A water sample total phosphorus detection device and detection method

Abstract

The present invention relates to the technical field of water quality detection, and discloses a water sample total phosphorus detection device, comprising a sample introduction system, a light source system, an analysis system, and a measurement and control system, and also comprising a spectroscopic system, wherein the spectroscopic system comprises a spectroscopic chamber, a spectroscope, a first reflector, a second reflector, and a guide mirror. A water sample total phosphorus detection method comprises the following steps: S1, preparing a water sample, S2, testing a water sample, S3, data screening, S4, testing a blank solution, and S5, calculating the total phosphorus content. The present invention provides a water sample total phosphorus detection device and a detection method, which can solve or at least alleviate the problems of existing water sample total phosphorus detection equipment, such as a single observation method, a low linear range, and inaccurate detection results.

Description

Technical Field

[0001] The present invention relates to the technical field of water quality detection, and in particular to a device and method for detecting total phosphorus in water samples. Background Art

[0002] Phosphorus is a key indicator of water pollution and eutrophication, and is one of the primary indicators for my country's implementation of total pollutant emission control. Phosphorus primarily originates from industrial and domestic wastewater. The large-scale discharge of these phosphorus-containing wastewaters increases phosphorus levels in water bodies, leading to eutrophication, mass mortality of fish and other organisms, and deteriorating water quality, resulting in a fishy odor. In recent years, the improvement and strengthening of national environmental protection regulations have mandated strict monitoring of pollutants, including total phosphorus, in various types of wastewater and river water.

[0003] Currently, inductively coupled plasma optical emission spectrometry (ICP-OES) is mostly used to determine total phosphorus in water. The core of an ICP-OES is the plasma. High-frequency, high-power energy flows through the working coil, creating a strong alternating electromagnetic field within the quartz torch. This ionizes the argon gas within, forming a stable, high-temperature discharge torch—the plasma. The sample aerosol is injected into the plasma through a central tube, forming an analytical channel approximately 2 mm in diameter. Due to the varying temperature distributions in different regions of the plasma, the analytical channel is divided into: an atomization zone (lower temperature), an atomic emission zone (higher temperature), and an ion emission zone (higher temperature).

[0004] Plasma observation methods include horizontal and vertical observation. Horizontal observation collects signals from the entire analytical channel, excluding the tail plume. Therefore, it offers greater sensitivity than vertical observation, which only collects signals from a localized region, and reduces the detection limit by 5-10 times. However, because horizontal observation collects signals from the entire analytical channel, including the atomization and atomic emission regions, which are not optimal for observation, while improving sensitivity, it also increases background noise and matrix effects, introducing interferences from readily ionized particles. Vertical observation collects light from the side of the plasma and measures the signal from the ion emission region (optimal observation region). Obviously, the signal from this region is not as strong as that from the entire analytical channel during horizontal observation, so its sensitivity is not as high as that of horizontal observation. However, the signal from this region provides the best signal-to-background ratio, especially in complex matrices. Furthermore, vertical observation does not collect light from the atomization and atomic emission regions within the plasma. Therefore, it is completely free of readily ionized interferences, offers excellent linear range, minimal matrix effects, and very low background, and is flexible and convenient. However, vertical observation requires adjusting the plasma height to ensure optimal observation quality. Furthermore, sample delivery also affects observation quality.

[0005] This scheme combines the advantages of horizontal observation and vertical observation, makes up for the defects of horizontal observation such as easy ionization interference, decreased linear range and large matrix effect, and proposes a more accurate detection scheme. Summary of the Invention

[0006] The purpose of the present invention is to overcome the deficiencies in the prior art, solve or at least alleviate the problems of the existing water sample total phosphorus detection equipment, such as a single observation method, a low linear range, and inaccurate detection results, and provide a water sample total phosphorus detection device and detection method.

