EP4004537A1 - Système pour la production d'une solution d'étalonnage - Google Patents

Système pour la production d'une solution d'étalonnage

Info

Publication number
EP4004537A1
EP4004537A1 EP20771460.1A EP20771460A EP4004537A1 EP 4004537 A1 EP4004537 A1 EP 4004537A1 EP 20771460 A EP20771460 A EP 20771460A EP 4004537 A1 EP4004537 A1 EP 4004537A1
Authority
EP
European Patent Office
Prior art keywords
liquid component
receiving device
gaseous components
metering valves
feeding
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
Application number
EP20771460.1A
Other languages
German (de)
English (en)
Inventor
Ivanka ATANASOVA-HÖHLEIN
Carolin Schütt
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Siemens Energy Global GmbH and Co KG
Original Assignee
Siemens Energy Global GmbH and Co KG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Siemens Energy Global GmbH and Co KG filed Critical Siemens Energy Global GmbH and Co KG
Publication of EP4004537A1 publication Critical patent/EP4004537A1/fr
Pending legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26—Oils; Viscous liquids; Paints; Inks
    • G01N33/28—Oils, i.e. hydrocarbon liquids
    • G01N33/2835—Specific substances contained in the oils or fuels
    • G01N33/2841—Gas in oils, e.g. hydrogen in insulating oils
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N2030/042—Standards

