CN114235730A - Seawater nutrient salt online monitoring system and seawater nutrient salt detection method - Google Patents
Seawater nutrient salt online monitoring system and seawater nutrient salt detection method Download PDFInfo
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- CN114235730A CN114235730A CN202210154665.2A CN202210154665A CN114235730A CN 114235730 A CN114235730 A CN 114235730A CN 202210154665 A CN202210154665 A CN 202210154665A CN 114235730 A CN114235730 A CN 114235730A
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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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
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Abstract
The invention discloses an online monitoring system and a detection method for seawater nutritive salt, wherein the monitoring system comprises a sealed cabin, a main control module, a detection module, a reagent accommodating device, a liquid inlet interface and an air interface; the detection module comprises a first detection module, a second detection module, a third detection module and a fourth detection module, wherein the first detection module, the second detection module, the third detection module and the fourth detection module are independently arranged and used for detecting nitrate and nitrite; during detection, the first detection module, the second detection module, the third detection module and the fourth detection module work independently, detect different nutritive salts in the seawater respectively, and introduce the air mass in the detection to defoam. The invention has the advantages of high detection precision, small drift amount, stable and reliable operation, small detection reagent amount and small detection waste liquid amount, and can simultaneously or independently complete the in-situ online analysis and monitoring of 5 nutrient salts of nitrate, nitrite, ammonia nitrogen, phosphate and silicate.
Description
Technical Field
The invention relates to the technical field of water quality monitoring, in particular to an online seawater nutrient salt monitoring system and a seawater nutrient salt detection method.
Background
The nutritive salt in the seawater mainly comprises inorganic nitrogen, active phosphate, active silicate and other components, and is a necessary nutrient element for the growth of the marine phytoplankton. The different concentrations and compositions of nutritive salt in seawater not only can influence the primary productivity of the ocean, but also can produce the regulation effect on the community structure of phytoplankton, thereby influencing the structure of the marine ecosystem. Therefore, the monitoring of the concentration distribution and the change of the nutritive salt in the seawater has important scientific significance for evaluating the eutrophication of the water body, and understanding the geochemical cycle of nitrogen, phosphorus and silicon elements in the ocean and the key process of an ocean ecosystem.
At present, the analysis of nutritive salt in seawater mainly adopts a method of sampling on site and measuring in a laboratory, and the method has the defects of poor real-time performance, easy pollution of a sample to be measured, waste of manpower and material resources and the like.
The existing on-line seawater nutrient salt analyzers are used for measuring nutrient salts in seawater, but due to the limitation of the volume of the analyzers, the existing on-line seawater nutrient salt analyzers generally adopt a single module to detect in sequence, seawater to be detected flows in a plurality of detection modules, the detection of the nutrient salts is carried out when the seawater to be detected flows to a specific detection module, the measurement error is generally about-20% to +45%, the measurement error is large, and the reagent consumption is high. The last decades of marine monitoring research have demonstrated that the existing on-line seawater nutrient salt analyzers cannot meet the increasingly urgent need for marine ecological environment monitoring and protection.
Therefore, there is a need to provide a new technical solution to solve the above problems.
Disclosure of Invention
In order to solve the technical problem, the application provides an online monitoring system for seawater nutrient salts, which can improve the online monitoring precision of the seawater nutrient salts, reduce the generation of waste liquid in the detection process of the seawater nutrient salts and reduce water body pollution.
An online monitoring system for seawater nutrient salt comprises:
sealing the cabin;
the main control module is arranged in the sealed cabin;
the detection module is arranged in the sealed cabin and comprises a first detection module for detecting nitrate and nitrite, a second detection module for detecting phosphate, a third detection module for detecting ammonium salt and a fourth detection module for detecting silicate; the first detection module, the second detection module, the third detection module and the fourth detection module are arranged independently;
the reagent containing device is arranged outside the sealed cabin and is communicated with the detection module through a pipeline;
the liquid inlet interface is communicated with the detection module;
an air interface in communication with the detection module.
