CN112903414A - Multi-parameter automatic water quality analysis method and system - Google Patents
Multi-parameter automatic water quality analysis method and system Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 91
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- 238000004737 colorimetric analysis Methods 0.000 claims abstract description 43
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- 238000011161 development Methods 0.000 claims description 24
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
Abstract
The invention relates to the field of automatic water quality monitoring, in particular to a multi-parameter automatic water quality analysis method, which comprises a direct colorimetric analysis method, a chromogenic colorimetric analysis method, a digestion-chromogenic colorimetric analysis method and an air-blowing desorption-ultraviolet Fourier transform analysis method; the multi-parameter water quality automatic analysis system comprises a metering part, a reaction part and a detection part, wherein the metering part comprises a first pump and a multi-way valve, the reaction part comprises a reaction chamber, a second pump and a three-way valve, the detection part comprises a first light source, a second light source, a gas flow cell, a liquid flow cell, a light splitter and a spectrometer, and the reaction chamber comprises a first reaction chamber and a second reaction chamber. The invention is compatible with various detection methods, and realizes multi-index detection; the required reagents are few in types and small in consumption; the high integration application realizes the sharing of the spectrograph for detecting gas and liquid, and effectively reduces the system cost.
Description
Technical Field
The invention relates to the field of automatic water quality monitoring, in particular to a multi-parameter automatic water quality analysis method and system.
Background
Quality of water automatic monitoring instrument has been widely used in the detection of natural water, sewage, process water, drinking water, domestic water etc, hexavalent chromium monitor automatic correction position color comparison device for disclosing be "CN 102735681B", including the instrument installation panel, characterized by, be equipped with the colour comparison tube backup pad on the instrument installation panel, liquid detection colour comparison tube is fixed in the colour comparison tube backup pad, colour comparison tube backup pad upper end sets up the colour comparison tube upper cover, colour comparison tube backup pad lower extreme sets up the colour comparison tube lower cover, liquid detection colour comparison tube and colour comparison tube lower cover taper fit installation, the lower port of liquid detection colour comparison tube passes the colour comparison tube lower cover, links to each other with advance the drain pipe. The device can self-correct the position, simple structure, and is small, simple to operate, the maintenance of being convenient for, the practicality is wide, can install among different color comparison systems.
This device still has a number of disadvantages: (1) one instrument can only detect one index, and multiple indexes need multiple instruments; (2) conventional water quality indexes such as chemical oxygen demand, ammonia nitrogen, total phosphorus, total nitrogen and the like are generally detected by a wet chemical method, 2-3 different reagents are required for detection of each index, the detection period is long, the reagent consumption is large, the waste liquid amount is large, and the maintenance amount is large; when the chemical oxygen demand is measured by adopting a probe type spectrum method, although the detection is quick and the maintenance amount is small, the chemical oxygen demand is easily interfered by turbidity, an optical detection window is not easy to clean and cannot be automatically calibrated or automatically zeroed, and the numerical value drift is large after long-time measurement; (3) when ammonia nitrogen is measured by adopting a probe type ion selective electrode method, although the detection is quick and the maintenance amount is small, the electrode is easily subjected to temperature influence to cause signal drift, the service life of the electrode is limited, automatic calibration cannot be realized, and the numerical value drift is large after long-time measurement.
Disclosure of Invention
The invention aims to overcome the defects of the existing scheme and provides a multi-parameter automatic water quality analysis method and system, which have the advantages of multi-parameter detection, low reagent consumption, rapid detection and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a multi-parameter automatic water quality analysis method comprises a direct colorimetric analysis method, a chromogenic colorimetric analysis method, a digestion-chromogenic colorimetric analysis method comprising a digestion reaction and a chromogenic reaction, and an air-blowing-off-ultraviolet Fourier transform analysis method, and the analysis method is carried out according to the following steps:
(1) running the digestion reaction of the digestion-color development colorimetric analysis method and generating a digestion solution;
(2) running a direct colorimetric analysis method;
(3) running a colorimetric method;
(4) operating an air stripping-ultraviolet Fourier transform analysis method;
(5) and injecting the digestion solution into the liquid flow cell in several times, and operating the color reaction of the digestion-color development colorimetric analysis method.