[0007] To achieve the above objectives, the present invention provides the following technical solutions: a water sample total phosphorus detection device, comprising a sample introduction system, a light source system, an analysis system, and a measurement and control system, and further comprising a spectroscopic system, wherein the spectroscopic system divides the light source generated by the vertically arranged light source system into vertical light and horizontal light, and transmits the vertical light and the horizontal light to the analysis system at intervals, and the spectroscopic system comprises:

[0008] The spectroscopic chamber includes a vertical chamber and a horizontal chamber, wherein the vertical chamber is located above the light source system and the horizontal chamber is located on one side of the light source system. A longitudinal light inlet is provided on the bottom surface of the vertical chamber and is coaxial with the light source system. A transverse light inlet is provided on the side surface of the horizontal chamber and faces the upper part of the light source system.

[0009] A spectrometer is tilted and rotatably disposed in the horizontal chamber at one end close to the light source system. The reflector has multiple hollow areas evenly distributed around its circumference, and light entering the transverse light inlet passes through one of the hollow areas and enters the analysis system.

[0010] A first reflector and a second reflector, which are used to reflect light entering from the longitudinal light inlet to the beam splitter, wherein the first reflector and the second reflector are both fixedly arranged on the top of the vertical chamber, and the first reflector and the second reflector are respectively located above the light source system and the beam splitter;

[0011] A guide mirror is used to guide the light passing through the spectroscope and the light reflected by the spectroscope to the analysis system.

[0012] In order to further realize the present invention, the following technical solutions may be preferably used:

[0013] Preferably, it also includes:

[0014] A first housing, wherein the sample injection system, the light source system and the spectroscopic system are all located in the first housing, and an exhaust port is provided on the top of the first housing;

[0015] The second shell, the analysis system and the measurement and control system are both located in the second shell, the second shell is located on one side of the first shell, and the light reflected by the guide mirror passes through the first shell and the second shell into the analysis system.

[0016] Preferably, the light source system comprises:

[0017] a sampling tube, the lower end of which is connected to the sampling system;

[0018] An auxiliary gas pipe is coaxially sleeved on the outside of the sample inlet pipe, and the lower part of the auxiliary gas pipe is connected to the argon gas source;

[0019] A cooling air pipe is coaxially sleeved on the auxiliary air pipe, and the lower portion of the cooling air pipe is connected to an argon gas source;

[0020] The high-frequency coil is fixedly sleeved on the outer side of the upper end of the cooling air pipe.

[0021] Preferably, the injection system comprises:

[0022] An atomizer, which is used to atomize the sample, and the atomizer outlet is fixedly connected to the lower end of the sample inlet tube;

[0023] A peristaltic pump is used to deliver the sample to the nebulizer.

[0024] Preferably, an adjustment component is further included, which is used to adjust the height position of the light source system, and the adjustment component includes:

[0025] An adjustment box, wherein the lower portion of the light source system is longitudinally slidably arranged on the top surface of the adjustment box, and the atomizer is located in the adjustment box;

[0026] An air jet port is provided at the lower portion of the auxiliary air pipe and is located in the regulating box, and the jet direction of the air jet port is vertically upward and toward the top plate of the regulating box;

[0027] The spring is used to drive the atomizer and the light source system to move upward relative to the adjustment box.

[0028] Preferably, the auxiliary air pipe includes an upper guide section and a lower jet section, the lower part of the guide section is longitudinally slidably arranged on the top surface of the regulating box, the jet section is located on the lower side of the top surface of the regulating box, and the multiple jet ports are evenly distributed on the top surface of the jet section, and the diameter value of the jet section is greater than the diameter value of the guide section.

[0029] Preferably, the adjustment assembly further comprises a guide mechanism, and the guide mechanism comprises:

[0030] An directional sleeve, the directional sleeve is vertically fixedly arranged at the lower part of the regulating box;

[0031] A lifting sleeve, wherein the lower portion of the lifting sleeve is longitudinally slidably sleeved in the directional sleeve, the upper end of the lifting sleeve abuts against the lower portion of the atomizer, and the waste liquid outlet of the atomizer is located in the lifting sleeve;

[0032] The spring is slidably sleeved on the outside of the directional sleeve, the lower end of the spring is fixed to the adjustment box, and the upper end of the spring is against the lifting sleeve.

