EP4630796A1 - Verfahren zum kontinuierlichen bestimmen des lactose-, protein- und fettgehaltes von milch - Google Patents
Verfahren zum kontinuierlichen bestimmen des lactose-, protein- und fettgehaltes von milchInfo
- Publication number
- EP4630796A1 EP4630796A1 EP23813297.1A EP23813297A EP4630796A1 EP 4630796 A1 EP4630796 A1 EP 4630796A1 EP 23813297 A EP23813297 A EP 23813297A EP 4630796 A1 EP4630796 A1 EP 4630796A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- content
- lactose
- fat
- protein
- medium
- 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.)
- Withdrawn
Links
Classifications
-
- 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
- G01N33/02—Food
- G01N33/04—Dairy products
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N22/00—Investigating or analysing materials by the use of microwaves or radio waves, i.e. electromagnetic waves with a wavelength of one millimetre or more
Definitions
- the invention relates to a method for, in particular continuously, determining a lactose content a, protein content b and fat content c of a flowable medium, in particular milk, a milk substitute and/or a milk product, and a measuring arrangement for determining a lactose content a, protein content b and fat content c of a flowable medium, in particular milk, a milk substitute and/or a milk product.
- Microwaves can be used to determine the physical quantities of permittivity and loss factor of a medium in a process line. From these two quantities - measured either at one or across many different frequencies - conclusions can be drawn about application-specific parameters, for example the proportion of water in a mixture of water and other non-polar or slightly polar components or a solid content in a liquid medium.
- the established transmission-Z-reflection measurement is described in L.F. Chen, C.K. Ong, C.P. Neo, V.V. Varadan, V. K. Varadan - “Microwave Electronics, Measurement and Materials Characterization”, John Wiley & Sons Ltd., 2004.
- the microwave signal is coupled to the medium in a container or measuring tube at two different positions, the scattering parameters (transmission and, if applicable, reflection) between these coupling structures are measured and the measured scattering parameters are used to calculate the physical properties of the medium.
- WO 2018/121927 A1 teaches a measuring arrangement for analyzing properties of a flowing medium using microwaves.
- the measuring arrangement has an electrically insulating lining layer on the inner surface of the measuring tube. This lining layer forms a dielectric waveguide via which a microwave signal can at least partially pass from a first microwave antenna to a second microwave antenna.
- One application for such a measuring arrangement is the determination of solid fractions in the liquid medium to be conveyed.
- WO 2021/099152 A1 teaches a microwave antenna which has a front section in contact with the medium via which the excitation signal is emitted into the medium.
- Milk and (intermediate) products derived from it can be described as a mixture of different components consisting mainly of water, milk fat and other solids, with the other solids essentially comprising proteins, carbohydrates (including in particular lactose) and small amounts of minerals.
- the proportions of these components are important parameters for controlling and regulating the processes that Process and quality control, and the balancing of product flows. It is usual to determine the proportions using laboratory samples according to standard procedures. This means that only a few samples can be evaluated and that an analysis result is only available with a significant delay after sampling. A process-related spectroscopic analysis in the infrared range with automated sampling is possible, but firstly this is very costly and secondly only based on the small volume of samples taken at comparatively long time intervals. Such an analysis is therefore only partially suitable for process control.
- DE102017131269A1 discloses a method for continuously determining the fat content of milk with varying solids content using a Coriolis flow meter and a microwave sensor. This type of measuring device can be integrated into the processes for processing milk. The disadvantage of the disclosed solution is that it is not possible to separate the solids for the precise determination of the protein and lactose content.
- the invention is based on the object of providing a remedy.
- the object is achieved by the method according to claim 1 and the measuring arrangement according to claim 13.
- the method according to the invention for, in particular continuously, determining a lactose content a, protein content b and fat content c of a, in particular flowable, medium, in particular milk, a milk substitute and/or a milk product, comprising the method steps:
- the frequency spectrum has an upper limit of 50 GHz, in particular 25 GHz and preferably 14 GHz, wherein the frequency spectrum has a lower limit of 10 MHz, in particular 50 MHz and preferably 85 MHz;
- the lactose contribution can be distinguished and measured from the protein contribution despite very similar density and permittivity.
- the method according to the invention is suitable, for example, for use in a microwave sensor which is designed to determine the solid content in a flowable, aqueous medium.
- the reference in the sense of the invention is a mathematical quantity which describes the basic contribution of the respective portion to the determined relative permittivity.
- the reference can comprise a mathematical function of the relative permittivity or its real or imaginary part as a function of the frequency.
- the mathematical quantity can also be a frequency-dependent vector.
- One embodiment provides that only the real part of the relative permittivity is used to determine the lactose content a, protein content b and fat content c.