Preferably, the detection module comprises an injection device and a photoelectric detection device; the injection device includes a syringe pump and a multi-position valve, the syringe pump being in communication with the multi-position valve.
Preferably, the photoelectric detection device comprises a flow cell, a light source and a receiver; the flow cell, the light source and the receiver are configured to detect and reference light paths; the flow cell is in communication with the multi-position valve.
Preferably, the device further comprises a waste liquid storage device; the waste liquid storage device is communicated with the flow cell.
Preferably, the system also comprises a handheld terminal; the handheld terminal is connected with the main control module in a wired communication or wireless communication mode.
A seawater nutrient salt detection method utilizes the seawater nutrient salt on-line monitoring system to detect seawater nutrient salt, and comprises the following steps:
respectively measuring the absorbance values of the deionized water and the standard solution;
drawing a standard curve according to the concentrations of the deionized water and the standard solution, and the absorbance values of the deionized water and the standard solution;
fully mixing a water sample with a detection reagent, and measuring the absorbance value of the mixture of the water sample and the detection reagent;
and (3) bringing the absorbance value of the mixture of the water sample and the detection reagent into a standard curve and calculating to obtain the concentration parameter of the nutrient salt to be detected in the water sample.
Preferably, when the absorbance values of the deionized water, the standard solution and the detection reagent are detected, air is introduced into the seawater nutrient salt online monitoring system for defoaming.
Preferably, the method for detecting nitrite comprises:
respectively extracting a quantitative water sample, a quantitative detection reagent A and quantitative air, and fully mixing in a circulating push-out and suction mode to obtain a mixture A;
pushing the mixture A into a photoelectric detection device to detect the absorbance value of the mixture A;
and substituting the absorbance value of the mixture A into a nitrite detection standard curve for operation to obtain the concentration parameter of nitrite in the water sample.
Preferably, the detection method of nitrate comprises:
a quantitative water sample is extracted and pushed into a first detection module for reduction to obtain a mixture B;
taking the mixture B and the quantitative detection reagent A to be fully mixed in a circulating pushing-out and sucking-in mode to obtain a mixture C;
pushing the mixture C into a photoelectric detection device to detect the absorbance value of the mixture C;
and substituting the absorbance value of the mixture C into a nitrate detection standard curve for operation to obtain the concentration parameter of the nitrate in the water sample.
Preferably, the phosphate detection method comprises:
respectively extracting a quantitative water sample, a quantitative detection reagent B, a quantitative detection reagent C and quantitative air, and fully mixing in a circulating push-out and suction manner to obtain a mixture D;
pushing the mixture D into a photoelectric detection device to detect the absorbance value of the mixture D;
and substituting the absorbance value of the mixture D into a phosphate detection standard curve for operation to obtain the concentration parameter of phosphate in the water sample.
Preferably, the detection method of the ammonium salt comprises:
heating the third detection module to a preset temperature;
a quantitative water sample, a quantitative detection reagent D and quantitative air are extracted and fully mixed in a circulating push-out and suction mode to obtain a mixture E;
pumping a certain amount of detection reagent E and fully mixing the detection reagent E and the mixture E in a circulating push-out and suction mode to obtain a mixture F;
pumping a certain amount of detection reagent F and fully mixing the detection reagent F and the mixture F in a circulating push-out and suction mode to obtain a mixture G;
pushing the mixture G into a photoelectric detection device to detect the absorbance value of the mixture G;
and substituting the absorbance value of the mixture G into an ammonium salt detection standard curve for operation to obtain the concentration parameter of the ammonium salt in the water sample.