[0033] Preferably, a partition is horizontally arranged in the middle of the regulating box, the directional sleeve is fixedly arranged on the upper side of the partition, and a waste liquid bottle is placed at the lower part of the regulating box. The waste liquid bottle is located below the partition, and the upper end opening of the waste liquid bottle faces the waste liquid port of the atomizer.

[0034] A method for detecting total phosphorus in a water sample comprises the following steps:

[0035] S1. Prepare a water sample by mixing the liquid to be tested with concentrated nitric acid to obtain a water sample, wherein the volume ratio of the liquid to be tested to the concentrated nitric acid is 50:1;

[0036] S2, water sample detection, the water sample prepared in step S1 is sent to the light source system through the sampling system for ionization, and is monitored in real time by the analysis system. During this process, the measurement and control system controls the spectrometer to rotate at a uniform speed, and controls the amount of water sample entering the light source system to increase at a uniform speed. At the beginning, one of the hollow areas of the spectrometer corresponds to the horizontal light inlet. At this time, the analysis system detects the phosphorus concentration c1. The spectrometer rotates, and the light from the vertical light inlet is reflected to the spectrometer through the first and second reflectors, causing the analysis system to detect the phosphorus concentration c2. The spectrometer continues to rotate at a uniform speed and detects phosphorus concentrations c3, c4...c n 、c n+1 ;

[0037] S3, data screening, the adjacent two phosphorus concentrations obtained in step S2 are grouped together, and the optimal group of phosphorus concentrations c is screened out. N and c N+1 ;

[0038] S4, blank solution detection, distilled water is sent to the light source system through the sampling system for ionization, and detected by the analysis system to obtain the phosphorus concentration c0;

[0039] S5, calculate the total phosphorus content, according to the c in step S3 N and c N+1 Calculate the total phosphorus content of the water sample using c0 in step S4;

[0040]

[0041] Where W P is the total phosphorus content, c N and c N+1 is the phosphorus concentration of the water sample obtained from the standard curve, c0 is the phosphorus concentration of the blank solution obtained from the standard curve, V is the volume of the water sample, t s Take multiples of the points.

[0042] Preferably, in step S3, when a group of phosphorus concentrations When the phosphorus concentration of this group is the effective phosphorus concentration, the effective phosphorus concentration of the group with the smallest subscript is the optimal phosphorus concentration cN and c N+1 .

[0043] The beneficial effects of the present invention are:

[0044] 1. The present invention observes the light source system from the vertical direction and the horizontal direction through the spectroscopic system. The observations in the two directions are performed alternately. By comparing the data from the two directions, the data interfered by easy ionization is eliminated to obtain the optimal data, thereby ensuring the accuracy of the detection.

[0045] 2. The present invention adjusts the height position of the light source system in real time through an adjustment component, and maintains the optimal observation position when observing in the horizontal direction. During detection, the flow of argon in the auxiliary air pipe drives the sample in the sample injection tube to be ejected. Gradually increasing the flow rate of argon in the auxiliary air pipe will also increase the amount of sample ejected from the sample injection tube, and the position of the atomic emission zone will also rise accordingly. A portion of the argon in the auxiliary air pipe is ejected from the jet port and sprayed toward the top plate of the regulating box. The reaction force of the ejected air flow drives the light source system to move downward, so that the ion emission zone (optimal observation zone) is always located at the height position of the horizontal light inlet. Not only can the detection sample be detected at different ejection volumes, but the accuracy of the detection can also be guaranteed. BRIEF DESCRIPTION OF THE DRAWINGS

[0046] Figure 1 It is a schematic structural diagram of the sample injection system, light source system and spectroscopic system of the present invention.

[0047] Figure 2 For the present invention Figure 1 Structural cross-sectional view.

[0048] Figure 3 For the present invention Figure 2 Cross-sectional view at AA in the middle.

[0049] Figure 4 It is a structural schematic diagram of the present invention.

[0050] Figure 5 It is a structural cross-sectional view of the present invention.

[0051] Figure 6 Schematic diagram of the structure of the spectroscope of the present invention.

[0052] Figure 7 It is a schematic structural diagram of the sample injection system, light source system and adjustment component of the present invention.

[0053] Figure 8 For the present invention Figure 7 Structural cross-sectional view.

