CN110542667B - Portable rapid water quality detector and water quality detection method - Google Patents
Portable rapid water quality detector and water quality detection method Download PDFInfo
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Abstract
The invention discloses a portable rapid water quality detector and a water quality detection method, and belongs to the technical field of water quality analysis and detection. The LED light source and detection assembly comprises a four-way light cuvette, an LED light source intensity detection module, an ultraviolet absorption light intensity detection module and a fluorescence light intensity detection module; the LED light source is used for emitting ultraviolet light to the four-way light cuvette, and the ultraviolet absorption light intensity detection module is used for detecting the light intensity of the ultraviolet light which is not absorbed after passing through the four-way light cuvette; the fluorescence intensity detection module is used for detecting the fluorescence intensity excited by the liquid to be detected in the four-way light cuvette; the LED light source intensity detection module is arranged between the LED light source and the corresponding light transmission surface and is used for detecting the light intensity of ultraviolet light emitted by the LED light source in real time; the portable rapid water quality detector provided by the invention can be used after being started, and the water quality detection by using the device can more accurately reflect the composition of substances contained in the liquid to be detected.
Description
Technical Field
The invention belongs to the technical field of water quality analysis and detection, and particularly relates to a portable rapid water quality detector and a water quality detection method, which can rapidly detect natural organic matters and aromatic artificially synthesized compounds dissolved in water.
Background
The soluble organic matters comprise macromolecular polysaccharide and protein substances, humus with medium molecular weight, fulvic acid and building block type small molecular substances, and are widely existing in various natural water bodies, sewage and drinking water. Methods for analytically detecting the concentration level of soluble organics mainly include chemical methods and spectroscopic methods. The indexes of chemical oxygen demand, total organic carbon and the like are chemical method indexes reflecting the concentration of the soluble organic matters, and the concentration of the total organic carbon of the soluble organic matters in the city tap water taking the Yangtze river as a water source is between 1mg/L and 3 mg/L. The spectrometry mainly comprises an ultraviolet-visible absorbance method and a fluorescence spectrometry, and compared with a chemical method, the spectrometry does not need chemical reagents and has the advantages of sensitivity, rapidness, easiness in operation and the like.
The ultraviolet absorption method mainly utilizes the strong ultraviolet absorption of aromatic compounds in the wavelength range of 240nm to 300nm, so that macromolecular proteins, humic acid, fulvic acid and some compounds containing benzene ring structures in water can be detected by the ultraviolet absorbance method. The fluorescence of the soluble organic matters mainly comprises protein fluorescence, humus fluorescence, chlorophyll and other pigment fluorescence. The emission wavelength range of the protein fluorescence is 310nm to 360nm; the emission wavelength range of the humus fluorescence is 400-500nm; the peak wavelength of chlorophyll fluorescence is about 685 nm. The protein fluorescent signal is mainly used for detecting substances containing phenol or aniline structures in water and comprises macromolecular proteins, humus, fulvic acid, tryptophan and tyrosine and some small molecular compounds containing phenol or aniline structures; humic substances fluorescence mainly detects substances containing polycyclic aromatic structures such as humic acid, fulvic acid, naphthol, naphthylamine, quinine, pterin and the like in water.
In recent years, river growth, intelligent water service, construction of a distributed water treatment facility, a cooling circulating water system of a building, a market after installation and maintenance of a water purifier and the like all generate great demands on handheld equipment for rapidly testing soluble organic matters, however, the existing ultraviolet absorption or fluorescence spectrometry equipment mainly adopts a xenon lamp or mercury lamp light source and has the defects of large volume, complex optical structure, high power consumption, high cost and the like. The LED has the advantages of small volume, low power consumption, low cost, good monochromaticity, low operation voltage, high-speed frequent switching and the like, and has great application value in the field of portable water quality detection. The existing hand-held rapid water quality analyzer mainly adopts a light-emitting diode (LED) with visible light wavelength (wavelength range is 380-780 nm) to detect indexes such as residual chlorine in water by combining a specific chemical reagent, and a deep ultraviolet LED light source with wavelength below 300nm is needed for detecting soluble organic matters. For example, chinese patent publication No. CN206177817U, publication No. 2017-05-17 discloses a portable hand-held water quality rapid detection device, which emits ultraviolet light through an emitting tube to excite soluble organic matters in water to generate fluorescence, however, the application of the utility model does not define whether the emitting tube is a light emitting diode LED, and similarly, only a fluorescence detection method is used.
