CN216669721U - Water quality total nitrogen analyzer - Google Patents
Water quality total nitrogen analyzer Download PDFInfo
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- CN216669721U CN216669721U CN202121914191.4U CN202121914191U CN216669721U CN 216669721 U CN216669721 U CN 216669721U CN 202121914191 U CN202121914191 U CN 202121914191U CN 216669721 U CN216669721 U CN 216669721U
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 86
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 37
- 230000029087 digestion Effects 0.000 claims abstract description 111
- 230000002572 peristaltic effect Effects 0.000 claims abstract description 96
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 55
- 238000006243 chemical reaction Methods 0.000 claims abstract description 47
- 239000007788 liquid Substances 0.000 claims abstract description 43
- 238000001514 detection method Methods 0.000 claims abstract description 34
- 239000002699 waste material Substances 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 19
- 239000010453 quartz Substances 0.000 claims description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 19
- 238000003760 magnetic stirring Methods 0.000 claims description 13
- 238000011084 recovery Methods 0.000 claims description 11
- 229910052724 xenon Inorganic materials 0.000 claims description 11
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 10
- 239000011229 interlayer Substances 0.000 claims description 8
- 239000010410 layer Substances 0.000 claims description 5
- 230000003287 optical effect Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 238000005259 measurement Methods 0.000 abstract description 10
- 238000004458 analytical method Methods 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 3
- 238000007254 oxidation reaction Methods 0.000 abstract description 3
- 238000005070 sampling Methods 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000012423 maintenance Methods 0.000 abstract description 2
- 238000002798 spectrophotometry method Methods 0.000 abstract description 2
- 239000012153 distilled water Substances 0.000 description 16
- 239000000243 solution Substances 0.000 description 10
- 238000002835 absorbance Methods 0.000 description 8
- 238000011161 development Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 238000011088 calibration curve Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000012544 monitoring process Methods 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000008237 rinsing water Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002352 surface water Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229910052805 deuterium Inorganic materials 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 125000001477 organic nitrogen group Chemical group 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/152—Water filtration
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- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The utility model provides a water quality total nitrogen analyzer, which comprises: the device comprises a reagent metering assembly, a digestion assembly, a reaction tank assembly, an ultraviolet photoelectric detection assembly, a single chip microcomputer, a plurality of three-way pinch valves and a plurality of peristaltic pumps, wherein the reagent metering assembly, the digestion assembly, the reaction tank assembly and the ultraviolet photoelectric detection assembly are connected through various liquid conveying channels, and each electronic component is electrically connected with the single chip microcomputer. The utility model realizes the automatic, rapid and accurate analysis of the total nitrogen content in water by fully automating the steps of total nitrogen complete detection such as sampling, metering, mixing, digestion, ultraviolet spectrophotometry detection and the like. The reagent metering assembly is high in metering precision and good in stability; the digestion reaction adopts an ultraviolet light assisted catalytic oxidation digestion technology, so that the high-efficiency digestion of a water sample can be realized under normal pressure, and the digestion time is shortened. The utility model has the advantages of accurate measurement, good stability, automatic calibration, less maintenance and the like, and has wide application prospect.
Description
Technical Field
The utility model belongs to the technical field of environmental monitoring, relates to a water quality online analyzer, and particularly relates to a water quality total nitrogen online analyzer.
Background
Total Nitrogen (TN), which is the total amount of various forms of inorganic and organic nitrogen in water, is one of the important indexes for measuring water quality. With the implementation of the policies of 'river growth system' and 'lake growth system', the water quality is more and more emphasized by governments of all levels in China. The traditional total nitrogen analysis method needs sampling on site and bringing back to a laboratory for analysis, is time-consuming and labor-consuming, and cannot be monitored in real time, and the water quality total nitrogen online analyzer becomes a main means for continuously monitoring water quality conditions in departments of environmental protection, water conservancy and the like, can continuously, stably and reliably provide accurate and rapid monitoring data, and has large market demand.
The domestic water quality detecting instrument is started late, the total nitrogen analyzing instrument is large in size, high in power consumption, low in data accuracy and relatively high in failure rate. And meanwhile, the total nitrogen is detected and quantified according to Lambert-beer law, wherein A is equal to epsilon, b.c (A is absorbance, epsilon is molar absorption coefficient of a chromogenic substance, b is optical path of the colorimetric pool, and c is concentration of a substance to be detected), and the calculation formula of the absorbance is as follows: a ═ A220-2A275Therefore, it is necessary to measure the absorbance of ultraviolet light at a wavelength of 220nm and a wavelength of 275 nm. At present, most of light sources of imported instruments and domestic instruments are deuterium lamps, the starting voltage of 800 plus 1000V is needed, certain danger is caused, and a light receiving end is needed to be installed and connected with a spectrometer to read the absorbance of ultraviolet light at the wavelength of 220nm and the wavelength of 275nm, so that the manufacturing cost of the instrument is high.