[0054] Figure 9 Schematic diagram of the structure of the auxiliary trachea of the present invention.

[0055] Figure 10This is a structural cross-sectional view of the auxiliary trachea of the present invention.

[0056] The accompanying drawings are:

[0057] 1-spectrometric chamber; 2-longitudinal light inlet; 3-horizontal light inlet; 4-spectrometer; 5-first reflector; 6-second reflector; 7-guide mirror; 8-first outer shell; 9-second outer shell; 10-injection tube; 11-auxiliary air pipe; 12-cooling air pipe; 13-high-frequency coil; 14-atomizer; 15-regulating box; 16-injection nozzle; 17-spring; 18-directional sleeve; 19-lifting sleeve; 20-partition; 21-waste liquid bottle; 101-vertical chamber; 102-horizontal chamber; 1101-diversion section; 1102-injection section. DETAILED DESCRIPTION

[0058] In the description of the present invention, it should also be noted that, unless otherwise expressly specified or limited, the terms "disposed," "installed," "connected," and "connected" should be understood in a broad sense. For example, they may refer to fixed connections, detachable connections, or integral connections; they may refer to mechanical connections or electrical connections; they may refer to direct connections or indirect connections through an intermediate medium; and they may refer to internal communication between two components. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on the specific circumstances.

[0059] The following will be combined with the accompanying drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative work are within the scope of protection of the present invention. Example 1

[0060] Plasma observation methods include lateral and vertical observation. Horizontal observation collects signals from the entire analytical channel, excluding the tail plume. Therefore, it offers greater sensitivity than vertical observation, which only collects signals from a localized region, and reduces the detection limit by 5-10 times. However, because lateral observation collects signals from the entire analytical channel, including the atomization and atomic emission regions, which are not optimal for observation, while improving sensitivity, it also increases background noise and matrix effects, introducing interferences from readily ionized particles. Vertical observation collects light from the side of the plasma, measuring the signal from the ion emission region (optimal observation zone). Obviously, the signal in this region is not as strong as that from the entire analytical channel during lateral observation, so its sensitivity is not as high as that of lateral observation. However, the signal in this region provides the best signal-to-background ratio, especially in complex matrices. Furthermore, vertical observation does not collect light from the atomization and atomic emission regions within the plasma, eliminating any interferences from readily ionized particles. It offers excellent linear range, minimal matrix effects, and very low background, while also being flexible and convenient.

[0061] Reference Figure 1-Figure 7 A water sample total phosphorus detection device includes a sample introduction system, a light source system, an analysis system, and a measurement and control system. It also includes a spectroscopic system. The spectroscopic system divides the light generated by the vertically arranged light source system into vertical light and horizontal light, and transmits the vertical light and the horizontal light to the analysis system at intervals. The spectroscopic system includes:

[0062] The spectroscopic chamber 1 includes a vertical chamber 101 and a horizontal chamber 102. The vertical chamber 101 is located above the light source system, and the horizontal chamber 102 is located on one side of the light source system. A longitudinal light inlet 2 is provided on the bottom surface of the vertical chamber 101, and the longitudinal light inlet 2 is coaxially arranged with the light source system. A transverse light inlet 3 is provided on the side of the horizontal chamber 102, and the transverse light inlet 3 faces the upper part of the light source system.

[0063] The spectrometer 4 is tilted and rotatably disposed at one end of the horizontal chamber 102 near the light source system. The reflector has multiple hollow areas evenly distributed around its circumference. Light entering the horizontal light inlet 3 passes through one of the hollow areas and enters the analysis system.

[0064] A first reflector 5 and a second reflector 6 are used to reflect the light entering from the longitudinal light inlet 2 to the beam splitter 4. The first reflector 5 and the second reflector 6 are both fixedly disposed on the top of the vertical chamber 101. The first reflector 5 and the second reflector 6 are respectively located above the light source system and the beam splitter 4;

[0065] The guide mirror 7 is used to guide the light passing through the beam splitter 4 and the light reflected by the beam splitter 4 to the analysis system.

