• 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 comprises a method and plant for monitoring and optionally validating a clean-in-place (CIP) washing process by conducting measurements on a stream of rinsing water. In particular, the invention comprises a deaeration step in which rinsing water collected upon rinse of a container is deaerated prior to measurement, thus avoiding e.g. signal noise problems caused by the presence of air bubbles and ensuring measurement reproducibility.
    公开号:DK201870235A1
    申请号:DKP201870235
    申请日:2018-04-19
    公开日:2019-12-09
    发明作者:Egede Petersen Michael
    申请人:Purgatio A/S；
    IPC主号:
    专利说明:

    A method for measuring an entity of interest in a stream of rinsing water
    TECHNICAL FIELD
    The disclosure relates to a method and plant for measuring an entity of interest in a liquid stream, particularly an entity of interest in a stream of rinsing water, primarily in the context of clean-in-place (CIP) cleaning of containers used
    e.g. in pharmaceutical, food, beverage, or similar industries .
    BACKGROUND
    Various clean-in-place (CIP) processes for cleaning containers in pharmaceutical, food, beverage, or other industries are known from the prior art.
    US20060042665A1 discloses a method of cleaning equipment using CIP procedures and a pre-treatment solution prior to the conventional CIP cleaning process. The pre-treatment step improves the degree of softening of the soil, and thus facilitates its removal.
    US2006064954 and WO2016088725A1 disclose gas-liquid separation devices for deaerating the washing water used in a CIP system. In both disclosures, gas-liquid separation is performed by centrifugal force of an impeller on a shaft which rotates in a casing.
    DK 2018 70235 A1
    The above disclosures provide methods for CIP cleaning and deaerating washing water. However, none of the disclosures include a sensor system for monitoring the internal cleaning process .
    Sensor systems for monitoring internal cleaning of e.g. a container by conducting measurements on the cleaning liquid are known from other prior art.
    For example, US20170282225A1 discloses an invention, wherein during the cleaning process cleaning liquid is sprayed onto the inner wall of the tank container. The uniform distribution of the cleaning liquid and its degree of contamination are monitored by calorimetric flow measurement. For this purpose, a heating element is disposed in the flow-off area of the cleaning liquid.
    US7682460 provides a method for cleaning chemical process and hydrocarbon processing apparatuses, wherein cleaning is performed by establishing a closed flow circulation loop, under specific operating conditions and in the presence of hydrocarbon-based fluids. The cleaning method is monitored by performing analyses such as e.g. viscosity and density analysis on the circulating hydrocarbon-based fluid.
    EP1882914A2 discloses a method that involves arranging a measuring point, which represents a measuring position, at a wall surface of a tank, a container, or a pipe. A temporally stepwise or continuous varying signal (S(t)) for presence of a medium or media composite characteristics is received and
    DK 2018 70235 A1 evaluated at the measuring point. Molecules of the medium arrived into a region of the measuring point are detected by a sensor. Temporal variation of the signal (dS/dt) or rate of change of temporal variation (dS/dt2) of alternating electrical field is detected as a characteristic signal for evaluating the signal.
    None of the publications US20170282225A1, US7682460, and EP1882914A2 comprise a deaeration or more generally a degassing step for deaerating/degassing the rinsing liquid prior to measurement.
    It is an object of the present invention to provide a method and plant that allows for precise and reproducible measurement of an entity of interest in a stream of rinsing water in a CIP cleaning system. The entity of interest could be e.g. the concentration of a compound or contaminant. The method and plant can be used e.g. for monitoring a cleaning process and for validation of washing effectiveness of same cleaning process. Validation of washing effectiveness is of particular interest e.g. when cleaning containers, tanks, pipes, or other equipment that must meet cleanliness requirements, as is often the case in e.g. pharmaceutical, food, beverage, or similar industries. Said object of the invention is achieved by the features of the independent claims. Further implementation forms are apparent from the dependent claims, the summary, the description, and the figures.
    DK 2018 70235 A1
    SUMMARY
    According to a first aspect, the invention comprises a method for measuring an entity of interest in a stream of rinsing water,
    a. supplying a stream of water to a unit previously subjected to a washing process for rinsing at least a part of the surfaces of the washed unit,
    b. supplying a stream of air to the washed unit,
    c. collecting a mixture of water and air at an outlet of the unit,
    d. deaerating the mixture of water and air to produce an aqueous stream, and
    e. measuring the concentration of an entity of interest in the aqueous stream.