Definitions

  • the object of the present invention to at least partially remedy the above-described disadvantages of known systems and methods for producing a calibration solution.
  • the method according to the invention or the system according to the invention should be as versatile and user-friendly as possible.
  • a liquid component is preferably one Standard conditions understood at least partially fluid component, in particular an oil.
  • the liquid component can preferably be in the form of a transformer oil, in particular in the form of a mineral oil, a silicone oil or a synthetic, natural ester or the like.
  • the gaseous components can preferably be in the form of substances that are gaseous under standard conditions, in particular in the form of high-purity gases, which are advantageously present with an analytical accuracy of at least 2.0, in particular at least 3.0.
  • hydrogen, methane, ethane, ethylene, acetylene, propane, propylene, carbon monoxide, carbon dioxide, oxygen, nitrogen and / or methanol can be used as gases.
  • the receiving device can advantageously be provided according to the invention so that the receiving device is at least partially formed from an elastomer, for example a laminate reinforced elastomer, in particular at least partially from a rubber.
  • An embodiment of the receiving device in the form of an elastomer enables a pressure equalization within the receiving device in a simple manner when adding the components, so that the addition of the components does not lead to a pressure increase within the receiving device and it is therefore not necessary to add the volume to be supplied beforehand via a syringe or the like before supplying a component remove.
  • the design of the receiving device in the form of an elastomer resistant to the insulating liquid and / or laminate-reinforced elastomer in particular eliminates the complicated and health-endangering step of mercury pressure compensation provided according to the prior art.
  • the receiving device in addition to an embodiment of the receiving device in the form of rubber or natural rubber, the receiving device can also be formed in the form of silicone rubber or vulcanizates or the like. With regard to a compact arrangement and a simple introduction of supply and discharge connections, the receiving device in question can advantageously be designed in the shape of a cuboid. Alternatively, other shapes, in particular spherical, oval or rectangular shapes, are also conceivable.
  • the first feed unit comprises a feed pump and a line system for conveying the liquid component into the receiving device.
  • the delivery pump for delivering the liquid component is preferably designed in the form of a liquid pump, in particular in the form of an oil pump.
  • the line system can preferably be formed in the form of metal, in particular in the form of stainless steel lines, which can likewise advantageously be chemically resistant to the liquid component used.
  • a line system made of metal is not only more stable and more resistant to chemical substances, but also generally more sealed to the environment than conventional hose systems or similar.
  • the first feed unit has a vacuum pump and a line system for degassing the liquid component.
  • the vacuum pump and the line system serve to effectively remove gases dissolved in the liquid component, which in the context of the invention should only be supplied in precisely defined quantities during the preparation of the calibration solution, so that it makes sense for the preparation of precisely concentrated calibration solutions, in advance all within to remove dissolved gases from the liquid component.
  • collecting devices for collecting parts of the liquid component between the Vacuum pump and the storage location of the liquid component to be degassed can be provided.
  • a reservoir for storing the liquid component, the reservoir preferably being connected to the feed pump and / or the vacuum pump via the line system.
  • Such a connection makes it possible, in particular, to establish a continuous cycle of possible supply and degassing of the liquid component.
  • the access to the feed pump should advantageously be arranged at the bottom of the reservoir and the access to the vacuum pump should be arranged at the cover of the reservoir in order to ensure that the vacuum pump only removes the gaseous substances from the liquid component and the feed pump only conveys the purified liquid component.
  • the second feed unit has at least three, preferably at least five, in particular more than five metering valves for feeding the definable amount of a plurality of different gaseous components.
  • different amounts of a gaseous component can preferably be introduced via the individual metering valves.
  • the metering valves can preferably be in the form of gas metering valves.
  • the quantities to be supplied can be regulated, for example, via the volumes, in particular the line diameter and / or the line length, or also via the time of introduction.
  • the invention can also advantageously provide that the metering valves are connected to one another via a first and second fluid path, a first fluid path preferably for transferring the liquid component and the second fluid path for transferring a plurality of gaseous components is provided.
  • the intended separation of the fluid paths in particular, minimizes the cleaning effort and the number of necessary rinsing processes.
  • the metering valves have a coupling path for coupling the first and second fluid paths, the coupling path being designed in such a way that this an access between the first and second fluid paths in a closed state of FIG Metering valves closes and releases the metering valves in an open state.
  • the second fluid path can be completely protected from contamination with the liquid component by allowing access to the second fluid path via the coupling path only when a metering valve is opened, so that the gas is directed into part of the first fluid path for a definable period can be, which can then preferably be passed directly into the receiving device.
  • the opening time of the metering valve as well as the line cross-section and the length of the metering valve in question, the addition of a gas can be precisely controlled.
  • the metering valves are in the form of pneumatically and / or electrically and / or magnetically operated valves.
  • a gas supply unit for supplying a plurality of gaseous components, the gas supply unit having a plurality of supply and discharge lines , wherein the supply and discharge lines can preferably be connected to the second fluid path.
  • a control unit is provided for automatic control of the gas supply unit and the metering valves in order to automatically and finely metered addition of a plurality of different gaseous components to the liquid Ensure component.
  • a control unit can be software-controlled, for example, and thus enable a clearly more precisely determinable opening duration of the metering valves, which advantageously correlates with the type and size and the pre-pressure of the gaseous components to be introduced.
  • the individual system components can be connected to one another preferably via control lines or the like.
  • the individual components can also be connected to one another wirelessly or contactlessly via Bluetooth, WLAN, Zigbee or the like.
  • the liquid component Before a liquid component is supplied by means of a first supply unit, the liquid component can preferably be degassed by means of the first supply unit, in particular by means of a vacuum pump integrated within the first supply unit and a correspondingly arranged line system.
