EP4669949A1 - Probenentnahmevorrichtung zur entnahme einer probe aus einem ein flüssiges medium führenden anlagenteil sowie verfahren zur entnahme einer solchen probe - Google Patents
Probenentnahmevorrichtung zur entnahme einer probe aus einem ein flüssiges medium führenden anlagenteil sowie verfahren zur entnahme einer solchen probeInfo
- Publication number
- EP4669949A1 EP4669949A1 EP24706731.7A EP24706731A EP4669949A1 EP 4669949 A1 EP4669949 A1 EP 4669949A1 EP 24706731 A EP24706731 A EP 24706731A EP 4669949 A1 EP4669949 A1 EP 4669949A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- sample
- sampling
- line arrangement
- medium
- section
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/20—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials
- G01N1/2035—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials by deviating part of a fluid stream, e.g. by drawing-off or tapping
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N2001/1062—Sampling under constant temperature, pressure, or the like
- G01N2001/1068—Cooling sample below melting point
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/20—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials
- G01N1/2035—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials by deviating part of a fluid stream, e.g. by drawing-off or tapping
- G01N2001/205—Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials by deviating part of a fluid stream, e.g. by drawing-off or tapping using a valve
Definitions
- Sampling device for taking a sample from a part of a system carrying a liquid medium and method for taking such a sample
- the invention relates to a sampling device for taking a sample from a liquid medium located in a system, with a sample holder into which the sample taken can be introduced via a feed device, and to a method for taking a sample from a liquid medium located in a part of the system by means of a sample holder into which the sample is introduced via a feed device, and further to a use of such a sample holder device and an application of the method.
- a sampling device for taking a sample from a liquid medium of this type conducted in a system has a feed device which is coupled or can be coupled to a suitable location in the system and to which a receptacle is assigned on the output side in order to feed the sample taken from the liquid medium in a specific quantity.
- Another sampling device and a method for taking a sample from a liquid medium conducted in a system, in particular for the analysis of biological material, is shown in US 5 902 746 A.
- the liquid medium can be frozen and the seal can be opened again by supplying electrical energy while heating.
- a sampling device shown in DE 1 955 988 A is designed in particular for sampling liquid metals and for chemically analyzing liquid metal melts for impurities in nuclear reactor circuits.
- the repeated taking of a sample from a liquid medium in a system is useful, and often even necessary, in order to determine changes in the properties of the medium by analyzing the sample.
- a sample taken from the liquid medium while the system is in operation such as a chemical reactor, thermal storage facility or other storage facility which uses, for example, molten inorganic salts, nitrate salts, chloride salts or carbonate salts at temperatures of 150 °C to 800 °C as a working medium or heat transfer medium
- the long-term stability of the salt and of the components brought into contact with it can be checked and suitable measures can be taken.
- taking a sample using conventional sampling devices of the type mentioned is cumbersome, time-consuming and, due to the manual sampling, potentially dangerous.
- the present invention is based on the object of providing a sampling device of the type mentioned at the outset, with which an automated sampling of samples from the ongoing operation of a system or from a system part thereof (such as a pipeline, tank or other components) is made possible as safely and reproducibly as possible, and of specifying a corresponding method and an application.
- the feed device has a line arrangement which, on the input side, is provided with a connection unit which is or can be coupled to a part of the system in a medium-conducting manner and, on the output side, is provided with a discharge section which is or can be connected to the sample holder in a medium-conducting manner and which has an openable and closable closure device.
- an automated sampling of samples is achieved during ongoing operation of the system without endangering people, so that a practical repeated and reproducible sampling of the samples is possible, especially at higher temperatures of e.g. between 100 °C and 1600 °C, preferably between 150 °C and 800 °C, such as with molten inorganic salts in a system as a working medium or heat transfer medium.
- the automated sampling designed in this way is also used for other liquid media, for example corrosive media.
- the sampling can be carried out, controlled or regulated precisely using a control device.
- the fact that the feed device has a pressure reduction device in an inlet area contributes to precise sampling.
- a precisely reproducible, defined sampling is further facilitated by the fact that the pressure reducing device has a pipe with a reduced cross-section relative to the connection unit or a nozzle part with a narrowing part directed towards the inlet side.
- the pressure reduction device has a pressure compensation device or flow limiting device arranged downstream of the nozzle part, if present, in particular designed as a passive fluidic valve, for example a Tesla valve.
