CN110031437A - A kind of trace level high-accuracy portable dissolved oxygen measuring device based on fluorescence method - Google Patents
A kind of trace level high-accuracy portable dissolved oxygen measuring device based on fluorescence method Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
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Abstract
The invention discloses a kind of trace level high-accuracy portable dissolved oxygen measuring device based on fluorescence method, belongs to dissolved oxygen detection field.The device includes portable housing, storage battery power supply module, power management module, flow cell, high-precision fluorescence measurement probe, fluorescence cap, temperature sensor, optical signal amplification module, photoelectric conversion module, signal conditioning module, current output module, voltage transformation module, pre-amplifying module, A/D conversion module, cpu controller, liquid crystal display, bluetooth module, memory, indicator light, buzzer, control button.Apparatus of the present invention can realize that dissolved oxygen concentration is the high-acruracy survey of 0 ~ 2000ppb Gamma Magnitude, measurement error is 0.5ppb, within 10 minutes measurement period time, the continuous powered operation of battery 48 hours, it is not influenced by disturbing factors such as water sample flow velocity, water pollutants, improves the stability of measuring device.
Description
Technical field
The invention belongs to dissolved oxygen detection technique fields.It is related to a kind of dissolved oxygen measuring device based on fluorescence method, especially
It is a kind of high precision measuring device of measurable micro rank.
Background technique
Water of Power Plants vapour system dissolved oxygen content is the important means for controlling equipment corrosion and scaling and salification.General control
The dissolved oxygen of water supply is less than 7 μ g/L, and the detection of dissolved oxygen concentration is mainly the following method in solution: iodimetric titration, optics point
Analysis method and electrochemical methods etc..In these methods, iodimetric titration is a kind of traditional dissolved oxygen sensing method, but stability
Difference, time-consuming, and program is cumbersome, is unable to satisfy continuous measurement request；Electrochemistry embrane method needs to be replaced frequently diaphragm and electrolyte,
And influenced by impurity such as Sulfide in water, measurement accuracy is not high, and stability is poor, the result that same experimental conditions are first measured
Difference is also larger, therefore, develops that a kind of precision is high, stability is good, easy to operate, cheap, integrated level is high, small in size is convenient for
The detection cell that carries, can be used for real-time detection dissolved oxygen concentration, for promoting dissolved oxygen concentration context of detection to be of great significance.
Fluorescent optical sensor is a kind of high sensitivity, preferably a kind of sensor of stability, is surveyed using the dissolved oxygen of its method
Measuring instrument has preferable repeatability and stability.Currently, the producer of domestic research and development fluorescence method dissolved oxygen instrument is seldom, and product matter
Amount is all undesirable, and domestic many scholars have also carried out some researchs.Such as: Shen Duhai et al. proposes a kind of based on narrowband Internet of Things
The online fluorescence method dissolved oxygen device of net, the narrowband technology of Internet of things by using low-power consumption and the micro process using low-power consumption
Device can be used for a long time using battery power supply, and communication distance mainly solves the problems, such as communication distance, but do not have up to several kilometers
Have measurement accuracy is improved (Shen Duhai, Lin Liteng, a kind of online fluorescence method dissolved oxygen device based on narrowband Internet of Things,
Application number: 201720602395.1)；Liu Fengyan et al. proposes a kind of preparation method of fluorescence method dissolved oxygen sensor diaphragm,
Fluorescence colloidal sol is sprayed on substrate using pyrolytic coating technology, the range and thickness of spraying are controlled, thickness has been obtained
Uniform fluorescence method dissolved oxygen sensor diaphragm, this method only study the diaphragm of dissolved oxygen sensing instrument, can't be straight
Connect using carry out dissolved oxygen sensing (Liu Fengyan, Liu Zhenfeng, Liu Jingjing, Zhao Anjun, a kind of fluorescence method dissolved oxygen sensor diaphragm
Preparation method, application number: 201810875080.3)；Hong Zhen et al. proposes a kind of high-precision dissolved oxygen biography based on fluorescence method
Sensor, provided dissolved oxygen sensor can realize long-term Unattended remote monitoring；Dissolved oxygen is obtained using phase difference calculating
Concentration, but the key parameters such as the measurement accuracy of proposed sensor, response time (Hong Zhen, Li Yan, Pan Xiaoman, one kind are not referred to
High-precision dissolved oxygen sensor based on fluorescence method, application number: 201710653350.1).It is announced in these patent documents
Technical solution provides new approaches for high-accuracy portable dissolved oxygen measuring device, and this patent is different from the above technology, proposes
Dissolved oxygen measuring device can realize concentration be 0~2000ppb Gamma Magnitude high-acruracy survey, measurement error 0.5ppb, survey
It measures within 10 minutes cycle time, the continuous powered operation of battery 48 hours.