Disclosure of Invention
In order to solve the problems, the utility model discloses an on-line analyzer for total nitrogen in water quality, which has the advantages of accurate measurement, good stability, safe detection light source and relatively low detection signal measurement cost and provides reliable guarantee for long-term and accurate monitoring of total nitrogen in water quality.
In order to achieve the above purpose, the utility model provides the following technical scheme:
an online analyzer for total nitrogen in water, comprising: the device comprises a reagent metering component, a digestion component, a reaction tank component, an ultraviolet photoelectric detection component, a single chip microcomputer, a plurality of three-way pinch valves and a plurality of peristaltic pumps; the reagent metering assembly, the digestion assembly, the reaction tank assembly and the ultraviolet photoelectric detection assembly are connected through various liquid conveying channels, and each electronic component is electrically connected with the single chip microcomputer;
the reagent metering assembly comprises two groups of transparent quartz metering tubes, the lower ends of the two metering tubes are respectively connected with a first three-way pinch valve and a second three-way pinch valve, the left sides of the first three-way pinch valve and the second three-way pinch valve are connected with a reagent bottle, and the right sides of the first three-way pinch valve and the second three-way pinch valve are connected with the digestion assembly; the upper end of the metering pipe is connected with three-way electromagnetic air valves, all the three-way electromagnetic air valves are linearly connected in series and are connected with the first peristaltic pump through the left side of a third three-way pinch valve, photoelectric switches are respectively arranged at the upper part and the lower part of the side surface of the metering pipe, and the generated electric signals indirectly control the three-way electromagnetic air valves, the first to third three-way pinch valves and the first peristaltic pump to operate through a single chip microcomputer; the first to third three-way pinch valves are connected with the first peristaltic pump;
the digestion assembly main body is a digestion tube, the bottom of the digestion assembly main body is provided with a sample inlet, the upper part of the digestion assembly main body is provided with an overflow port, the heating sheet is wrapped outside the whole digestion assembly main body, a temperature sensor is embedded between the heating sheet and the digestion tube, and an ultraviolet lamp tube is inserted into an opening at the upper part of the digestion tube; the heating plate is electrically connected with the temperature sensor and the singlechip, and the singlechip collects data of the temperature sensor and controls the heating plate and the ultraviolet lamp tube to work; the digestion tube sample inlet is connected to the left side of a sixth three-way pinch valve, the right side of a third three-way pinch valve, the right sides of a first three-way pinch valve and a second three-way pinch valve, a second peristaltic pump and a third peristaltic pump, and the overflow port is connected to the left side of an eighth three-way pinch valve;
the reaction tank assembly comprises a reaction tank, magnetic stirring blades and a stirring motor, and a sample inlet at the bottom of the reaction tank is connected with a fourth peristaltic pump;
the ultraviolet photoelectric detection assembly is an opaque box body, a light source is arranged on one side of the ultraviolet photoelectric detection assembly, a diode detector is arranged on the other side of the ultraviolet photoelectric detection assembly, a quartz colorimetric pool is arranged at a position close to the diode detector, the upper opening and the lower opening of the colorimetric pool are connected with the liquid conveying channel, and the light source and the diode detector are electrically connected with the single chip microcomputer;
the fourth peristaltic pump is connected with a sixth three-way pinch valve, the left side of the sixth three-way pinch valve is connected with the digestion assembly, the right side of the sixth three-way pinch valve is connected with the left side of a seventh three-way pinch valve, the right side of the seventh three-way pinch valve is connected with the waste liquid barrel, the left side of the eighth three-way pinch valve is connected with the waste liquid barrel, and the right side of the eighth three-way pinch valve is connected with the cleaning water recovery barrel.
Further, the light source is a flash xenon lamp with safe voltage, and the diode detector is a 220nm/275nm diode detector.
Further, there are several optical lenses between the flash xenon lamp and the 220nm/275nm diode detector.
Furthermore, the digestion tube is a double-layer hollow quartz digestion tube, the bottom of the digestion tube is provided with an interlayer sample inlet, and the upper part of the digestion tube is provided with an interlayer overflow port.
Furthermore, the lower ends of the two groups of transparent quartz metering tubes are provided with ellipsoidal tubes, and the photoelectric switch is positioned above the ellipsoidal tubes.
Further, the liquid passage includes a plurality of three-way joints.
Compared with the prior art, the utility model has the following advantages and beneficial effects:
1. the method fully automates the steps of total nitrogen complete detection such as sampling, metering, mixing, digestion, ultraviolet spectrophotometry detection and the like, realizes automatic, rapid and accurate analysis of the total nitrogen content in water, has the advantages of accurate metering, good stability, automatic calibration, less maintenance and the like, and has wide application prospect.
2. The utility model has 4 sample feeding channels, can be automatically switched according to the requirement at regular time, and realizes the functions of automatic calibration of standard samples and the like.
3. The recovery system of the utility model distinguishes cleaning water and waste liquid, and greatly reduces the amount of waste liquid generated by the system.