Based on the above factors, chinese patent publication No. CN104198391B, publication No. 2017-02-15, discloses an ultraviolet fluorescent double-signal water quality detection device using an LED as a light source and an application method thereof, wherein the device consists of a sample collecting part and a detection part. The method comprises the steps of selecting a deep ultraviolet LED lamp light source and a photoelectric detector component with specific wavelengths according to a three-dimensional fluorescence spectrum, detecting fluorescence intensity and ultraviolet absorption with specific wavelengths simultaneously, and calculating the ratio between the fluorescence intensity and the corresponding ultraviolet absorption. The invention has no consumption of chemical reagent, can realize the detection of the total concentration change of the soluble organic matters in the water body, can reflect the change of the concentration of fluorescent components such as proteins or humus, and provides an online detection device. The invention discloses an ultraviolet fluorescence three-signal water quality sensor and application thereof, wherein the publication number is CN105181667B, and the publication date is 2017-10-17, and the ultraviolet fluorescence three-signal water quality sensor comprises a light path part and a signal control processing part, wherein the light path part comprises 1 UV LED, a sample cell, an ultraviolet detector, a fluorescence detector A and a fluorescence detector B; the signal control processing part comprises a power supply module, a signal amplifier A, a signal amplifier B, a signal amplifier C, an analog-to-digital converter and a microprocessor. The method has the advantages of no consumption of chemical reagents, capability of realizing real-time detection of the total concentration change of the soluble organic matters in the water body, capability of reflecting the real-time change of the concentration of fluorescent components such as proteins or humus and the like, and capability of being used for on-line prediction of the disinfection by-product generation potential and the degradation degree of micro pollutants in the advanced oxidation process. However, in the two applications, a single ultraviolet LED is used as a light source, and an ultraviolet method and a fluorescence method are adopted to simultaneously measure ultraviolet absorbance values and protein or humus fluorescence signals so as to realize the detection of the concentration of soluble organic matters in water; therefore, there is a problem that, firstly, the intensity of the deep ultraviolet LED light source has a large fluctuation, the light intensity is attenuated by about 1% after the light source is continuously turned on for 10 seconds, the light intensity is attenuated by about 5% after the light source is continuously turned on for 5 minutes, and secondly, the light source can keep a certain degree of relative stability after ten minutes of heat engine is needed, but the accuracy and the rapidity of the whole instrument in spectrum detection generally need to be improved.
Disclosure of Invention
1. Problems to be solved
Aiming at the problems of low accuracy and low detection speed in the existing water quality detection device and the water quality detection process, one of the purposes of the invention is to provide a portable rapid water quality detector, which is added with a light source intensity detection module, does not need to start up and preheat, and can simultaneously improve the detection speed and the accuracy of detection results;
The second objective of the present invention is to provide a method for rapidly detecting soluble organic matters in water, which adds a correction calculation step of light source signals, and effectively corrects the light source signals to eliminate internal masking effects.
2. Technical proposal
In order to solve the problems, the technical scheme adopted by the invention is as follows:
The portable rapid water quality detector comprises a handheld shell, wherein an LED light source and a detection assembly are arranged in the handheld shell, and the detection assembly comprises a four-way light cuvette with four light transmission surfaces, an LED light source intensity detection module, an ultraviolet absorption light intensity detection module and a fluorescence light intensity detection module; the LED light source, the ultraviolet absorption light intensity detection module and the fluorescent light intensity detection module are arranged on the periphery of the four-way light cuvette in a surrounding manner and respectively correspond to different light transmission surfaces; the ultraviolet absorption light intensity detection module is arranged at the relative position of the LED light source (namely, the light transmission surface corresponding to the LED light source and the light transmission surface corresponding to the ultraviolet absorption light intensity detection module are two opposite light transmission surfaces of the four-way cuvette) and used for detecting the light intensity of the un-absorbed ultraviolet light after passing through the four-way cuvette, and the fluorescent light intensity detection module is arranged at one side of the four-way cuvette (the light transmission surface corresponding to the fluorescent light intensity detection module and the light transmission surface corresponding to the LED light source are two adjacent light transmission surfaces of the four-way cuvette) and used for detecting the fluorescent light intensity in the four-way cuvette;
The LED light source intensity detection module is arranged on one side of the LED light source and used for detecting the light intensity of ultraviolet light emitted by the LED light source in real time.
Preferably, the LED light source is a deep ultraviolet light emitting diode LED light source, the central wavelength range of which is 250-300 nm, more preferably 265-285 nm, and most preferably 275nm.
Preferably, the LED light source intensity detection module is composed of a gallium nitride-based ultraviolet photodiode (the gallium nitride-based ultraviolet photodiode is manufactured by Zhenjiang gallium core photoelectric limited company, and has a specification of TO-46 package) and an operational amplifier circuit, wherein a feedback resistor in the operational amplifier circuit adopts an M omega-level resistance resistor.
Preferably, the ultraviolet absorption light intensity detection module is composed of a gallium nitride-based ultraviolet photodiode (the gallium nitride-based ultraviolet photodiode is produced by Zhenjiang gallium core photoelectric limited company, the specification is TO-46 package) or a silicon-based photodiode and an operational amplifier circuit, and a k omega-level resistance is adopted as a feedback resistor in the operational amplifier circuit.
Preferably, the fluorescent light intensity detection module comprises a first fluorescent light intensity detection module and a second fluorescent light intensity detection module which are respectively arranged at two sides of the four-way light cuvette.
Preferably, the transmission wavelength range of the bandpass filter of the first fluorescent light intensity detection module is 325-360 nm; the transmission wavelength range of the band-pass filter of the second fluorescent light intensity detection module is 400-480 nm, and the cut-off rate of the band-pass filter on light outside the band-pass wavelength range is higher than 99.9%;
Specifically, the fluorescence intensity detection module consists of a band-pass filter, a silicon-based photodiode and an operational amplifier circuit, wherein the band-pass filter is tightly attached to the surface of the silicon-based photodiode, and the band-pass filter and the silicon-based photodiode are packaged into a whole by adopting a round hollow metal cap; the operational amplifier circuit converts a current signal into a voltage signal in a transimpedance operational amplifier mode, and noise signal interference is eliminated through the low-pass filter circuit.
