CN112014461A - Detection system and method for multi-index analysis of milk - Google Patents

Detection system and method for multi-index analysis of milk Download PDF

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Publication number
CN112014461A
CN112014461A CN201910451465.1A CN201910451465A CN112014461A CN 112014461 A CN112014461 A CN 112014461A CN 201910451465 A CN201910451465 A CN 201910451465A CN 112014461 A CN112014461 A CN 112014461A
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ultrasonic
microwave
milk
detection
index analysis
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刘川
郑礼龙
王辛尧
王禹浪
陈飞
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Chuzhou Commscope Testing Equipment Co ltd
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Chuzhou Commscope Testing Equipment Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/02Analysing fluids
    • G01N29/024Analysing fluids by measuring propagation velocity or propagation time of acoustic waves
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N22/00Investigating or analysing materials by the use of microwaves or radio waves, i.e. electromagnetic waves with a wavelength of one millimetre or more
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N22/00Investigating or analysing materials by the use of microwaves or radio waves, i.e. electromagnetic waves with a wavelength of one millimetre or more
    • G01N22/04Investigating moisture content
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N29/00Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
    • G01N29/02Analysing fluids
    • G01N29/032Analysing fluids by measuring attenuation of acoustic waves
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00Indexing codes associated with group G01N29/00
    • G01N2291/01Indexing codes associated with the measuring variable
    • G01N2291/011Velocity or travel time
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00Indexing codes associated with group G01N29/00
    • G01N2291/01Indexing codes associated with the measuring variable
    • G01N2291/015Attenuation, scattering
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00Indexing codes associated with group G01N29/00
    • G01N2291/02Indexing codes associated with the analysed material
    • G01N2291/022Liquids
    • G01N2291/0228Aqueous liquids
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2291/00Indexing codes associated with group G01N29/00
    • G01N2291/02Indexing codes associated with the analysed material
    • G01N2291/028Material parameters
    • G01N2291/02809Concentration of a compound, e.g. measured by a surface mass change

Abstract

The invention discloses a detection system and a detection method for multi-index analysis of milk, and belongs to the field of detection systems. Aiming at the problems of single detection mode, expensive and huge instrument of the existing milk in the prior art, the invention provides a detection system and a method for multi-index analysis of milk. The system comprises an ultrasonic detection system and a microwave detection system, wherein the ultrasonic detection system and the microwave detection system are arranged in a detection area and are connected with an external control system. By combining the microwave detection technology and the ultrasonic detection technology, the method realizes accurate, rapid and efficient detection of indexes of milk, such as fat, protein, non-fat milk solid, lactose, water mixing rate, mastitis and the like.

Description

Detection system and method for multi-index analysis of milk
Technical Field
The invention relates to the field of detection systems, in particular to a detection system and a detection method for multi-index analysis of milk.
Background
(1) Necessity and common detection technology of milk detection
The milk is a necessary nutritional food in our daily life, contains rich protein, minerals, vitamins and carbohydrates, and plays an important role in human health. In recent years, with the improvement of living standard and health requirements of people, the milk cultivation and dairy product processing industry develops rapidly, and in order to ensure the quality of milk and dairy products, the quality of the milk needs to be controlled and checked in the processes of milk production, raw milk purchase, milk processing and transportation so as to meet national standards, and some milk products do not meet the national standard indexes, so that people feel uncomfortable once drinking the milk products and even can bring serious consequences. For this reason, manufacturers of milk products generally equip them with various instruments and devices dedicated to the quality detection of milk samples. The milk quality detection mainly comprises the measurement of the content of the internal components of the milk, the detection of harmful substances and adulteration, and the like. The traditional milk quality inspection mostly adopts a national standard method, namely a chemical analysis method. Because of the long analysis time and high cost of chemical methods, rapid, non-contact and automatic detection methods are proposed, and the current market mainly comprises a mid-infrared spectrum method, a near-infrared spectrum analysis method and an ultrasonic analysis method. Corresponding commercial instruments are available for both infrared spectroscopy and ultrasonic analysis. In addition, the microwave has wide application prospect in milk analysis as a new technology.
In the chemical analysis method, the national standard has strict regulations on various indexes and detection of dairy products such as fresh milk, pasteurized milk, sterilized milk and the like. If fat is measured by the method of Rotzingguotry, the reported mass fraction result needs to be accurate to 0.01%; the Kjeldahl method measures the protein, and the difference between the two parallel measurement results is not more than 1.5 percent of the average value of the two measurements; the lactose is tested by high pressure liquid chromatography and a Leaine-Enon method, and the difference between the two parallel measurement results is not more than 5 percent of the average value; although the chemical method is well developed, the detection process is complex, the testing time is too long, the technical requirement is high, and the assay cost is high, so that the requirements of purchasing a large amount of raw milk and analyzing the processed components of the milk product cannot be met.
The fast developed infrared spectrum detection method in the field of dairy product quality analysis has the advantages of no need of pretreatment of samples, low consumption, no chemical time, fast analysis and the like, and can be accepted by authorities. A plurality of electronic detection instruments with infrared detection principles are produced at home and abroad to replace chemical detection. Such as a multifunctional dairy analyzer of the swedish Foss company, a snap (tm) series milk component analyzer of the Idexx company in the united states, a milk adulterating analyzer of the mitsunda instruments ltd. Although the instruments are accurate in measurement, due to the fact that the instruments are expensive and large in one-time investment, most dairy products enterprises are difficult to accept, actual requirements of common dairy production are not met, and wide application of the instruments is restricted.