    The inventor of the present invention has realized that air bubbles in the rinsing water may cause problems by influencing measurements, rendering measurement imprecise and unreproducible. Step d of the present invention removes air bubbles that might otherwise influence measurement of the aqueous stream in step e.
    To obtain a uniform cleaning of the unit, a stream of air is supplied concurrently with the stream of water during rinse. The stream of air is used to prepare a pressure above the atmospheric pressure to propel emptying of the unit and to avoid build-up of a standing water phase inside the washed unit, also referred to as the CIP client, during rinse.
    DK 2018 70235 A1
    The method according to the invention may find use in various applications, incl. cleaning of e.g. bottles for beverages, reaction chambers for chemicals, containers for wastewater, etc .
    In a possible implementation form of the first aspect, the method further comprises the steps of
    f. comparing the measured concentration of the entity of interest with a predetermined concentration and
    g. determining that the washing process is validated if the measured concentration is at or below the predetermined concentration.
    The effect of steps f and g is to assess and validate the effectiveness of the washing process.
    The measurement of the entity of interest may be performed as a single occurrence, or the measurement may be repeated as required by the circumstances. In a possible implementation of the invention, the steps a to f are repeated if the measured concentration is above a predetermined concentration.
    The effect hereof is to control the washing process and to ensure that the wash is thorough and that the washed unit meets specified requirements if necessary.
    The deaeration may be performed batchwise or continuously as required by the circumstances. When performed batchwise, the deaeration is preferably performed immediately prior to the measuring of the entity of interest to avoid air bubbles in the measured sample. In a possible implementation form of the invention, the mixture of water and air is continuously
    DK 2018 70235 A1 deaerated to allow for continuous or discrete measuring of the entity of interest.
    The effect hereof is to continuously remove air bubbles that might otherwise influence a later measuring step and, thus, to generate a deaerated stream of rinsing water that can be subjected to measurement.
    While it may be useful in certain embodiments of the invention to perform discrete measurements, it may often be preferred that the concentration of the entity of interest is measured continuously. The effect hereof is to obtain continuous measurement data on the deaerated rinsing water, allowing for immediate intervention when the concentration of the entity of interest is at, below and/or above a predetermined concentration. Such continuous monitoring may be advantageous e.g. in pharmaceutical production to ensure e.g. patient security.
    When discrete measurements are performed, analysis may take a certain amount of time before the result is available. Hence, this type of measurement will result in a certain lag in response time. It may therefore often be preferred that the measuring of the concentration of an entity of interest in the aqueous stream is performed continuously as an in-line or on-line process.
    The entity of interest may be selected among a plurality of possibilities. In a certain implementation form of the invention, the entity of interest is one or more of Total Organic Carbon (TOC), O2, CO2, pH, bioburden, or conductivity.
    DK 2018 70235 A1
    The effect hereof is to determine composition, contamination, chemical properties, and/or physical properties of the deaerated rinsing water, thereby assessing the state of the washed unit and monitoring the washing process.
    According to a second aspect, the invention comprises a plant for measuring an entity of interest in a stream of rinsing water, comprising a unit previously subjected to a washing process, an inlet for supply of a stream of water for rinsing at least a part of the surfaces of the washed unit, an inlet for supplying a stream of air to the washed unit, an outlet of the unit capable of collecting a mixture of water and air, a deaerator for producing an aqueous stream of the mixture of water and air, and a sensor for measuring the concentration of an entity of interest in the aqueous stream.
    The plant allows for the implementation of possible embodiments of the method according to the invention, in which a previously washed unit can be rinsed without build-up of any standing water phase inside the unit during rinse and in which the rinsing water is deaerated prior to measurement, thus removing air bubbles that might otherwise influence measurement. Inlets may e.g. be in the form of jets, nozzles, sprinklers, spray heads, etc.
    In order to infer and assess the effectiveness of the washing process and thereby the state of cleanliness of the container, measurements are compared to predetermined and/or predefined standards, e.g. predetermined concentrations. While the comparison may be carried out or supervised by a human, having
    DK 2018 70235 A1 a computer software to perform the task in an automated process may often be preferred.