[0066] The water sample total phosphorus detection device also includes:

[0067] The first housing 8, the sample injection system, the light source system and the spectroscopic system are all located in the first housing 8, and an exhaust port is provided on the top of the first housing 8, through which the light source system is cooled;

[0068] The second shell 9 , the analysis system and the measurement and control system are all located in the second shell 9 . The second shell 9 is located on one side of the first shell 8 . The light reflected by the guide mirror 7 passes through the first shell 8 and the second shell 9 into the analysis system.

[0069] The light source system is observed from the vertical and horizontal directions through the spectroscopic system. The observations in the two directions are performed alternately. By comparing the data from the two, the data interfered by easy ionization is eliminated to obtain the optimal data, thereby ensuring the accuracy of the detection. Example 2

[0070] In the technical solution of embodiment 1, although the advantages of horizontal observation and vertical observation are combined, when vertical observation is performed through the horizontal light inlet 3, it cannot be guaranteed that the horizontal light inlet 3 corresponds to the ion emission area for optimal observation, which will affect the detection results.

[0071] Experiments show that the plasma length increases with the increase of gas flow. For example, when the argon flow rate increases from 1.8×10⁻ 4 kg / s increases to 3.4×10⁻ 4 kg / s, the plasma length increases from 260 mm to 550 mm. The optimal ion emission region is located at the top of the plasma and also increases with the increase in plasma length. However, the position of transverse light inlet 3 is fixed. When the plasma length increases with the ionized gas flow rate, the ion emission region moves above transverse light inlet 3. At this time, transverse light inlet 3 observes the atomic emission region, which cannot achieve optimal observation effect.

[0072] To this end, conventional detection equipment requires a constant gas flow rate at the ionization point during testing, thereby maintaining the ion emission region in a set position. However, the sample discharge volume is proportional to the gas flow rate at the ionization point. When the gas flow rate is constant, the sample discharge volume is also essentially constant, which limits the detection range of the detection equipment. This makes it difficult to detect low concentrations of the test component in the sample.

[0073] Reference Figure 1-Figure 7 In this embodiment, the light source system includes an injection tube 10, an auxiliary air tube 11, a cooling air tube 12 and a high-frequency coil 13. The lower end of the injection tube 10 is connected to the injection system, the auxiliary air tube 11 is coaxially sleeved on the outside of the injection tube 10, and the lower part of the auxiliary air tube 11 is connected to the argon gas source. The cooling air tube 12 is coaxially sleeved on the outside of the auxiliary air tube 11, and the lower part of the cooling air tube 12 is connected to the argon gas source. The high-frequency coil 13 is fixedly sleeved on the outer side of the upper end of the cooling air tube 12.

[0074] The sampling system includes a nebulizer 14 and a peristaltic pump. The nebulizer 14 is used to atomize the sample. The mist outlet of the nebulizer 14 is fixedly connected to the lower end of the sampling tube 10 . The peristaltic pump is used to transport the sample to the nebulizer 14 .

[0075] The water sample total phosphorus detection device also includes an adjustment component, which is used to adjust the height position of the light source system. The adjustment component includes an adjustment box 15, an air jet 16 and a spring 17. The lower part of the light source system is longitudinally slidably arranged on the top surface of the adjustment box 15. The atomizer 14 is located in the adjustment box 15. The air jet 16 is arranged at the lower part of the auxiliary air pipe 11 and is located in the adjustment box 15. The spray direction of the air jet 16 is vertically upward and toward the top plate of the adjustment box 15. The spring 17 is used to drive the atomizer 14 and the light source system to move upward relative to the adjustment box 15.

[0076] In order to optimize the product structure, in this embodiment, the auxiliary air pipe 11 includes an upper guide section 1101 and a lower jet section 1102. The lower part of the guide section 1101 is longitudinally slidably set on the top surface of the regulating box 15, and the jet section 1102 is located on the lower side of the top surface of the regulating box 15. Multiple jet ports 16 are evenly distributed on the top surface of the jet section 1102, and the diameter value of the jet section 1102 is greater than the diameter value of the guide section 1101.