4. The reagent metering component has high metering precision and good stability; the digestion reaction adopts an ultraviolet light assisted catalytic oxidation digestion technology, so that the high-efficiency digestion of a water sample can be realized under normal pressure, and the digestion time is shortened.
5. The light source of the ultraviolet photoelectric detection assembly uses a flashing xenon lamp, the safety voltage can be lightened, and the circuit safety is improved; a plurality of optical lenses are arranged between the light source and the detector, so that ultraviolet light emitted by the flashing xenon lamp is condensed in front of the colorimetric pool and penetrates through the colorimetric pool to ensure that the reaction liquid absorbs the ultraviolet light, and the ultraviolet light is orderly, dispersedly and uniformly irradiated on the whole 220nm/275nm diode detector light receiving surface after passing through the colorimetric pool, thereby improving the measurement accuracy.
Drawings
FIG. 1 is a schematic structural diagram of an on-line analyzer for total nitrogen in water provided by the utility model.
Fig. 2 is a connection block diagram of electrical elements of the water quality total nitrogen online analyzer provided by the utility model.
Description of reference numerals:
P1-P4: first to fourth peristaltic pumps, T1-T8: first to eighth three-way pinch valves, C: three-way joint, S1-S2: reagent bottle, S3: distilled water bottle, S4-S5: specific concentration sample bottle, S6: waste liquid barrel, S7: cleaning water recovery tub, a: reagent metering assembly, a1-a 2: first and second three-way solenoid gas valves, A3-a 6: first to fourth photoelectric switches, a 7-A8: quartz metering tube, X: digestion assembly, X1: ultraviolet lamp, X2: quartz digestion tube, X3: temperature sensor, X4: heating sheet, X5: heat insulation sponge layer, M: reaction cell assembly, M1: reaction cell, M2: magnetic stirrer fan blade, M3: stirring motor, L: ultraviolet photodetection assembly, L1: flash xenon lamp, L2: colorimetric cell, L3: 220nm/275nm diode detector.
Detailed Description
The present invention will be further illustrated with reference to the accompanying drawings and specific embodiments, which are to be understood as merely illustrative of the utility model and not as limiting the scope of the utility model.
The utility model provides an online analyzer for total nitrogen in water quality, as shown in figures 1 and 2, comprising: the device comprises a reagent metering component A, a digestion component X, a reaction pool component M, an ultraviolet photoelectric detection component L, a plurality of peristaltic pumps (P1-P4), and 4 sample feeding channels, a plurality of reagent sub-channels, a plurality of conveying sub-channels, a plurality of waste liquid sub-channels, a plurality of three-way pinch valves (T1-T8) and a plurality of three-way joints C which are used for connecting the components. The digestion assembly is connected with the reagent metering assembly through the reagent sub-channel, the sample introduction channel is used for metering and conveying water samples to the digestion assembly, the reaction tank assembly is connected with the digestion assembly through the conveying sub-channel, the ultraviolet photoelectric detection assembly is connected with the reaction tank assembly through the conveying sub-channel, waste liquid generated by each assembly is uniformly discharged into the waste liquid recovery barrel through the waste liquid sub-channel, and the cleaning water is uniformly discharged into the cleaning water recovery part through the waste liquid sub-channel. The singlechip is not drawn in fig. 1, but electronic components in each pump, valve, reagent metering assembly, digestion assembly, reaction tank assembly and ultraviolet photoelectric detection assembly are electrically connected with and controlled by the singlechip, and the connection schematic diagram is shown in fig. 2. In the utility model, one side of the three-way pinch valve is opened, and the other side is closed inevitably, all pumps are closed in the initial state, the left side of the three-way pinch valve (T1-5, 7-8) is opened, and the right side of the three-way pinch valve T6 is opened. The various liquid conveying channels are made of oxidation-resistant and corrosion-resistant hoses.
Specifically, the sample feeding channel comprises two peristaltic pumps (P2, P3) and two three-way pinch valves (T4, T5), and four channels are formed by opening and closing the peristaltic pumps and the pinch valves. The first channel is closed, the peristaltic pump P3 is closed, the peristaltic pump P2 is started to be opened to directly extract the surface water sample, and the surface water sample is pumped into the digestion assembly; when the right side of the three-way pinch valve T4 is closed, the peristaltic pump P2 is closed, and the peristaltic pump P3 is opened to draw distilled water in the distilled water bottle S3 to the digestion assembly; a third channel, wherein the right side of the three-way pinch valve T4 is opened, the left side of the three-way pinch valve T5 is opened, the peristaltic pump P2 is closed, and the peristaltic pump P3 is opened to pump the sample 3 in the sample bottle S4 with specific concentration to the digestion assembly; and a fourth channel, wherein the right side of the three-way pinch valve T4 is opened, the right side of the three-way pinch valve T5 is opened, the peristaltic pump P2 is closed, and the peristaltic pump P3 is opened to pump the sample 4 in the sample bottle S5 with the specific concentration to the digestion assembly.