(2) Features and advantages of ultrasonic testing
The application of ultrasonic technology is one of the milk detection methods worth popularizing. The technology utilizes the interaction between high-frequency sound waves and substances to acquire the physicochemical properties of the interior of the measured substances. The detection method of the ultrasonic propagation characteristics mainly measures the speed of sound and the sound attenuation of the ultrasonic propagation characteristics in milk. Through a large number of experiments, an empirical mathematical relationship between the components of part of the milk and the ultrasonic characteristics is established. At present, various ultrasonic milk component analyzers are available, and the prediction precision CV value can reach the level of 5%.
The invention discloses a device for analyzing and detecting the content of liquid milk components by using a low-energy ultrasonic detection technology, which is a Chinese patent with the patent number of CN 2837841Y and the name of a milk sample rapid detector, and mainly aims to detect the content of fat, protein and non-fat Solid (SNF) and the like.
The invention discloses a Chinese invention patent with the patent number of CN 100573133C and the name of method and detecting instrument for improving the ultrasonic detection precision of milk quality, and discloses a basic method and instrument for reducing the temperature influence and improving the model prediction precision in the ultrasonic detection of milk quality. The method establishes the correlation correction model between the ultrasonic parameters and the concentration of the main components of the milk at a plurality of temperature points in the heating process of the milk, thereby calculating the content of each component of the unknown milk.
The invention discloses an ultrasonic milk component analyzer, which is a Chinese invention patent with the patent number of CN 1194225C and the name of ultrasonic milk component analyzer, and utilizes an ultrasonic detection technology and a multiple linear regression equation to analyze components of multi-phase liquid, can detect and analyze fat, protein, non-fat milk solid, density, freezing point and water adding rate in milk at one time, and utilizes ultrasonic to detect the content of milk components.
U.S. patent No. US 20030051535a1 entitled "Characterization of fluids using ultrasonic reflection" discloses a method for characterizing physical properties of fluids using ultrasonic reflection. The method determines the physical property of interest by correlating certain properties of the reflected ultrasound waves with the measured physical properties of the fluid. The invention is particularly suitable for the online detection of food solutions such as milk, tomato sauce, syrup, chocolate, other candies and the like.
(3) Features and advantages of microwave detection technique
The microwave technology has the advantages of low cost, environmental protection, capability of testing the opaque liquid and the like. The basic properties of microwaves are generally represented by three characteristics, namely penetration, reflection and absorption. The microwave sensor detects microwave emission in a certain frequency band, and performs penetration, reflection and absorption in a milk sample, and finally reflected signals are collected and analyzed. In the process, the difference between the signal emission and the feedback is determined by the characteristics of the milk samples with different component contents, wherein the dielectric properties of the milk samples are the main characteristics, so that the feedback signal is used as a characteristic signal of the sample to analyze, and the qualitative or quantitative analysis can be carried out on the sample. At present, the milk detection method and the milk detection equipment based on the microwave principle are not widely applied.
The invention discloses a detection system for harmful substances in liquid milk, which is a Chinese invention patent with the patent number of CN 103743762B and named as a detection device for harmful impurities in liquid milk, and comprises modules such as a microwave signal generator, a microwave circuit, a microwave sensor and the like, wherein the detection system detects the amplitude of electromagnetic waves, the fragrance and the current intensity or the impedance variable quantity according to the induced polarization effect of charged ions of different substances in the liquid milk in a microwave electromagnetic field, and finally obtains the melamine content in the liquid milk.
The patent number is US 006462321B2, entitled "Microwave assisted content analyzer", and discloses a content analysis method. The method can analyze the water content of the material, the contents of fat, oil, volatile matters except water and the like by utilizing microwave radiation.
In addition to the milk detection technology, the Chinese invention patent with the patent number of CN 101769866B and named as a milk component detection device and method discloses a milk detection method combining ultrasonic and near infrared spectrum technologies. The method uses an ultrasonic self-excitation frequency measurement technology to evaluate the background interference of the milk components, automatically classifies near-infrared spectrum models and realizes the rapid, automatic and efficient detection of the conventional components of the milk.
In summary, the existing milk quality inspection methods and apparatuses have advantages and disadvantages and are mostly applied to a single principle. Therefore, a multi-principle multi-parameter milk sample analysis system or equipment with low cost and high performance suitable for the current situation of the milk industry is developed, and the requirements of the milk industry on production and consumption are met to a greater extent.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems of single detection mode, expensive and huge instrument of the existing milk in the prior art, the invention provides a detection system and a method for multi-index analysis of milk. By combining the microwave detection technology and the ultrasonic detection technology, the method realizes accurate, rapid and efficient detection of indexes of milk, such as fat, protein, non-fat milk solid, lactose, water mixing rate, mastitis and the like.
2. Technical scheme
The purpose of the invention is realized by the following technical scheme.
A detection system for milk multi-index analysis comprises an ultrasonic detection system and a microwave detection system, wherein the ultrasonic detection system and the microwave detection system are arranged in a detection area and are connected with an external control system.
Furthermore, the ultrasonic detection system comprises an ultrasonic transducer, and the ultrasonic transducer detects the liquid to be detected in the ultrasonic testing area.
Furthermore, the ultrasonic transducer comprises an ultrasonic transducer left side and an ultrasonic transducer right side which are respectively arranged at two ends of the ultrasonic testing area.
Furthermore, the ultrasonic transducer is electrically connected with the ultrasonic driving circuit and the analog-to-digital conversion module, and the control processor is electrically connected with the ultrasonic driving circuit and the analog-to-digital conversion module.
Furthermore, the ultrasonic testing area is an ultrasonic testing container, and a liquid inlet of the ultrasonic testing container and a liquid outlet of the ultrasonic testing container are respectively connected with the ultrasonic testing conveying pipeline and the ultrasonic liquid drainage pipeline.