    In a possible implementation form of the second aspect, the plant comprises a computer software program capable of comparing the measured concentration of the entity of interest with a predetermined concentration of the entity of interest and determining that the washing process is validated if the measured concentration is at or below the predetermined concentration .
    The effect hereof is that the washing effectiveness and the cleanliness control and validation are performed in the most efficient manner, thus saving time and manpower.
    Compounds requiring marketing approval by an authority such as e.g. a food or drug authority need to fulfill certain requirements with regards to e.g. reproducibility of the preparation process. Meeting such requirements requires a reproducible cleaning process for cleaning of equipment used e.g. in handling, preparation, storage, processing, etc. of the compounds. The plant according to the invention is capable of accommodating the requirements of any authority, notably an authority for granting marketing approval for pharmaceutical products.
    The washed unit may be e.g. a holder, vessel, repository, receptacle, tank, pipe, tube, barrel, etc. In a possible implementation form of the second aspect, the washed unit is a container previously used for accommodating a compound requiring marketing approval by an authority.
    DK 2018 70235 A1
    The effect hereof is that the present invention can be used to wash and validate the washing of a container used e.g. in handling, preparation, storage, processing, etc. of a compound requiring marketing approval by an authority.
    The rinsing water is collected, preferably continuously, at the outlet of the unit and without build-up of any standing water phase in the unit. Furthermore, the rinsing water is supplied, preferably continuously, to the deaerator for deaeration prior to measurement. While the rinsing water may flow naturally from the unit to the deaerator, flow or transport of the rinsing water may also be achieved e.g. by overpressure in the unit and/or by using a pumping system.
    In a possible implementation form of the second aspect, a pump is used for transporting the collected mixture of water and air from the outlet of the unit to the deaerator. The effect hereof is to supply a sufficient amount of the rinsing water to the deaerator to avoiding the build-up of a standing water phase.
    In a possible implementation form of the second aspect, the pump is a side channels pump or water ring pump. The effect hereof is to ensure the most effective transport of the mixture of the rinsing water and the air bubbles.
    Deaeration of the rinsing water prior to measurement may be achieved by various means and apparatuses, incl. e.g. by sonication and stirring under reduced pressure (vacuum degasification), gas-liquid separation membranes, thermal
    DK 2018 70235 A1 regulation, etc. In a possible implementation form of the second aspect, the deaerator is a cyclone. The effect hereof is to efficiently produce a deaerated aqueous stream that can be subjected to measurement, using an in-line unit operation.
    For measurement of the entity of interest in the aqueous stream, a range of different measuring systems, sensors, and/or combinations thereof may be used. In a possible implementation form of the second aspect, the sensor is one or more of pH electrode, TOC sensor, bioburden sensor, oxygen sensor, CO2 sensor, or conductivity sensor. The effect hereof is to ensure proper measurement of the entity of interest.
    The method and plant of the present invention may find use in various applications and contexts in which measurement of an entity of interest in a liquid stream, particularly in an aqueous stream, is desired. In a possible implementation form of the first aspect and its implementation forms or the second aspect and its implementation forms, the invention comprises validating a washing process of a unit previously used for accommodating a compound requiring marketing approval by an authority.
    The effect hereof is to provide a method and plant that can be used e.g. in the handling, preparation, storage, processing, etc. of a compound requiring marketing approval by an authority.
    These and other aspects will be apparent from and the embodiment(s) described below.
    DK 2018 70235 A1
    BRIEF DESCRIPTION OF THE DRAWINGS
    In the following detailed portion of the present disclosure, the aspects, embodiments, and implementations will be explained in more detail with reference to the example embodiments shown in the drawings, in which:
    Fig. 1 is a simplified scheme of a possible embodiment of the present invention, showing a clean-in-place (CIP) plant with an integrated deaerator for deaerating rinsing water and with an integrated sensor for performing measurements on the deaerated rinsing water.
    Fig. 2 is a plot with measurement results obtained in a possible embodiment of the present invention. The plot shows measured total organic carbon (TOC) data vs. time, as collected online and continuously in a stream of deaerated rinsing water in a CIP plant with an integrated hydrocyclone for deaerating the rinsing water and with an integrated sensor .