[0077] The height position of the light source system is adjusted in real time by adjusting the components, maintaining the optimal observation position when observing in the vertical direction. During detection, the flow of argon gas in the auxiliary gas pipe 11 drives the sample in the sample injection tube 10 to be ejected. Gradually increasing the flow rate of argon gas in the auxiliary gas pipe 11 will also increase the amount of sample ejected from the sample injection tube 10, and the position of the ion emission zone will also rise accordingly. A portion of the argon gas in the auxiliary gas pipe 11 is ejected from the jet port 16 and sprayed toward the top plate of the regulating box 15. The reaction force of the ejected air flow drives the light source system downward, so that the atomic emission zone is always located at the height position of the horizontal light inlet 3. This not only allows the detection of the test sample at different ejection amounts, but also ensures the accuracy of the detection.

[0078] By gradually limiting the number and size of the air jets 16 through experiments, the airflow rates ejected from the upper and lower ends of the light source system are in a specific ratio, thereby ensuring that the observation area of the transverse light inlet 3 is always located within the ion emission region during detection.

[0079] At the same time, the sample ejection volume can be gradually changed to achieve the best observation effect; when the content of the detection component in the sample is small, the ionized detection component increases with the sample ejection volume, and is easier to be detected, thereby expanding the detection range. Example 3

[0080] In the technical solution of Example 2, the height position of the ion emission region can be automatically adjusted according to the argon gas flow rate, so that it automatically corresponds to the transverse light inlet 3, ensuring that vertical observation is always carried out at the optimal observation position. However, due to the limited thickness of the top plate of the adjustment box 15, the light source system will tilt to a certain extent during the raising and lowering, and it is impossible to ensure that the ion emission region is accurately aligned with the transverse light inlet 3.

[0081] Reference Figure 1-Figure 7 The adjustment component also includes a guiding mechanism, which includes a directional sleeve 18 and a lifting sleeve 19. The directional sleeve 18 is vertically fixed to the lower part of the adjustment box 15, and the lower part of the lifting sleeve 19 is longitudinally slidably fitted into the directional sleeve 18. The upper end of the lifting sleeve 19 is against the lower part of the atomizer 14. The waste liquid port of the atomizer 14 is located in the lifting sleeve 19. The spring 17 is slidably fitted onto the outside of the directional sleeve 18. The lower end of the spring 17 is fixed to the adjustment box 15, and the upper end of the spring 17 is against the lifting sleeve 19.

[0082] In order to optimize the product structure and facilitate the collection of waste liquid generated in the atomizer 14, a partition 20 is horizontally arranged in the middle of the regulating box 15, and the directional sleeve 18 is fixedly arranged on the upper side of the partition 20. A waste liquid bottle 21 is placed at the lower part of the regulating box 15. The waste liquid bottle 21 is located below the partition 20, and the upper end opening of the waste liquid bottle 21 faces the waste liquid port of the atomizer 14. Example 4

[0083] A method for detecting total phosphorus in a water sample comprises the following steps:

[0084] S1. Prepare a water sample by mixing the liquid to be tested with concentrated nitric acid to obtain a water sample, wherein the volume ratio of the liquid to be tested to the concentrated nitric acid is 50:1;

[0085] S2, water sample detection, the water sample prepared in step S1 is sent to the light source system through the sampling system for ionization, and is monitored in real time by the analysis system. During this process, the measurement and control system controls the spectrometer 4 to rotate at a uniform speed, and controls the amount of water sample entering the light source system to increase at a uniform speed. At the beginning, one of the hollow areas of the spectrometer 4 corresponds to the horizontal light inlet 3. At this time, the analysis system detects the phosphorus concentration c1. The spectrometer 4 rotates, and the light from the vertical light inlet 2 is reflected to the spectrometer 4 through the first reflector 5 and the second reflector 6, causing the analysis system to detect the phosphorus concentration c2. The spectrometer 4 continues to rotate at a uniform speed and detects phosphorus concentrations c3, c4...c n 、c n+1 ;

[0086] S3, data screening, the adjacent two phosphorus concentrations obtained in step S2 are grouped together, and the optimal group of phosphorus concentrations c is screened out. N and c N+1 ;

[0087] S4, blank solution detection, distilled water is sent to the light source system through the sampling system for ionization, and detected by the analysis system to obtain the phosphorus concentration c0;

[0088] S5, calculate the total phosphorus content, according to the c in step S3 N and c N+1 Calculate the total phosphorus content of the water sample using c0 in step S4;

[0089]

[0090] Where W P is the total phosphorus content, c N and c N+1 is the phosphorus concentration of the water sample obtained from the standard curve, c0 is the phosphorus concentration of the blank solution obtained from the standard curve, V is the volume of the water sample, t s Take multiples of the points.