Furthermore, one or more temperature sensors I are arranged in the ultrasonic testing area, the ultrasonic testing conveying pipeline and/or the ultrasonic liquid discharging pipeline.
Furthermore, the microwave detection system comprises a microwave detection chip, and the liquid to be detected is detected through a microwave test area of the microwave detection chip.
Furthermore, the microwave detection chip comprises a PCB substrate and a double-ring structure single-port SRR arranged on the PCB substrate.
Furthermore, the double-ring structure single-port SRR is composed of an inner ring and an outer ring, the outer ring is a single-opening ring which is opened towards one side of the PCB substrate, the inner ring is a single-opening ring which is arranged in the outer ring, a gap is arranged between the inner ring and the outer ring, and the opening direction of the inner ring is perpendicular to the opening direction of the outer ring.
Furthermore, the microwave test area is a micro-channel which is respectively connected with a microwave liquid inlet pipeline and a microwave liquid outlet pipeline. The microwave liquid inlet pipeline is connected with the microwave detection conveying pipeline.
Furthermore, one or more temperature sensors II are arranged in the microwave test area, the microwave detection conveying pipeline, the microwave liquid inlet pipeline and/or the microwave liquid outlet pipeline.
Furthermore, the microwave detection system further comprises,
the radio frequency connector is connected with the microwave detection chip and receives and transmits video signals;
the directional coupler extracts forward and backward microwave signals and transmits them to the amplitude-phase detector;
an amplitude-phase detector for converting the RF signal into a DC voltage signal;
and the microwave signal source is connected with the directional coupler and is connected with the control processor.
Furthermore, the liquid to be detected is divided into two paths through the liquid inlet hose, the liquid conveying pipe and the two-way valve, and the two paths of liquid respectively enter the ultrasonic detection area and the microwave detection area.
Furthermore, the liquid detected by the ultrasonic detection area and the microwave detection area enters the liquid discharge hose after passing through the pipe joint until reaching the waste liquid outlet.
Furthermore, the control system is connected with the control processor, and the control processor carries out detection and calculation on the ultrasonic detection system and the microwave detection system.
Furthermore, the device also comprises a shielding constant temperature container, and the detection parts of the ultrasonic detection system and the microwave detection system are arranged in the shielding constant temperature container.
Furthermore, the device also comprises a heating mechanism which is arranged in the shielding constant temperature container and used for heating the liquid to be detected of the ultrasonic detection system and the microwave detection system in the shielding constant temperature container.
Further, the heating mechanism is a heating wire.
Furthermore, the device also comprises a variable voltage power supply which supplies power to the control processor.
A detection method for milk multi-index analysis comprises the following steps: the liquid to be measured is detected by a microwave and ultrasonic detection system, a microwave detection signal measures the characteristic peak frequency and the characteristic peak S11 value of a microwave spectrum, the ultrasonic detection signal mainly measures the sound velocity and sound attenuation of ultrasonic wave propagation, information of measurement parameters is collected by the system and then transmitted to a control processor for data analysis, preliminary data results are respectively selected and brought into a preset model for analysis, data processing is completed, parameter results required to be measured are obtained, and data are output to obtain detection results.
Further, the predetermined models include milk component models and mastitis parameter models.
Further, the step of obtaining the model is as follows,
A. respectively preparing a series of standard solutions with different concentrations of each component according to the milk component parameters, and measuring by using a standard method to obtain the standard value of each component of the sample;
B. then, performing instrument detection on the prepared milk standard sample, and inputting a corresponding measurement information value;
C. the modeling of the milk components comprises two parts of microwave measurement information and ultrasonic measurement information;
D. and establishing a multi-parameter linear regression model for the standard value and the measurement parameter of each measurement component of the milk sample by a partial least square method to obtain an analysis model of each component index.
Further, the microwave measurement information of step C includes the frequency of the characteristic value and the S11 value, and the ultrasonic measurement information includes the sound velocity and the sound attenuation.
Furthermore, the correlation correction model between the milk components and the microwave frequency and the microwave attenuation coefficient S11 and between the ultrasonic sound velocity and the ultrasonic attenuation coefficient is as follows:
Ci=ki+kfif+kSiS+kviv+kαiα
wherein Ci is the mass percentage concentration of the ith milk component; f is the frequency value of the characteristic peak of the milk, unit GHz, S is the value of the characteristic peak S11, unit dB; v is the ultrasonic sound velocity of the measured milk, and the unit is m/s; alpha is the ultrasonic attenuation coefficient of milk, and the unit is dB/cm; ki. kfi, kSi, kvi, and k α i are regression coefficients of the ith milk component measurement model.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
according to the scheme, the milk detection system and method combining microwave and ultrasonic technologies use a plurality of modeling parameters reflecting different physicochemical properties of milk, so that the modeling parameters contain more milk component information, and the accuracy of model prediction is improved. And can provide information for judging mastitis of milk besides detecting the concentration of the milk component. Therefore, the invention simultaneously realizes the rapid, accurate, automatic and efficient detection of the conventional components of the milk and mastitis indexes. The detection equipment has small volume, light weight and high response speed, can be widely applied to pastures, dairy product processing plants and dairy product detection units, and can also be used for continuously monitoring milk in real time so as to realize the quality control of processed products.
Drawings
FIG. 1 is a design diagram of a micro-fluidic chip of a microwave sensor;
FIG. 2 is a schematic view of a microwave and ultrasonic measurement control system;
FIG. 3 is a diagram of a microwave and ultrasonic combined detection system;
FIG. 4 is a flow chart of milk detection parameter modeling;
FIG. 5 is a flow chart of milk testing;
FIG. 6 is a graph of the microwave detection results of milk with different water mixing rates.