The first to third three-way pinch valves (T1-T3) are connected with a first peristaltic pump P1, the peristaltic pump P4 is connected with a three-way pinch valve T6, the left side of the three-way pinch valve T6 is connected with the digestion assembly, and the right side of the three-way pinch valve T7 is connected with the left side of the three-way pinch valve T6. The right side of the three-way pinch valve T7 is connected with a waste liquid barrel. The left side of the three-way pinch valve T8 is connected with a waste liquid barrel S6, and the right side is connected with a washing water recovery barrel S7.
The reagent metering assembly comprises two groups of transparent quartz metering tubes (A7 and A8) which are used for metering a reagent 1 and a reagent 2 respectively. The lower end of each metering tube is connected with a three-way pinch valve (T1, T2), the two three-way pinch valves are connected with a reagent bottle on the left side, the digestion assembly is connected with the right side through a reagent sub-channel, when the left side is opened, a reagent can be sucked into the metering tubes for metering, and when the right side is opened, the reagent which completes metering is discharged into the digestion assembly. The upper end of the metering pipe is connected with three-way electromagnetic air valves (A1, A2), and the three-way electromagnetic air valves are linearly connected in series and are connected with a peristaltic pump P1 through the left side of a three-way pinch valve T3. The right side of the three-way pinch valve T3 is connected with a digestion assembly digestion pipe X2, and the right side of the three-way pinch valve (T1 and T2) is connected with a digestion assembly digestion pipe X2. The lower end of the metering tube is provided with an ellipsoid-shaped tube, the upper part and the lower part of the side surface are respectively provided with a photoelectric switch, and the photoelectric switches are positioned above the ellipsoid-shaped cavity. When the reagent 1 is metered, the left side of the three-way pinch valve T1, the left side of the three-way pinch valve T3 and the three-way electromagnetic air valves (A1 and A2) of the quartz metering tube A7 are opened, the peristaltic pump P1 rotates anticlockwise, and the reagent 1 is pumped into the quartz metering tube A7. When the liquid level of the reagent 1 in the metering tube reaches the photoelectric switch A3 above, the right side of the three-way pinch valve T1 is opened, the peristaltic pump P1 rotates clockwise, and the reagent 1 is injected into the digestion tube of the digestion assembly. When the liquid level of the reagent 1 drops to the photoelectric switch A4 at the lower part, the left side of the three-way pinch valve T1 is opened, and the peristaltic pump P1 is stopped. The metered volume of reagent 1 is equal to the cross-sectional area in the metering tube multiplied by the height difference of the upper and lower level switches. Reagent 2 metering is based on another group of quartz metering tubes, only A2 of the three-way electromagnetic air valve is opened during metering, and other procedures are similar to reagent 1 metering.
The digestion assembly main body is a double-layer hollow quartz digestion tube X2, an interlayer sample inlet is formed in the bottom of the digestion assembly main body, an interlayer overflow port is formed in the upper portion of the digestion assembly main body, a heating sheet X4 is wrapped outside the whole digestion assembly main body, a temperature sensor X3 is embedded between the heating sheet X4 and the digestion tube, and an ultraviolet lamp tube X1 is inserted into a hollow position from an upper opening of the digestion tube X2. The ultraviolet lamp X1, the heating plate X4 and the temperature sensor X3 are electrically connected with the single chip microcomputer, the heating plate X4 is controlled by the single chip microcomputer, the single chip microcomputer collects data X3 of the temperature sensor, and the digestion assembly is wholly wrapped by a heat insulation sponge layer X5. A sample inlet at the bottom of the digestion tube X2 is communicated with the left side of a sixth three-way pinch valve T6, the right side of a third three-way pinch valve T3, the right side of a first three-way pinch valve T1, the right side of a second three-way pinch valve T2, a second peristaltic pump P2 and a third peristaltic pump P3. An overflow port of the digestion pipe X2 is connected to the left side of an eighth three-way pinch valve T8. During digestion, a water sample and a reagent are sequentially injected into an interlayer space of the digestion tube, an ultraviolet lamp is turned on to provide ultraviolet light to the periphery, and meanwhile, a heating sheet starts to work; when the temperature value received by the single chip microcomputer from the temperature sensor is lower than a preset low value, the single chip microcomputer keeps the heating sheet open and heats the liquid in the digestion tube; when the temperature value received by the singlechip reaches a preset high value, the heating sheet is controlled to be disconnected, heating is stopped, and overlarge pressure in the pipe caused by overhigh temperature is prevented; the right side of the three-way pinch valve T3 is opened, and the peristaltic pump P1 rotates clockwise to pump air into the interlayer space of the digestion tube, so that the water sample is ensured to be subjected to thorough digestion reaction.
