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 apparatus, which comprises a sample introduction system, a light source system, an analysis system and a measurement and control system, and further comprises a light splitting system, and the light splitting system comprises a light splitting chamber, a light splitting mirror, a first reflective mirror, a second reflective mirror and a guide mirror. The invention relates to a water sample total phosphorus detection method, which comprises: S1, water sample preparation, S2, water sample detection, S3, data screening, S4, blank solution detection, and S5, total phosphorus content calculation. The invention provides a water sample total phosphorus detection device and a detection method, which can solve or at least alleviate the problems of single observation mode, relatively low linear range and inaccurate detection result of the existing water sample total phosphorus detection equipment.

Description

Technical Field

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

[0002] Phosphorus is an important indicator of the degree of water pollution and eutrophication, and is also one of the main indicators for my country to implement total pollutant emission control. Phosphorus mainly comes from industrial wastewater and domestic wastewater. The large-scale discharge of these phosphorus-containing wastewaters increases the phosphorus content in the water, leading to eutrophication of the water, the death of a large number of fish and other organisms, and the deterioration of water quality with a fishy smell. In recent years, with the improvement and strengthening of national environmental protection laws and regulations, strict monitoring of pollutant indicators including total phosphorus in various types of wastewater and river water is required.

[0003] At present, inductively coupled plasma emission spectrometer (ICP-0ES) is mostly used to determine total phosphorus in water quality. One of the cores of inductively coupled plasma emission spectrometer is plasma. Its working coil is passed with high-frequency and high-power energy to form a strong alternating electromagnetic field in the quartz torch tube, so that the argon gas in it is ionized to form a stable, high-temperature discharge torch - plasma. The aerosol of the sample is sprayed into the plasma through the central tube to form an analysis channel of about Φ2mm. Due to the different temperature distributions in different areas of the plasma, the entire analysis channel is divided into: atomization area (lower temperature), atomic emission area (higher temperature) and ion emission area (higher temperature).

[0004] Plasma observation methods are divided into horizontal observation and vertical observation. Horizontal observation collects signals from the entire analysis channel except the tail flame, so its sensitivity is better than vertical observation that only collects signals from local areas, and the detection limit is reduced by 5-10 times. However, because horizontal observation collects signals from the entire analysis channel including the atomization zone and the atomic emission zone, and these two areas are not the best observation areas, horizontal observation increases background noise and matrix effects while improving sensitivity, and introduces easy ionization interference. Vertical observation collects light from the side of the plasma and measures the signal of the ion emission zone (the best observation area). Obviously, the signal in this area is not as strong as the signal of the entire analysis channel during horizontal observation, so its sensitivity is not as high as that of horizontal observation, but the signal in this area can provide the best signal-to-background ratio, especially under complex matrices, its signal-to-background ratio is more outstanding. At the same time, vertical observation does not collect light signals from the atomization zone and the atomic emission zone in the plasma, so it does not have easy ionization interference at all, has a very good linear range, very small matrix effect and very low background, and is flexible and convenient. However, vertical observation requires adjusting the height position of the plasma to ensure the observation effect. At the same time, the sample delivery volume also affects the observation effect.

[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, reduced 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 having a single observation method, a low linear range, and inaccurate detection results, and to provide a water sample total phosphorus detection device and a detection method.

[0007] To achieve the above object, the present invention provides the following technical solution: 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 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: The spectroscopic chamber comprises a vertical chamber and a horizontal chamber, wherein the vertical chamber is located above the light source system, the horizontal chamber is located on one side of the light source system, a longitudinal light inlet is arranged on the bottom surface of the vertical chamber, and the longitudinal light inlet is arranged coaxially with the light source system, and a transverse light inlet is arranged on the side surface of the horizontal chamber, and the transverse light inlet faces the upper part of the light source system; A spectroscope, which is tilted and rotatably arranged at one end of the horizontal chamber close to the light source system, and the circumference of the reflector is evenly distributed with a plurality of hollow areas, and the light entering from the transverse light inlet passes through one of the hollow areas and enters the analysis system; A first reflector and a second reflector, which are used to reflect the 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; A guiding mirror is used to guide the light passing through the beam splitter and the light reflected by the beam splitter to the analysis system.

[0008] In order to further realize the present invention, the following technical solutions may be preferably selected: Preferably, it also includes: A first housing, wherein the sample injection system, the light source system and the light splitting system are all located in the first housing, and an exhaust port is provided at the top of the first housing; A 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.