The reference numbers in the figures illustrate:
1. a liquid inlet hose; 2. an infusion pump; 3. a delivery pipe; 4. a two-way valve; 5. detecting a conveying pipeline by microwave; 6. ultrasonic detection of the conveying pipeline; 7. shielding the constant-temperature container; 8. heating wires; 9. the ultrasonic transducer is arranged on the left side; 10. ultrasonically detecting a liquid inlet of the container; 11. an ultrasonic testing area; 12. acoustically detecting a container liquid outlet; 13. the right side of the ultrasonic transducer; 14. a temperature sensor I; 15. an ultrasonic drainage pipeline; 16. a drain hose; 17. a waste liquid outlet; 18. a temperature sensor II; 19. a microwave liquid outlet pipeline; 20. a pipe joint; 21. a microwave detection chip; 22. a microwave test zone; 23. a radio frequency connector; 24. a microwave liquid inlet pipeline; 25. a directional coupler; 26. a magnitude-phase detector; 27. a microwave signal source; 28. a control processor; 29. the ultrasonic drive circuit and the analog-to-digital conversion module; 30. a variable voltage power supply; 31. and (5) controlling the system.
Detailed Description
The invention is described in detail below with reference to the drawings and specific examples.
Example 1
Cow mastitis affects the quality of milk production and is a very important index in milk detection. At present, the detection of the mastitis of the dairy cattle is mainly judged by milk physicochemical properties such as the somatic cell number, the conductivity and the like of the milk. The traditional milk component detection instrument, such as a milk detector based on technologies such as ultrasonic waves, infrared spectroscopy and the like, cannot detect mastitis of the milk. The high-frequency microwave sensor based on the liquid dielectric constant detection principle can judge whether the cow has mastitis or not through the change of the dielectric constant in the milk. Therefore, the microwave detection technology and the ultrasonic detection technology are combined, so that the main components of the milk, such as fat, protein, lactose, non-fat milk solid and the like, and the index of the mastitis of the milk can be detected simultaneously. In addition, the ultrasonic technology and the microwave technology are different based on the detection principle of the milk components, and the two detection technologies reflect different properties of the milk components, so that the ultrasonic technology and the microwave technology are combined to obtain a more accurate milk component detection result.
The scheme designs a detection system for milk multi-index analysis, which comprises an ultrasonic detection system and a microwave detection system, wherein the ultrasonic detection system and the microwave detection system are arranged in a detection area and are connected with an external control system. FIG. 3 is a block diagram of the microwave and ultrasonic combined detection system, showing the hardware components of the microwave and ultrasonic combined detection system. Liquid to be detected is sucked into the detection system through the liquid inlet pipe by the stepping motor type peristaltic pump, the liquid to be detected enters the microwave detection system and the ultrasonic detection system which are connected in parallel sequentially through the control of the two-way valve, and the flow rate of the liquid to be detected of the two detection systems and the discharge of waste liquid are controlled by the microcontroller through controlling the peristaltic pump.
The ultrasonic detection system comprises an ultrasonic transducer, and the ultrasonic transducer detects the liquid to be detected in the ultrasonic test area 11. The ultrasonic transducer comprises an ultrasonic transducer left 9 and an ultrasonic transducer right 13 which are respectively arranged at two ends of the ultrasonic testing area 11. The ultrasonic transducer is electrically connected with the ultrasonic drive circuit and the analog-to-digital conversion module 29, and the control processor 28 is electrically connected with the ultrasonic drive circuit and the analog-to-digital conversion module 29. The ultrasonic testing area 11 is an ultrasonic testing container, and an ultrasonic testing container liquid inlet 10 and an ultrasonic testing container liquid outlet 12 of the ultrasonic testing container are respectively connected with the ultrasonic testing conveying pipeline 6 and the ultrasonic liquid drainage pipeline 15. One or more temperature sensors I14 are provided in the ultrasonic testing zone 11, the ultrasonic testing delivery conduit 6 and/or the ultrasonic drainage conduit 15. The ultrasonic testing container is a circular tube-shaped cavity, and ultrasonic transducers are respectively arranged on two sides of the container and used as ultrasonic transmitting and receiving probes. The ultrasonic emission circuit is controlled by the micro control processor to be emitted by the ultrasonic probe emission end, and after the signal is received by the ultrasonic probe at the other end of the container, the ultrasonic signal is returned to the micro control processor for processing by the receiving circuit.
FIG. 2 is a schematic diagram of a microwave and ultrasonic measurement control system. The microwave detection system comprises a microwave detection chip 21, and the liquid to be detected is detected through a microwave test area 22 of the microwave detection chip 21. The microwave detection chip 21 includes a PCB substrate and a dual-ring structure single-port SRR disposed on the PCB substrate. The double-ring structure single-port SRR is composed of an inner ring and an outer ring, the outer ring is a single-opening ring which is opened towards one side of the PCB substrate, the inner ring is a single-opening ring which is arranged in the outer ring, a gap is arranged between the inner ring and the outer ring, and the opening direction of the inner ring is perpendicular to the opening direction of the outer ring.
The core component of the microwave detection system is a micro-fluidic chip of a microwave sensor, the microwave chip is connected with the control system through a radio frequency connector of the SMA interface, microwave signals are transmitted and received, and data processing is carried out on the signals.