Summary of the invention
Technical problem solved by the present invention is providing a kind of trace level dissolved oxygen of high-accuracy portable based on fluorescence method
Measuring device, the device compared to traditional measurement method, overcome traditional dissolved oxygen measuring device can not precise measurement it is micro-
The shortcomings that magnitude other dissolved oxygen content and it can effectively shorten response time of sensor measurement.Not by dirty in water sample flow velocity, water
The influence for contaminating the disturbing factors such as object, improves the stability of measuring device.
To solve the above problems, present invention provide the technical scheme that the device includes portable housing, storage battery power supply
Module, power management module, flow cell, high-precision fluorescence measurement probe, fluorescence cap, temperature sensor, optical signal amplification module,
Photoelectric conversion module, signal conditioning module, current output module, voltage transformation module, pre-amplifying module, A/D conversion module,
Cpu controller, liquid crystal display, bluetooth module, memory, indicator light, buzzer, control button.
The CPU control mainboard is located in shell, and driving circuit, periphery are provided with memory, liquid crystal display
Screen, bluetooth module, power management module, indicator light, buzzer, control button.
The measurement sensor based on fluorescence method includes excitation light source, reference power source, fluorescence cap, and the signal of measurement passes through
It crosses optical signal amplification module, photoelectric conversion module, signal conditioning module, current output module and reaches main control chip.
The fluorescence current signal reaches CPU control by voltage transformation module, pre-amplifying module, A/D conversion module
Device processed.
The trace level high precision measuring device based on fluorescence method is by being mounted on the storage battery power supply of bottom.
The dissolved oxygen measuring device, it can be achieved that dissolved oxygen concentration is the high-acruracy survey of 0~2000ppb Gamma Magnitude,
Measurement error is 0.5ppb, within 10 minutes measurement period time.
The battery is mounted on the bottom of device housing, output voltage 24V, and the continuous powered operation 48 of battery is small
When, without connecing power supply, Portable movable can be carried out.
The high-precision fluorescence measurement probe distal end is by two light emitting diodes (emitting feux rouges and blue light respectively), photoelectricity
Detector and fluorescence cap composition.The fluorescent material of fluorescence cap front end is a kind of special ruthenium metallic compound, fluorescent material coating
Allowing below the polyester paillon that passes through of gas molecule, polyester foil piece upper surface applied one layer of black every luminescent material, to avoid
The interference of other fluorescent materials in daylight and water
The high-precision fluorescence measurement pop one's head in work when, the blue light of modulation shines on fluorescent material, fluorescent material by
Excitation generates red fluorescence.Since " quenching " of oxygen molecule acts on, the fluorescence intensity of excitation and time are related to oxygen concentration；Oxygen
Sub- concentration is higher, and the fluorescence intensity of excitation is lower, and the time of generation is shorter.The feux rouges of excitation detected by photoelectric sensing module,
And be compared with reference optical signal, phase difference is calculated, is compared with internal calibration value, to calculate oxygen molecule concentration, is passed through
Linearisation and temperature-compensating are crossed, 4-20mA current signal is exported
The dissolved oxygen fluorescence method measuring probe is connected in flow cell, and the direct vertical impact probe of water flow should be avoided,
There are buffer runners.
The dissolved oxygen measuring device can carry out signal communication by HART protocol and bluetooth module.
Above-mentioned a kind of trace level high-accuracy portable dissolved oxygen measuring device based on fluorescence method provided by the invention is used
Way is: as a kind of Gamma Magnitude dissolved oxygen measuring device, being widely used in electric field boiler water, brewery's wort fermentation process oxygen consumption
The industrial circles such as amount, ocean water pollution.Overcoming traditional dissolved oxygen measuring device can not accurate measuring trace quantity rank dissolved oxygen
The shortcomings that content and it can effectively shorten response time of sensor measurement.Not by water sample flow velocity, water pollutant etc. interfere because
The influence of element, improves the stability of measuring device.
The present invention has the advantage that compared with prior art:
1) device can based on fluorescence method measurement Gamma Magnitude dissolved oxygen concentration, it can be achieved that dissolved oxygen concentration be 0~
The high-acruracy survey of 2000ppb Gamma Magnitude, measurement error 0.5ppb.
2) the device measurement period time greatly shortened time of measuring within 10 minutes.