- the feed device has a laminarization section, in particular designed det as a dosing lance, wherein the laminarization section in the embodiment according to one of claims 2 to 4 is arranged downstream of the pressure reducing device in the flow direction.
- closure device can be controlled automatically and/or time-dependently depending on the sample size to be taken and/or the temporal sequence of the sampling.
- the closure device which is preferably arranged in the outlet region of the feed device, has a tempering device which, for closing, has a freezing device that forms a closure plug by freezing the medium, in particular by free or forced convection, and for opening, has a heating device that dissolves the closure plug, in particular by preventing convection by means of an insulating body or air flow inhibitor.
- a structure which is advantageous for the function consists in the fact that the freezing device has a fan which generates a cooling air flow around a line section of the line arrangement, in particular around the laminarization section.
- the heating device has an actively energized trace heating system and/or is operated passively using the heat of the supplied medium.
- the measures that contribute to good function and efficiency of the temperature control device are that the temperature control device has a heat conducting unit that is thermally connected to the line arrangement, in particular provided with cooling fins. Precise controllability or adjustability of the sampling is also advantageously supported by the fact that the feed device has a pressure difference regulating device assigned to the line arrangement, which comprises a pressure regulating unit arranged in a bypass line, which effects a pressure difference regulation in particular over the area of the temperature control device.
- sampling device further consists in that the feed device is provided on the output side with an adjustment device having a sampling part and a waste removal part, which comprises an adjustment part mounted on a support unit, wherein the sample holder is assigned to the sampling part and a waste holder is assigned to the waste removal part.
- the adjustment part is preferably held on the system part with a fastening part.
- the adjustment device is designed as a linear table or rotary table, which further comprises a guide part and a drive unit for adjusting the adjustment part from a rest position in which the discharge section of the line arrangement is closed, into a waste removal position in which the waste removal part is assigned to the discharge section of the line arrangement or into a sample removal position in which the sample removal part is assigned to the discharge section of the line arrangement, and back.
- Advantageous embodiments of the method consist in that the flow path is closed by freezing the medium in a section of the line arrangement to form a plug and that the flow path is opened by dissolving the plug using heat, and further in that before taking the sample, a waste amount of medium is directed into a waste receptacle by opening the flow path and then closing it.
- Fig. 1 is a schematic representation of a sampling device connected to a part of a plant
- Fig. 2 shows a sampling device according to Fig. 1 supplemented with a pressure difference regulating device
- Fig. 3 shows another embodiment of the sampling device in perspective view
- Fig. 4 shows a partially cutaway section of the sampling device according to Fig. 3 in its connection area on the system part and
- Fig. 5 shows a further section of the sampling device according to Fig. 3 in its receiving area for the sample.
- Fig. 1 shows an embodiment of a sampling device 1, which is coupled to a system part 2 of a system (not shown in detail) by means of a connection unit 10.
- the system with the system part 2 carries a liquid medium, which generally has a corrosive effect on components of the system that come into contact with it.
- the system is a chemical reactor or thermal or other storage device that uses molten inorganic salt, such as nitrate salt, chloride salt or carbonate salt, at a higher temperature in the range between 100 °C and 1600 °C, often between 150 °C and 800 °C, as a working medium. medium or heat transfer medium is used.
- the liquid medium is usually under increased pressure, e.g. in the order of a few bar or a few tens of bars.
- the sampling device 1 has a feed device comprising the connection unit 10 and a line arrangement 4 connected thereto, via which a sample taken from the liquid medium guided in the system is fed into a sample receptacle 16.
- the line arrangement 4 has, following the connection unit 10, a pipe 11 whose cross-section is reduced compared to the inlet section of the connection unit 10, which leads to the sample receptacle 16 via a pressure compensation device 12 or a flow limiter, which is designed, for example, as a Tesla valve, via a further section of the line arrangement 4 in which a closure device is arranged.
- the sample receptacle 16 can be assigned to a discharge section of the line arrangement 4 provided with an outlet, alternating with a waste receptacle 15, such as a waste container.
- a predeterminable or predetermined quantity of the liquid medium taken from the system can be set automatically by appropriate time-dependent and/or quantity-dependent control of a control device controlling the sampling device 1, in particular the closure device, to obtain a defined sample, for example also under control by means of a control device. This results in reproducible sampling, e.g. at predeterminable time intervals or depending on events, without endangering an operator and/or operator-dependent errors.