- One embodiment provides that only the imaginary part of the relative permittivity is used to determine the lactose content a, protein content b and fat content c.
- the imaginary part of the relative permittivity can also be used to determine the individual proportions of lactose, protein and fat.
- the imaginary part of the real permittivity describes a loss term that arises when the molecules in the medium are constantly repolarized. This loss term is made up of polarization and conductivity losses. The conductivity losses are particularly evident at low frequencies, which is why conductivity compensation of the imaginary part must be carried out for media with high conductivity (e.g. milk).
- the proportion of conductivity can be calculated using the following equation:
- the electrical conductivity can be determined using a conductivity sensor. This can be part of the measuring system and thus integrated into the process line or as an external handheld device designed to determine or determine the conductivity of a sample of the medium. Alternatively, the electrical conductivity of the medium can also be specified by the user.
- the milk is modelled as a four-component system in the calculation, with the components including fat, lactose, proteins and water.
- the water content of the medium is between 55, in particular 80 and 95 wt%.
- the working point defines a water content or fixed water content range, whereby at least the lactose reference, the protein reference and/or the fat reference of different working points differ.
- the operating point is determined by the user.
- the advantage of taking the expected water content into account is the greater accuracy that can be achieved when determining the individual proportions.
- An operating point in the sense of the invention includes exactly one concrete water content that is known or assumed by the user, or a water content range that includes a large number of water contents.
- lactose reference, the protein reference and the fat reference can be linearized at the specified operating point.
- the relative permittivity depends on the temperature and the measurement frequency.
- a temperature measurement that takes into account the temperature dependence of the medium properties enables the desired accuracy.
- lactose, protein and fat references are each temperature dependent.
- lactose reference has a frequency-dependent
- Lactose vector l wherein the protein reference comprises a frequency dependent protein vector p, wherein the fat reference comprises a frequency dependent fat vector /.
- lactose content a, protein content b and fat content c is determined/can be determined using the equation where A is where the basis vectors v lt v 2 and v 3 are obtained from an orthogonalization procedure of the
- the matrix can comprise the vector products of the basis vectors and the corresponding component vector, or alternatively can already be present as a parameter matrix, i.e. with vector products already executed in the measurement arrangement.
- the basis vectors can also be stored as equations that describe the frequency-dependent behavior of the relative permittivity, or the real part or the imaginary part.
- the measuring arrangement according to the invention for determining a lactose content a, protein content b and fat content c of a flowable medium, in particular milk, a milk substitute and/or a milk product comprises:
- the at least two microwave antennas are arranged on the measuring tube, wherein a first microwave antenna of the at least two microwave antennas has at least a first measuring range, wherein a second microwave antenna of the at least two microwave antennas has at least a second measuring range, wherein the first measuring range and the second measuring range together cover a frequency range of 10 MHz to 50 GHz, in particular 50 MHz to 25 GHz and preferably 85 MHz to 14 GHz.
- the converter electronics comprise an electronic memory, wherein the fat reference and a frequency-dependent fat vector are stored in the memory.
- Fig. 1 a first embodiment of the method according to the invention
- Fig. 2 a second embodiment of the method according to the invention.
- Fig. 3 the real part of the relative permittivity as a function of frequency for a lactose reference, a protein reference and a fat reference;
- Fig. 4 an embodiment of the measuring arrangement according to the invention.
- Fig. 1 shows a first embodiment of the method according to the invention, which can be carried out or is to be carried out by means of a measuring arrangement with a microwave antenna.
- a working point is determined.
- the working point determines the water content of the medium to be monitored or the water content range in which the water content to be expected for the medium lies.
- a water content of between 55, in particular 80 and 95 wt.% is assumed.
- the setting of the working point can be carried out by the operator of the measuring arrangement on a corresponding display of the Measuring arrangement on site or via a central monitoring unit that is connected to the measuring arrangement either contactlessly or with a cable.
- a frequency-dependent relative permittivity of the medium is determined over a frequency range of a frequency spectrum.
- the real part of the relative permittivity is determined and used to determine the individual components in the medium.
- the frequency spectrum has an upper limit of 50 GHz, in particular 25 GHz and preferably 14 GHz and a lower limit of 10 MHz, in particular 50 MHz and preferably 85 MHz.
- This is done using a microwave sensor. The microwave sensor is set up to send a microwave signal into the medium and to measure it again after it has interacted with the medium. Based on the measured microwave signal, the real part of the relative permittivity for the frequency band of the microwave signal is determined.
- a temperature sensor can be provided for this purpose, which is part of the measuring arrangement.
- the temperature of the medium can be determined via a temperature sensor that is separate from the measuring arrangement. In this case, the current temperature of the medium is provided to the converter electronics.
- a fourth process step IV 1, the determined real part of the relative permittivity is corrected or compensated depending on the measured temperature.