Preferably, the detection method of the silicate comprises the following steps:
respectively extracting a quantitative water sample, a detection reagent G and air, and fully mixing in a circulating push-out and suction mode in a flow cell to obtain a mixture H;
taking a certain amount of detection reagent H and the mixture H, and fully mixing in a circulating push-out and suction mode to obtain a mixture I;
taking a certain amount of detection reagent I and the mixture I, and fully mixing in a circulating push-out and suction mode to obtain a mixture J;
pushing the mixture J into a photoelectric detection device to detect the absorbance value of the mixture J;
and substituting the absorbance value of the mixture J into a silicate detection standard curve for operation to obtain the concentration parameter of silicate in the water sample. Compared with the prior art, the application has at least the following beneficial effects:
the seawater nutrient salt on-line monitoring system adopts mutually independent detection modules to detect seawater nutrient salt, has high detection precision, small drift amount, stable and reliable operation, small detection reagent amount and small detection waste liquid amount, can simultaneously or independently realize in-situ on-line analysis and monitoring of 5 nutrient salts of nitrate, nitrite, ammonium salt, phosphate and silicate, is suitable for buoys, shore bases, ships and laboratories, and improves the real-time on-line monitoring capability of seawater nutrient salt in marine ecological environment;
when the seawater nutritive salt is detected, the influence of the water color on the detection is deducted by adopting an actual water sample, so that the interference of environmental factors is avoided; the reference light path in the detection module controls the brightness of the LED, and detection inconsistency caused by LED attenuation is reduced, so that the detection precision is improved; the method of introducing the air mass for defoaming effectively avoids the influence of small bubbles in the detection flow path on the detection result, and meanwhile, the air mass can also seal the detection pool, so that other liquid is prevented from entering the detection pool, the detection pool is not polluted, and the detection precision is further improved; the instrument reagent directly contacts with the environmental water body, so that the influence of the environmental temperature on the detection is reduced, and meanwhile, the water body temperature is utilized to avoid the reagent from losing efficacy in a high-temperature environment.
Drawings
FIG. 1 is a schematic diagram of the overall structure of an on-line monitoring system for seawater nutrient salts according to the present invention;
FIG. 2 is a schematic structural diagram of a seawater nutrient salt on-line monitoring system of the present invention with a hidden protective cover;
FIG. 3 is a schematic diagram of the internal structure of an on-line monitoring system for seawater nutrient salts according to the present invention;
FIG. 4 is a schematic structural diagram of a photoelectric detection device of an online seawater nutrient salt monitoring system according to the present invention;
FIG. 5 is a schematic view of the overall process of a method for detecting seawater nutrient salts according to the present invention.
Wherein the figures include the following reference numerals:
1. the device comprises a protective cover, 2, a sealed cabin, 3, a handle, 4, a waterproof joint, 5, a liquid inlet interface, 6, an air interface, 7, a reagent accommodating device fixing piece, 8, a supporting rod, 9, a supporting plate, 10, a main control module, 11, a power supply module, 12, a communication module, 13, a first detection module, 14, a second detection module, 15, a third detection module, 16 and a fourth detection module; 17. reagent containing device, 18, photoelectric detection device;
201. a deck lid 202, a deck body;
1801. the flow cell 1802, detect light source, 1803, reference light source, 1804, detect fixing base, 1805, reference light path receiver, 1806, detection light path receiver.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions of the present application will be described in detail and completely with reference to the following specific embodiments of the present application and the accompanying drawings. It should be apparent that the described embodiments are only some of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
As shown in fig. 1, an online monitoring system for seawater nutrient salts comprises: a protective cover 1, a sealed cabin 2 and a handle 3. The protective cover 1 covers the outside of the sealed cabin 2 and is used for protecting the sealed cabin 2. The handle 3 is fixed on the top of the sealed cabin 2 and is used for fixing the seawater nutrient salt online monitoring system with an external buoy or a ship body and the like for monitoring.
As shown in fig. 2 and with reference to fig. 3, the capsule 2 comprises a lid 201 and a body 202. The waterproof connector 4, the liquid inlet interface 5 and the air interface 6 are all arranged on the upper portion of the cabin cover 201, and the liquid inlet interface 5 is communicated with an external detection water sample pipe or a detection reagent pipe and is used for enabling a water sample or a detection reagent to enter the cabin body 202 for corresponding detection. The waterproof connector 4 is used for electrically connecting components inside the sealed cabin 2 with external parts. The air interface 6 is used for introducing external air into the sealed cabin 2 for introducing air in the seawater nutrient salt detection. The reagent holding device fixing member 7 is provided on the outer wall of the chamber body 202 for fixing the reagent holding device 17.