3) device is powered using portable storage battery, the continuous powered operation of battery 48 hours, can be into without connecing power supply
Row Portable movable.
4) device is not influenced by disturbing factors such as water sample flow velocity, water pollutants, improves the stability of measuring device.
Detailed description of the invention
Fig. 1 is the structural block diagram of apparatus of the present invention.
Fig. 2 is apparatus of the present invention 4-20mA current input circuit figure.
Fig. 3 is apparatus of the present invention A/D conversion circuit figure.
Fig. 4 is apparatus of the present invention display screen circuit block diagram.
Specific embodiment
In order to which the purpose of the present invention, technical solution, advantage and uniqueness is more clearly understood, with reference to the accompanying drawing,
The present invention will be described in detail.It should be appreciated that described herein, the specific embodiments are only for explaining the present invention, but not
For limiting the present invention.
As shown in Figure 1, for a kind of trace level high-accuracy portable dissolved oxygen measuring device based on fluorescence method of the present invention, it should
Device includes portable housing, storage battery power supply module, power management module, flow cell, high-precision fluorescence measurement probe, fluorescence
Cap, temperature sensor, optical signal amplification module, photoelectric conversion module, signal conditioning module, current output module, voltage conversion
Module, pre-amplifying module, A/D conversion module, cpu controller, liquid crystal display, bluetooth module, memory, indicator light, bee
Ring device, control button.
As shown in Figure 1, being located in shell for the CPU control mainboard, and driving circuit, periphery are provided with storage
Device, liquid crystal display, bluetooth module, power management module, indicator light, buzzer, control button.
It is that 32 RSIC of ARM cortex-M3 framework are mono- as shown in Figure 1, being STM32 for the CPU master chip
Piece machine.With the port enhancing I/O abundant and peripheral resources abundant.Processor control circuit is the minimum based on STM32
System, including reset circuit, crystal oscillator and debugging interface etc..What crystal oscillator was selected is 8MHz without source crystal oscillator, and both ends pass through respectively
The capacity earth of 22pF.
As shown in Figure 1, include excitation light source, reference power source, fluorescence cap for the measurement sensor based on fluorescence method,
The signal of measurement reaches master control core by optical signal amplification module, photoelectric conversion module, signal conditioning module, current output module
Piece.
As shown in Figure 1, being mounted on the bottom of device housing for the battery, output voltage 24V, battery is continuously supplied
Electricity work 48 hours, without connecing power supply, can carry out Portable movable.
As shown in Fig. 2, for the 4-20mA current signal of the fluorescence method dissolved oxygen test output, measurement sensor front end
It is made of two light emitting diodes (emitting feux rouges and blue light respectively), photodetector and fluorescence cap.The fluorescence of fluorescence cap front end
Substance is a kind of special ruthenium metallic compound, and fluorescent material is coated in below the polyester paillon for allowing gas molecule to pass through, and is gathered
Ester paillon upper surface applied one layer of black every luminescent material, to avoid the interference of other fluorescent materials in daylight and water.When work,
The blue light of modulation shines on fluorescent material, and fluorescent material is generated red fluorescence by excitation.Since " quenching " of oxygen molecule acts on,
The fluorescence intensity of excitation and time are related to oxygen concentration；Oxygen molecule concentration is higher, and the fluorescence intensity of excitation is lower, the time of generation
It is shorter.The feux rouges of excitation is detected by photoelectric sensor, and is compared with reference optical signal, and phase difference is calculated, with inside
Calibration value compares, to calculate oxygen molecule concentration, by linearisation and temperature-compensating, exports 4-20mA current signal.
As shown in Fig. 2, being the 4-20mA current signal figure, each channel will be inputted using a switch (SW1)
Circuit switching to activation channel.There is the resistance (R3) of a 150k_ on each channel, it is a part of bandpass filter,
Additional protection is provided to switch SW1 simultaneously.Input is directly connected to current input terminal, to ensure the ADC_IP of AD5700-1
Pin can receive correct voltage level.Need carefully to calculate R1, C3, R6, the combination of R7, to ensure AD5700-1's
The voltage of HART_OUT pin is not less than GND signal under the input signal of 25Hz, 4mA-20mA.
As shown in figure 3, be the device A/D conversion circuit figure, ADS1255 using four-wire system (clock cable SCLK,
Data In-Line DIN, DOL Data Output Line DOUT and chip select line CS) SPI communication modes.ADS1255 can only operate in SPI communication
Under slave pattern, the register of ADS1255 on piece is controlled by master controller, these registers are read or write by serial ports.Serial ports
It is low level that CS must be kept when communication.In SPI transmit process, data are synchronously sent and received, SCLK and DIN,
DOUT synchronizing moving, SCLK signal keep completely to avoid loss of data .DIN combination SCLK for sending number to ADS1255
According to effective in the failing edge of SCLK；DOUT combination SCLK is used to read data from ADS1255, effective in the rising edge of SCLK.