Fig. 1 is a design diagram of a micro-fluidic chip of a microwave sensor. The microwave sensor on the left in the figure is a single-port open resonator ring structure containing a double-ring structure. The microwave sensor is designed and manufactured on the PCB, so that the manufacturing cost is greatly reduced, and the microwave sensor can be suitable for more working scenes. The double-ring circuit trace on the PCB is processed and manufactured by a method of copper plating, light masking and exposure corrosion. Wherein the outer ring is a microwave exciter and the inner ring is a ring resonator. The exciter ring is soldered to an SMA connector that transmits the signal to a custom signal processor. Microwave signals of different frequencies are initially fed back into the outer loop. These signals are then coupled to the inner loop. The gap on the inner ring is designed to generate an electric field at its top. The microwave microfluidic chip is a microwave sensor fabricated on a PCB substrate. And adhering a silica gel pad carved with a micro-fluid channel on a microwave sensor substrate, aligning the micro-channel to the gap of the inner ring of the sensor, and adhering a PTFE or glass cover plate processed with a micro-channel liquid inlet and outlet on the microwave sensor through a double-sided adhesive tape, thereby constructing the sealed micro-fluid channel. Wherein the microchannel has a design diameter width of 1 mm. Of course, other widths may be used as long as the microfluidic detection is ensured to be performed smoothly. The microwave test area 22 is the micro-channel and is respectively connected with a microwave liquid inlet pipeline 24 and a microwave liquid outlet pipeline 19. The microwave liquid inlet pipeline 24 is connected with the microwave detection conveying pipeline 5. One or more temperature sensors II18 are arranged in the microwave test area 22, the microwave detection conveying pipeline 5, the microwave liquid inlet pipeline 24 and/or the microwave liquid outlet pipeline 19. The specific model of the pipeline and the valve for ultrasonic and microwave detection can be designed according to the requirement, has no strict requirement on the specific material model, and can be replaced by components with similar functions.
The microwave detection system further comprises a microwave detection unit,
the radio frequency connector 23 is connected with the microwave detection chip 21 and receives and transmits video signals;
the directional coupler 25 extracts forward and backward microwave signals and transmits them to the amplitude-phase detector;
an amplitude-phase detector 26 for converting the RF signal into a dc voltage signal;
and a microwave signal source 27 connected with the directional coupler 25 and connected with the control processor 28.
This control system can replace the conventional microwave vector network analyzer VNA. The microcontroller is used to control the generation of the microwave signal and to collect amplitude and phase difference data from the amplitude and phase detector 26. The directional coupler 25 extracts the forward and backward microwave signals and transmits them to the amplitude-phase detector 26. The amplitude and phase detector 26 converts the radio frequency signal into a dc voltage signal, and the amplitude and phase detector converts the high frequency signal into a low frequency signal for the analog-to-digital converter ADC. In the conventional vector network analyzer VNA structure, multi-stage mixing is used for the down-conversion operation, but due to the complexity, the integrated amplitude and phase detector 26ad8302 is adopted in the present scheme to directly down-convert the high frequency signal. System complexity and cost are greatly reduced, but at the same time performance and stability are sacrificed, unlike conventional microwave network analyzers, which use mixers to convert frequency. Conventional schemes typically mix the frequency with a local oscillator and an input signal, which typically have a difference of a few MHz or KHz, which is the bandwidth of the measurement. The mixed signal is sampled by the ADC and back-end digitally processed. The whole process can be regarded as in-phase quadrature IQ modulation and demodulation to analyze real part amplitude and imaginary part phase information. An analog-to-digital converter ADC embedded in the microcontroller takes samples of the signal from the gain detector and transmits and stores the read dc voltage to digital data. In the next step, the control processor 28 communicates with the upper computer of the PC and uploads the collected data to the PC. The processed and calibrated test results are displayed on a graphical user interface GUI and reorganized for further data processing. These are circuit parts, which are grommets independent of the water circuit. The final product should be a PCB board and encapsulated with a metal shielding can. One end is connected to the microwave sensor through the SMA, and the other end is connected to the computer for data communication. The liquid to be detected is divided into two paths through a liquid inlet hose 1, an infusion pump 2, a delivery pipe 3 and a two-way valve 4, and the two paths of liquid respectively enter an ultrasonic detection area and a microwave detection area.
The liquid detected in the ultrasonic detection area and the microwave detection area passes through the pipe joint 20 and enters the liquid discharge hose 16 to the waste liquid outlet 17.
The control system 31 is connected to the control processor 28, and the control processor 28 performs detection and calculation of the ultrasonic detection system and the microwave detection system. The control system 31 is a PC and a corresponding embedded system.
The ultrasonic detection system and the microwave detection system are characterized by further comprising a shielding constant temperature container 7, wherein detection parts of the ultrasonic detection system and the microwave detection system are arranged in the shielding constant temperature container 7. The liquid heating device further comprises a heating mechanism, wherein the heating mechanism is arranged in the shielding constant-temperature container 7 and is used for heating liquid to be detected of an ultrasonic detection system and a microwave detection system in the shielding constant-temperature container 7. The heating mechanism is a heating wire 8, and preferably further comprises a variable voltage power supply 30, and the variable voltage power supply 30 supplies power to the control processor 28. Since the detection results of the microwaves and the ultrasonic waves are affected by environmental factors such as temperature, the detection systems of the microwaves and the ultrasonic waves are placed in the shielded thermostatic container 7. A temperature sensor and an electric heating wire 8 are installed in the container. The temperature sensor is not necessarily arranged at the outlet, the influence of the temperature sensor on the detection sample and the detection process is mainly considered to be reduced at the outlet, the temperature sensor is more accurate to arrange at the outlet, and the basic detection is not influenced at other parts. The control processor can control the temperature circuit to use the electric heating wire to keep the temperature of the test container according to the temperature measurement result of the temperature sensor. The temperature sensor, the heating wire 8 and the shielding container 7 are used for temperature control and shielding, so that better detection effect and better accuracy can be ensured. The variable voltage power supply 30 is required only by performing variable voltage during alternating current power supply, and the variable voltage power supply 30 is not required during direct current power supply.
