor, in a housing (6) as sensor components, an electromagnetic radiation source (2) for emitting a predetermined wavelength range, one permeable to the radiation and with the fluid to be examined (5) brought into contact with the reflection body (1) and a detector (3) for the reflected radiation and further serving to carry out the measurement and operation of serving components (16, 17, 18). According to the invention, before the gas-tight closure of the housing (6), in particular to avoid a measured value drift and to keep the radiation paths of CO 2, in the housing (6) and / or in a with the interior (7) of the housing (6). connectable or connected receiving space (7a) of an additional housing (6a) before the gas-tight closing of the inner space (7) and / or the receiving space (7a) C02 getter material (8) is introduced
    公开号:AT512375A1
    申请号:T1884/2011
    申请日:2011-12-23
    公开日:2013-07-15
    发明作者:Michael Dipl Ing Imre；Johann Dipl Ing Loder；Gerhard Dipl Ing Dr Pfeifer
    申请人:Anton Paar Gmbh；
    IPC主号:
    专利说明:

    The invention relates to a method according to the preamble of claim 1 and an ATR sensor according to the preamble of claim 3.
    The invention serves to measure the CO 2 content of fluids, wherein the fluids can also consist of several components. In particular, in this way liquids, e.g. Beverages are examined, which are composed of several components. It is usually difficult to measure CO2 contained in fluids because CO 2 is an inactive gas. One way to measure C02 is the so-called ATR (Attenuated Total Reflection) method.
    The technique of measuring C02 via attenuated total reflection, also known as multiple internal reflection, has been used for many years for C02 analysis. In ATR spectroscopy, the effect of using a light beam at the interface between an optically denser medium having the refractive index n1 and an optically thinner medium having the refractive index n2 (n1> n2) is totally reflected when the angle of incidence of the light beam to the interface exceeds the critical angle of total reflection. For the limiting angle, sinG = n2 / n1.
    At the interface, the light beam exits into the optically thinner medium and interacts with it. Behind the reflecting surface, the so-called evanescent wave forms, with a penetration depth in the range of the wavelength. The penetration depth dp depends on the two refractive indices m and n2, the wavelength λ used and the angle of incidence Θ.
    λ
    If the optically thinner medium absorbs the penetrating radiation, the totally reflected beam is weakened. The attenuation or partial extinction is dependent on the wavelength and the spectrum of the totally reflected radiation can be used analogously to the transmission measurement for the spectroscopic evaluation. From the transmission or extinction spectrum can be concluded that the composition of the optically thinner medium.
    Furthermore, the determination of low and lowest concentration ingredients from the absorption of infrared radiation is a known method of detecting CO 2. It exploits the fact that molecules are vibrated by infrared radiation of selected wavelengths. For example, dissolved CO 2 has a characteristic absorption band in the range around 4.3 pm. About the
    Lambert-Beer's law allows the absorption to be translated into precise concentrator measurements. It describes Εχ = - lg (l / lo) = εχ-c.d with Εχ absorption at the wavelength λ I intensity of the transmitted light l0 intensity of the incident light εχ extinction coefficient c concentration d layer thickness of the irradiated body.
    The two basic principles are advantageously used together in the measurement of the CO 2 content in fluids.
    In Fig. 1, a known ATR sensor is shown. The core of the ATR sensor is a reflection body, which is transparent in the region of interest for the radiation used, in particular IR radiation in the range of 4.3 μm, and has a high refractive index. Known, in particular crystalline, materials for such optical reflection bodies are, for example, sapphire, ZnSe, Ge, Sl, thallium bromide, YAG, spinel etc. Frequently, the reflection body is designed in such a way that the intensity yield is increased by multiple reflections in its interior. Other sensor components are more suitable for one or more radiation sources
    Frequency (ranges), optionally means for frequency selection and one or more detectors for the reflected radiation; These can also be carried out frequency-selective. An evaluation unit stores the intensities measured at the detector and supports the evaluation of the data or converts the measured intensities into the associated CO 2 concentrations. At least the sensor components are installed in the interior of a housing. In this housing are also the required further components, e.g. Lines, seals, frequency selection means, etc., arranged. The measuring surface of the reflection body is brought into contact with the fluid to be measured.