Preferably, an electronic control system is further arranged in the handheld housing of the portable rapid water quality detector, and the electronic control system comprises a main board circuit and a power supply;
The main board circuit is provided with a singlechip, a wireless communication module and a USB interface; the singlechip is used for receiving voltage signals generated by the LED light source intensity detection module, the ultraviolet absorption light intensity detection module and the fluorescent light intensity detection module, converting the voltage signals into digital signals for storage (storing the digital signals on a memory of the singlechip), and outputting the digital signals to the upper computer by connecting the USB interface with an interface of the upper computer (such as a mobile phone/a computer) through a data line/transmitting the digital signals to the upper computer through a wireless communication module;
the singlechip controls the LED light source to work in a constant-brightness or stroboscopic mode through the constant-current driving circuit;
the power supply is of a type capable of being repeatedly charged and discharged, such as a storage battery, a lithium battery and the like, and is connected with the USB interface by a data line for charging.
Preferably, the electronic control system further comprises a display screen and keys; the display screen is connected with the singlechip through a circuit and receives and displays digital signals output by the singlechip in real time; the key is connected with the singlechip through a circuit and used for controlling the working state and parameter input of the water quality detector;
the display screen is located in the middle of the handheld shell, and the keys comprise a power key, a zero calibration key, a reading key, a return key and a setting key, wherein each key is located in a key area at the rear of the handheld shell.
Preferably, the front part of the handheld shell is an optical test area, a shading cassette is formed inside the handheld shell, and the LED light source and the detection assembly are positioned in the shading cassette; interference of sunlight on fluorescent signal detection can be avoided.
Preferably, the hand-held shell is provided with a switchable flip cover at a position corresponding to the four-way light cuvette; the four-way light cuvette is convenient to take and place.
The method for detecting the water quality by using the portable rapid water quality detector comprises the following specific steps:
(1) Pressing a power button and starting a water quality detector;
(2) Opening a flip cover, putting a cuvette containing ultrapure water into a water quality detector, covering the flip cover, pressing a zero calibration key, wherein the value measured by an ultraviolet absorption light intensity detection module is I 0, the value measured by an LED light source intensity detection module is L 0, and the values measured by two fluorescent signal detection modules are A 0 and B 0 respectively;
(3) Opening a flip cover, taking a cuvette containing tryptophan water solution with the concentration of N 0, wherein N 0 is preferably 100 mug/L (in the specific embodiment part, the schematic description is made by taking N 0 as an example, the concentration is 100 mug/L), putting fluorescent signal calibration liquid serving as a fluorescent light intensity detection module A into a water quality detector, covering the flip cover, pressing a calibration key, and measuring the value A 1 by the fluorescent light intensity detection module A; calculating a calibration coefficient for the k A signal according to a formula k A＝(A1-A0)/N0;
Opening a flip cover, placing a quinine sulfate aqueous solution with the concentration of M 0, wherein M 0 is preferably 100 mug/L (in the specific embodiment part, M 0 is taken as an example to make a schematic description), taking a fluorescent signal calibration solution of a fluorescent light intensity detection module B as an example, into a water quality detector, covering the flip cover, pressing a calibration key, taking the value measured by the fluorescent light intensity detection module B as B 1, and calculating a signal calibration coefficient as k B according to a formula k B＝(B1-B0)/M0;
(4) Opening a flip cover, putting a cuvette containing a water sample to be detected into a water quality detector, covering the flip cover, pressing a reading key, wherein the value measured by an ultraviolet absorption light intensity detection module is I s, the value measured by an LED light source intensity detection module is L s, and the values measured by a fluorescent light intensity detection module A and a fluorescent light intensity detection module B are A s、Bs respectively; the display screen displays four measurement values, wherein
The light intensity signal L is expressed as a unit of percent, and the calculation formula is L= (L s/L0);
The ultraviolet absorbance UVA is expressed in cm -1 and the formula is uva=log (I s/I0)+log(Ls/L0);
log (L s/L0) is a correction term for the change in ultraviolet absorbance caused by the change in light intensity;
The unit of the fluorescence signal F A is a free dimension unit, the equivalent concentration is the concentration of the corresponding fluorescence calibration liquid, the calculation formula is F A＝(As-A0)/kA*10(0.5*UVA);kA which is a fluorescence equivalent concentration calibration coefficient, and 10 (0.5*UVA) which is an internal covering calibration item;
The unit of the fluorescence signal F B is a free dimension unit, the equivalent concentration is the concentration of the corresponding fluorescence calibration liquid, the calculation formula is F B＝(Bs-B0)/kB*10(0.5*UVA),kB which is a fluorescence equivalent concentration calibration coefficient, and 10 (0.5*UVA) which is an internal covering calibration item;
(5) And (5) repeating the step (4) to continue testing other water samples.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
(1) The portable rapid water quality detector provided by the invention is provided with the LED light source intensity detection module, the ultraviolet absorption light intensity detection module and the fluorescent light intensity detection module, so that the relatively broad spectrum of ultraviolet signals and the selectivity and sensitivity of fluorescent signals can be comprehensively utilized, more water quality information about soluble organic matters can be reflected, and the portable rapid water quality detector is suitable for various water samples;
The LED light source emits ultraviolet light to the four-way light cuvette, excites two signals of protein fluorescence and humus fluorescence generated by liquid to be detected in the four-way light cuvette, detects the fluorescence intensity of excited pre-detection wavelength by utilizing the fluorescence intensity detection module, and detects the light intensity of ultraviolet light which is not absorbed after passing through the four-way light cuvette by utilizing the ultraviolet absorption light intensity detection module to obtain corresponding ultraviolet absorbance signals; meanwhile, the LED light source intensity detection module can be used for detecting the light intensity of ultraviolet light emitted by the LED light source in real time, and correcting the detected ultraviolet absorbance signal according to the light intensity, so that the influence of light source intensity measurement errors can be weakened to the maximum extent, the component information of soluble organic matters in the water body to be detected can be acquired more truly and accurately, and the sensitivity is high;
in addition, because the LED light source intensity detection module can be used for detecting the light intensity of ultraviolet light emitted by the LED light source in real time, the water quality detector can be directly measured after being started, the time consumed by starting up and preheating operation is saved, and the water quality detector is convenient and quick and high in efficiency.