According to the scheme, the ultrasonic detection system comprises a micro-control processor, an ultrasonic driving circuit, an analog-to-digital conversion module, an ultrasonic transducer and the like. The drive circuit and the analog-to-digital conversion of ultrasonic waves are controlled by the micro-control processor, the ultrasonic waves are transmitted to the ultrasonic transducer, ultrasonic signals are transmitted and received for a sample to be detected, and then the ultrasonic signals enter the micro-control processor to complete data processing through reverse signal collection and transmission.
The core of the system is a microwave and ultrasonic detection system which is connected in parallel, and mainly comprises a micro-fluidic chip of a microwave sensor, a microwave signal control system, an ultrasonic detection cavity, an ultrasonic transducer which is used for transmitting and receiving ultrasonic waves in the cavity, and a driving circuit and a control system of the ultrasonic waves, which are indispensable parts of the system. The control system of microwave and ultrasonic wave has been explained by fig. 2, and fig. 3 mainly describes the water circuit operation and temperature control system of the detection system. Peristaltic pumps, tubing and valves help achieve parallel operation of the microwave and ultrasound systems. Because the microwave detection system uses the microfluidic chip, the width of the microchannel is only 1mm, so the flow rate of the microwave system is smaller than that of the ultrasonic system, and the pipe diameter entering and exiting the microwave system has the process of changing from large to small and from small to large. The microwave micro-fluidic chip has small pipeline and small flow. The function of the two-way valve is to control the liquid sample not to enter the microwave detection conveying pipeline 5 and the ultrasonic detection conveying pipeline 6 at the same time, namely, the detection liquid firstly enters the microwave system through the microwave detection conveying pipeline 5 by the control of the valve, at the moment, the ultrasonic detection conveying pipeline 6 is closed, and no liquid enters the ultrasonic system. When the microwave detection is finished, the microwave detection conveying pipeline 5 is closed and the ultrasonic detection conveying pipeline 6 is opened under the control of the two-way valve 4, so that the detection liquid enters the ultrasonic detection system. The heating wires, the temperature sensors and the constant-temperature shielding container in the system are mainly used for realizing the functions of adjusting and controlling the temperature, and meanwhile, the constant-temperature shielding container also has the function of shielding the external microwave signal interference.
A detection method for milk multi-index analysis comprises the following steps: the liquid to be measured is detected by a microwave and ultrasonic detection system, a microwave detection signal measures the characteristic peak frequency and the characteristic peak S11 value of a microwave spectrum, the ultrasonic detection signal mainly measures the sound velocity and sound attenuation of ultrasonic wave propagation, information of measurement parameters is collected by the system and then transmitted to the control processor 28 for data analysis, and through preliminary data results, the preliminary data results are respectively selected and taken into a preset model for analysis to complete data processing, so that parameter results required to be measured are obtained, and data are output to obtain detection results. The preset models comprise milk component models and mastitis parameter models.
In order to realize the purpose of milk detection, the patent provides a milk multi-parameter detection method, which comprises the steps of establishing a parameter model and detecting milk.
The establishment of the parameter model comprises the steps of sample pretreatment, chemical analysis method measurement, microwave information acquisition, ultrasonic information acquisition, analysis model establishment, model storage and the like.
The milk detection method comprises the steps of microwave signal measurement, ultrasonic signal measurement, microwave information acquisition, ultrasonic information acquisition, data analysis, model determination, data processing and data output.
FIG. 4 shows the main process of classification modeling of milk detection parameters in the present invention. The detection parameters of the milk are divided into two parts of main component indexes and mastitis indexes of the milk, and the milk is modeled in different modes respectively. The main ingredient indexes of the milk comprise fat, protein, non-fat milk solid, lactose and water mixing rate indexes.
The steps for obtaining the model are as follows,
A. respectively preparing a series of standard solutions with different concentrations of each component according to the milk component parameters, and measuring by using a standard method to obtain the standard value of each component of the sample;
B. then, performing instrument detection on the prepared milk standard sample, and inputting a corresponding measurement information value;
C. the modeling of the milk components comprises two parts of microwave measurement information and ultrasonic measurement information; the microwave measurement information includes the frequency of the characteristic value and the S11 value, and the ultrasonic measurement information includes the sound velocity and the sound attenuation.
D. And establishing a multi-parameter linear regression model for the standard value and the measurement parameter of each measurement component of the milk sample by a partial least square method to obtain an analysis model of each component index.
The correlation correction model of the milk components, the microwave frequency and the microwave attenuation coefficient S11 and the correlation correction model of the ultrasonic sound velocity and the ultrasonic attenuation coefficient is as follows:
Ci=ki+kfif+kSiS+kviv+kαiα
wherein Ci is the mass percentage concentration of the ith milk component; f is the frequency value of the characteristic peak of the milk, unit GHz, S is the value of the characteristic peak S11, unit dB; v is the ultrasonic sound velocity of the measured milk, and the unit is m/s; alpha is the ultrasonic attenuation coefficient of milk, and the unit is dB/cm; ki. kfi, kSi, kvi, and k α i are regression coefficients of the ith milk component measurement model. The regression coefficient is calculated by measuring the standard value of each parameter of a series of milk samples with different concentrations and by a partial least square method according to a modeling process.
Different from a modeling mode of milk component indexes, milk mastitis is detected mainly by taking a variation curve map of an S11 response value in a frequency range of 1-3GHz through microwave detection as collected information, a corresponding database is established through detection of a large number of milk samples containing mastitis and milk samples not containing mastitis, modeling is performed through a Machine learning model of a Support Vector Machine, the Support Vector Machine (SVM) is a commonly-used Machine learning algorithm for binary classification of data, model construction and calculation are directly performed through calling a data packet in software, and the method is an existing scheme. And finally, summarizing the models of various milk detection indexes into a milk detection classification model library.