    DETAILED DESCRIPTION
    Fig. 1 shows a simplified scheme of a possible embodiment of the plant of the present invention. The plant comprises a container 1 to be washed.
    The container 1 may e.g. be of a kind used in pharmaceutical, food, beverage, or similar industries. The container 1 may be, but does not have to be, made of stainless steel.
    DK 2018 70235 A1
    Prior to washing, the container 1 may have been used for containing a liquid, e.g. water, with e.g. a product, compound, mixture of compounds, or an active ingredient dissolved or otherwise contained therein. Possible products could be e.g. pharmaceutical products such as e.g. insulin, protein, polypeptide, or a drug, dairy products such as e.g. cheese, whey, milk, or sour milk, or food or beverage products .
    The container 1 is a sealed container. In the embodiment of Fig. 1, the container 1 has an inlet 2 for water and an inlet 3 for air. The inlets 2 & 3 are used for supplying water and air during rinse. In an alternative embodiment, water and air may be supplied through one and the same inlet. An additional inlet 4 for supplying cleaning fluids during wash is also shown in Fig. 1. Further additional inlets may be present in alternative embodiments of the invention.
    A possible washing procedure for washing the inner of the container could comprise the steps 1) pre-rinse to drain, 2) base wash with recirculation using e.g. 2-5 % sodium hydroxide (NaOH) at elevated temperature (e.g. 80 °C), 3) inter-rinse to drain, 4) acid wash with e.g. cold nitric acid (HNOs) for neutralizing the NaOH of the base wash (note that due to its oxidizing nature, nitric acid promotes the resistance of stainless steel to corrosion), 5) inter-rinse to drain, and ) final rinse .
    During rinse, inner surfaces of the container 1 are rinsed with water and air. The water and air streams are supplied concurrently. Possibly, the air is in the form of compressed
    DK 2018 70235 A1 air. The air stream functions to ensure a uniform rinse and prevents build-up of a standing water phase inside the container. The ratio between water and air is such that the air helps propelling the water out of the container 1. This is accomplished when using roughly an amount of air that is two-to-three times the amount of water. The mixture of water and air, also referred to as the rinsing water, exits the container 1 through an outlet 5.
    After exiting the container 1, the rinsing water enters into a connected hydrocyclone 7 via a pump 6. The function of the pump 6 is to assist or enable transport of the collected rinsing water from the outlet 5 to the hydrocyclone 7. The pump 6 should be suited for container emptying and CIP return applications where air and gas is entrained in the pumped liquid. The pump 6 can be of type side channel pump or water ring pump. Examples of applicable pumps are CSA series pumps (closed coupled sanitary centrifugal pumps with open impeller and independent shaft support) and ASH series pumps (close coupled sanitary self-priming pumps with independent shaft support), as produced by CSF Inox S.p.A., or the Alfa Laval LKH Prime UltraPure pump. In case the container 1 is e.g. a pressurized container with sufficiently high gauge pressure (e.g. of 0.5-0.2 bar), no pump may be needed to transport the rinsing water from the container 1 to the hydrocyclone 7. In a pressureless container, e.g. in a container that is open to the surroundings, a pump will generally be needed in order to pump out the mixture of water and air from the container.
    In the hydrocyclone 7, the rinsing water is separated into a predominantly gas phase (air) and a predominantly aqueous
    DK 2018 70235 A1 phase (water), the latter also referred to as aqueous stream. That is, the hydrocyclone 7 functions to continuously deaerate the rinsing water collected from the container 1, thereby producing a deaerated aqueous stream that can be readily subjected to online measurement and analysis by a sensor without signal noise or other disturbances caused by the presence of air bubbles. In principle, any hydrocyclone capable of such water/gas separation can be used. The separated air exits through an outlet 8, typically in the form of a vent, at the top of the hydrocyclone while the separated aqueous stream exits through an outlet 9 at the bottom of the hydrocyclone.