    In the simplest form, an ATR sensor comprises a reflection body formed by a crystal as an optically active element which enables the internal reflections, a radiation source and a detector. The reflection body protrudes with its measuring surface into the fluid to be examined, either directly into the process stream or into the fluid contained in a container. Such ATR sensors thus have at least three sensor components arranged in a suitable manner with respect to each other. The optically 3 3 '' '' ♦ '' t '' · · · · · · · · ·.... · »» »» Active element or the reflection body is gas-tight pressed against the housing or connected with this pressure and gas-tight, eg by means of O-ring or inelastic seals, e.g. made of PEEK, TEFLON etc.
    It was found that such ATR sensors are faulty, in particular that a long-term drift exists, with which the measured actual values deviate more and more from the actual measured values. For this reason, it has been necessary to calibrate or readjust such measuring devices at regular, relatively short intervals.
    The aim of the invention is to create a measuring method or an ATR sensor with which these disadvantages are avoided. ATR sensors according to the invention should also be largely temperature-resistant in order to survive high-temperature cleaning processes in operation which such sensors must undergo in practice, in particular if they are used for the measurement of food products.
    These objects are achieved in a method of the type mentioned in that prior to the gas-tight sealing of the housing, in particular to avoid a measured value drift and to keep the radiation paths of CO 2, in the housing and / or connected to the interior of the housing or connected Receiving space of an additional housing before the gas-tight sealing of the housing and / or the receiving space of the additional housing C02 getter material is introduced. An ATR sensor of the type mentioned above is characterized in that in the interior of the gas-tightly sealed housing and / or in a gas-tightly connected to the interior or connectable receiving space of an additional housing C02 getter material is included.
    Accurate and lengthy investigations to find out the cause of the unexplainable sensor - to - sensor long - term drift revealed that this long - term drift is mainly due to outgassing of CO 2 from the used electrical sensor components and the other components required for the measurement enclosed in the interior of the housing. The C02 outgassing these sensor components and components directly influences the measurement since it enters the radiation path and influences the electromagnetic radiation guided from the radiation source to the detector. Since the components and sensor components in the housing unavoidably and continuously deliver low or very small amounts of CO 2, it has hitherto been the case in practice that the measured values differ and the sensor has been in use, the more so from the initially adjusted or deviate from calibrated setpoints.
    With the getter material inserted or enclosed in the housing, it is now possible to decombine the successively outgassing CO 2 and thus to maintain the calibration of the ATR sensor to its exact initial value.
    It is advantageous if the CO 2 getter material is introduced in at least one quantity which comprises CO 2 outgassing CO 2 from the sensor components and components contained in the housing and / or in the additional housing over a period of time which is at least the expected lifetime of the ATR sensor or at least the time period until for opening the housing and / or additional housing for required maintenance and / or adjustment purposes, can accommodate. This creates a largely calibration-free and maintenance-free ATR sensor. At predetermined maintenance times, which are determined in particular by the replacement of the required seals, which age under process conditions, and possibly also by maintenance of the electrical and optical components, and the getter material can be replaced. According to the invention, a virtually drift-free CO 2 sensor is created, which requires minimal maintenance over its entire service life.
    It is advantageous if the CO 2 getter material on heating, preferably at a temperature of 200 to 1000 ° C, preferably at 300 to 600 ° C, C02 in its interior receives and binds and thus its surface for receiving more C02 molecules provides. Such a porous getter material has the ability to absorb the bound on its surface C02 molecules in its interior when heated and can thus absorb at temporary reactivation over the lifetime of the ATR sensor C02 and repeatedly provides free surface areas for recording or Addition of new from the sensor components and components outgassing C02 molecules available.