As shown in fig. 3, the capsule 2 has a cavity therein, and the support plate 9 has a plurality of layers and is disposed in the capsule 2 to divide the cavity into a plurality of independent spaces. The supporting plate 9 is fixedly supported by the supporting rod 8, and the stability of the supporting plate 9 is improved. The main control module 10, the power supply module 11, the communication module 12 and the detection module are all fixed in the sealed cabin 2. The detection modules comprise a first detection module 13 for detecting nitrate or nitrite, a second detection module 14 for detecting phosphate, a third detection module 15 for detecting ammonium salts and a fourth detection module 16 for detecting silicates. First detection module 13, second detection module 14, third detection module 15 and fourth detection module 16 set up each other independently, can carry out independent detection to nitrate or nitrite, phosphate, ammonium salt and silicate respectively for do not receive the pollution between each detection module, and this kind of structure can shorten the circulation pipeline, under the condition of a small amount of water samples, can detect out corresponding nutritive salt content, reduces detect reagent's use, reduce the production of detection waste liquid when improving detection precision. The first detection module 13 has a cadmium ring therein for reducing nitrate. The detection module comprises an injection device (not shown in the figures) comprising a syringe pump and a multi-position valve, the syringe pump being in communication with the multi-position valve, and a photo detection device 18. The injection pump and the multi-position valve are of conventional models sold in the market.
The reagent holding device 17 is disposed outside the sealed cabin 2 through the reagent holding device fixing member 7, and is used for detecting the holding of the reagent, and is preferably a reagent holding bag made of a flexible material. The reagent containing device 17 is communicated with the detection module through a pipeline and the liquid inlet interface 5. The detection reagent is fast deteriorated or even invalid after the temperature exceeds 30 ℃, the detection precision is influenced, and the temperature of the existing in-situ nutrient salt analyzer cabin exceeds 40 ℃ or even higher due to heat release of a plurality of components in the operation, so that the detection reagent has great influence on the monitoring of the seawater nutrient salt. Reagent accommodate device 17 sets up in sealed cabin 2 outsidely, and with external sea water contact, because the sea water temperature can not exceed 30, utilize the sea water to preserve, can effectively prevent that the detect reagent is rotten, simultaneously, detect reagent temperature and sea water are with the temperature, improve and detect the precision, can save sealed cabin 2's volume simultaneously. In addition, an air interface 6 is communicated with the detection module and used for introducing air in the detection of the seawater nutrient salt.
As shown in fig. 4, the photo-detecting device 18 includes a flow cell 1801, a detection light source 1802, a reference light source 1803, a detection holder 1804, a reference light path receiver 1805 and a detection light path receiver 1806. The flow cell 1801 is communicated with the multi-position valve, so that liquid and gas in the multi-position valve can be pumped into the flow cell 1801 under the action of the syringe pump.
The detection light source 1802 is fixed on the detection fixing seat 1804, and the light beam emitted by the detection light source 1802 passes through the flow cell 1801 and then is received by the detection light path receiver 1806, so as to form a detection light path. The reference light source 1803 is fixed on the detection fixing seat 1804, and a light beam emitted by the reference light source 1803 passes through the flow cell 1801 and is received by the reference light path receiver 1805, so as to form a reference light path.
The detection light source 1802 and the reference light source 1803 both adopt single-wavelength LED light sources, and the wavelength selection of the LED light sources for different nutrient salts is different, specifically: the photoelectric detection device 18 in the first detection module 13 for detecting nitrate or nitrite is an LED light source with the wavelength of 550 nm; the photoelectric detection device 18 in the second detection module 14 for detecting phosphate is an LED light source with the wavelength of 880 nm; the photoelectric detection device 18 in the third detection module 15 for detecting ammonium salt is an LED light source with the wavelength of 660 nm; the fourth detection module 16 for detecting silicates is chosen as an LED light source at 820 nm.