(2) According to the method for carrying out water quality detection by using the portable rapid water quality detector provided by the invention, the ultraviolet absorbance UVA is obtained by calculating the numerical value measured by the LED light source intensity detection module and the numerical value measured by the ultraviolet absorption light intensity detection module, wherein the change of the ultraviolet absorbance caused by the light intensity change can be effectively corrected by adding the LED light source intensity detection numerical value, so that the most practical ultraviolet absorbance UVA is obtained;
the fluorescence signal can be corrected for internal masking effect according to the ultraviolet absorbance signal, so that the fluorescence signal can still keep linearity in a higher concentration range (ultraviolet absorbance is more than 0.10cm -1), and the most accurate fluorescence signal is obtained.
Drawings
FIG. 1 is a hand-held housing of a portable rapid water quality detector provided by the present invention;
FIG. 2 is a schematic diagram showing the layout of an LED light source and a detection assembly of the portable rapid water quality detector provided by the invention;
FIG. 3 is a schematic perspective view of an LED light source and a detection assembly of the portable rapid water quality detector provided by the invention;
FIG. 4 is a linear regression fit of humus fluorescence signals to International humus Association standards SRNOM concentrations;
FIG. 5 is a linear regression fit of protein fluorescent signal to tryptophan concentration;
FIG. 6 linear regression fit of UV absorbance UVA280 signal to International humus Association standards SRNOM concentration;
In the figure: 1. a hand-held housing; 2. a display screen; 3. a key region; 301. a key; 4. a flip cover; 5. an LED light source; 6. a four-way light cuvette; 601. a first light-transmitting surface; 602. a second light-transmitting surface; 603. a light-transmitting surface III; 604. a light-transmitting surface IV; 7. an ultraviolet absorption light intensity detection module; 8. a fluorescent light intensity detection module; 801. a first fluorescent light intensity detection module; 802. a second fluorescent light intensity detection module; 9. the LED light source intensity detection module; 10. a light shielding cassette.
Detailed Description
It should be noted that, when an element is referred to as being "mounted" on/disposed on "another element, it can be directly on the other element or two elements may be directly integrated; when an element is referred to as being "connected" to another element, it can be directly connected to the other element or be directly integrated with the two elements. Also, the terms such as "upper", "lower", "left", "right", "front", "rear", "middle", "first", "second", "third", "fourth", etc. are used herein for descriptive purposes only and are not intended to limit the scope of the invention, which may be otherwise and may be embodied without substantial modification to the technical context.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs; the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The invention is further described below in connection with specific embodiments.
Example 1
The portable rapid water quality detector provided by the invention has the overall appearance shown in fig. 1, and is provided with a handheld shell 1, wherein the front part in the handheld shell 1 is provided with an optical test area, and the rear part of the optical test area is provided with an electronic control system, and as shown in fig. 2 and 3, the optical test area is internally provided with an LED light source 5 and a detection component, and the detection component comprises a four-way light cuvette 6 with four light transmission surfaces, an LED light source intensity detection module 9, an ultraviolet absorption light intensity detection module 7 and a fluorescent light intensity detection module 8; the LED light source 5, the ultraviolet absorption light intensity detection module 7 and the fluorescent light intensity detection module 8 are arranged around the periphery of the four-way light cuvette 6 and correspond to different light transmission surfaces respectively, specifically, the LED light source 5 corresponds to a first light transmission surface 601, the ultraviolet absorption light intensity detection module corresponds to a third light transmission surface 603, the fluorescent light intensity detection module 8 corresponds to a second light transmission surface 602 and/or a fourth light transmission surface 604 which are adjacent to the first light transmission surface 601, the first light transmission surface 601 and the third light transmission surface 603 are two opposite light transmission surfaces of the four-way light cuvette 6, and the second light transmission surface 602 and the fourth light transmission surface 604 are other two opposite light transmission surfaces of the four-way light cuvette 6; the LED light source 5 is used for emitting ultraviolet light to the four-way light cuvette 6, the ultraviolet absorption light intensity detection module 7 is used for detecting the light intensity of the ultraviolet light which is not absorbed after passing through the four-way light cuvette 6, and the fluorescent light intensity detection module 8 is used for detecting the fluorescent light intensity of the pre-detection wavelength which is excited by the liquid to be detected and passes through the four-way light cuvette 5; the LED light source intensity detection module 9 is disposed between the LED light source 5 and the first light-transmitting surface 601, and is configured to detect the light intensity of the ultraviolet light emitted by the LED light source in real time. The four-way light cuvette 6, the LED light source intensity detection module 9, the ultraviolet absorption light intensity detection module 7 and the fluorescent light intensity detection module 8 are all arranged inside a shading cassette 10 in an optical test area, and the hand-held shell 1 is provided with a switchable flip cover 4 at a place corresponding to the place where the four-way light cuvette 5 is arranged.