    The outlet at the bottom of the hydrocyclone 7 is connected to a sensor 10 to which the aqueous stream is exposed for measuring a specified property, e.g. conductivity, Total Organic Carbon (TOC), pH, and/or bioburden. Measurements on the aqueous stream are carried out online and/or inline and continuously by the sensor 10 in e.g. a flow cell. An example of an applicable sensor could be the Thornton 5000TCC1 sensor with M800 multi-parameter transmitter that uses ultraviolet (UV) oxidation with differential conductivity to determine TOC concentrations .
    The sensor 10 is connected to a controlling software 11 that monitors the measurement. The software 11 is capable of comparing measured values with predetermined or pre-defined values, determining if a measured value, e.g. a measured concentration value, is below, at, or above the predetermined value, thereby accessing e.g. the degree of cleanliness of the container 1 and, ultimately, validating the overall
    DK 2018 70235 A1 washing process if the measured value is at or below the predetermined value. After measurement, the aqueous stream may be recirculated back into the container 1, optionally after being supplemented with fresh water, or it may be discarded to drain.
    Fig. 2 shows a plot with measurement results obtained in a possible embodiment of the present invention. Total organic carbon (TOC) was measured vs. time online and continuously in a stream of deaerated rinsing water in a CIP plant with an integrated hydrocyclone for deaerating the rinsing water prior to measurement and with an integrated sensor. In the embodiment used in Fig. 2, measurement was performed on a minor partial stream of rinsing water diverted from the main stream of rinsing water. The minor partial stream of rinsing water was sent directly to drain after measurement.
    At time ca. 13:41:00, common table sugar (sucrose) corresponding to an amount of 20 sugar granules was added to the container of the plant, resulting in a rapid increase in the total organic carbon content from 14 ppb to 98 ppb. Following recirculation with 400 L of clean water, the organic carbon content dropped to 23 ppb. That is, the 20 granules of table sugar raised the TOC concentration from 14 ppb to 23 ppb .
    Deaeration of the rinsing water prior to measurement removed air bubbles from the rinsing water, allowing for the measurements shown in Fig. 2.
    DK 2018 70235 A1
    The various aspects and implementations have been described in conjunction with various embodiments herein. However, other variations to the disclosed embodiments can be understood and effected by those skilled in the art in practicing the claimed subject-matter, from a study of the drawings, the disclosure, and the appended claims. In the claims, the word comprising does not exclude other elements or steps, and the indefinite article a or an does not exclude a plurality. A single processor or other unit may fulfill the functions of several items recited in the claims.
    The mere fact that certain measures are recited in mutually different dependent claims does not indicate that a combination of these measured cannot be used to advantage. A computer program may be stored/distributed on a suitable medium, such as an optical storage medium or a solid-state medium supplied together with or as part of other hardware, but may also be distributed in other forms, such as via the Internet or other wired or wireless telecommunication systems.
    The reference signs used in the claims shall not be construed as limiting the scope.
    权利要求:
    Claims (15)
    [1] 1. A method for measuring an entity of interest in a stream of rinsing water,
    a. supplying a stream of water to a unit previously subjected to a washing process for rinsing at least a part of the surfaces of the washed unit,
    b. supplying a stream of air to the washed unit,
    c. collecting a mixture of water and air at an outlet of the unit,
    d. deaerating the mixture of water and air to produce an aqueous stream, and
    e. measuring the concentration of an entity of interest in the aqueous stream.
    [2] 2. The method according to claim 1, further comprising the steps of
    f. comparing the measured concentration of the entity of interest with a predetermined concentration and
    g. determining that the washing process is validated if the measured concentration is at or below the predetermined concentration.
    [3] 3. The method according to claims 1 or 2, wherein the steps a to f are repeated if the measured concentration is above the predetermined concentration.
    [4] 4. The method according to anyone of the claims 1 to 3, wherein the mixture of water and air is continuously deaerated.
    DK 2018 70235 A1
    [5] 5. The method according to anyone of the claims 1 to wherein the concentration of the entity of interest measured continuously.
    [6] 6. The method according to anyone of the claims 1 to 5, wherein the measuring of the concentration of an entity of interest in the aqueous stream is performed continuously as an in-line or on-line process.
    [7] 7. The method according to anyone of the claims 1 to 6, wherein the entity of interest is one or more of Total Organic
    Carbon (TOC), O2, CO2, pH, bioburden, or conductivity.