The reaction cell assembly M comprises a reaction cell M1, a magnetic stirring fan M2 and a stirring motor M3. The sample inlet at the bottom of the reaction tank is connected with a peristaltic pump P4, the peristaltic pump P4 is connected with a three-way pinch valve T6, the left side of the three-way pinch valve T6 is connected with a digestion tube, and the right side of the three-way pinch valve T6 is connected with an ultraviolet photoelectric detection assembly. The reaction tank is also connected with a waste liquid pipeline, and can empty waste liquid. The left side of the three-way pinch valve T6 is opened, and the digestion water sample in the digestion tube can be input into the reaction tank when the peristaltic pump P4 rotates clockwise, and the digestion water sample is further uniformly stirred and radiated in the reaction tank to obtain the color developing solution. The problems of water mist generation on the side surface of the colorimetric pool, change of the refractive index in the colorimetric pool and the like are easily caused by overhigh temperature of the color developing solution, so that the analysis error of photoelectric detection can be reduced by uniformly mixing and cooling the digestion solution.
The shell of the ultraviolet photoelectric detection component L is an opaque rectangular box body, a flashing xenon lamp L1 with safe voltage is arranged on one side, a 220nm/275nm diode detector L3 is arranged on the other side, a quartz colorimetric pool L2 is arranged at the position close to the diode detector, and a plurality of optical lenses are arranged among the ultraviolet photoelectric detection component L, the ultraviolet photoelectric detection component L and the quartz colorimetric pool L2, so that light rays of the flashing xenon lamp passing through the colorimetric pool can uniformly irradiate the whole 220nm/275nm diode detector light receiving surface. The upper and lower ports of the colorimetric pool L2 are connected with a liquid conveying channel, the upper end is connected to the lower end of a three-way pinch valve T8, and the lower end is connected to the left side of a three-way pinch valve T7. The flashing xenon lamp and the diode detector are electrically connected with the singlechip, and the electric signal collected by the diode detector is transmitted to the singlechip. During detection, light emitted by the flashing xenon lamp passes through the colorimetric pool filled with color development liquid to reach the light receiving surface of the diode detector, and the single chip microcomputer collects two electric signals from the diode detector, wherein the two electric signals respectively represent the ultraviolet light intensity at the wavelength of 220nm and the ultraviolet light intensity at the wavelength of 275 nm.
Based on the above water total nitrogen analyzer, water sample test experiments as shown in examples 1-4 were performed. The composition of the reagent 1 is 40g/L potassium persulfate solution; the composition of the reagent 2 is 32g/L sodium hydroxide and 53g/L boric acid solution.
Example 1 Total Nitrogen Low concentration Water sample test (0.05 to 7mg/L)
The structure of the online analyzer for total nitrogen in water quality of the embodiment is shown in fig. 1, before the analyzer operates, reagents 1 and 2 in bottles S1 and S2 and distilled water in a bottle S3 are required to be supplemented, and the analysis is performed according to the following specific steps:
step 1, pipeline rinsing
And (3) rotating the sample feeding channel I and the peristaltic pump P2 anticlockwise, and extracting a water sample to fill the digestion tube. Subsequently, the left side of the three-way pinch valve T6 was opened, the peristaltic pump P2 was stopped, the peristaltic pump P4 was rotated clockwise to pump rinse water into the reaction cell, and magnetic stirring was simultaneously initiated. After the magnetic stirring is stopped, the right side of the three-way pinch valve T6 is opened, the peristaltic pump P4 rotates anticlockwise, the rinsing water sample is pumped into the colorimetric pool through the left side of the three-way pinch valve T7, and is discharged into the rinsing water recovery barrel through the right side of the three-way pinch valve T8.
The peristaltic pump P4 rotates clockwise, the residual rinse water in the colorimetric pool is pumped into the reaction pool, then the right side of the three-way pinch valve T7 is opened, the peristaltic pump P4 rotates counterclockwise, and a small amount of rinse water left in the reaction pool is emptied along the waste liquid pipeline.
Step 2, reagent metering
The left side of the three-way pinch valve T6 is closed, the peristaltic pump P1 rotates anticlockwise, and reagent 1 and reagent 2 are sequentially pumped into the reagent metering assembly to be metered. After metering is completed, the right side of the three-way pinch valve (T1-T2) is opened, and the peristaltic pump P1 rotates clockwise to pump the completed quantitative reagent 1 and reagent 2 into the digestion tube.
The left side of the three-way pinch valve T1, the left side of the three-way pinch valve T3 and the three-way electromagnetic air valve (A1-A2) are opened, the peristaltic pump P1 rotates anticlockwise, and the reagent 1 is pumped into the quartz metering tube A7. When the singlechip receives a signal of the photoelectric switch A3, the right side of the three-way pinch valve T1 is opened, the peristaltic pump P1 rotates clockwise, and the reagent 1 is injected into the digestion tube. The adding amount of the reagent 1 is 2mL, when the liquid level of the reagent 1 drops to a photoelectric switch A4 at the lower part, the left side of a three-way pinch valve T1 is opened, and a peristaltic pump P1 is stopped. The adding amount of the reagent 2 is 2mL, the reagent is metered through a quartz metering tube A8, a three-way electromagnetic air valve is only opened A2, and other procedures are similar to the metering of the reagent 1.