As an embodiment of the present invention, the seawater nutrient salt online monitoring system further includes a waste liquid storage device (not shown in the figure), which is communicated with the flow cell and can store a detection reagent and a water sample mixture after detection, so as to prevent seawater pollution caused by direct discharge.
As an embodiment of the present invention, the seawater nutrient salt on-line monitoring system further comprises a handheld terminal (not shown in the figure). The handheld terminal can be electrically connected with the power supply module 11 through a line and is powered on site by the power supply module 11. The hand-held terminal is connected with the main control module 10 through the communication module 12 in a wired communication or wireless communication mode. The wired communication is preferably R485 communication. The wireless communication is preferably any one of bluetooth communication, infrared communication or zigbee communication. The handheld terminal adopts IP65 waterproof grade, and has good waterproof performance. Because the existing in-situ nutrient salt analyzer mainly depends on a communication part and a notebook computer to carry out equipment debugging, data transmission and in-situ calibration in a wired connection mode, the handheld terminal can improve the convenience of in-situ debugging and calibration of the seawater nutrient salt on-line monitoring system equipment in the invention in view of the fact that the notebook computer is easy to wet in the marine seawater environment and does not have 220V power supply, and the notebook computer needs to be operated by two hands and is extremely poor in convenience.
The on-line monitoring system for seawater nutrient salt of the invention is compared with the parameters of the WIZ in-situ nutrient salt analyzer of Systea corporation in Italy as shown in the following table:
the components of the seawater nutrient salt on-line monitoring system device are closely connected to form a complete whole, the seawater nutrient salt on-line monitoring function can be realized, the detection precision of nutrient salt in seawater is improved, compared with the existing device, the seawater nutrient salt on-line monitoring system device has a good monitoring effect, the components cannot be separately split, and the corresponding technical problems of the seawater nutrient salt on-line monitoring system device cannot be solved by the superposition of the separate components with similar functions.
As shown in fig. 5, the invention also provides a method for detecting seawater nutrient salts, which uses the online monitoring system for seawater nutrient salts to detect seawater nutrient salts, and comprises the following steps:
s1, respectively measuring the absorbance values of the deionized water and the standard solution;
s2, drawing a standard curve according to the concentrations of the deionized water and the standard solution, and the absorbance values of the deionized water and the standard solution;
s3, fully mixing the water sample with the detection reagent, and determining the absorbance value of the mixture of the water sample and the detection reagent;
and S4, bringing the absorbance value of the mixture of the water sample and the detection reagent into a standard curve and calculating to obtain the concentration parameter of the nutrient salt to be detected in the water sample.
Wherein, the absorbance calculation formula is as follows:
wherein A is the absorbance value of the light,
is the photovoltage value of deionized water, standard solution or water sample,
the photovoltage value of the mixture of the deionized water, the standard solution or the water sample and the detection reagent;
the formula for calculating the concentration of the sample is as follows:
wherein
Is the concentration value of the sample,
is the absorbance value of the water sample,
is the absorbance value of the deionized water,
is the absorbance value of the standard solution,
concentration values of the standard solutions.
In addition, when the absorbance values of the deionized water, the standard solution and the detection reagent are detected, air is introduced into the seawater nutrient salt online monitoring system, so that the small bubbles can be broken and fused with the introduced air after contacting the introduced air, and defoaming is realized.
As an embodiment of the invention, in the detection process, the mixture of the water sample and the detection reagent can be collected for a plurality of times to detect the photovoltaic value, the influence of the photovoltaic value caused by different factors such as chromaticity, turbidity or pH value in the water sample can be effectively eliminated, the water sample is repeatedly extracted and pushed out for 3-5 times, and the effects of wetting and washing the water sample tube, the injector, the detector, isolating the pollution caused by the reverse absorption of waste liquid and the like can be achieved.