- the closure device is designed in a special way by means of a tempering device 13.
- a part of the extracted liquid medium itself is used as a closure element to close the line arrangement 4, in particular in its outlet area, in that it is heated by means of the tempering device 13 in a section of the line arrangement.
- Order 4 is cooled to below its solidification temperature, so that a sealing plug forms through freezing.
- the temperature control device 13 has a cooling device, for example comprising a fan 132, by means of which a cooling air flow is generated around the relevant line section carrying the liquid medium.
- the line section is expediently provided with a heat conduction unit 131, e.g. having cooling fins.
- the sealing plug saves on other sealing components and avoids corrosion reactions and the resulting functional impairments.
- the fan 132 can be switched off and the heat of the supplied liquid medium itself can be used as a passive heat source.
- the temperature control device 13 is provided with a heating device 130 as auxiliary heating, which is designed, for example, as an electrical heating device, and the heat of which is used, for example, for heating the pipe. B. when the fan 132 is switched on, the heat is fed via the heat conduction unit 131 to the line section with the closure plug, which dissolves or melts as a result, so that the liquid medium reaches the sample holder 16 in a regulated manner.
- the amount of liquid medium guided through the line arrangement 4, in particular also the relevant section thereof, as well as the cooling capacity of the temperature control device 13 and the heating energy are coordinated with one another in such a way that a relevant amount of the liquid medium reaches the sample holder 16 as a sample under control or regulation of the closure device designed in this way by means of the control device.
- the sampling device 1 also has the waste receptacle 15, which can be assigned to the outlet of the line arrangement 4 in a waste removal function by means of the adjustment device 3 instead of the sample receptacle 16.
- the closure device for example the temperature control device 13, can also be used for this purpose. be controlled by supplying heat in such a way that the line arrangement 4 is opened to discharge the waste quantity of the liquid medium into the waste receptacle 15 by dissolving the closure plug.
- the sample receptacle 16 can then be assigned to the outlet of the line arrangement 4 again in order to take a relevant (current) quantity of the liquid medium from the system as a sample.
- the line arrangement 4 can be closed by actuating the closure device, for example by forming the closure plug.
- the sampling device 1 shown in Fig. 1 therefore works, for example, as follows: Before sampling, all controllable components, in particular the closure device or temperature control device 13, are switched off.
- the heat conduction unit 131, in particular the cooling fins, are dimensioned such that free convection is sufficient to dissipate the heat coming from the hot system part 2 and to hold a solidified closure plug or salt plug in the area of the line arrangement 4 with the heat conduction unit 131.
- the waste receptacle 15 with the waste container is assigned to the discharge section or is arranged under the outlet.
- both the fan 132 and the heat source of the heating device 130 are switched off.
- the heating device 130 is dimensioned such that it can quickly melt the plug in the relevant section of the line arrangement 4 despite the additional cooling effect of the fan 132.
- the medium or liquid salt flows into the waste receptacle with the waste container.
- the medium flow or salt flow is regulated by the pressure compensation device 12 or the flow limiter, in particular in the form of the Tesla valve.
- the heating device 130 can now be switched off briefly, whereby the temperature in the relevant section of the line arrangement 4 drops extremely due to the strong cooling effect of the fan 132 and a sealing plug forms again.
- the medium flow is now briefly interrupted.
- the sample holder 16 with a sample container is now assigned to the discharge section or moved under the outlet of the same.
- the heating device 130 with the heat source is now switched on again and the sealing plug melts again.
- the medium now flows into the sample holder 16 in a regulated manner through the pressure compensation device 12 or the flow limiter, in particular the Tesla valve. An interruption of the medium flow can also be dispensed with.
- the heating device 130 is first switched off.
- the fan 132 initially remains switched on in order to reduce the temperature in the relevant section of the line arrangement 4 as quickly as possible. A sealing plug forms again. The fan 132 is now also switched off.
- liquid molten salt for example, can be advantageously defined as a liquid medium and reproducibly extracted from a relevant plant, such as from a thermal energy storage facility in the field of solar thermal power plants or from salt-based reactors, such as endothermic or exothermic reactors.
- a pressure difference regulation device 17 which has a bypass to the line arrangement 4 with a pressure regulation unit 170.