Step 3, sample introduction
And a sample introduction channel I, wherein a peristaltic pump P2 rotates anticlockwise, the flow rate (V) of the peristaltic pump is fixed, the first dose volume V of the water sample introduction is t multiplied by V, and the water sample quantification is realized by setting the rotation time (t) of the peristaltic pump. In this case, 40mL of water sample was drawn into the digestion tube.
The uv lamp and heating plate in the digestion module were turned on and the mixed liquor was heated to 90 ℃. Then the peristaltic pump P1 rotates clockwise, the right side of the three-way pinch valve T3 is opened, air is continuously blown into the digestion tank, and the digestion of the total nitrogen is accelerated for 10 min.
Step 5, colorimetric measurement
After digestion is finished, the left side of the three-way pinch valve (T3, T6) is opened, and the peristaltic pumpAnd (3) pumping the digestion solution into the reaction tank by clockwise rotation of P4, starting magnetic stirring, and naturally radiating heat by the digestion solution to obtain the color development solution. 5min later, the right side of the three-way pinch valve T6 is opened, the left side of the three-way pinch valve (T7-8) is opened, the peristaltic pump P4 rotates counterclockwise, the color development liquid is pumped into the ultraviolet photoelectric detection component for photoelectric measurement, and the absorbance A is measured220、A275。
The mass concentration ρ of total nitrogen can be calculated by the formula (2)
Wherein,
a-measured target absorbance value (A ═ A)220-2A275)
b1Intercept of calibration curve for low total nitrogen concentration
a1Slope of calibration curve for low total nitrogen concentration
After the measurement is completed, the peristaltic pump P4 is rotated clockwise to pump the residual color developing solution in the colorimetric pool into the reaction pool. Then the right side of the three-way pinch valve T7 is opened, the peristaltic pump P4 rotates anticlockwise, and the color development liquid left in the reaction tank is emptied along the waste liquid pipeline.
The left side of the three-way pinch valve T6, the right side of the three-way pinch valve T4 and the peristaltic pump P2 are closed, and the peristaltic pump P3 is opened to draw distilled water to fill the digestion tube. Subsequently, the left side of the three-way pinch valve T6 was opened, the peristaltic pump P4 was opened to pump distilled water into the reaction cell, and magnetic stirring was simultaneously started. After the magnetic stirring is stopped, the right side of the three-way pinch valve T6 is opened, the peristaltic pump P4 rotates anticlockwise, the distilled water sample is pumped into the colorimetric pool through the left side of the three-way pinch valve T7, and is discharged into the cleaning water recovery barrel through the right side of the three-way pinch valve T8.
Then the peristaltic pump P4 rotates clockwise to pump the residual distilled water in the colorimetric pool into the reaction pool, then the right side of the three-way pinch valve T7 is opened, the peristaltic pump P4 rotates counterclockwise to drain the residual distilled water in the reaction pool along the waste liquid pipeline.
The washing was repeated once.
Example 2 Total Nitrogen high concentration Water sample test (7 to 100mg/L)
The structure and the composition, the initial state and the reagent bottle loading of the water quality total phosphorus on-line analyzer provided by the embodiment of the utility model are the same as those of the embodiment 1.
In this example, the steps of the total nitrogen high concentration water sample test are the same as those in example 1 except for step 3, step 4 and step 5. In the step 3, distilled water is required to be introduced to dilute the water sample, and the calibration curve in the step 5 is correspondingly changed, specifically as follows:
step 3, sample introduction (dilution)
The first sample feeding channel rotates anticlockwise through a peristaltic pump P2, and a water sample is extracted to the digestion tube; a sample feeding channel II, the right side of the three-way pinch valve T4 and the peristaltic pump P2 are closed, and the peristaltic pump P3 clockwise pumps distilled water (S3) to the digestion tube; the flow rate (v) of the peristaltic pump is fixed, and the water sample is quantitatively extracted by setting the rotation time (t) of the peristaltic pump
The volume of distilled water is extracted
The total injection amount is 40 mL.
The uv lamp and heating plate in the digestion module were turned on and the mixed liquor was heated to 95 ℃. Then the peristaltic pump P1 rotates clockwise, the right side of the three-way pinch valve T3 is opened, air is continuously blown into the digestion tank, and the digestion of the total nitrogen is accelerated for 20 min.
Step 5, colorimetric measurement
After digestion is finished, the left side of the three-way pinch valve (T3 and T6) is opened, the peristaltic pump P4 rotates clockwise, digestion liquid is pumped into the reaction tank, magnetic stirring is started simultaneously, and the digestion liquid naturally dissipates heat to obtain color development liquid. 5min later, the right side of the three-way pinch valve T6 is opened, the left side of the three-way pinch valve (T7-8) is opened, the peristaltic pump P4 rotates counterclockwise, the color development liquid is pumped into the ultraviolet photoelectric detection component for photoelectric measurement, and the absorbance A is measured220、A275。
The mass concentration ρ of total nitrogen can be calculated by the formula (3)
Wherein,
a-measured target absorbance value (A ═ A)220-2A275)
bnIntercept of calibration curve for high total nitrogen concentration
anSlope of calibration curve for high total nitrogen concentration
After the measurement is completed, the peristaltic pump P4 is rotated clockwise to pump the residual color developing solution in the colorimetric pool into the reaction pool. Then the right side of the three-way pinch valve T7 is opened, the peristaltic pump P4 rotates anticlockwise, and the color development liquid left in the reaction tank is emptied along the waste liquid pipeline.