The electronic control system comprises the display screen 2, and in addition, the electronic control system comprises a key 301, a main board circuit and a power supply connected with the main board circuit and the singlechip through a circuit, wherein the singlechip, a wireless communication module, a USB interface and a miniature buzzer are arranged on the main board circuit; the singlechip is used for receiving voltage signals generated by the LED light source intensity detection module 9, the ultraviolet absorption light intensity detection module 7 and the fluorescent light intensity detection module 8, converting the voltage signals into digital signals to be stored (stored on a memory of the singlechip), and outputting the digital signals to the host computer through a USB interface by utilizing the connection of a data line and the host computer (such as a mobile phone/a computer) interface, or transmitting the digital signals to the host computer through a wireless communication module (the wireless communication module used in the specific embodiment is a CC2530 chip of TI company, which is a 2.4-GHz short-distance wireless communication chip based on IEEE 802.15.4 standard); in addition, the singlechip controls the LED light source to work in a constant-brightness or stroboscopic mode through the constant-current driving circuit; the power supply supplies power to an electronic control system and an LED light source of the whole water quality detector, the display screen 2 is connected with the singlechip through a circuit, receives and displays digital signals output by the singlechip in real time, and the key 301 is connected with the singlechip through the circuit and is used for controlling the working state of the water quality detector and/or inputting parameters; the micro buzzer is connected with the singlechip through a circuit, and the singlechip controls the micro buzzer to sound for state prompt when the key is pressed or the test is completed.
The LED light source 5 is a deep ultraviolet light emitting diode LED light source (manufactured by Qingdao Jiesh electric Co., ltd., specification is TO-39 package, light emission angle is 7 °), of course, the LED light source 5 having a wavelength appropriately selected within the center wavelength range of 250 TO 300nm, for example, the LED light source 5 having a wavelength range of 265 TO 285nm, or the LED light source 5 having a wavelength of 275nm may be arbitrarily selected.
The LED light source intensity detection module 9 is composed of a gallium nitride-based ultraviolet photodiode (the gallium nitride-based ultraviolet photodiode is manufactured by Zhenjiang gallium core photoelectric limited company, and has the specification of TO-46 package) and an operational amplifier circuit, wherein a feedback resistor in the operational amplifier circuit adopts an MΩ -level resistance resistor.
The ultraviolet absorption light intensity detection module 7 can be composed of a gallium nitride-based ultraviolet photodiode (the gallium nitride-based ultraviolet photodiode is produced by Zhenjiang gallium core photoelectric limited company, the specification is TO-46 package) and an operational amplifier circuit, and also can be composed of a silicon-based photodiode (a high-quality silicon photodiode provided by Beijing-based phototechnology limited company; model 1.5mm UVC photodiode) and an operational amplifier circuit, wherein feedback resistors in the operational amplifier circuit are k omega-level resistance resistors.
The fluorescence intensity detection module 8 consists of a band-pass filter, a silicon-based photodiode (high-quality silicon photodiode provided by Beijing-sensitive optical technology Co., ltd.; model 1.5mm UVC photodiode) and an operational amplifier circuit, wherein the band-pass filter is tightly attached to the surface of the silicon-based photodiode, and the band-pass filter and the silicon-based photodiode are packaged into a whole by adopting a round hollow metal cap; the operational amplifier circuit converts a current signal into a voltage signal in a transimpedance operational amplifier mode, and noise signal interference is eliminated through the low-pass filter circuit.
As shown in fig. 2 and 3, the fluorescent light intensity detection module 8 includes a first fluorescent light intensity detection module 801 and a second fluorescent light intensity detection module 802 that are respectively arranged on two sides of the four-way cuvette, one of the two detection modules corresponds to the second light transmitting surface 602, and the other detection module corresponds to the fourth light transmitting surface 604. Wherein, the transmission wavelength range of the band-pass filter of the fluorescent light intensity detection module I801 is 325-360 nm; the transmission wavelength range of the band-pass filter of the second fluorescent light intensity detection module 802 is 400-480 nm, and the cut-off rate of the band-pass filter to light outside the band-pass wavelength range is higher than 99.9%.
The singlechip of the electronic control system is an existing singlechip (Single-Chip Microcomputer), is an integrated circuit chip, and is a small and perfect microcomputer system formed by integrating functions (possibly including a display driving circuit, a pulse width modulation circuit, an analog multiplexer, an A/D converter and the like) such as a central processing unit CPU, a random access memory RAM, a read-only memory ROM, a plurality of I/O ports, an interrupt system, a timer/counter and the like with data processing capacity on a piece of silicon wafer by adopting a very large scale integrated circuit technology; the power source may be a battery or lithium battery, as long as it can be repeatedly charged by connecting a data line to the USB interface. The keys 310 in the key section 3 include a power key, a zero calibration key, a reading key, a back key, and a set key.