The multi-parameter automatic water quality analysis method simultaneously comprises a direct colorimetric analysis method, a color development colorimetric analysis method, a digestion-color development colorimetric analysis method comprising a digestion reaction and a color development reaction, and an air blowing-off-ultraviolet Fourier transform analysis method, and in a measurement period, the methods are carried out according to specific steps, and the direct colorimetric analysis method, the color development colorimetric analysis method and the air blowing-off-ultraviolet Fourier transform analysis method are sequentially carried out while the digestion reaction is carried out, wherein the direct colorimetric method can be used for measuring water quality indexes such as COD, BOD, TOC, chromaticity, turbidity, nitrate nitrogen and the like, and compared with a probe type instrument, the multi-parameter automatic water quality analysis method can be automatically cleaned, automatically zero-setting a spectrometer and automatically calibrating the spectrometer; the color development colorimetric method can be used for measuring plasma state water quality indexes of phosphate, nitrite, silicate and ionic state heavy metal, the digestion-color development colorimetric method can be used for measuring total state water quality indexes of total phosphorus, total nitrogen, total state heavy metal and the like, the air blowing-off-ultraviolet colorimetric analysis method can be used for measuring water quality indexes of ammonia nitrogen, sulfide and the like which can be converted into volatile molecular states, and complex chemical reaction is not required: the invention realizes multi-parameter detection, greatly improves the detection efficiency and realizes quick detection.
Meanwhile, the invention needs few types of reagents and small consumption, and the direct colorimetric analysis method does not need to use reagents; the digestion-color development colorimetric method can share a digestion reagent, realize one-time digestion and multiple color development, realize multi-index rapid detection and reduce the variety and consumption of the reagent; the air stripping-ultraviolet colorimetric analysis method only needs one pH adjusting reagent; the detection sample used in the invention can complete multiple detections once, thus greatly reducing the dosage of the detection reagent; and the digestion solution in the digestion-color development colorimetric analysis method is injected into the liquid flow cell for multiple times and then the color development reaction is operated, so that the multiple utilization of the digestion solution in sequence is realized, and the reagent usage amount of the reaction is further reduced.
The invention also shares the spectrograph for detecting gas and liquid, realizes high integration application and effectively reduces the system cost.
The digestion reaction in the step (1) is carried out under the conditions of heating to the temperature of not higher than 90 ℃ and ultraviolet light oxidation.
The gas stripping-ultraviolet Fourier transform analysis method in the step (4) comprises the following steps: mixing a sample and a pH adjusting reagent, heating and pumping air to blow off substances to be detected in the sample, collecting light signals by a spectrometer for analysis after ultraviolet and visible light beams penetrate through a gas flow cell and a light splitter, and calculating the concentration of the substances to be detected by a Fourier transform algorithm.
The heating is controlled by resistance wires; and/or ultraviolet light oxidation is realized by adopting an ultraviolet lamp and a photocatalytic substance.
A multi-parameter water quality automatic analysis system applied to the multi-parameter water quality automatic analysis method comprises a metering part, a reaction part, a detection part and a metering part; the metering part comprises a first pump and a multi-way valve, the reaction part comprises a reaction chamber, a second pump and a three-way valve, and the detection part comprises a first light source, a second light source, a gas flow cell, a liquid flow cell, a light splitter and a spectrometer.
The reaction chamber comprises a first reaction chamber and a second reaction chamber, an ultraviolet lamp is arranged on the inner wall of the first reaction chamber, a first quartz glass container is fixed at the center of the first reaction chamber, a resistance wire is wound on the outer wall of the first reaction chamber, and a photocatalytic substance is placed inside the first reaction chamber.
The first quartz glass container is provided with an upper outlet and a lower outlet, the upper outlet of the first quartz glass container is communicated with the air, and the lower outlet of the first quartz glass container is connected with the multi-way valve through a pipeline; and/or
The photocatalytic substance is a titanium dioxide nanotube or a carbon nanotube. The titanium dioxide nanotube and the carbon nanotube have a series of advantages of high photocatalytic efficiency, no toxicity, environmental protection, low cost and the like, and are in accordance with the use environment and the use equipment of the invention.
A second quartz glass container is fixed in the center of the second reaction chamber, a resistance wire is wound on the outer wall of the second quartz glass container, the second quartz glass container is provided with an upper outlet and a lower outlet, and the upper outlet of the second quartz glass container is connected with a three-way valve through a pipeline; the gas flow cell is provided with an upper outlet and a lower outlet, the three-way valve comprises a normally open end and a normally closed end, the normally open end of the three-way valve is communicated with air, and the normally closed end is connected with the upper outlet of the gas flow cell through a pipeline; the lower outlet of the second quartz glass container is divided into two paths, one path is connected with the multi-way valve through a pipeline, the other path is connected with the second through pipeline, and the second pump is connected with the lower outlet of the gas flow cell through a pipeline.