A method for detecting seawater nutrient salt comprises a nitrite detection method, a nitrate detection method, a phosphate detection method, an ammonium salt detection method and a silicate detection method.
The nitrite detection adopts a naphthyl ethylenediamine colorimetric method, and specifically, the nitrite detection method comprises the following steps:
step Sa1, extracting 0.3ml of water sample;
step Sa2, extracting 0.1ml of sulfanilamide-naphthylethylenediamine hydrochloride-hydrochloric acid aqueous solution;
step Sa3, extracting 0.1ml of air;
step Sa4, pushing out 0.5ml of a mixture A consisting of a water sample, sulfanilamide-naphthylethylenediamine hydrochloride-hydrochloric acid aqueous solution and air, sucking in 0.5ml of the mixture A, and fully mixing the mixture A in a circulating pushing-out and sucking-in mode according to 0.5ml of the mixture A;
step Sa5, pushing the fully mixed mixture a into the photodetection device 18, turning on the light source;
step Sa6, reading the absorbance value of the mixture A, and turning off the light source;
and step Sa7, substituting the absorbance value of the mixture A into the standard curve A and calculating to obtain the concentration parameter of the nitrite in the water sample.
The nitrate detection adopts a cadmium ring reduction-naphthalene ethylenediamine colorimetric method, and specifically, the nitrate detection method comprises the following steps:
step Sb1, extracting 0.65ml of water sample;
step Sb2, pushing the water sample into a cadmium ring of the first detection module 13 for reduction, and respectively pushing out and sucking in 0.2ml to obtain a mixture B;
step Sb3, taking 0.3ml of mixture B;
step Sb4, taking 0.1ml of sulfanilamide-naphthylethylenediamine hydrochloride-hydrochloric acid aqueous solution;
step Sb5, taking 0.1ml of air;
step Sb6, pushing out 0.5ml of mixture C consisting of the mixture B, the detection reagent A and air, sucking in 0.5ml, and fully mixing in a circulating pushing-out and sucking-in mode of 0.5 ml;
step Sb7, pushing the fully mixed mixture C into the photodetection device 18, and turning on the light source;
step Sb8, reading the absorbance value of the mixture C, and turning off the light source;
step Sb9, substituting the absorbance value of the mixture C into a standard curve B and calculating to obtain the concentration parameter of the nitrate in the water sample;
the phosphate is detected by adopting a phosphomolybdic blue colorimetric method, and specifically, the phosphate detection method comprises the following steps:
step Sc1, extracting 0.2ml of water sample;
step Sc2, extracting 0.1ml of ammonium molybdate-antimony potassium tartrate-sulfuric acid aqueous solution;
step Sc3, extracting 0.1ml ascorbic acid aqueous solution;
step Sc4, extracting 0.1ml of air;
step Sc5, pushing out 0.5ml of a mixture D consisting of a water sample, an ammonium molybdate-antimony potassium tartrate-sulfuric acid aqueous solution, an ascorbic acid-acetone aqueous solution and air, sucking in 0.5ml, and fully mixing in a 0.5ml circulating pushing-out and sucking-in mode;
step Sc6, pushing the fully mixed mixture D into the photoelectric detection device 18, and turning on a light source;
step Sc7, reading the absorbance value of the mixture D, and turning off the light source;
and step Sc8, substituting the absorbance value of the mixture D into the standard curve C and calculating to obtain the concentration parameter of phosphate in the water sample.