[0009] Preferably, the light source system comprises: A sampling tube, the lower end of which is connected to the sampling system; 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 an argon gas source; A cooling air pipe, which is coaxially sleeved outside the auxiliary air pipe, and the lower part of the cooling air pipe is connected to the argon gas source; The high frequency coil is fixedly sleeved on the outer side of the upper end of the cooling air pipe.

[0010] Preferably, the injection system comprises: An atomizer, which is used to atomize the sample, and the atomizer outlet is fixedly connected to the lower end of the sample injection tube; A peristaltic pump is used to deliver the sample to the nebulizer.

[0011] Preferably, it also includes an adjustment component, which is used to adjust the height position of the light source system, and the adjustment component includes: An adjustment box, wherein the lower part 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; An air jet port, the air jet port is arranged at the lower part 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; The spring is used to drive the atomizer and the light source system to move upward relative to the adjustment box.

[0012] Preferably, the auxiliary air duct 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.

[0013] Preferably, the adjustment assembly further comprises a guide mechanism, and the guide mechanism comprises: An directional sleeve, the directional sleeve is vertically fixedly arranged at the lower part of the regulating box; 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; 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.

[0014] Preferably, a partition is laterally arranged in the middle of the regulating box, the directional sleeve is fixedly arranged on the upper side of the partition, 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.

[0015] A method for detecting total phosphorus in a water sample comprises the following steps: 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 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 corresponds to the horizontal light inlet. At this time, the analysis system detects the phosphorus concentration c1, the spectroscope rotates, and the light from the vertical light inlet is reflected to the spectroscope through the first reflector and the second reflector, and causes the analysis system to detect the phosphorus concentration c2. The spectroscope continues to rotate at a uniform speed and detects 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 injection 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 and c0 in step S4 to calculate the total phosphorus content of the water sample;

[0016] 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.

[0017] 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 c N and c N+1 .

[0018] The beneficial effects of the present invention are: 1. The present invention observes the light source system from the vertical direction and the horizontal direction through the spectroscopic system, and the observations in the two directions are performed alternately. By comparing the data of the two, the data interfered by easy ionization is eliminated to obtain the optimal data, thereby ensuring the accuracy of the detection.

[0019] 2. The present invention adjusts the height position of the light source system in real time through the 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 injection tube to be ejected. Gradually increasing the flow rate of argon in the auxiliary air pipe will also increase the sample ejection amount in the injection tube, and the position of the atomic emission area will also increase accordingly. A part of the argon in the auxiliary air pipe is ejected from the jet port and sprayed toward the top plate of the adjustment box. The reaction force of the ejected air flow drives the light source system to move downward, so that the ion emission area (optimal observation area) is always located at the height position of the horizontal light inlet, which can not only detect the test sample at different ejection amounts, but also ensure the accuracy of the detection. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a schematic diagram of the structure of the sample injection system, light source system and spectroscopic system of the present invention.

[0021] Figure 2 For the present invention Figure 1 Structural cross-section view.

[0022] Figure 3 For the present invention Figure 2 Cross-sectional view at AA in the middle.

[0023] Figure 4 It is a schematic diagram of the structure of the present invention.

[0024] Figure 5 It is a structural cross-sectional view of the present invention.

[0025] Figure 6 It is a schematic structural diagram of the spectroscope of the present invention.

[0026] Figure 7 It is a schematic diagram of the structure of the sample injection system, light source system and adjustment component of the present invention.

[0027] Figure 8 For the present invention Figure 7 Structural cross-section view.

[0028] Fig. 9 It is a schematic diagram of the structure of the auxiliary airway of the present invention.

[0029] Fig.10 It is a structural cross-sectional view of the auxiliary airway of the present invention.

[0030] The accompanying drawings are marked as follows: 1-spectrometer chamber; 2-longitudinal light inlet; 3-lateral 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-adjustment box; 16-injection port; 17-spring; 18-directional sleeve; 19-lifting sleeve; 20-partition; 21-waste liquid bottle; 101-vertical chamber; 102-horizontal chamber; 1101-guiding section; 1102-injection section. DETAILED DESCRIPTION

[0031] In the description of the present invention, it is also necessary to explain that, unless otherwise clearly specified and limited, the terms "set", "install", "connect", and "connect" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two elements. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0032] The following will be combined with the 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 described embodiments 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. Embodiment 1