The liquid flow cell is provided with an upper outlet and a lower outlet, the upper outlet of the liquid flow cell is communicated with air, and the lower outlet of the liquid flow cell is connected with the multi-way valve through a pipeline.
The first light source emits ultraviolet visible light beams, and light signals are collected by a spectrometer for analysis after the ultraviolet visible light beams penetrate through the gas flow cell and the light splitter; the second light source emits ultraviolet visible light beams, and light signals are collected by the spectrometer for analysis after the ultraviolet visible light beams penetrate through the liquid flow cell and the light splitter; the light splitter comprises one of a light splitter, a light splitting prism and a beam splitting quartz fiber. All optical components of the invention can also be packaged by black and non-reflective plastic or metal materials to eliminate stray light interference.
In conclusion, the invention has the following beneficial effects:
(1) one analyzer is compatible with various detection methods to realize multi-index detection; (2) the required reagents are few in types and small in consumption; (3) the high integration application realizes the sharing of the spectrograph for detecting gas and liquid, and effectively reduces the system cost.
Drawings
FIG. 1 is a schematic diagram of a system configuration according to the present invention.
Fig. 2 is a schematic diagram of another system configuration of the present invention.
In the figure: 1. a first pump; 2. a multi-way valve; 3. a first reaction chamber; 4. an ultraviolet lamp; 5. a first quartz glass container; 6. a photocatalytic substance; 7. a second reaction chamber; 8. a second glass container; 9. a three-way valve; 10. a second pump; 11. A first light source; 12. a gas flow cell; 13. a second light source; 14. a liquid flow cell; 15. a light splitter; 16. a spectrometer.
Detailed Description
The invention is further described with reference to the following detailed description and accompanying drawings.
Example 1
In embodiment 1 shown in fig. 1, a multi-parameter automatic water quality analysis system includes a metering portion, a reaction portion, a detection portion, and a metering portion; the metering part comprises a first pump 1 and a multi-way valve 2, the reaction part comprises a first reaction chamber 3, a second reaction chamber 7, a second pump 10 and a three-way valve 9, the detection part comprises a first light source 11, a second light source 13, a gas flow cell 12, a liquid flow cell 14, a light splitter 15 and a spectrometer 16, wherein:
the first pump 1 is connected with a common channel of the multi-way valve 2 through a pipeline, and other channels of the multi-way valve 2 are connected with a sample, an oxidant, an alkali reagent, a color developing agent, a reducing agent and waste liquid, a first reaction chamber 3, a second reaction chamber 7 and a liquid flow cell 14; an ultraviolet lamp 4 is arranged on the inner wall of the first reaction chamber 3, a first quartz glass container 5 is fixed in the center of the first reaction chamber 3, a resistance wire is wound on the outer wall of the first quartz glass container, and a photocatalytic substance 6 is placed in the first quartz glass container; the upper outlet of the first quartz glass container 5 is communicated with the air, and the lower outlet is connected with the multi-way valve 2 through a pipeline; the photocatalytic substance 6 is a titanium dioxide nanotube; a second quartz glass container 8 is fixed in the center of the second reaction chamber 7, and a resistance wire is wound on the outer wall of the second quartz glass container 8; an upper outlet of the second quartz glass container 8 is connected with a common channel of the three-way valve 9 through a pipeline, a normally open end of the three-way valve 9 is communicated with air, and a normally closed end of the three-way valve 9 is connected with an upper outlet of the gas flow cell 12 through a pipeline; the lower outlet is divided into two paths, one path is connected with the multi-way valve 2 through a pipeline, the other path is connected with the second pump 10 through a pipeline, and the second pump 10 is connected with the lower outlet of the gas flow cell 12 through a pipeline; the upper outlet of the liquid flow cell 14 is communicated with air, and the lower outlet is connected with the multi-way valve 2 through a pipeline; the first light source 11 emits ultraviolet visible light beams, and light signals are collected by the spectrometer 16 for analysis after the ultraviolet visible light beams penetrate through the gas flow cell 12 and the light splitter 15; the second light source 13 emits ultraviolet visible light beams, and light signals are collected by the spectrometer 16 for analysis after the ultraviolet visible light beams penetrate through the liquid flow cell 14 and the light splitter 15; the light splitter is a light splitting sheet, and all optical components are packaged by black and non-reflective plastic materials so as to eliminate stray light interference.