The operation principle of the portable rapid water quality detector for water quality detection is as follows:
Pressing a power button and starting a water quality detector; the power supply supplies power to the whole water quality detector (an electronic control system, an LED light source 5 and detection components), the singlechip controls the LED light source 5 to emit ultraviolet light towards the four-way cuvette 6 in a constant-brightness or stroboscopic mode through a circuit, meanwhile, an LED light source intensity detection module 9 starts to detect the intensity of the ultraviolet light emitted by the LED light source 5, a part of the ultraviolet light emitted by the LED light source 5 is absorbed by soluble organic matters in liquid to be detected in the four-way cuvette 6 and generates fluorescence, and the fluorescence is detected 8 by a fluorescence light intensity detection module positioned on the side surface of the four-way cuvette 6; a part of ultraviolet light passes through the four-way cuvette 6 and is detected by an ultraviolet absorption light intensity detection module 7 opposite to the LED light source, and a small part of ultraviolet light is detected by an LED light source intensity detection module 9 arranged on the side face;
the ultraviolet absorption light intensity detection module 7, the fluorescent light intensity detection module 8 and the LED light source intensity detection module 9 transmit detection data thereof to the singlechip in the form of analog voltage, the singlechip converts the received detection data into digital data and stores the digital data in a memory of the singlechip, and meanwhile, the digital data are transmitted to the display screen 2 through a circuit, the detection result is displayed on the display screen 2, in addition, the digital signal obtained by converting the singlechip is transmitted to the upper computer through a USB interface of the water quality detector by utilizing a data line to be connected with the upper computer (such as a mobile phone/a computer); or the digital signal obtained by the conversion of the singlechip is transmitted to the upper computer through the wireless connection between the wireless communication module and the upper computer;
The steps of carrying out water quality detection on the water samples 1 and 2 to be detected by using the portable rapid water quality detector are as follows:
(1) Pressing a power button and starting a water quality detector; if the parameters are required to be set, pressing a setting key to set the parameters;
(2) Opening the flip cover 4, putting a cuvette containing ultrapure water into a water quality detector, covering the flip cover 4, pressing a zero calibration key, wherein the value measured by the ultraviolet absorption light intensity detection module 7 is I 0, the value measured by the LED light source intensity detection module 9 is L 0, and the values measured by the fluorescent signal detection module I801 and the fluorescent signal detection module II 802 are A 0 and B 0 respectively;
(3) Opening the flip cover 4, taking a four-way light cuvette 6 containing tryptophan water solution with the concentration of 100 mug/L, putting the four-way light cuvette 6 serving as fluorescent signal calibration liquid of the fluorescent light intensity detection module I801 into a water quality detector, covering the flip cover 4, and pressing a calibration key, wherein the value measured by the fluorescent light intensity detection module I801 is A 1; calculating a calibration coefficient for the k A signal according to the formula k A＝(A1-A0)/100;
Opening the flip cover 4, putting a quinine sulfate aqueous solution with the concentration of 100 mug/L into a water quality detector as a fluorescent signal calibration solution of the fluorescent light intensity detection module II 802, covering the flip cover 4, pressing a calibration key, and calculating a k B signal calibration coefficient according to a formula k B＝(B1-B0)/100, wherein the measured value of the fluorescent light intensity detection module II 802 is B 1;
(4) Opening the flip 4, putting the four-way cuvette 6 containing the water sample 1 to be detected into a water quality detector, covering the flip, pressing a reading key, wherein the value measured by the ultraviolet absorption light intensity detection module 7 is I s, the value measured by the LED light source intensity detection module 9 is L s, and the values measured by the fluorescent light intensity detection module I801 and the fluorescent light intensity detection module II 802 are A s、Bs respectively; the display screen 2 displays four measured values, of which,
The light intensity signal L is expressed as a unit of percent, and the calculation formula is L= (L s/L0);
The ultraviolet absorbance UVA is expressed in cm -1 and the formula is uva=log (I s/I0)+log(Ls/L0);
log (L s/L0) is a correction term for the change in ultraviolet absorbance caused by the change in light intensity;
The unit of the fluorescence signal F A is a free dimension unit, the equivalent concentration is the concentration of the corresponding fluorescence calibration liquid, the calculation formula is F A＝(As-A0)/kA*10(0.5*UVA);kA which is a fluorescence equivalent concentration calibration coefficient, and 10 (0.5*UVA) which is an internal covering calibration item;
The unit of the fluorescence signal F B is a free dimension unit, the equivalent concentration is the concentration of the corresponding fluorescence calibration liquid, the calculation formula is F B＝(Bs-B0)/kB*10(0.5*UVA),kB which is a fluorescence equivalent concentration calibration coefficient, and 10 (0.5*UVA) which is an internal covering calibration item;
(5) And (4) pressing a return key, and repeating the step (4) to continue the test of the water sample 2 to be tested.
The specific detection results obtained are shown in table 1.