DIN and DOUT is connected by a bidirectional signal line with master controller.
As shown in figure 4, being the device display screen circuit block diagram, including LCD module and display subsystem.By LCD's
SEG (segment electrode) and COM (public electrode) with the SEG of HT1621 is corresponding with COM is connected.HT1621 has with lower interface and monolithic
The I/O mouth of machine is connected: wherein (CS) is chip selection signal, and WR is write operation, and RD is read operation, and DATA is data bit.Pass through software
Program controls and then controls the read-write operation of HT1621 to I/O.
It should be understood that for those of ordinary skills, it can be modified or changed according to the above description,
And all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (6)
1. a kind of trace level high-accuracy portable dissolved oxygen measuring device based on fluorescence method, it is characterised in that: including portable
Shell, storage battery power supply module, power management module, flow cell, high-precision fluorescence measurement probe, fluorescence cap, temperature sensor,
Optical signal amplification module, photoelectric conversion module, signal conditioning module, current output module, voltage transformation module, preposition amplification mould
Block, A/D conversion module, cpu controller, liquid crystal display, bluetooth module, memory, indicator light, buzzer, control button.
The CPU control mainboard is located in shell, and driving circuit, periphery are provided with memory, liquid crystal display, indigo plant
Tooth module, power management module, indicator light, buzzer, control button；
The measurement sensor based on fluorescence method includes excitation light source, reference power source, fluorescence cap, and the signal of measurement passes through light
Signal amplification module, photoelectric conversion module, signal conditioning module, current output module reach main control chip；
The fluorescence current signal reaches cpu controller by voltage transformation module, pre-amplifying module, A/D conversion module；
The trace level high precision measuring device based on fluorescence method is by being mounted on the storage battery power supply of bottom.
2. dissolved oxygen measuring device according to claim 1 is, it can be achieved that dissolved oxygen concentration is 0~2000ppb Gamma Magnitude
High-acruracy survey, measurement error 0.5ppb, within 10 minutes measurement period time.
3. battery according to claim 1 is mounted on the bottom of device housing, output voltage 24V, battery is continuously supplied
Electricity work 48 hours, without connecing power supply, can carry out Portable movable.
4. high-precision fluorescence measurement probe distal end according to claim 1 (emits feux rouges by two light emitting diodes respectively
And blue light), photodetector and fluorescence cap composition.The fluorescent material of fluorescence cap front end is a kind of special ruthenium metallic compound,
Fluorescent material is coated in below the polyester paillon for allowing gas molecule to pass through, polyester foil piece upper surface applied one layer of black every light
Material, to avoid the interference of other fluorescent materials in daylight and water.
5. the blue light of modulation shines on fluorescent material, glimmering when high-precision fluorescence measurement probe work according to claim 1
Stimulative substance is generated red fluorescence by excitation.Since " quenching " of oxygen molecule acts on, the fluorescence intensity of excitation and time and oxygen are dense
Degree is related；Oxygen molecule concentration is higher, and the fluorescence intensity of excitation is lower, and the time of generation is shorter.The feux rouges of excitation is by photoelectric sensing
Module detects, and is compared with reference optical signal, calculates phase difference, compares with internal calibration value, to calculate oxygen
Molecular concentration exports 4-20mA current signal by linearisation and temperature-compensating.
6. dissolved oxygen measuring device according to claim 1 can carry out signal communication by HART protocol and bluetooth module.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111537487A (en) * | 2020-05-25 | 2020-08-14 | 清华大学 | Temperature compensation method and device of optical oxygen sensor |
| CN113514431A (en) * | 2021-04-06 | 2021-10-19 | 中国农业大学 | Dissolved oxygen measuring method and device |
| CN114307903A (en) * | 2022-01-11 | 2022-04-12 | 深圳市刚竹医疗科技有限公司 | System circuit of double-channel QPCR instrument |
| CN114486828A (en) * | 2022-01-19 | 2022-05-13 | 安徽清大云博环保科技有限公司 | Dissolved oxygen analyzer capable of rapidly measuring |
| CN117723527A (en) * | 2024-02-08 | 2024-03-19 | 杭州柔谷科技有限公司 | Optimized control method of oxygen partial pressure sensor, electronic equipment and storage medium |
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Application publication date: 20190719 |