- the bypass is connected on the inlet side to the outlet area of the line arrangement 4 and the area of the waste receptacle 15 or sample receptacle 16 arranged there and is led back into an area in the flow direction upstream of the temperature control device 13 or the pressure compensation device 12, e.g. to the pipeline 11, as can be seen from Fig. 2.
- the pressure difference regulation device device 17 thus regulates the pressure difference between the internal system pressure and a sample chamber in which the sample is taken from the line arrangement 4, whereby the pressure difference control has self-regulating components.
- the pressure regulation unit 170 arranged in the bypass is based, for example, on the formation of a gas cushion or on the use of a flexible membrane.
- an output pressure of 1 bar is created in the area of the sample chamber at a system pressure of 20 bar, for example. This allows a reproducible sample to be taken in a defined and simple manner.
- the sampling device 1 is also connected to a system part 2 by means of a flange connection and a feed device with a line arrangement 4 is present, at the discharge section or outlet of which a sample holder 16 can be arranged alternately with a waste holder 15.
- the adjustment between the sample holder 16 in the sampling position and the waste holder 15 in the waste removal position is also carried out by means of an adjustment device 3, the adjustment device 3 in this embodiment being designed as a linear table.
- the line arrangement 4 also has a closure device which has a temperature control device 13, in particular of the structure described above, for the defined supply of liquid medium as a sample.
- a quantity of waste present in the line arrangement 4 is discharged into the waste holder 15 in a rinsing process.
- a dosing lance is installed, by means of which a laminarization section 14 is formed for the liquid medium passed through and a connection to a control slide present in the adjustment device 3 or an adjustment part is created, wherein the laminarization section 14 is closed by the control slide or opens in the waste removal position or the sample removal position.
- the liquid medium e.g. a salt flow
- the liquid medium e.g. a salt flow
- a nozzle section is formed in the inlet area of the line arrangement 4, which narrows continuously, e.g. conically, towards the inlet area or towards the system part 2 and causes an active pressure reduction of the liquid medium coming from the system part 2 by increasing the pipe cross-section at a constant flow rate.
- the subsequent pressure compensation device 12 for example the Tesla valve, then serves to further reduce the pressure or to equalize gas or medium pressures.
- the adjustment device 3 designed as a linear table has a guide part 30 and a drive unit 31 which, for example, engages by means of a gear in a rack for adjusting the adjustment part of the adjustment device 3.
- the adjustment part has a sample removal part 32 with the sample holder 16 and a waste removal part 36 which is coupled to the waste holder 15 and has a free jet piece 33 leading to the waste removal part 36, via which a waste quantity of the removed medium can be guided into the waste holder 15.
- the linear table can be provided with a closure part 34 for closing the outlet of the line arrangement 4 in a rest position and also with a freezing part 35 in order to form a closure plug by freezing the liquid medium in the outlet area of the line arrangement 4.
- a heating device can be integrated into the linear table as a trace heating device for dissolving the sealing plug for the removal of the liquid medium.
- the pressure compensation device 12, in particular the Tesla valve and the nozzle part 110, are permanently heated, for example passively by the heat of the liquid medium or salt circuit and/or actively heated to avoid plug formation.
- the laminarization section 14 or the dosing lance is unheated and is passively cooled from one side by the freezing part 35 in the neutral position (when the freezing part 35 is located underneath), so that a closure plug is formed in the laminarization section or the dosing lance, which prevents the medium flow from the freezing part 35 or the discharge section of the line arrangement 4 if no medium sample is taken.
- the heating device of the linear table in the area of the free jet piece 33 (zone 1), the sampling part 32 (zone 2) and the closure part 34 (zone 3) is switched on and heated to approx. 300 °C, for example.
- the adjustment part of the linear table moves from zone 3 (closure part) to the position of zone 1 (free jet piece) and liquid medium flows into the waste receptacle 15 or the waste container.
- the linear table After rinsing the sampling device, which can be determined, for example, based on the increase in weight of the waste receptacle or the waste container, the linear table is placed in the position of zone 2 (sample removal part). The sample holder or a sample container is filled with a relevant amount of liquid medium or salt. After filling the sample holder, the linear table is set to the position of the freezing part (zone 4). At the same time as the adjustment, the heating of the laminarization section 14 or the dosing lance is switched off by the heating device or trace heating. A sealing plug forms in the laminarization section 14.