The embodiment also provides a multi-parameter automatic water quality analysis method, which comprises the following steps:
(1) the multi-way valve 2 selects a sample channel and a reagent channel, the first pump 1 respectively pumps quantitative samples, oxidants and alkali reagents through a common channel of the multi-way valve 2 and injects the quantitative samples, the oxidants and the alkali reagents into a first quartz glass container 5 in the first reaction chamber 3;
(2) starting an ultraviolet lamp 4, starting a resistance wire wound on the outer wall of the first quartz glass container 5, and digesting the mixed solution for 15 minutes at a heating temperature of 70 ℃;
(3) the multi-way valve 2 selects a sample channel, and the first pump 1 extracts a quantitative sample through a common channel of the multi-way valve 2 and injects the quantitative sample into the liquid flow cell 14;
(4) the second light source 13 emits an ultraviolet visible light beam, and after passing through the liquid flow cell 14 and the optical splitter 15, the optical signal is collected by the optical spectrometer 16 for analysis, and the chemical oxygen demand is measured. After the signal collection is finished, the first pump 1 is matched with the multi-way valve 2 to discharge the sample in the liquid flow cell 14 to waste liquid and clean the sample;
(5) the multi-way valve 2 selects a sample channel and a reagent channel, the first pump 1 respectively extracts quantitative samples and alkali reagents through a common channel of the multi-way valve 2 and injects the quantitative samples and the alkali reagents into a second quartz glass container 8 in the second reaction chamber 7;
(6) the normally open end of the three-way valve 9 is closed, and the normally closed end is opened; starting a resistance wire wound on the outer wall of the second quartz glass container 8, and heating the mixed solution for 3 minutes at 50 ℃; simultaneously, the second pump 10 operates to blow air, ammonia in the mixed solution in the second quartz glass container 8 is blown off, and the ammonia enters the gas flow cell 12;
(7) after the second quartz glass container 8 is heated, the first light source 11 emits ultraviolet visible light beams, the ultraviolet visible light beams penetrate through the gas flow cell 12 and the light splitter 15, the light signals are collected by the spectrometer 16 for analysis, and the ammonia nitrogen concentration is calculated through a Fourier transform algorithm. After the signal acquisition is finished, the first pump 1 is matched with the multi-way valve 2 and the three-way valve 9, and the sample in the second quartz glass container 8 is discharged to waste liquid and cleaned;
(8) after the mixed solution in the first quartz glass container 5 is digested, the multi-way valve 2 selects a channel of the first reaction chamber 3, and the first pump 1 pumps half of the digested solution through a common channel of the multi-way valve 2 and injects the solution into the liquid flow cell 14;
(9) the second light source 13 emits an ultraviolet visible light beam, and after passing through the liquid flow cell 14 and the optical splitter 15, the optical signal is collected by the optical spectrometer 16 for analysis, and the total nitrogen is measured. After the signal collection is finished, the first pump 1 is matched with the multi-way valve 2 to discharge the sample in the liquid flow cell 14 to waste liquid and clean the sample;
(10) the multi-way valve 2 selects a reagent channel, the first pump 1 respectively pumps quantitative color developing agent and reducing agent through a common channel of the multi-way valve 2, and the color developing agent and the reducing agent are injected into a first quartz glass container 5 in the first reaction chamber 3 to perform color development reaction;
(11) the multi-way valve 2 selects a channel of the first reaction chamber 3, and the first pump 1 pumps the colored solution through a common channel of the multi-way valve 2 and injects the solution into the liquid flow cell 14;
(12) the second light source 13 emits an ultraviolet visible light beam, and after passing through the liquid flow cell 14 and the optical splitter 15, the optical signal is collected by the optical spectrometer 16 for analysis, and total phosphorus is measured. After the signal collection is finished, the first pump 1 is matched with the multi-way valve 2, the sample in the liquid flow cell 14 is discharged to waste liquid and cleaned, and the first quartz glass container 5 is cleaned;
(13) according to the steps, the pure water and the mixed standard liquid can be used for automatic calibration and spectrum zero setting.