  • a dosage of the liquid and / or the at least one gaseous component can in particular be automated or automatic by means of a control unit or the like.
  • the invention can also provide that after the liquid component and the various gaseous components have been fed in, the calibration solution is shaken, the calibration solution preferably being shaken for one to 24 hours.
  • shaking can preferably take place in the receiving device in question, which for this purpose is preferably separated from the outside via shut-off valves and can be transferred to a suitable shaker.
  • the volume of a liquid component can preferably be determined by measuring the weight and converting the known density of the liquid component in question, so that the volume does not have to be measured and a risk of contamination is prevented.
  • a sample can also be measured to verify the quality of the standard before using a calibration solution prepared according to the method in question.
  • the subject method for producing a calibration solution takes place at constant temperature and at constant pressure, which allows the concentrations to be converted to standard conditions (20 ° C. and 101.3 kPa).
  • FIG. 1 shows a schematic representation of a system according to the invention for producing a calibration solution for calibrating a gas chromatograph according to a first exemplary embodiment
  • FIG. 2b a schematic representation of the second feed unit according to the invention according to FIG. 2a with partially open metering valves
  • FIG. 3 shows a schematic representation of a method according to the invention for producing a calibration solution for calibrating a gas chromatograph according to a first exemplary embodiment.
  • FIG. 1 shows a schematic representation of a system 2 according to the invention for producing a calibration solution 4 for calibrating a gas chromatograph, having a liquid component 6 and at least one gaseous component 8 according to a first exemplary embodiment.
  • the system 2 in question comprises a receiving device 10 for receiving the liquid component 6 and a plurality of different gaseous components 8, a first supply unit 12 for supplying a definable amount of the liquid component 6 into the receiving device 10 and a second supply unit 14 for Feeding a definable amount of a plurality of different gaseous components 8 into the receiving device 10, the second feed unit 14 having a plurality of metering valves 16 - not shown here - for feeding the definable amount of a plurality of different gaseous components 8.
  • the receiving device 10 is in the present case in the form of an elastomer, in particular made of rubber. To prevent contamination of the calibration solution 4 produced within the receiving device 10, the receiving device 10 is also formed from an air-impermeable and preferably chemically resistant material.
  • the first feed unit 12 comprises a feed pump 18 and a line system 20 for conveying the liquid component 6 into the receiving device 10.
  • the feed unit 12 also comprises a vacuum pump 18 ′ and a further line system 24 for degassing the liquid component 6.
  • a reservoir 27 is also provided, which is connected to the feed pump 18 via the line system 20 and to the vacuum pump 18 ′ via the line system 24.
  • Such an arrangement is used to degas the liquid component 6, which is in the form of an insulating oil, preferably in the form of a mineral oil, a silicone oil or a synthetic ester, in that the gases dissolved within the liquid component 6 are discharged via the vacuum pump 18 '.
  • the liquid component 6 is meanwhile discharged via the feed pump 18 and made available again to the reservoir 27 within a circuit via the line system 20. During this transfer, the liquid Component 6 of the receiving device 10 are fed via shut-off valves 17. As can be seen, a large number of further shut-off valves 17 are arranged distributed over the system 2. With regard to the most flexible handling of the receiving device 10 while at the same time ensuring the production of a calibration solution 4 that is as pure as possible, the system 2 has a multi-way connection unit 34 for connecting the receiving device 10 to the first and / or second supply unit 12, 14, which is preferably in the form a 3-way cock or the like can be formed.
  • two collecting devices 22 for collecting residues of the liquid component 6 within the line system 24 are also provided between the reservoir 27 and the vacuum pump 18'.
  • FIG. 2a shows a schematic representation of a second feed unit 14 according to the invention for feeding a definable amount of a plurality of different gaseous components 8 into the receiving device 10 with completely closed metering valves 16a-16f.
  • the present six metering valves 16a-16f arranged next to one another are connected to one another via a first and second fluid path 26, 28, the first fluid path 26 being provided for transferring the liquid component 6 and the second fluid path 28 for transferring a plurality of gaseous components 8.
  • the metering valves 16 can be in the form of pneumatically and / or electrically and / or magnetically operated valves.
  • a plurality of gaseous components 8 are added to the fluid path 28 via the gas supply unit 32 for supplying a plurality of gaseous components 8 added, which in the present case has a plurality of supply and discharge lines, via which various gases can be supplied to the fluid path 28.
  • the fluid path 26 leads to the transfer of the liquid component 6 via the feed pump 18 and the receiving device 10, so that a volume of the liquid component 6 arranged within the receiving device 10 is constantly within or along the Fluid path 26 can be circulated.
  • FIG. 2b shows a schematic representation of a second feed unit 14 according to the invention according to FIG. 2a with partially open metering valves 16.
  • the valve 16e is open.
  • the valves 16a-16f have a coupling path 30 for coupling the first and second fluid paths 26, 28, which is designed in such a way that they provide access between the first and second fluid paths 26, 28 in a closed manner Closed state of the dosing valves 16 and released in the open state of the dosing valve 16e shown here, so that the gaseous component 8 introduced via the gas supply unit 32 can be introduced into the second fluid path 28 via the coupling path 30 of the dosing valve 16e and thus a new, third fluid path 29 for Transfer of a liquid component 6 mixed with a gaseous component 8 arises, via which the components 6, 8 are fed to the receiving device 10 and form the finished calibration solution 4.
  • the method according to the invention initially comprises a step of degassing 40 the liquid component 6 by means of a vacuum pump 18 ′ integrated within the first feed unit 12 and a correspondingly arranged line system 24, before a subsequent second step feed 42 a defined amount of the liquid component 6 in the receiving device 10 by means of the first supply unit 12 and, in the third step, supplying 44 of a defined amount of the plurality of different gaseous components 8 into the receiving device 10 by means of a second supply unit 14, the various gaseous components 8 being the
  • Receiving device 10 according to the method according to the invention can be fed in a defined quantity by means of the second feed unit 14 via a plurality of metering valves 16.
  • the method in question takes place at constant temperature and at constant pressure, so that the concentrations can be converted to standard conditions (20 ° C. and 101.3 kPa).