Fig. 5 illustrates a milk detection process: the milk passes through the peristaltic pump and enters the microwave and ultrasonic detection system in sequence. The microwave detection signal mainly measures the characteristic peak frequency of the microwave spectrum and the characteristic peak S11 value. The ultrasonic detection signal mainly measures the sound velocity and the acoustic attenuation of the ultrasonic wave propagation. The information of the measurement parameters is collected by the system and then transmitted to the controller for data analysis. And (4) respectively selecting and bringing the initial data results into proper models for analysis to complete data processing, thereby obtaining parameter results to be measured and outputting the data.
Milk is sucked into the detection system through the peristaltic pump, and the milk enters the microwave detection module firstly through the two-way control valve. When milk flows through the microwave micro-fluidic sensor, the microwave signal processing system can control the generation of microwave signals and collect and process microwave information fed back by milk liquid detection.
The microwave detection result obtained after the data processing is a graph of the frequency and the reflection coefficient S11 value as shown in fig. 6. The frequency of the liquid to be measured, such as milk, and the information of the value of S11 are collected and analyzed together with the detection information of the ultrasonic waves.
Through the control of the two-way valve, the milk sample can be sucked into the ultrasonic detection system through the peristaltic pump after passing through the microwave detection system. The ultrasonic testing area is a cylindrical cavity, and two ends of the cavity are respectively provided with an ultrasonic transducer for respectively realizing the transmission and the reception of ultrasonic signals. The ultrasonic signal processing system also controls the generation of microwave signals through the microprocessor and collects and processes microwave information fed back by detecting milk liquid through the driving circuit and the analog-to-digital converter. The collected ultrasonic information is the sound velocity and acoustic attenuation of the ultrasonic waves. The two ultrasonic parameters are collected with the frequency of the microwave and the S11 value parameters, and then are subjected to data analysis.
According to two types of multi-parameter models which are established before and comprise components of milk and mastitis, the system substitutes measured microwave and ultrasonic parameter values into the models for calculation, and obtains the result of the concentration value of the corresponding milk component and the information of whether mastitis exists. And finally, the system outputs the data obtained by detection and calculation through a computer or an embedded system.
According to the result of the measurement of the milk sample by the microwave sensor chip, as shown in fig. 6, the characteristic peak of the microwave measurement spectrum of the milk around 1.8GHz exists, and the characteristic peak of the milk with different water mixing rates can shift. Therefore, a milk water mixing rate model can be established according to the frequency of the characteristic peak value of the standard sample and the S11 value, and the microwave characteristic peak value of the measured sample is brought into the corresponding model, so that the water mixing rate value of the milk can be obtained. Besides the water mixing rate, the microwave detection can also detect components such as fat, protein, non-fat milk solid, lactose and the like of the milk, and the accuracy of the detection result is improved by combining with ultrasonic detection.
The invention and its embodiments have been described above schematically, without limitation, and the invention can be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The representation in the drawings is only one of the embodiments of the invention, the actual construction is not limited thereto, and any reference signs in the claims shall not limit the claims concerned. Therefore, if a person skilled in the art receives the teachings of the present invention, without inventive design, a similar structure and an embodiment to the above technical solution should be covered by the protection scope of the present patent. Furthermore, the word "comprising" does not exclude other elements or steps, and the word "a" or "an" preceding an element does not exclude the presence of a plurality of such elements. Several of the elements recited in the product claims may also be implemented by one element in software or hardware. The terms first, second, etc. are used to denote names, but not any particular order.

Claims (24)

1. A detecting system for milk multi-index analysis is characterized in that: the system comprises an ultrasonic detection system and a microwave detection system, wherein the ultrasonic detection system and the microwave detection system are arranged in a detection area and are connected with an external control system.
2. A test system for multi-index analysis of milk according to claim 1, wherein: the ultrasonic detection system comprises an ultrasonic transducer, and the ultrasonic transducer detects the liquid to be detected in the ultrasonic test area (11).
3. A test system for multi-index analysis of milk according to claim 2, wherein: the ultrasonic transducer comprises an ultrasonic transducer left side (9) and an ultrasonic transducer right side (13) which are respectively arranged at two ends of the ultrasonic testing area (11).
4. A detection system for milk multi-index analysis according to claim 2 or 3, characterized in that: the ultrasonic transducer is electrically connected with the ultrasonic drive circuit and the analog-digital conversion module (29), and the control processor (28) is electrically connected with the ultrasonic drive circuit and the analog-digital conversion module (29).
5. A test system for multi-index analysis of milk according to claim 2, wherein: the ultrasonic testing area (11) is an ultrasonic testing container, and an ultrasonic testing container liquid inlet (10) and an ultrasonic testing container liquid outlet (12) of the ultrasonic testing container are respectively connected with an ultrasonic testing conveying pipeline (6) and an ultrasonic liquid drainage pipeline (15).
6. A test system for multi-index analysis of milk according to claim 5, characterized in that: one or more temperature sensors I (14) are arranged in the ultrasonic testing area (11), the ultrasonic detection conveying pipeline (6) and/or the ultrasonic liquid discharge pipeline (15).
7. A test system for multi-index analysis of milk according to claim 1, wherein: the microwave detection system comprises a microwave detection chip (21), and the liquid to be detected is detected through a microwave test area (22) of the microwave detection chip (21).