Table 1 detection results of water quality detection of water sample to be detected by using the portable rapid water quality detector provided in this embodiment
In addition, a series of concentration gradient international humus standard substances SRNOM and tryptophan are detected according to the method, the obtained linear regression curves of ultraviolet absorbance signals, fluorescence signal values and standard test solution concentrations are shown in fig. 4 (humus fluorescence), fig. 5 (protein fluorescence) and fig. 6 (ultraviolet absorbance UVA 280), and the linear fitting degree is more than 0.998, so that the method has good accuracy; the lower detection limit of the fluorescence method is as low as 20ppb, and the sensitivity is high.
Comparative example 1
The portable rapid water quality tester of this comparative example is basically the same as that of example 1, except that there is no LED light source intensity detection module 4;
the portable rapid water quality detector provided in example 1 and this comparative example was used to perform water quality detection on the water sample 3 to be detected, and the steps of performing water quality detection on the water sample 3 to be detected using the portable rapid water quality detector provided in this comparative example were as follows: (1) pressing a power key to start a water quality detector; if the parameters are required to be set, pressing a setting key to set the parameters;
(2) Opening a flip cover, putting a cuvette containing ultrapure water into a water quality detector, covering the flip cover, pressing a zero calibration key, wherein the value measured by the ultraviolet absorption light intensity detection module 7 is I 0, and the values measured by the first fluorescent signal detection module 801 and the second fluorescent signal detection module 802 are A 0 and B 0 respectively;
(3) Opening a flip cover, taking a four-way light cuvette 6 containing tryptophan water solution with the concentration of 100 mug/L, placing the four-way light cuvette 6 serving as fluorescent signal calibration liquid of a fluorescent light intensity detection module I801 into a water quality detector, covering the flip cover, and pressing a calibration key, wherein the value measured by the fluorescent light intensity detection module I801 is A 1; calculating a calibration coefficient for the k A signal according to the formula k A＝(A1-A0)/100;
Opening a flip cover, putting a quinine sulfate aqueous solution with the concentration of 100 mug/L into a water quality detector as fluorescent signal calibration liquid of a fluorescent light intensity detection module II 802, covering the flip cover, pressing a calibration key, and calculating a k B signal calibration coefficient according to a formula k B＝(B1-B0)/100, wherein the measured value of the fluorescent light intensity detection module II 802 is B 1;
(4) Opening the flip 4, putting the four-way light cuvette 6 containing the water sample 3 to be detected into a water quality detector, covering the flip, pressing a reading key, wherein the value measured by the ultraviolet absorption light intensity detection module 7 is I s, and the values measured by the fluorescent light intensity detection module I801 and the fluorescent light intensity detection module II 802 are A s、Bs respectively; the display screen 2 displays four measurement values, of which
The ultraviolet absorbance UVA is expressed in cm -1 and the formula is uva=log (I s/I0);
log (L s/L0) is a correction term for the change in ultraviolet absorbance caused by the change in light intensity;
The unit of the fluorescence signal F A is a free dimension unit, the equivalent concentration is the concentration of the corresponding fluorescence calibration liquid, the calculation formula is F A＝(As-A0)/kA*10(0.5*UVA);kA which is a fluorescence equivalent concentration calibration coefficient, and 10 (0.5*UVA) which is an internal covering calibration item;
The unit of the fluorescence signal F B is a free dimension unit, the equivalent concentration is the concentration of the corresponding fluorescence calibration liquid, the calculation formula is F B＝(Bs-B0)/kB*10(0.5*UVA),kB which is a fluorescence equivalent concentration calibration coefficient, and 10 (0.5*UVA) which is an internal covering calibration term.
The specific detection results obtained are shown in Table 2.
Table 2 results of water quality detection of water sample 3 to be detected using the portable rapid water quality detector provided in example 1 and this comparative example, respectively
As can be seen from Table 3, the portable rapid water quality detector provided in this comparative example, compared with example 1, has no LED light source intensity detection mode module for correcting the ultraviolet light source, the obtained fluorescence signal is attenuated by about 1.4% compared with the fluorescence signal measured by the scheme of example 1, the obtained ultraviolet absorbance signal is 0.0148cm -1 higher than the ultraviolet absorbance signal 0.0087cm -1 measured by the scheme of example 1 by 0.0061cm -1, and the relative increase is 70% due to the error caused by the attenuation of 1.4% by the light source.