- the sampling device 1 can be used in any fluid system that works with liquid, corrosive media, in particular in Temperatures above 100 °C, preferably above 150 °C. Samples can be taken automatically for later analysis during operation, without the need to change operating parameters, as may be necessary for a person taking the sample in order not to endanger them. Samples are or can be taken automatically, with appropriate control using control technology. Samples can be taken at predefined times, e.g. at constant intervals, or depending on events, including at weekends or at night. Samples are taken in a reproducible manner and always in the same way. Due to the intrinsic pressure control, samples can also be taken from pressurized areas without endangering people.
- the sampling device can be easily adapted to the system or system part 2 (such as a pressurized pipe, container, valve or the like). Pressure fluctuations in system parts are compensated by the sampling device with simple components, whereby a corresponding pressure reduction or pressure difference regulation also takes place when sampling between the internal system pressure and the sample chamber.
- system or system part 2 such as a pressurized pipe, container, valve or the like.
- the sample is taken from a representative, relevant medium-carrying area of the system, so that sampling from dead space volumes or non-representative edge areas is avoided.
- the sample is advantageously taken from a continuously flowing free jet, for example, and in particular after flushing the sampling device with system fluid, whereby the medium flow or salt flow can be interrupted in a controlled manner.
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102023104568.7A DE102023104568A1 (de) | 2023-02-24 | 2023-02-24 | Probenentnahmevorrichtung zur Entnahme einer Probe aus einem ein flüssiges Medium führenden Anlagenteil sowie Verfahren zur Entnahme einer solchen Probe |
| PCT/EP2024/054315 WO2024175607A1 (de) | 2023-02-24 | 2024-02-20 | Probenentnahmevorrichtung zur entnahme einer probe aus einem ein flüssiges medium führenden anlagenteil sowie verfahren zur entnahme einer solchen probe |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP4669949A1 true EP4669949A1 (de) | 2025-12-31 |
Family
ID=90014310
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP24706731.7A Pending EP4669949A1 (de) | 2023-02-24 | 2024-02-20 | Probenentnahmevorrichtung zur entnahme einer probe aus einem ein flüssiges medium führenden anlagenteil sowie verfahren zur entnahme einer solchen probe |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US20260219139A1 (de) |
| EP (1) | EP4669949A1 (de) |
| CN (1) | CN120202399A (de) |
| DE (1) | DE102023104568A1 (de) |
| WO (1) | WO2024175607A1 (de) |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE757692A (fr) | 1969-11-07 | 1971-04-01 | Siemens Ag | Dispositif combine pour la prise d'echantillons et la distillation sousvide |
| DE2443559C2 (de) * | 1974-09-11 | 1984-01-12 | Interatom Internationale Atomreaktorbau Gmbh, 5060 Bergisch Gladbach | Vorrichtung zur Entnahme von Proben aus einem Flüssigmetall führenden Kreislauf |
| FR2740222B1 (fr) | 1995-10-23 | 1997-11-14 | Bio Merieux | Ensemble de traitement d'un echantillon en milieu liquide, notamment d'un materiel biologique |
| DE102004039378A1 (de) * | 2004-08-13 | 2006-02-23 | Hte Ag The High Throughput Experimentation Company | Vorrichtung zur kontrollierten Entnahme von Fluidproben aus Druckbehältern |
| DE102010031097A1 (de) | 2010-07-08 | 2012-01-12 | Voith Patent Gmbh | Probenentnahme |
| CN113405852A (zh) * | 2021-07-21 | 2021-09-17 | 西安热工研究院有限公司 | 一种高温高压流体自动减压限流取样装置及方法 |
-
2023
- 2023-02-24 DE DE102023104568.7A patent/DE102023104568A1/de active Pending
-
2024
- 2024-02-20 US US19/148,694 patent/US20260219139A1/en active Pending
- 2024-02-20 EP EP24706731.7A patent/EP4669949A1/de active Pending
- 2024-02-20 WO PCT/EP2024/054315 patent/WO2024175607A1/de not_active Ceased
- 2024-02-20 CN CN202480004759.9A patent/CN120202399A/zh active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| DE102023104568A1 (de) | 2024-08-29 |
| CN120202399A (zh) | 2025-06-24 |
| US20260219139A1 (en) | 2026-07-30 |
| WO2024175607A1 (de) | 2024-08-29 |
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