- the lactose, protein and/or fat references provided can be temperature-dependent.
- the lactose content a, the protein content b and the fat content c are calculated based on the determined real part and depending on a provided lactose reference, a protein reference and a fat reference.
- a four-component system is assumed for the milk, the milk substitute, the milk product and/or the milk substitute product.
- the components are fat, lactose, proteins and water.
- the lactose reference, the protein reference and/or the fat reference are adapted to the respective operating point. This means that the lactose reference, the protein reference and the fat reference can be linearized at the respective operating point.
- the lactose reference is a frequency-dependent lactose vector l.
- the protein reference which comprises a frequency-dependent protein vector p
- the fat reference which accordingly comprises a frequency-dependent fat vector f.
- the lactose vector l the protein vector p and the fat vector f, the lactose content a, protein content b and fat content c can be determined according to:
- the matrix A is used to transform the vectors l, p and / into the orthogonal system.
- the individual references can also be stored as mathematical functions.
- Fig. 2 shows a second embodiment of the method according to the invention, which can be carried out or is to be carried out using a measuring arrangement with a microwave antenna.
- a first method step 1,2 an operating point is determined.
- the operating point determines the water content of the medium to be monitored or the water content range in which the water content expected for the medium lies.
- the operating point can be determined by the operator of the measuring arrangement on a corresponding display of the measuring arrangement on site or via a central monitoring unit that is connected to the measuring arrangement either contactlessly or by cable.
- a frequency-dependent relative permittivity of the medium is determined over a frequency range of a frequency spectrum.
- the imaginary part of the relative permittivity is determined and used to determine the individual components in the medium.
- the frequency spectrum has an upper limit of 50 GHz, in particular 25 GHz and preferably 14 GHz and a lower limit of 10 MHz, in particular 50 MHz and preferably 85 MHz.
- the imaginary part is determined using a microwave sensor. The microwave sensor is set up to send a microwave signal into the medium and to measure it again after it has interacted with the medium. Based on the measured microwave signal, the imaginary part of the relative permittivity for the frequency band of the microwave signal is determined.
- a temperature sensor can be provided for this purpose, which is part of the measuring arrangement.
- the temperature of the medium can be measured via a temperature sensor that is separate from the measuring arrangement.
- the current temperature of the medium is provided to the converter electronics.
- a fourth method step VI, 2 the electrical conductivity of the medium is measured.
- a conductivity sensor can be provided for this purpose, which is part of the measuring arrangement.
- the conductivity of the medium can be determined using a conductivity sensor that is separate from the measuring arrangement. In this case, the current conductivity in the medium is provided to the converter electronics.
- the determined imaginary part of the relative permittivity is corrected or compensated depending on the temperature and conductivity.
- the lactose, protein and/or fat references provided can be temperature and/or conductivity dependent.
- the lactose content a, the protein content b and the fat content c are calculated based on the determined imaginary part and depending on a provided lactose reference, a protein reference and a fat reference.
- Fig. 3 shows the real part of the relative permittivity as a function of the frequency for a protein reference 201, a lactose reference 202 and a fat reference 203.
- the individual references are each the difference between two reference measurements of different reference media, which only differ in the water content and in one of the remaining three components (protein, lactose and fat). This also means that two components of the reference media are essentially identical.
- the lactose and fat content of the two reference media are essentially identical.
- the water content of the two reference media is between 87 and 92 wt%.
- the course of the protein reference 201 is parabolic in sections and has a minimum at approx. 5 GHz.
- the protein and fat content of the two reference media are essentially identical.
- the water content of the two reference media is between 87 and 92% by weight.
- the curve of the Lactose Reference 202 is parabolic and has a minimum at approx. 8 GHz.
- Fig. 4 shows an embodiment of the measuring arrangement 100 according to the invention for determining a lactose content a, protein content b and fat content c of a flowable medium, in particular milk, a milk substitute and/or a milk product.
- the measuring arrangement 100 comprises a measuring tube 101 for guiding the medium and two microwave antennas 116, 118 arranged opposite one another.
- the microwave antenna 116 is designed to feed a microwave signal into the medium when the medium is present in the measuring tube.
- the microwave signal covers a frequency range of 10 MHz to 50 GHz, in particular 50 MHz to 25 GHz and preferably 85 MHz to 14 GHz.
- an additional pair of microwave antennas can be provided.
- the two measuring ranges of the two microwave antenna pairs together cover the frequency range from 10 MHz to 50 GHz, in particular 50 MHz to 25 GHz and preferably 85 MHz to 14 GHz.
- the microwave antenna 118 is designed to measure the microwave signal sent into the medium by the microwave antenna 116.
- the measured microwave signal is provided to a converter electronics 102, which is designed to carry out the method according to the invention.