[0091] In step S3, when a group of phosphorus concentrations When the phosphorus concentration of this group is the effective phosphorus concentration, the effective phosphorus concentration of the group with the smallest subscript is the optimal phosphorus concentration c N and c N+1 .

[0092] The above are only preferred specific embodiments of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with this technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solutions and inventive concepts of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. A water sample total phosphorus detection device, comprising a sample introduction system, a light source system, an analysis system and a measurement and control system, characterized in that: The system further includes a light splitting system, which splits the light source generated by the vertically arranged light source system into vertical light and horizontal light, and transmits the vertical light and the horizontal light to the analysis system at intervals. The light splitting system includes: A spectroscopic chamber (1) comprising a vertical chamber (101) and a horizontal chamber (102), wherein the vertical chamber (101) is located above the light source system, and the horizontal chamber (102) is located on one side of the light source system. A longitudinal light inlet (2) is provided on the bottom surface of the vertical chamber (101), and the longitudinal light inlet (2) is coaxially arranged with the light source system. A transverse light inlet (3) is provided on the side surface of the horizontal chamber (102), and the transverse light inlet (3) faces the upper part of the light source system. A spectroscope (4) is tilted and rotatably arranged at one end of the horizontal chamber (102) close to the light source system, and a plurality of hollow areas are evenly distributed around the circumference of the spectroscope (4). Light entering from the transverse light inlet (3) passes through one of the hollow areas and enters the analysis system; a first reflector (5) and a second reflector (6), which are used to reflect light entering from the longitudinal light inlet (2) to the beam splitter (4); the first reflector (5) and the second reflector (6) are both fixedly arranged on the top of the vertical chamber (101); the first reflector (5) and the second reflector (6) are respectively located above the light source system and the beam splitter (4); a guide mirror (7) for guiding the light passing through the spectroscope (4) and the light reflected by the spectroscope (4) to the analysis system; The injection system comprises: An atomizer (14) for atomizing the sample, wherein the atomizer (14) has a mist outlet fixedly connected to the lower end of the light source system; a peristaltic pump for delivering the sample to the nebulizer (14); Also included is an adjustment component for adjusting the height position of the light source system, the adjustment component comprising: An adjustment box (15), wherein the lower portion of the light source system is longitudinally slidably disposed on the top surface of the adjustment box (15), and the atomizer (14) is located inside the adjustment box (15); An air jet (16), the air jet (16) being arranged at the lower portion of the auxiliary air pipe (11) and located in the regulating box (15), with the jetting direction of the air jet (16) being vertically upward and toward the top plate of the regulating box (15); The spring (17) is used to drive the atomizer (14) and the light source system to move upward relative to the adjustment box (15).

2. A water sample total phosphorus detection device according to claim 1, characterized in that, Also includes: A first housing (8), wherein the sample injection system, the light source system and the light splitting system are all located in the first housing (8), and an exhaust port is provided at the top of the first housing (8); A second housing (9), wherein the analysis system and the measurement and control system are both located in the second housing (9), and the second housing (9) is located on one side of the first housing (8). Light reflected by the guide mirror (7) passes through the first housing (8) and the second housing (9) and enters the analysis system.

3. A water sample total phosphorus detection device according to claim 1, characterized in that, The light source system comprises: A sampling tube (10), the lower end of which is connected to the sampling system; An auxiliary gas pipe (11) is coaxially sleeved on the outside of the sample inlet pipe (10), and the lower part of the auxiliary gas pipe (11) is connected to an argon gas source; A cooling air pipe (12) is coaxially sleeved on the outside of the auxiliary air pipe (11), and the lower part of the cooling air pipe (12) is connected to an argon gas source; The high-frequency coil (13) is fixedly sleeved on the outer side of the upper end of the cooling air pipe (12).