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Pathology (AREA)
  • Immunology (AREA)
  • General Physics & Mathematics (AREA)
  • General Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Medicinal Chemistry (AREA)
  • Food Science & Technology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

L'invention concerne un système (2) pour la production d'une solution d'étalonnage (4) pour l'étalonnage d'un chromatographe en phase gazeuse, comprenant un constituant liquide (6) et au moins un constituant gazeux (8), comprenant un dispositif de réception (10) destiné à recevoir le constituant liquide (6) et une pluralité de différents constituants gazeux (8), une première unité d'alimentation (12) permettant d'alimenter le dispositif de réception (10) en une quantité définissable du constituant liquide (6), une seconde unité d'alimentation (14) permettant d'alimenter le dispositif de réception (10) en une quantité définissable d'une pluralité de différents constituants gazeux (8), la seconde unité d'alimentation (14) comprenant une pluralité de valves doseuses (16) pour l'alimentation de la quantité définissable d'une pluralité de différents constituants gazeux (8).
EP20771460.1A 2019-09-11 2020-08-31 Système pour la production d'une solution d'étalonnage Pending EP4004537A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102019213820.9A DE102019213820A1 (de) 2019-09-11 2019-09-11 System zur Herstellung einer Kalibrierlösung
PCT/EP2020/074200 WO2021047931A1 (fr) 2019-09-11 2020-08-31 Système pour la production d'une solution d'étalonnage

Publications (1)

Publication Number Publication Date
EP4004537A1 true EP4004537A1 (fr) 2022-06-01

Family

ID=72473506

Family Applications (1)

Application Number Title Priority Date Filing Date
EP20771460.1A Pending EP4004537A1 (fr) 2019-09-11 2020-08-31 Système pour la production d'une solution d'étalonnage

Country Status (3)

Country Link
EP (1) EP4004537A1 (fr)
DE (1) DE102019213820A1 (fr)
WO (1) WO2021047931A1 (fr)

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE29802891U1 (de) * 1998-02-19 1998-04-09 Raak Juergen Mischmodul zum kontinuierlichen Mischen und Dosieren
US7950296B2 (en) * 2007-06-01 2011-05-31 Siemens Industry, Inc. Continuous flow sample introduction apparatus and method
US8438969B2 (en) * 2010-05-06 2013-05-14 Dr Pepper/Seven Up, Inc. Apparatus and method for dissolving gases in a beverage
US9239322B2 (en) * 2011-01-23 2016-01-19 Serveron Corporation Electrical apparatus oil sampler and conditioner for solid state sensors
CN204065038U (zh) * 2014-06-30 2014-12-31 杭州申昊科技股份有限公司 一种标准油样配制装置
CN106872613B (zh) * 2015-12-14 2020-03-13 中国电力科学研究院 一种变压器标准油样配制装置及其操作方法

Also Published As

Publication number Publication date
WO2021047931A1 (fr) 2021-03-18
DE102019213820A1 (de) 2021-03-11

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