    It is expedient if the CO 2 getter material is temperature-resistant up to 200 ° C., preferably 150 ° C., with regard to its CO 2 affinity. In the case of a necessary device cleaning during use, which takes place at the specified temperatures, or in high-temperature measurements, the getter remains active.
    The sensor may have a directly integrated control and evaluation or have a transducer, with a remote unit for the display and operation of the sensor, such as a PC or display and control devices. Several sensors can also be monitored simultaneously via interfaces and their data can be read out and used for process control.
    It may be advantageous if in addition to the C02 getter material further getter materials in the interior of the housing and / or in the receiving space of
    Housing additional housing that bind and / or absorb carbonaceous gases and / or water vapor. Thus, at most occurring influence of other gas molecules can be excluded.
    It may be structurally advantageous if a connection for a purge gas line is formed on the housing and / or additional housing or a purge gas line is connected.
    In principle, it is also possible that the C02 getter material is introduced into the receiving space of an additional housing, which is connected via an optionally closable with a closure unit line with the interior of the housing and / or in the interior of the housing and / or in the receiving space means for Forced circulation, preferably a fan, which is arranged in the interior and / or in the receiving space atmosphere. It may also be expedient if a gas-tight closable wall opening for exchanging or refilling C02 getter material is formed in the housing and / or in the additional housing.
    In order to increase the service life and absorption capacity of the getter material, it can be provided that a heater for the CO 2 getter material is provided for activating or reactivating the CO 2 getter material in the housing and / or in the additional housing.
    In the following the invention will be explained in more detail with reference to the drawings, for example.
    FIG. 2 shows a comparable ATR sensor according to the invention with the ATR sensor shown in FIG. 1, in which getter material is located in the interior of the housing. 3 shows an embodiment of an ATR sensor according to the invention, in which the getter material is located in a receiving space of an additional housing connected to the interior of the housing. 4 shows an embodiment of an ATR sensor, in which the getter material is located in its own receiving space, which can be connected to the interior of the housing, of an additional housing which is equipped with a heating device.
    Fig. 2 shows an embodiment of an ATR sensor in which an ATR element, i. a reflecting body 1 formed by a crystal is arranged. The housing 6 is inserted with an outer wall 10 with seals 11 in a line 5a for a fluid 5. An electromagnetic radiation source 2 radiates into the reflection body 1 electromagnetic radiation having a predetermined wavelength range, which is reflected after multiple reflection at the boundary surfaces 15 of the reflection body 1 to the fluid to be examined 5 in a detector 3.
    The fluid 5 to be examined can be guided in a line 5a or is arranged in a container. Provision must be made for the reflection body 1 to be in appropriate contact with the fluid 5 to be examined, in particular liquids. In the interior 7 of the housing 6, in addition to the sensor components which are absolutely necessary for the measurement, all other components required for carrying out the measurement are indicated, which are indicated at 18. In the interior 7 of the housing 6 is Gettermateriai 8. Furthermore, in the interior 7 means for moving the inner atmosphere, e.g. a fan 9 may be provided, which supply the getter material 8 from the sensor components located in the interior 7 and further components and also the self-exiting C02 molecules 12. As soon as a C02 molecule hits the surface of the getter material 8, it is bound.
    The housing 6 of the ATR sensor is designed so that the smallest leakage rates to the environment or external spaces and the fluid to be examined 5 are present. This is achieved by a completely closed housing 6 and by vacuum-tight passages or seals 16 for any lines 17. Furthermore, the electrical connections and the seat of the reflection body 1 with regard to the process environment are designed pressure and temperature resistant. The housing 6 can be made resistant to chemicals especially for special applications.