The invention also comprises a direct colorimetric analysis method, a chromogenic colorimetric analysis method, a digestion-chromogenic colorimetric analysis method comprising a digestion reaction and a chromogenic reaction, and an air-blowing-off-ultraviolet Fourier transform analysis method, wherein in a measurement period, the methods are carried out according to specific steps, and the direct colorimetric analysis method, the chromogenic colorimetric analysis method and the air-blowing-off-ultraviolet Fourier transform analysis method are sequentially carried out while the digestion reaction is carried out, wherein the direct colorimetric method can be used for measuring water quality indexes such as COD, BOD, TOC, chromaticity, turbidity, nitrate nitrogen and the like, and compared with a probe type instrument, the method can be automatically cleaned, can automatically zero a spectrometer, and can be automatically calibrated; the color development colorimetric method can be used for measuring plasma state water quality indexes of phosphate, nitrite, silicate and ionic state heavy metal, the digestion-color development colorimetric method can be used for measuring total state water quality indexes of total phosphorus, total nitrogen, total state heavy metal and the like, and the air blowing-off-ultraviolet colorimetric analysis method can be used for measuring water quality indexes of ammonia nitrogen, sulfide and the like which can be converted into volatile molecular states without carrying out complex chemical reaction. The above reaction is particularly suitable for measuring the chemical oxygen demand, ammonia nitrogen, total phosphorus and total nitrogen of the sample in the present embodiment. The invention realizes multi-parameter detection, greatly improves the detection efficiency and realizes quick detection.
Meanwhile, the invention needs few types of reagents and small consumption, and the direct colorimetric analysis method does not need to use reagents; the digestion-color development colorimetric method can share a digestion reagent, realize one-time digestion and multiple color development, realize multi-index rapid detection and reduce the variety and consumption of the reagent; the air stripping-ultraviolet colorimetric analysis method only needs one pH adjusting reagent; the detection sample used in the invention can complete multiple detections once, thus greatly reducing the dosage of the detection reagent; and the digestion solution in the digestion-color development colorimetric analysis method is injected into the liquid flow cell for multiple times and then the color development reaction is operated, so that the multiple utilization of the digestion solution in sequence is realized, and the reagent usage amount of the reaction is further reduced.
Example 2
In embodiment 2 shown in fig. 2, a multi-parameter automatic water quality analysis system includes a metering portion, a reaction portion, a detection portion, and a metering portion; the metering part comprises a first pump 1 and a multi-way valve 2, the reaction part comprises a first reaction chamber 3, a second pump 10 and a three-way valve 9, the detection part comprises a first light source 11, a second light source 13, a gas flow cell 12, a liquid flow cell 14, a light splitter 15 and a spectrometer 16, wherein:
the first pump 1 is connected with a common channel of the multi-way valve 2 through a pipeline, and other channels of the multi-way valve are connected with a sample, an alkali reagent, a first color developing agent, a second color developing agent, a reducing agent, waste liquid, a first reaction chamber 3 and a liquid flow cell 14; a first quartz glass container 5 is fixed in the center of the first reaction chamber 3, and a resistance wire is wound on the outer wall of the first quartz glass container 5; the upper outlet of the first quartz glass container 5 is connected with the common channel of the three-way valve 9 through a pipeline, the normally open end of the three-way valve 9 is communicated with the air, and the normally closed end of the three-way valve 9 is connected with the upper outlet of the gas flow cell 12 through a pipeline; the lower outlet is divided into two paths, one path is connected with the multi-way valve 2 through a pipeline, the other path is connected with the second pump 10 through a pipeline, and the second pump 10 is connected with the lower outlet of the gas flow cell 12 through a pipeline; the upper outlet of the liquid flow cell 14 is communicated with air, and the lower outlet is connected with the multi-way valve 2 through a pipeline; the first light source 11 emits ultraviolet visible light beams, and light signals are collected by the spectrometer 16 for analysis after the ultraviolet visible light beams penetrate through the gas flow cell 12 and the light splitter 15; the second light source 9 emits ultraviolet visible light beams, and light signals are collected by the spectrometer 16 for analysis after the ultraviolet visible light beams penetrate through the liquid flow cell 10 and the light splitter 11; the beam splitter 15 is a beam splitter prism, and all optical components are packaged by black and non-reflective metal materials to eliminate stray light interference.