EXAMPLE 3 Low concentration Standard sample calibration test (X mg/L, and X. ltoreq.7 mg/L)
The structure, composition and initial state of the water quality total phosphorus on-line analyzer in the embodiment are the same as those in the embodiment 1. Before the instrument is operated, the bottles S1 and S2, namely reagent 1 and reagent 2, are filled with distilled water in the bottle S3, and the bottle S4 is filled with a standard sample with the concentration of X mg/L.
The standard sample calibration test procedure was the same as in example 1 except for steps 1 and 3.
Step 1, pipeline rinsing
A sample feeding channel III is formed, the right side of the three-way pinch valve T4 and the left side of the three-way pinch valve T5 are opened, and the peristaltic pump P3 rotates clockwise to draw a standard sample (S4) to the digestion assembly; subsequently, the left side of the three-way pinch valve T6 was opened, the peristaltic pump P3 was stopped, the peristaltic pump P4 was rotated clockwise to pump the standard sample into the reaction cell, and magnetic stirring was simultaneously started. After the magnetic stirring is stopped, the right side of the three-way pinch valve T6 is opened, the peristaltic pump P4 rotates anticlockwise, the standard sample is pumped into the colorimetric pool through the left side of the three-way pinch valve T7, and is discharged into the cleaning water recovery barrel through the right side of the three-way pinch valve T8.
The peristaltic pump P4 rotates clockwise, the residual rinse water in the colorimetric pool is pumped into the reaction pool, then the right side of the three-way pinch valve T7 is opened, the peristaltic pump P4 rotates counterclockwise, and a small amount of rinse water left in the reaction pool is emptied along the waste liquid pipeline.
Step 3, sample introduction
And a third sample feeding channel, wherein the right side of the three-way pinch valve T4 and the left side of the three-way pinch valve T5 are opened, and the peristaltic pump P3 rotates clockwise to draw the standard sample (S4) to the digestion assembly. The flow rate V of the peristaltic pump is fixed, the first dose volume V of the standard sample is t multiplied by V, and the water sample is quantified by setting the rotation time (t) of the peristaltic pump. In this case, 40mL of water sample was drawn into the digestion tube.
Calculating by formula (2) in step 5 to obtain the detection concentration rho of the standard sample1The detection deviation amplitude of the instrument low-concentration standard sample is
Example 4 high concentration Standard sample calibration test (X mg/L, and X > 7mg/L)
The structure, composition and initial state of the water quality total phosphorus on-line analyzer in the embodiment are the same as those in the embodiment 1. Before the instrument is operated, the reagent bottles 1 and 2 in the bottles S1 and S2 are filled, the distilled water in the bottle S3 is filled, and the standard sample with the concentration of X mg/L in the bottle S5 is filled.
The standard sample calibration test procedure was the same as in example 2 except for steps 1 and 3.
Step 1, pipeline rinsing
A sample feeding channel IV, wherein the right side of the three-way pinch valve T4 and the right side of the three-way pinch valve T5 are opened, and the peristaltic pump P3 rotates clockwise to draw a standard sample (S5) to the digestion tube; subsequently, the left side of the three-way pinch valve T6 was opened, the peristaltic pump P3 was stopped, the peristaltic pump P4 was rotated clockwise to pump the standard sample into the reaction cell, and magnetic stirring was simultaneously started. After the magnetic stirring is stopped, the right side of the three-way pinch valve T6 is opened, the peristaltic pump P4 rotates anticlockwise, the standard sample is pumped into the colorimetric pool through the left side of the three-way pinch valve T7, and is discharged into the cleaning water recovery barrel through the right side of the three-way pinch valve T8.
The peristaltic pump P4 rotates clockwise, the residual rinse water in the colorimetric pool is pumped into the reaction pool, then the right side of the three-way pinch valve T7 is opened, the peristaltic pump P4 rotates counterclockwise, and a small amount of rinse water left in the reaction pool is emptied along the waste liquid pipeline.
Step 3, sample introduction (dilution)
A sample feeding channel IV, wherein the right side of the three-way pinch valve T4 and the right side of the three-way pinch valve T5 are opened, and the peristaltic pump P3 rotates clockwise to draw a standard sample (S5) to the digestion tube; the right side of the sample inlet channel II, a three-way pinch valve T4 and a peristaltic pump P2 are closed, and the peristaltic pump P3 is used for pumping distilled water (S3) to the digestion tube clockwise; the flow rate (v) of the peristaltic pump is fixed, and the water sample is quantitatively extracted by setting the rotation time (t) of the peristaltic pump
The volume of distilled water is extracted
The total injection amount is 40 mL.