    The getter material 8 is advantageously chosen such that its activation energy is as small as possible. The getter material 8 is a chemically reactive material which can bind to its surface either by absorption or by chemical bonding C02. It is advantageous if the CO 2 molecules precipitated on the free surfaces can be removed from the surface by heating in such a way that they penetrate into the interior of the getter material 8, thus making room for the attachment of further CO 2 molecules to the surface is created, whereby a reactivation of the getter material 8 is possible.
    In order to be able to use such getter materials 8 advantageously in ATR sensors according to the invention, getter material 8 is introduced into the interior space 7, which has a sufficiently large surface area in order to be able to set all C02 molecules outgassing for a given operating time. Alternatively, it can be provided that getter material 8 is used, which can be regenerated by heating. It is also possible that the getter material 8 is flushed out by supplying a flushing gas and the CO 2 molecules leaving are removed. This rinsing is advantageously carried out at elevated temperature of the getter material 8. ♦ ♦ ♦ ♦ ♦ ♦ ♦ ♦ ♦ · 4 ♦ · ♦ »> ♦ · · · ·· ···· »**« · # · #
    Well replaceable getter materials 8 are, for example, barium, aluminum and / or magnesium alloys; Titanium and platinum are also suitable for this purpose. Non-evaporable getter materials 8 can also be used, as are known, for example, from vacuum technology. These form stable compounds with CO2 and even at higher temperatures absorbed CO2 molecules are not released from the getter material. An example of such getter materials 8 is zirconium, for example.
    As shown in FIG. 3, it is also possible to connect the housing interior 7 to the inner or receiving space 7a of an additional housing 6a and to place the getter material 8 or further getter material 8 in the receiving space 7a. Via a fan 9, the atmosphere of the inner space 7 is exchanged with the atmosphere of the receiving space 7a, and the outgassed C02 molecules are conveyed from the housing interior 7 to the getter material 8. The additional housing 6a may be designed to be removable or gas-tight connectable to the housing 6, for example via a provided in the connecting line 6c shut-off device 6d, as it is dargesteift in Fig. 4.
    If recorded CO 2 molecules form a protective passivation layer on the getter surface, the getter material 8 can be reactivated by heating after a predetermined period of time. Depending on the material, the activation temperature can be 200 to 1000 °. Upon activation, the temperature increase causes the C02 molecules or molecule compounds bound to the getter surface to be mobilized and diffuse into the getter volume, so that the surface becomes receptive again. Such activation of the getter material 8 could, for example, in the cleaning of the outer surface of the housing 6 in operation at the intended elevated cleaning temperature or by its own heating device 18 which is arranged in the interior 7 of the housing 6 or in the receiving space 7a of the auxiliary housing 6a. The heating device 18 is supplied or controlled by a current source or control unit 17.
    As shown in Fig. 4, purge gas may be supplied into the housing 6 and / or the auxiliary housing 6a via a purge gas inlet 19 and a purge gas outlet 20.
    权利要求:
    Claims (12)
    [1]
    1, A method for measuring the CO2 content of fluids with an ATR sensor, in a housing (6) as sensor components, an electromagnetic radiation source (2) for emitting a predetermined wavelength range, one for the radiation permeable and with the examined Having fluid (5) can be brought into contact reflection body (1) and a detector (3) for the reflected radiation and further serving for the measurement and operation of serving components (16, 17, 18), characterized in that prior to the gas-tight sealing of Housing (6), in particular to avoid a measured value drift and to keep the radiation paths of CO2, in the housing (6) and / or in a with the interior (7) of the housing (6) connectable or connected receiving space (7a) of an additional housing ( 6 a) before the gas-tight closing of the inner space (7) and / or the receiving space (7 a) C02 getter material (8) is introduced.
    [2]
    2. The method according to claim 1, characterized in that the C02 getter material (8) is introduced in at least an amount which outgassing from the sensor components and components contained in the housing (6) and / or additional housing (6a) C02 over a period of time, at least the expected life of the ATR sensor or at least the time to open the housing (6) and / or additional housing (6a) for required maintenance and / or adjustment purposes record can accommodate.