    [8] 8. A plant for measuring an entity of interest in a stream of rinsing water, comprising a unit previously subjected to a washing process,
    an inlet for supply of a stream of water for rinsing at least a part of the surfaces of the washed unit, an inlet for supplying a stream of air to the washed
    unit,
    an outlet of the unit capable of collecting a mixture of
    water and air, a deaerator for producing an aqueous stream of the mixture of water and air, and a sensor for measuring the concentration of an entity of interest in the aqueous stream.
    [9] 9. The plant according to claim 8, wherein the plant further comprises a computer software program capable of comparing the measured concentration of the entity of interest with a predetermined concentration of the entity of interest and
    DK 2018 70235 A1 determining that the washing process is validated if the measured concentration is at or below the predetermined concentration.
    [10] 10. The plant according to anyone of the claims 8 or 9, wherein, the washed unit is a container previously used for accommodating a compound requiring marketing approval by an authority.
    [11] 11. The plant according to anyone of the claims 8 to 10, wherein a pump is used for transporting the collected mixture of water and air from the outlet of the unit to the deaerator.
    [12] 12.
    The plant according to anyone of the claims 8 to 11, wherein the pump is a side channels pump or water ring pump.
    [13] 13. The plant according to anyone of the claims 8 to 12 wherein the deaerator is a cyclone.
    [14] 14. The plant according to anyone of the claims 8 to 13 wherein the sensor is one or more of pH electrode, TOC sensor bioburden sensor, oxygen sensor, CO2 sensor, or conductivity sensor.
    [15] 15. Use of the method according to claims 1 to 7 or the plant according to claims 8 to 14 for validating a washing process of a unit previously used for accommodating a compound requiring marketing approval by an authority.
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    同族专利:
    公开号 | 公开日
    EP3557235A2|2019-10-23|
    EP3557235A3|2019-11-06|
    DK180097B1|2020-04-30|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    DE19741242C1|1997-09-18|1999-07-08|Diversey Lever Gmbh|Plant for cleaning a bottling plant|
    JP2000334402A|1999-05-31|2000-12-05|Clenvy Corp|Vacuum vapor cleaning device|
    ITME20020007A1|2002-06-10|2003-12-10|Marcello Ferrara|METHOD, PLANT, CHEMICAL PRODUCTS AND MONITORING SYSTEM FOR THE CLEANING OF PETROLEUM EQUIPMENT AND THEIR CLEANING BY GAS FREE.|
    US6767408B2|2002-12-18|2004-07-27|Hydrite Chemical Co.|Monitoring device and method for operating clean-in-place system|
    US8114222B2|2004-08-27|2012-02-14|Ecolab Usa Inc.|Method for cleaning industrial equipment with pre-treatment|
    CN1895719B|2005-06-21|2012-06-27|株式会社海上|Degassing apparatus and ultrasonic wave washing apparatus using the same|
    EP1882914B1|2006-07-25|2018-06-06|Sontec Sensorbau GmbH|Method and assembly for determining the presence or status of a medium or a mixture|
    DE102008056522A1|2008-11-08|2010-05-12|Hammann Wasser-Kommunal Ingenieurgesellschaft für kommunale Dienstleistungen mbH|Stationary device for cleaning pipes in building e.g. public building such as sports hall, has regulating valves provided in each individual line strand for optionally supplying pressure or discharging water to pipe|
    CN103245765B|2013-04-24|2015-12-30|北京南风科创应用技术有限公司|A kind of Oceanic parameter measurement system|
    DE102016205573B3|2016-04-05|2017-02-16|Ifm Electronic Gmbh|Method for carrying out a cleaning process in a tank container|
    法律状态:
    2019-12-09| PAT| Application published|Effective date: 20191020 |
    2020-04-30| PME| Patent granted|Effective date: 20200430 |
    优先权:
    申请号 | 申请日 | 专利标题
    DKPA201870235A|DK180097B1|2018-04-19|2018-04-19|A method for measuring an entity of interest in a stream of rinsing water|DKPA201870235A| DK180097B1|2018-04-19|2018-04-19|A method for measuring an entity of interest in a stream of rinsing water|
    EP19169166.6A| EP3557235A3|2018-04-19|2019-04-15|A method for measuring an entity of interest in a stream of rinsing water|
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