4. A water sample total phosphorus detection device according to claim 1, characterized in that, The auxiliary air pipe (11) comprises an upper guide section (1101) and a lower jet section (1102), wherein the lower portion of the guide section (1101) is longitudinally slidably arranged on the top surface of the regulating box (15), and the jet section (1102) is located on the lower side of the top surface of the regulating box (15), and the plurality of jet ports (16) are evenly distributed on the top surface of the jet section (1102), and the diameter of the jet section (1102) is greater than the diameter of the guide section (1101).

5. A water sample total phosphorus detection device according to claim 1, characterized in that, The adjustment assembly further includes a guide mechanism, which includes: A directional sleeve (18), wherein the directional sleeve (18) is vertically fixedly disposed at the lower portion of the regulating box (15); A lifting sleeve (19), wherein the lower portion of the lifting sleeve (19) is longitudinally slidably sleeved in the directional sleeve (18), the upper end of the lifting sleeve (19) abuts against the lower portion of the atomizer (14), and the waste liquid outlet of the atomizer (14) is located in the lifting sleeve (19); The spring (17) is slidably sleeved on the outside of the directional sleeve (18), the lower end of the spring (17) is fixed to the adjustment box (15), and the upper end of the spring (17) is against the lifting sleeve (19).

6. A water sample total phosphorus detection device according to claim 5, characterized in that, A partition (20) is laterally arranged in the middle of the regulating box (15), and the directional sleeve (18) is fixedly arranged on the upper side of the partition (20). A waste liquid bottle (21) is placed at the lower part of the regulating box (15), and the waste liquid bottle (21) is located below the partition (20). The upper end opening of the waste liquid bottle (21) faces the waste liquid outlet of the atomizer (14).

7. A method for detecting total phosphorus in a water sample, according to a device for detecting total phosphorus in a water sample according to any one of claims 1 to 6, characterized in that: The following steps are involved: S1. Prepare a water sample by mixing the liquid to be tested with concentrated nitric acid to obtain a water sample, wherein the volume ratio of the liquid to be tested to the concentrated nitric acid is 50:1; S2, water sample detection, the water sample prepared in step S1 is sent to the light source system through the sampling system for ionization, and is monitored in real time by the analysis system. During this process, the measurement and control system controls the spectroscope (4) to rotate at a uniform speed, and controls the amount of water sample entering the light source system to increase at a uniform speed. At the beginning, one of the hollow areas of the spectroscope (4) corresponds to the horizontal light inlet (3). At this time, the analysis system detects the phosphorus concentration c1. The spectroscope (4) rotates, and the light from the vertical light inlet (2) is reflected to the spectroscope (4) through the first reflector (5) and the second reflector (6), and is guided to the analysis system to detect the phosphorus concentration c2. The spectroscope (4) continues to rotate at a uniform speed to detect phosphorus concentrations c3, c4...c n 、c n+1 ; S3, data screening, the adjacent two phosphorus concentrations obtained in step S2 are grouped together, and the optimal group of phosphorus concentrations c is screened out. N and c N+1 ; S4, blank solution detection, distilled water is sent to the light source system through the sampling system for ionization, and detected by the analysis system to obtain the phosphorus concentration c0; S5, calculate the total phosphorus content, according to the c in step S3 N and c N+1 Calculate the total phosphorus content of the water sample using c0 in step S4; Where W P is the total phosphorus content, c N and c N+1 is the phosphorus concentration of the water sample obtained from the standard curve, c0 is the phosphorus concentration of the blank solution obtained from the standard curve, V is the volume of the water sample, t s Take multiples of the points.

8. A method for detecting total phosphorus in water samples according to claim 7, characterized in that, In step S3, when a group of phosphorus concentrations When the phosphorus concentration of this group is the effective phosphorus concentration, the effective phosphorus concentration of the group with the smallest subscript is the optimal phosphorus concentration c N and c N+1 .

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