    [3]
    3, ATR sensor, in particular for measuring the CO 2 content of fluids, in a housing (6) as sensor components an electromagnetic radiation source (2) for emitting a predetermined wavelength range, a permeable to the radiation and with the fluid to be examined (5 ) and a detector (3) for the reflected radiation and further required for carrying out the measurement and operation components, characterized in that in the interior (7) of the gas-tight housing (6) and / / or in a with the interior (7) gastight connected or connectable receiving space (7a) of an additional housing (6a) C02 getter material (8) is included.
    [4]
    4. ATR sensor according to claim 3, characterized in that the C02 ~ getter material (8) on heating, preferably at a temperature of 200 to 1000 ° C, preferably at 300 to 600 ° C, C02 in its interior receives and binds and so that its surface is available for the uptake of further C02 molecules. ·· Q ···································································································. «Ftftftft» «·« «« «* * ♦
    [5]
    5. ATR sensor according to claim 3 or 4, characterized in that the C02 getter material (8) up to 200 ° C, preferably 150 ° C, with respect to its C02 affinity temperature resistant.
    [6]
    6. ATR sensor according to one of claims 3 to 5, characterized in that in the interior (7) and / or in the receiving space (7a) as serving to carry out the measurement and operation components control and / or evaluation units (18), Transducer seals (16), lines (17), receptacle for the COz getter material (8) and / or electronic components are arranged.
    [7]
    7. ATR sensor according to one of claims 3 to 6, characterized in that in addition to the C02 getter material (8) further getter materials in the interior (7) of the housing (6) and / or in the receiving space (7a) of the additional housing (6a ), which bind and / or absorb carbonaceous gases and / or water vapor.
    [8]
    8. ATR sensor according to one of claims 3 to 7, characterized in that on the housing (6) and / or on the additional housing (6a) is formed a connection (19) for a purge gas line or a purge gas line is connected.
    [9]
    9. ATR sensor according to one of claims 3 to 8, characterized in that the C02 getter material (8) in the receiving space (7a) of an additional housing (6a) is introduced, which can be shut off via a possibly with a closure unit (6d) line (6c) is connected to the interior (7) of the housing (6).
    [10]
    10. ATR sensor according to one of claims 3 to 9, characterized in that in the interior (7) of the housing (6) and / or in the receiving space (7 a) means (9) for forced circulation, preferably a fan, in the interior (7) and / or in the receiving space (7a) located atmosphere is arranged.
    [11]
    11. ATR sensor according to one of claims 3 to 10, characterized in that in the housing (6) and / or in the additional housing (6a) a gas-tight closable wall opening for replacement or refilling of C02 getter material (8) is formed.
    [12]
    12. ATR sensor according to one of claims 3 to 11, characterized in that for activating or reactivating the C02 getter material (8) in the housing (6) and / or in the additional housing (6a), a heating device (18) for the C02- Getter material (8) is provided. Vienna, December 23, 2011
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    ATA1884/2011A|AT512375B1|2011-12-23|2011-12-23|METHOD AND SENSOR FOR MEASURING THE CO2 CONTENT OF FLUIDS|ATA1884/2011A| AT512375B1|2011-12-23|2011-12-23|METHOD AND SENSOR FOR MEASURING THE CO2 CONTENT OF FLUIDS|
    EP12455011.2A| EP2607887A3|2011-12-23|2012-12-20|Method and sensor for measuring the carbon dioxide content of fluids|
    DE202012013546.5U| DE202012013546U1|2011-12-23|2012-12-20|Sensor for measuring the CO2 content of fluids|
    US13/724,776| US9063083B2|2011-12-23|2012-12-21|Method and sensor device for measuring a carbon dioxide content in a fluid|
    CN201210599030.XA| CN103257125B|2011-12-23|2012-12-21|For measuring the method for CO2 content and the sensor of fluid|
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