- the converter electronics 102 can be mechanically connected to the microwave antenna. If the determination of the individual components takes place in the converter electronics 102 on site, the converter electronics 102 has an electronic memory 103 in which the fat reference and a frequency-dependent fat vector f are stored. Alternatively, the determination of the individual components can take place in a higher-level computing unit that communicates with the converter electronics 102 via cable or wirelessly.
- the measuring arrangement has a temperature sensor 104, which is arranged in a lateral opening of the measuring tube 101 and is positioned such that it is in contact with the medium when the medium is present.
- the temperature of the medium can also be determined via a temperature sensor arranged on the outer surface of the measuring tube and not in contact with the medium.
- the temperature sensor 104 is electrically connected to the converter electronics 102 and is designed to provide current measured values of the temperature to the converter electronics 102.
- the measuring arrangement 100 also has a conductivity sensor 105, which, like the temperature sensor 104, is arranged in a lateral opening of the measuring tube 101 and is designed to determine the electrical conductivity of the medium.
- the conductivity sensor 105 can be designed to be in contact with the medium or not.
- the conductivity sensor 105 is electrically connected to the converter electronics 102 and is designed to provide the converter electronics 102 with measured values of the electrical conductivity.
- the previous description of the illustrated embodiment refers to a transmission measuring method in which the microwave signal is generated with a microwave antenna and measured by another microwave antenna usually positioned opposite.
- the embodiment shown can also be operated in reflection mode.
- the first microwave antenna 116 is designed to emit a microwave signal into the medium and at the same time to measure the microwave signal that is subject to interaction with the medium.
- the second microwave antenna 118 is also designed to emit a microwave signal into the medium and to measure the microwave signal that is subject to interaction with the medium.
- the second microwave antenna 118 is not necessarily arranged opposite the first microwave antenna 116 in this case.
- the microwave signal generated by the first microwave antenna 116 covers a first measuring range, while the second microwave antenna 118 covers a second measuring range.
- the two measuring ranges together cover a frequency range from 10 MHz to 50 GHz, in particular 50 MHz to 25 GHz and preferably 85 MHz to 14 GHz.
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Electromagnetism (AREA)
- Medicinal Chemistry (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102022132798.1A DE102022132798A1 (de) | 2022-12-09 | 2022-12-09 | Verfahren zum kontinuierlichen Bestimmen des Lactose-, Protein- und Fettgehaltes von Milch |
| PCT/EP2023/081999 WO2024120783A1 (de) | 2022-12-09 | 2023-11-16 | Verfahren zum kontinuierlichen bestimmen des lactose-, protein- und fettgehaltes von milch |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP4630796A1 true EP4630796A1 (de) | 2025-10-15 |
Family
ID=88969697
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP23813297.1A Withdrawn EP4630796A1 (de) | 2022-12-09 | 2023-11-16 | Verfahren zum kontinuierlichen bestimmen des lactose-, protein- und fettgehaltes von milch |
Country Status (4)
| Country | Link |
|---|---|
| EP (1) | EP4630796A1 (de) |
| CN (1) | CN120265975A (de) |
| DE (1) | DE102022132798A1 (de) |
| WO (1) | WO2024120783A1 (de) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120310541A1 (en) * | 2009-11-25 | 2012-12-06 | Gil Katz | Online determination of inter alia fat, protein, lactose, somatic cell count and urea in milk by dielectric spectroscopy between 0.3 mhz and 1.4 ghz using chemometric evaluation |
| DE102016125809A1 (de) | 2016-12-28 | 2018-06-28 | Endress+Hauser Flowtec Ag | Messanordnung zur Analyse von Eigenschaften eines strömenden Mediums mittels Mikrowellen |
| DE102017131269A1 (de) | 2017-12-22 | 2019-06-27 | Endress+Hauser Flowtec Ag | Verfahren und Vorrichtung zur Milchfettmessung |
| DE102019131504A1 (de) | 2019-11-21 | 2021-05-27 | Endress + Hauser Flowtec Ag | Antennenanordnung zur Abstrahlung von Mikrowellen und Messanordnung mit mindestens einer solchen Antennenanordnung |
-
2022
- 2022-12-09 DE DE102022132798.1A patent/DE102022132798A1/de active Pending
-
2023
- 2023-11-16 EP EP23813297.1A patent/EP4630796A1/de not_active Withdrawn
- 2023-11-16 WO PCT/EP2023/081999 patent/WO2024120783A1/de not_active Ceased
- 2023-11-16 CN CN202380083346.XA patent/CN120265975A/zh active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| CN120265975A (zh) | 2025-07-04 |
| DE102022132798A1 (de) | 2024-06-20 |
| WO2024120783A1 (de) | 2024-06-13 |
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