The embodiment also provides a multi-parameter automatic water quality analysis method, which comprises the following steps:
(1) the multi-way valve 2 selects a sample channel, and the first pump 1 extracts a quantitative sample through a common channel of the multi-way valve 2 and injects the quantitative sample into the liquid flow cell 14;
(2) the second light source 13 emits ultraviolet visible light beams, and after passing through the liquid flow cell 14 and the light splitter 15, the light signals are collected by the spectrometer 16 for analysis, and nitrate is measured. After the signal collection is finished, the first pump 1 is matched with the multi-way valve 2 to discharge the sample in the liquid flow cell 14 to waste liquid and clean the sample;
(3) the multi-way valve 2 selects a sample channel and a reagent channel, the first pump 1 respectively extracts quantitative samples and a first color developing agent through a common channel of the multi-way valve 2, and the quantitative samples and the first color developing agent are injected into the liquid flow cell 14 for color development reaction;
(4) the second light source 13 emits ultraviolet visible light beams, and after passing through the liquid flow cell 14 and the light splitter 15, the light signals are collected by the spectrometer 16 for analysis, and nitrite is measured. After the signal collection is finished, the first pump 1 is matched with the multi-way valve 2 to discharge the sample in the liquid flow cell 14 to waste liquid and clean the sample;
(5) the multi-way valve 2 selects a sample channel and a reagent channel, the first pump 1 respectively extracts quantitative samples, a second color developing agent and a reducing agent through a common channel of the multi-way valve 2, and injects the quantitative samples, the second color developing agent and the reducing agent into the liquid flow cell 14 for color development reaction;
(6) the second light source 13 emits an ultraviolet visible light beam, and after passing through the liquid flow cell 14 and the optical splitter 15, the optical signal is collected by the optical spectrometer 16 for analysis, and the phosphate is measured. After the signal collection is finished, the first pump 1 is matched with the multi-way valve 2 to discharge the sample in the liquid flow cell 10 to waste liquid and clean the sample;
(7) the multi-way valve 2 selects a sample channel and a reagent channel, the first pump 1 respectively pumps quantitative samples and alkali reagents through a common channel of the multi-way valve 2 and injects the quantitative samples and the alkali reagents into a first quartz glass container 5 in the first reaction chamber 3;
(8) the normally open end of the three-way valve 9 is closed, and the normally closed end is opened; starting a resistance wire wound on the outer wall of the first quartz glass container 5, and heating the mixed solution for 3 minutes at 50 ℃; simultaneously, the second pump 10 operates to blow air, ammonia in the mixed solution in the first quartz glass container 5 is blown off, and the ammonia enters the gas flow cell 12;
(9) after the first quartz glass container 5 is heated, the first light source emits ultraviolet visible light beams, the ultraviolet visible light beams penetrate through the gas flow cell 12 and the light splitter 15, the light signals are collected by the spectrometer 16 to be analyzed, and the ammonia nitrogen concentration is calculated through a Fourier transform algorithm. After the signal collection is finished, the first pump 1 is matched with the multi-way valve 2 and the three-way valve 9, and the sample in the first quartz glass container 5 is discharged to waste liquid and cleaned;
(10) according to the steps, the pure water and the mixed standard liquid can be used for automatic calibration and spectrum zero setting.
Example 3
A multi-parameter water quality automatic analysis system comprises a metering part, a reaction part, a detection part and a metering part; the metering part comprises a first pump 1 and a multi-way valve 2, the reaction part comprises a first reaction chamber 3, a second reaction chamber 7, a second pump 10 and a three-way valve 9, the detection part comprises a first light source 11, a second light source 13, a gas flow cell 12, a liquid flow cell 14, a light splitter 15 and a spectrometer 16, wherein:
the first pump 1 is connected with a common channel of the multi-way valve 2 through a pipeline, and other channels of the multi-way valve 2 are connected with a sample, an oxidant, an alkali reagent, a color developing agent, a reducing agent and waste liquid, a first reaction chamber 3, a second reaction chamber 7 and a liquid flow cell 14; an ultraviolet lamp 4 is arranged on the inner wall of the first reaction chamber 3, a first quartz glass container 5 is fixed in the center of the first reaction chamber 3, a resistance wire is wound on the outer wall of the first quartz glass container, and a photocatalytic substance 6 is placed in the first quartz glass container; the upper outlet of the first quartz glass container 5 is communicated with the air, and the lower outlet is connected with the multi-way valve 2 through a pipeline; the photocatalytic substance 6 is a carbon nanotube; a second quartz glass container 8 is fixed in the center of the second reaction chamber 7, and a resistance wire is wound on the outer wall of the second quartz glass container 8; an upper outlet of the second quartz glass container 8 is connected with a common channel of the three-way valve 9 through a pipeline, a normally open end of the three-way valve 9 is communicated with air, and a normally closed end of the three-way valve 9 is connected with an upper outlet of the gas flow cell 12 through a pipeline; the lower outlet is divided into two paths, one path is connected with the multi-way valve 2 through a pipeline, the other path is connected with the second pump 10 through a pipeline, and the second pump 10 is connected with the lower outlet of the gas flow cell 12 through a pipeline; the upper outlet of the liquid flow cell 14 is communicated with air, and the lower outlet is connected with the multi-way valve 2 through a pipeline; the first light source 11 emits ultraviolet visible light beams, and light signals are collected by the spectrometer 16 for analysis after the ultraviolet visible light beams penetrate through the gas flow cell 12 and the light splitter 15; the second light source 13 emits ultraviolet visible light beams, and light signals are collected by the spectrometer 16 for analysis after the ultraviolet visible light beams penetrate through the liquid flow cell 14 and the light splitter 15; the beam splitter is a beam splitting quartz optical fiber, and all optical components are packaged by black and non-reflective plastic materials so as to eliminate stray light interference.