Claims (7)
1. A method for detecting water quality by using a portable rapid water quality detector is characterized in that:
The portable quick water quality detector comprises a handheld shell, and is characterized in that: an LED light source and a detection assembly are arranged in the handheld shell, and the detection assembly comprises a four-way light cuvette with four light transmission surfaces, an LED light source intensity detection module, an ultraviolet absorption light intensity detection module and a fluorescent light intensity detection module;
The LED light source, the ultraviolet absorption light intensity detection module and the fluorescent light intensity detection module are arranged on the periphery of the four-way light cuvette and respectively correspond to different light transmission surfaces; the LED light source is used for emitting ultraviolet light to the four-way light cuvette, the ultraviolet absorption light intensity detection module is arranged at the relative position of the LED light source and used for detecting the light intensity of the ultraviolet light which is not absorbed after passing through the four-way light cuvette, and the fluorescent light intensity detection module is arranged at one side of the four-way light cuvette and used for detecting the fluorescent light intensity of the liquid to be detected which is excited and passes through the four-way light cuvette;
the central wavelength range of the LED light source is 250-300 nm; the transmission wavelength range of the bandpass filter of the fluorescence intensity detection module is 325-480 nm;
the LED light source intensity detection module is arranged on one side of the LED light source and used for detecting the light intensity of ultraviolet light emitted by the LED light source in real time;
The fluorescent light intensity detection module comprises a fluorescent light intensity detection module I and a fluorescent light intensity detection module II; the first fluorescent light intensity detection module and the second fluorescent light intensity detection module are respectively arranged at two opposite sides of the four-way light cuvette
The water quality detection method comprises the following specific steps:
(1) Starting a water quality detector;
(2) Placing a cuvette containing ultrapure water into a water quality detector, wherein the numerical value measured by an ultraviolet absorption light intensity detection module is I 0, the numerical value measured by an LED light source intensity detection module is L 0, and the numerical values measured by two fluorescent signal detection modules are A 0 and B 0 respectively;
(3) Taking a cuvette containing tryptophan water solution with the concentration of N 0, and taking the cuvette as fluorescent signal calibration liquid of a fluorescent light intensity detection module A, and putting the cuvette into a water quality detector, wherein the value measured by the fluorescent light intensity detection module A is A 1; calculating a calibration coefficient for the k A signal according to a formula k A=(A1-A0)/N0;
The method comprises the steps of (1) putting a quinine sulfate aqueous solution with the concentration of M 0 into a water quality detector as fluorescent signal calibration liquid of a fluorescent light intensity detection module B, wherein the numerical value measured by the fluorescent light intensity detection module B is B 1, and calculating a k B signal calibration coefficient according to a formula k B=(B1-B0)/M0;
(4) Placing a cuvette containing a water sample to be detected into a water quality detector, wherein the value measured by an ultraviolet absorption light intensity detection module is I s, the value measured by an LED light source intensity detection module is L s, and the values measured by a fluorescent light intensity detection module A and a fluorescent light intensity detection module B are A s、Bs respectively; the display screen displays four measured values, wherein,
The light intensity signal L is expressed as a unit of percent, and the calculation formula is L= (L s/L0);
The ultraviolet absorbance UVA is expressed in cm -1 and the formula is uva=log (I s/I0)+log(Ls/L0);
log (L s/L0) is a correction term for the change in ultraviolet absorbance caused by the change in light intensity;
The unit of the fluorescence signal F A is a free dimension unit, the equivalent concentration is the concentration of the corresponding fluorescence calibration liquid, the calculation formula is F A=(As-A0)/kA×10 (0.5×UVA);kA which is a fluorescence equivalent concentration calibration coefficient, and 10 (0.5×UVA) which is an internal covering calibration item;
the unit of the fluorescence signal F B is a free dimension unit, the equivalent concentration is the concentration of the corresponding fluorescence calibration liquid, the calculation formula is F B=(Bs-B0)/kB×10 (0.5×UVA),kB which is a fluorescence equivalent concentration calibration coefficient, and 10 (0.5×UVA) which is an internal covering calibration item;
(5) And (5) repeating the step (4) to continue testing other water samples.
2. The method for water quality testing by using a portable rapid water quality tester according to claim 1, wherein: the LED light source intensity detection module consists of a gallium nitride-based ultraviolet photodiode and an operational amplification circuit, wherein a feedback resistor in the operational amplification circuit adopts an M omega-level resistance resistor.
3. The method for water quality detection by using a portable rapid water quality detector according to any one of claims 1 to 2, wherein the method comprises the following steps: the transmission wavelength range of the bandpass filter of the first fluorescent light intensity detection module is 325-360 nm; the transmission wavelength range of the band-pass filter of the second fluorescent light intensity detection module is 400-480 nm.
4. A method for water quality testing with a portable rapid water quality tester according to claim 3, wherein: an electronic control system is also arranged in the handheld shell, and comprises a main board circuit and a power supply;
The main board circuit is provided with a singlechip, a wireless communication module and a USB interface; the singlechip is used for receiving voltage signals generated by the LED light source intensity detection module, the ultraviolet absorption light intensity detection module and the fluorescent light intensity detection module, converting the voltage signals into digital signals for storage, or transmitting the digital signals to the upper computer through the USB interface/wireless communication module;
The singlechip controls the work of the LED light source through the constant current driving circuit;
The power supply is used for supplying power to the electronic control system, the LED light source intensity detection module, the ultraviolet absorption light intensity detection module and the fluorescent light intensity detection module, and can be charged through the USB interface.
5. The method for water quality testing with a portable rapid water quality tester according to claim 4, wherein: the electronic control system also comprises a display screen and keys;
The display screen is connected with the singlechip through a circuit and receives and displays digital signals output by the singlechip in real time;
The keys are connected with the singlechip through circuits and used for controlling the working state and parameter input of the water quality detector.
6. The method for water quality testing with a portable rapid water quality tester according to claim 5, wherein: the hand-held shell is provided with a switchable flip cover at a position corresponding to the four-way light cuvette.
7. The method for water quality testing with a portable rapid water quality tester according to claim 6, wherein: the handheld shell is internally provided with a shading cassette, and the LED light source and the detection assembly are positioned in the shading cassette.
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