8. A test system for multi-index analysis of milk according to claim 7, wherein: the microwave detection chip (21) comprises a PCB substrate and a double-ring structure single-port SRR arranged on the PCB substrate.
9. A test system for multi-index analysis of milk according to claim 8, wherein: the double-ring structure single-port SRR is composed of an inner ring and an outer ring, the outer ring is a single-opening ring which is opened towards one side of the PCB substrate, the inner ring is a single-opening ring which is arranged in the outer ring, a gap is arranged between the inner ring and the outer ring, and the opening direction of the inner ring is perpendicular to the opening direction of the outer ring.
10. A test system for multi-index analysis of milk according to claim 9, wherein: the microwave test area (22) is a micro-channel and is respectively connected with a microwave liquid inlet pipeline (24) and a microwave liquid outlet pipeline (19). The microwave liquid inlet pipeline (24) is connected with the microwave detection conveying pipeline (5).
11. A test system for multi-index analysis of milk according to claim 10, wherein: one or more temperature sensors II (18) are arranged in the microwave test area (22), the microwave detection conveying pipeline (5), the microwave liquid inlet pipeline (24) and/or the microwave liquid outlet pipeline (19).
12. A test system for multi-index analysis of milk according to claim 8, wherein: the microwave detection system further comprises a microwave detection unit,
the radio frequency connector (23) is connected with the microwave detection chip (21) and receives and transmits a video signal;
a directional coupler (25) extracts the forward and backward microwave signals and transmits them to an amplitude-phase detector;
an amplitude-phase detector (26) that converts the RF signal into a DC voltage signal;
and the microwave signal source (27) is connected with the directional coupler (25) and is connected with the control processor (28).
13. A test system for multi-index analysis of milk according to claim 1, wherein: the liquid to be detected is divided into two paths through a liquid inlet hose (1) through an infusion pump (2), a delivery pipe (3) and a two-way valve (4), and the two paths of liquid respectively enter an ultrasonic detection area and a microwave detection area.
14. A detection system for milk multi-index analysis according to claim 1 or 13, characterized in that: the liquid detected by the ultrasonic detection area and the microwave detection area enters the liquid discharge hose (16) after passing through the pipeline joint (20) until reaching the waste liquid outlet (17).
15. A test system for multi-index analysis of milk according to claim 1, wherein: the control system (31) is connected with the control processor (28), and the control processor (28) performs detection and calculation of the ultrasonic detection system and the microwave detection system.
16. A test system for multi-index analysis of milk according to claim 1, wherein: the ultrasonic detection system and the microwave detection system are characterized by further comprising a shielding constant temperature container (7), and the detection parts of the ultrasonic detection system and the microwave detection system are arranged in the shielding constant temperature container (7).
17. A test system for multi-index analysis of milk according to claim 1 or 16, wherein: the device also comprises a heating mechanism, wherein the heating mechanism is arranged in the shielding constant-temperature container (7) and is used for heating the liquid to be detected of the ultrasonic detection system and the microwave detection system in the shielding constant-temperature container (7).
18. A test system for multi-index analysis of milk according to claim 17, wherein: the heating mechanism is a heating wire (8).
19. A test system for multi-index analysis of milk according to claim 1, wherein: the system also comprises a variable voltage power supply (30), wherein the variable voltage power supply (30) supplies power to the control processor (28).
20. A detection method for milk multi-index analysis comprises the following steps: the liquid to be measured is detected by a microwave and ultrasonic detection system, a microwave detection signal measures the characteristic peak frequency and the characteristic peak S11 value of a microwave spectrum, the ultrasonic detection signal mainly measures the sound velocity and sound attenuation of ultrasonic wave propagation, information of measurement parameters is collected by the system and then transmitted to a control processor (28) for data analysis, and through preliminary data results, the information is respectively selected and brought into a preset model for analysis to complete data processing, so that parameter results required to be measured are obtained, and data are output to obtain detection results.
21. A detection method for milk multi-index analysis according to claim 20, characterized in that: the preset models comprise milk component models and mastitis parameter models.
22. The detecting method for the multi-index analysis of milk according to claim 21, wherein the step of obtaining the model is as follows,
A. respectively preparing a series of standard solutions with different concentrations of each component according to the milk component parameters, and measuring by using a standard method to obtain the standard value of each component of the sample;
B. then, performing instrument detection on the prepared milk standard sample, and inputting a corresponding measurement information value;
C. the modeling of the milk components comprises two parts of microwave measurement information and ultrasonic measurement information;
D. and establishing a multi-parameter linear regression model for the standard value and the measurement parameter of each measurement component of the milk sample by a partial least square method to obtain an analysis model of each component index.
23. The detecting method for the milk multi-index analysis according to claim 22, wherein the microwave measurement information in the step C includes the frequency of the characteristic value and the S11 value, and the ultrasonic measurement information includes sound velocity and sound attenuation.
24. The detecting method for the multi-index analysis of milk according to claim 22,
the correlation correction model of the milk components, the microwave frequency and the microwave attenuation coefficient S11 and the correlation correction model of the ultrasonic sound velocity and the ultrasonic attenuation coefficient is as follows:
Ci=ki+kfif+kSiS+kviv+kαiα
wherein Ci is the mass percentage concentration of the ith milk component; f is the frequency value of the characteristic peak of the milk, unit GHz, S is the value of the characteristic peak S11, unit dB; v is the ultrasonic sound velocity of the measured milk, and the unit is m/s; alpha is the ultrasonic attenuation coefficient of milk, and the unit is dB/cm; ki. kfi, kSi, kvi, and k α i are regression coefficients of the ith milk component measurement model.
CN201910451465.1A 2019-05-28 2019-05-28 Detection system and method for multi-index analysis of milk Pending CN112014461A (en)

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