Calculating by formula (3) in step 5 to obtain the detection concentration rho of the standard sample1The detection deviation amplitude of the high-concentration standard sample of the instrument is
The technical means disclosed in the utility model scheme are not limited to the technical means disclosed in the above embodiments, but also include the technical scheme formed by any combination of the above technical features. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and such improvements and modifications are also considered to be within the scope of the present invention.
Claims (6)
1. The utility model provides a quality of water total nitrogen on-line analyzer which characterized in that includes: the device comprises a reagent metering component, a digestion component, a reaction tank component, an ultraviolet photoelectric detection component, a single chip microcomputer, a plurality of three-way pinch valves and a plurality of peristaltic pumps; the reagent metering assembly, the digestion assembly, the reaction tank assembly and the ultraviolet photoelectric detection assembly are connected through various liquid conveying channels, wherein each electronic component is electrically connected with the single chip microcomputer;
the reagent metering assembly comprises two groups of transparent quartz metering tubes, the lower ends of the two metering tubes are respectively connected with a first three-way pinch valve and a second three-way pinch valve, the left sides of the first three-way pinch valve and the second three-way pinch valve are connected with a reagent bottle, and the right sides of the first three-way pinch valve and the second three-way pinch valve are connected with the digestion assembly; the upper end of the metering pipe is connected with three-way electromagnetic air valves, all the three-way electromagnetic air valves are linearly connected in series and are connected with the first peristaltic pump through the left side of a third three-way pinch valve, photoelectric switches are respectively arranged at the upper part and the lower part of the side surface of the metering pipe, and the generated electric signals indirectly control the three-way electromagnetic air valves, the first to third three-way pinch valves and the first peristaltic pump to operate through a single chip microcomputer; the first to third three-way pinch valves are connected with the first peristaltic pump;
the digestion assembly main body is a digestion tube, the bottom of the digestion assembly main body is provided with a sample inlet, the upper part of the digestion assembly main body is provided with an overflow port, the heating sheet is wrapped outside the whole digestion assembly main body, a temperature sensor is embedded between the heating sheet and the digestion tube, and an ultraviolet lamp tube is inserted into an opening at the upper part of the digestion tube; the heating plate is electrically connected with the temperature sensor and the singlechip, and the singlechip collects data of the temperature sensor and controls the heating plate and the ultraviolet lamp tube to work; the digestion tube sample inlet is connected to the left side of a sixth three-way pinch valve, the right side of a third three-way pinch valve, the right sides of a first three-way pinch valve and a second three-way pinch valve, a second peristaltic pump and a third peristaltic pump, and the overflow port is connected to the left side of an eighth three-way pinch valve;
the reaction tank assembly comprises a reaction tank, magnetic stirring blades and a stirring motor, and a sample inlet at the bottom of the reaction tank is connected with a fourth peristaltic pump;
the ultraviolet photoelectric detection assembly is an opaque box body, a light source is arranged on one side of the ultraviolet photoelectric detection assembly, a diode detector is arranged on the other side of the ultraviolet photoelectric detection assembly, a quartz colorimetric pool is arranged at a position close to the diode detector, the upper opening and the lower opening of the colorimetric pool are connected with the liquid conveying channel, and the light source and the diode detector are electrically connected with the single chip microcomputer;
the fourth peristaltic pump is connected with a sixth three-way pinch valve, the left side of the sixth three-way pinch valve is connected with the digestion assembly, the right side of the sixth three-way pinch valve is connected with the left side of a seventh three-way pinch valve, the right side of the seventh three-way pinch valve is connected with the waste liquid barrel, the left side of an eighth three-way pinch valve is connected with the waste liquid barrel, and the right side of the eighth three-way pinch valve is connected with the cleaning water recovery barrel.
2. The online analyzer for total nitrogen in water according to claim 1, wherein the light source is a flash xenon lamp with safe voltage, and the diode detector is a 220nm/275nm diode detector.
3. The online analyzer of total nitrogen in water according to claim 2, wherein there are several optical lenses between the scintillation xenon lamp and the 220nm/275nm diode detector.
4. The online analyzer for total nitrogen in water quality according to claim 1, wherein the digestion tube is a double-layer hollow quartz digestion tube, the bottom of the digestion tube is provided with an interlayer sample inlet, and the upper part of the digestion tube is provided with an interlayer overflow port.
5. The on-line analyzer for total nitrogen in water quality as claimed in claim 1, wherein the two sets of transparent quartz metering tubes have an ellipsoidal tube at the lower end, and the photoelectric switch is located above the ellipsoidal tube.
6. The on-line analyzer for total nitrogen in water according to claim 1, wherein the liquid conveying channel comprises a plurality of three-way joints.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202121914191.4U CN216669721U (en) | 2021-08-16 | 2021-08-16 | Water quality total nitrogen analyzer |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202121914191.4U CN216669721U (en) | 2021-08-16 | 2021-08-16 | Water quality total nitrogen analyzer |
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