The embodiment also provides a multi-parameter automatic water quality analysis method, which comprises the following steps:
(1) the multi-way valve 2 selects a sample channel and a reagent channel, the first pump 1 respectively pumps quantitative samples, oxidants and alkali reagents through a common channel of the multi-way valve 2 and injects the quantitative samples, the oxidants and the alkali reagents into a first quartz glass container 5 in the first reaction chamber 3;
(2) starting an ultraviolet lamp 4, starting a resistance wire wound on the outer wall of the first quartz glass container 5, and digesting the mixed solution for 15 minutes at a heating temperature of 70 ℃;
(3) the multi-way valve 2 selects a sample channel, and the first pump 1 extracts a quantitative sample through a common channel of the multi-way valve 2 and injects the quantitative sample into the liquid flow cell 14;
(4) the second light source 13 emits an ultraviolet visible light beam, and after passing through the liquid flow cell 14 and the optical splitter 15, the optical signal is collected by the optical spectrometer 16 for analysis, and the chemical oxygen demand is measured. After the signal collection is finished, the first pump 1 is matched with the multi-way valve 2 to discharge the sample in the liquid flow cell 14 to waste liquid and clean the sample;
(5) the multi-way valve 2 selects a sample channel and a reagent channel, the first pump 1 respectively extracts quantitative samples and alkali reagents through a common channel of the multi-way valve 2 and injects the quantitative samples and the alkali reagents into a second quartz glass container 8 in the second reaction chamber 7;
(6) the normally open end of the three-way valve 9 is closed, and the normally closed end is opened; starting a resistance wire wound on the outer wall of the second quartz glass container 8, and heating the mixed solution for 3 minutes at 50 ℃; simultaneously, the second pump 10 operates to blow air, ammonia in the mixed solution in the second quartz glass container 8 is blown off, and the ammonia enters the gas flow cell 12;
(7) after the second quartz glass container 8 is heated, the first light source 11 emits ultraviolet visible light beams, the ultraviolet visible light beams penetrate through the gas flow cell 12 and the light splitter 15, the light signals are collected by the spectrometer 16 for analysis, and the ammonia nitrogen concentration is calculated through a Fourier transform algorithm. After the signal acquisition is finished, the first pump 1 is matched with the multi-way valve 2 and the three-way valve 9, and the sample in the second quartz glass container 8 is discharged to waste liquid and cleaned;
(8) after the mixed solution in the first quartz glass container 5 is digested, the multi-way valve 2 selects a channel of the first reaction chamber 3, and the first pump 1 pumps half of the digested solution through a common channel of the multi-way valve 2 and injects the solution into the liquid flow cell 14;
(9) the second light source 13 emits an ultraviolet visible light beam, and after passing through the liquid flow cell 14 and the optical splitter 15, the optical signal is collected by the optical spectrometer 16 for analysis, and the total nitrogen is measured. After the signal collection is finished, the first pump 1 is matched with the multi-way valve 2 to discharge the sample in the liquid flow cell 14 to waste liquid and clean the sample;
(10) the multi-way valve 2 selects a reagent channel, the first pump 1 respectively pumps quantitative color developing agent and reducing agent through a common channel of the multi-way valve 2, and the color developing agent and the reducing agent are injected into a first quartz glass container 5 in the first reaction chamber 3 to perform color development reaction;
(11) the multi-way valve 2 selects a channel of the first reaction chamber 3, and the first pump 1 pumps the colored solution through a common channel of the multi-way valve 2 and injects the solution into the liquid flow cell 14;
(12) the second light source 13 emits an ultraviolet visible light beam, and after passing through the liquid flow cell 14 and the optical splitter 15, the optical signal is collected by the optical spectrometer 16 for analysis, and total phosphorus is measured. After the signal collection is finished, the first pump 1 is matched with the multi-way valve 2, the sample in the liquid flow cell 14 is discharged to waste liquid and cleaned, and the first quartz glass container 5 is cleaned;
(13) according to the steps, the pure water and the mixed standard liquid can be used for automatic calibration and spectrum zero setting.