The detection of the ammonium salt adopts a salicylic acid colorimetric method, and specifically, the detection method of the ammonium salt comprises the following steps:
step Sd1, heating the third detection module 15 to a preset temperature of 45 ℃;
step Sd2, extracting 0.3ml of water sample;
step Sd3, extracting 0.05ml of sodium citrate-sodium hydroxide aqueous solution;
step Sd4, extracting 0.05ml of air;
step Sd5, pushing out 0.5ml of mixture E consisting of the water sample, the sodium citrate-sodium hydroxide aqueous solution and air, sucking in 0.5ml of mixture E, and fully mixing in a 0.5ml circulating pushing-out and sucking mode;
step Sd6, extracting 0.05ml of sodium salicylate-sodium nitroprusside water solution;
step Sd7, sucking mixture E back into the syringe pump;
step Sd8, fully mixing a mixture F consisting of the mixture E and the sodium salicylate-sodium nitroprusside aqueous solution in a circulating push-out and suction mode of 0.5 ml;
step Sd9, extracting 0.05ml of sodium hydroxide-sodium hypochlorite aqueous solution;
step Sd10, fully mixing a mixture G consisting of the mixture F and a sodium hydroxide-sodium hypochlorite aqueous solution in a 0.5ml circulating push-out and suction mode;
step Sd11, pushing the fully mixed mixture G into the photoelectric detection device 18, and turning on a light source;
step Sd12, reading the absorbance value of the mixture G, and turning off the light source;
step Sd13, stopping heating the third detection module 15;
and step Sd14, substituting the absorbance value of the mixture G into the standard curve D and calculating to obtain the concentration parameter of the ammonium salt in the water sample.
The detection of the silicate adopts a silicon-molybdenum blue colorimetric method, and specifically, the detection method of the silicate comprises the following steps:
step Se1, extracting 0.3ml of water sample;
step Se2, extracting 0.05ml of ammonium molybdate-sulfuric acid aqueous solution;
step Se3, extracting 0.05ml of air;
step Se4, pushing out 0.5ml of a mixture H consisting of the water sample, the ammonium molybdate-sulfuric acid aqueous solution and air, sucking in 0.5ml of the mixture H, and then fully mixing the mixture H in a 0.5ml circulating pushing-out and sucking-in mode;
step Se5, extracting 0.05ml of oxalic acid aqueous solution;
step Se6, fully mixing a mixture I consisting of the mixture H and the oxalic acid aqueous solution in a circulating 0.5ml mode of pushing out and sucking in;
step Se7, extracting 0.05ml of ascorbic acid aqueous solution;
step Se8, mixing the mixture I with an ascorbic acid aqueous solution to obtain a mixture J, and fully mixing the mixture J in a 0.5ml circulating push-out and suction mode;
step Se9, pushing the fully mixed mixture J into the photoelectric detection device 18, and turning on a light source;
step Se10, reading the absorbance value of the mixture J;
and step Se11, substituting the absorbance value of the mixture J into the standard curve E and calculating to obtain the concentration parameter of the silicate in the water sample.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (12)
1. An online monitoring system for seawater nutrient salt is characterized by comprising:
sealing the cabin;
the main control module is arranged in the sealed cabin;
the detection module is arranged in the sealed cabin and comprises a first detection module for detecting nitrate and nitrite, a second detection module for detecting phosphate, a third detection module for detecting ammonium salt and a fourth detection module for detecting silicate; the first detection module, the second detection module, the third detection module and the fourth detection module are arranged independently;
the reagent containing device is arranged outside the sealed cabin and is communicated with the detection module through a pipeline;
the liquid inlet interface is communicated with the detection module;
an air interface in communication with the detection module.
2. The seawater nutrient salt on-line monitoring system of claim 1, wherein the detection module comprises an injection device and a photoelectric detection device; the injection device includes a syringe pump and a multi-position valve, the syringe pump being in communication with the multi-position valve.
3. The seawater nutrient salt on-line monitoring system of claim 2, wherein the photoelectric detection device comprises a flow cell, a light source and a receiver; the flow cell, the light source and the receiver are configured to detect and reference light paths; the flow cell is in communication with the multi-position valve.
4. The on-line seawater nutrient salt monitoring system of claim 3, further comprising a waste liquid storage device; the waste liquid storage device is communicated with the flow cell.
5. The seawater nutrient salt on-line monitoring system of claim 1, further comprising a handheld terminal; the handheld terminal is connected with the main control module in a wired communication or wireless communication mode.