Claims (10)
1. The multi-parameter automatic water quality analysis method is characterized by comprising a direct colorimetric analysis method, a chromogenic colorimetric analysis method, a digestion-chromogenic colorimetric analysis method comprising a digestion reaction and a chromogenic reaction, and an air-blowing desorption-ultraviolet Fourier transform analysis method, wherein the analysis method comprises the following steps:
(1) running the digestion reaction of the digestion-color development colorimetric analysis method and generating a digestion solution;
(2) running a direct colorimetric analysis method;
(3) running a colorimetric method;
(4) operating an air stripping-ultraviolet Fourier transform analysis method;
(5) and injecting the digestion solution into the liquid flow cell in several times, and operating the color reaction of the digestion-color development colorimetric analysis method.
2. The multiparameter automatic water quality analysis method according to claim 1, wherein the digestion reaction in step (1) is performed under ultraviolet light oxidation conditions with heating to a temperature of not higher than 90 ℃.
3. The multi-parameter automatic water quality analysis method according to claim 1, wherein the gas stripping-ultraviolet Fourier transform analysis method in the step (4) comprises the following steps: mixing a sample and a pH adjusting reagent, heating and pumping air to blow off substances to be detected in the sample, collecting light signals by a spectrometer for analysis after ultraviolet and visible light beams penetrate through a gas flow cell and a light splitter, and calculating the concentration of the substances to be detected by a Fourier transform algorithm.
4. The multi-parameter automatic water quality analysis method according to claim 1, wherein the heating is controlled by resistance wires; and/or
The ultraviolet light oxidation is realized by an ultraviolet lamp and a photocatalytic substance.
5. A multi-parameter water quality automatic analysis system applied to the multi-parameter water quality automatic analysis method of any one of claims 1 to 4 is characterized in that the multi-parameter water quality automatic analysis system comprises a metering part, a reaction part, a detection part and a metering part; the metering part comprises a first pump and a multi-way valve, the reaction part comprises a reaction chamber, a second pump and a three-way valve, and the detection part comprises a first light source, a second light source, a gas flow cell, a liquid flow cell, a light splitter and a spectrometer.
6. The multiparameter water quality automatic analysis system according to claim 5, wherein the reaction chamber comprises a first reaction chamber and a second reaction chamber, the inner wall of the first reaction chamber is provided with an ultraviolet lamp, the center of the first reaction chamber is fixed with a first quartz glass container, the outer wall of the first reaction chamber is wound with a resistance wire, and a photocatalytic substance is placed inside the first reaction chamber.
7. The automatic multi-parameter water quality analysis system according to claim 6, wherein the first quartz glass container is provided with an upper outlet and a lower outlet, the upper outlet of the first quartz glass container is communicated with air, and the lower outlet of the first quartz glass container is connected with the multi-way valve through a pipeline; and/or
The photocatalytic substance is a titanium dioxide nanotube or a carbon nanotube.
8. The multi-parameter automatic water quality analysis system according to claim 7, wherein a second quartz glass container is fixed in the center of the second reaction chamber, a resistance wire is wound on the outer wall of the second quartz glass container, the second quartz glass container is provided with an upper outlet and a lower outlet, and the upper outlet of the second quartz glass container is connected with a three-way valve through a pipeline; the gas flow cell is provided with an upper outlet and a lower outlet, the three-way valve comprises a normally open end and a normally closed end, the normally open end of the three-way valve is communicated with air, and the normally closed end is connected with the upper outlet of the gas flow cell through a pipeline; the lower outlet of the second quartz glass container is divided into two paths, one path is connected with the multi-way valve through a pipeline, the other path is connected with the second through pipeline, and the second pump is connected with the lower outlet of the gas flow cell through a pipeline.
9. The automatic multi-parameter water quality analysis system according to claim 5, wherein the liquid flow cell is provided with an upper outlet and a lower outlet, the upper outlet of the liquid flow cell is communicated with air, and the lower outlet of the liquid flow cell is connected with the multi-way valve through a pipeline.
10. The multiparameter water quality automatic analysis system according to claim 5, wherein the first light source emits an ultraviolet visible light beam, and after passing through the gas flow cell and the light splitter, a spectrometer collects light signals for analysis; the second light source emits ultraviolet visible light beams, and light signals are collected by the spectrometer for analysis after the ultraviolet visible light beams penetrate through the liquid flow cell and the light splitter; the light splitter comprises one of a light splitter, a light splitting prism and a beam splitting quartz fiber.
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