6. A seawater nutrient salt detection method is characterized in that the seawater nutrient salt detection is carried out by using the seawater nutrient salt on-line monitoring system of claims 1-5, and comprises the following steps:
respectively measuring the absorbance values of the deionized water and the standard solution;
drawing a standard curve according to the concentrations of the deionized water and the standard solution, and the absorbance values of the deionized water and the standard solution;
fully mixing a water sample with a detection reagent, and measuring the absorbance value of the mixture of the water sample and the detection reagent;
and (3) bringing the absorbance value of the mixture of the water sample and the detection reagent into a standard curve and calculating to obtain the concentration parameter of the nutrient salt to be detected in the water sample.
7. The method for detecting seawater nutrient salt of claim 6, wherein air is introduced into the online seawater nutrient salt monitoring system for defoaming when detecting the absorbance values of the deionized water, the standard solution and the detection reagent.
8. The method for detecting seawater nutrient salt as claimed in claim 7, wherein the method for detecting nitrite comprises:
respectively extracting a quantitative water sample, a quantitative detection reagent A and quantitative air, and fully mixing in a circulating push-out and suction mode to obtain a mixture A;
pushing the mixture A into a photoelectric detection device to detect the absorbance value of the mixture A;
and substituting the absorbance value of the mixture A into a nitrite detection standard curve for operation to obtain the concentration parameter of nitrite in the water sample.
9. The method for detecting seawater nutrient salts as claimed in claim 7, wherein the method for detecting nitrate comprises:
a quantitative water sample is extracted and pushed into a first detection module for reduction to obtain a mixture B;
taking the mixture B and the quantitative detection reagent A to be fully mixed in a circulating pushing-out and sucking-in mode to obtain a mixture C;
pushing the mixture C into a photoelectric detection device to detect the absorbance value of the mixture C;
and substituting the absorbance value of the mixture C into a nitrate detection standard curve for operation to obtain the concentration parameter of the nitrate in the water sample.
10. The method for detecting seawater nutrient salts as claimed in claim 7, wherein the method for detecting phosphate comprises:
respectively extracting a quantitative water sample, a quantitative detection reagent B, a quantitative detection reagent C and quantitative air, and fully mixing in a circulating push-out and suction manner to obtain a mixture D;
pushing the mixture D into a photoelectric detection device to detect the absorbance value of the mixture D;
and substituting the absorbance value of the mixture D into a phosphate detection standard curve for operation to obtain the concentration parameter of phosphate in the water sample.
11. The method for detecting seawater nutrient salt of claim 7,
the detection method of the ammonium salt comprises the following steps:
heating the third detection module to a preset temperature;
a quantitative water sample, a quantitative detection reagent D and quantitative air are extracted and fully mixed in a circulating push-out and suction mode to obtain a mixture E;
pumping a certain amount of detection reagent E and fully mixing the detection reagent E and the mixture E in a circulating push-out and suction mode to obtain a mixture F;
pumping a certain amount of detection reagent F and fully mixing the detection reagent F and the mixture F in a circulating push-out and suction mode to obtain a mixture G;
pushing the mixture G into a photoelectric detection device to detect the absorbance value of the mixture G;
and substituting the absorbance value of the mixture G into an ammonium salt detection standard curve for operation to obtain the concentration parameter of the ammonium salt in the water sample.
12. The method for detecting seawater nutrient salt as claimed in claim 7, wherein the method for detecting silicate comprises:
respectively extracting a quantitative water sample, a detection reagent G and air, and fully mixing in a circulating push-out and suction mode in a flow cell to obtain a mixture H;
taking a certain amount of detection reagent H and the mixture H, and fully mixing in a circulating push-out and suction mode to obtain a mixture I;
taking a certain amount of detection reagent I and the mixture I, and fully mixing in a circulating push-out and suction mode to obtain a mixture J;
pushing the mixture J into a photoelectric detection device to detect the absorbance value of the mixture J;
and substituting the absorbance value of the mixture J into a silicate detection standard curve for operation to obtain the concentration parameter of silicate in the water sample.
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