[0033] The observation methods of plasma are divided into horizontal observation and vertical observation. Horizontal observation collects the signal of the entire analysis channel except the tail flame, so its sensitivity is better than vertical observation which only collects the signal of the local area, and the detection limit is reduced by 5-10 times. However, because horizontal observation collects the signal of the entire analysis channel including the atomization zone and the atomic emission zone, and these two areas are not the best observation areas, horizontal observation increases the background noise and matrix effect while improving the sensitivity, and introduces easy ionization interference. Vertical observation collects light from the side of the plasma and measures the signal of the ion emission zone (the best observation area). Obviously, the signal in this area is not as strong as the signal of the entire analysis channel during horizontal observation, so its sensitivity is not as high as that of horizontal observation, but the signal in this area can provide the best signal-to-background ratio, especially under complex matrices, its signal-to-background ratio is more outstanding. At the same time, vertical observation does not collect the light signal of the atomization zone and the atomic emission zone in the plasma, so it does not have easy ionization interference at all, has a very good linear range, very small matrix effect and very low background, and is flexible and convenient.

[0034] Reference Figure 1-Figure 7A water sample total phosphorus detection device includes a sample introduction system, a light source system, an analysis system and a measurement and control system, and also includes a spectroscopic system. 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. The spectroscopic system includes: 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. The spectroscope 4 is tilted and rotatably disposed at one end of the horizontal chamber 102 close to the light source system. The circumference of the spectroscope is evenly distributed with multiple hollow areas. The light entering the horizontal 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 the light entering from the longitudinal light inlet 2 to the beam splitter 4, and the first reflector 5 and the second reflector 6 are both fixedly arranged on the top of the vertical chamber 101, and the first reflector 5 and the second reflector 6 are respectively located above the light source system and the beam splitter 4; 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.

[0035] The water sample total phosphorus detection device also includes: A first housing 8, in which the sample introduction system, the light source system and the light splitting system are all located. An exhaust port is provided on the top of the first housing 8, through which the light source system is cooled; 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, and the light reflected by the guide mirror 7 passes through the first shell 8 and the second shell 9 into the analysis system.

[0036] 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 directions, the data interfered by easy ionization is eliminated to obtain the optimal data, thereby ensuring the accuracy of the detection. Embodiment 2

[0037] 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 result.

[0038] 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⁻ 4kg / s, the plasma length increases from 260 mm to 550 mm. The best observed ion emission region is located at the top of the plasma, and will also increase with the increase of plasma length. The position of the transverse light inlet 3 is fixed. When the plasma length increases with the increase of ionized gas flow, the ion emission region moves to the top of the transverse light inlet 3. At this time, the atomic emission region is observed by the transverse light inlet 3, and the best observation effect cannot be achieved.

[0039] Therefore, conventional detection equipment requires that the gas flow rate at the ionization point be a fixed value during detection, so that the ion emission area is kept at the set position. However, the sample ejection volume is proportional to the gas flow rate at the ionization point. When the gas flow rate is a fixed value, the sample ejection volume is also basically a fixed value, which limits the detection range of the detection equipment. When the content of the detection component in the sample is small, it is not easy to detect it.

[0040] Reference Figure 1-Figure 7 In this embodiment, the light source system includes an injection tube 10, an auxiliary air pipe 11, a cooling air pipe 12 and a high-frequency coil 13. The lower end of the injection tube 10 is connected to the injection system, the auxiliary air pipe 11 is coaxially sleeved on the outside of the injection tube 10, the lower part of the auxiliary air pipe 11 is connected to the argon gas source, the cooling air pipe 12 is coaxially sleeved on the outside of the auxiliary air pipe 11, the lower part of the cooling air pipe 12 is connected to the argon gas source, and the high-frequency coil 13 is fixedly sleeved on the outer side of the upper end of the cooling air pipe 12.

[0041] 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 .

[0042] 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, and the injection 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.

[0043] 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 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. A plurality of 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.

[0044] The height position of the light source system is adjusted in real time by adjusting the components, and the light source system is kept at the optimal observation position when observing in the vertical direction. During detection, the flow of argon in the auxiliary air pipe 11 drives the sample in the injection tube 10 to be ejected. Gradually increasing the flow rate of argon in the auxiliary air pipe 11 will also increase the amount of sample ejected from the injection tube 10, and the position of the ion emission zone will also rise accordingly. A portion of the argon in the auxiliary air 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 to move downward, so that the atomic emission zone is always located at the height position of the horizontal light inlet 3, which can not only detect the test sample at different ejection amounts, but also ensure the accuracy of the detection.

[0045] By gradually limiting the number and size of the jets 16 through experiments, the gas volumes ejected from the upper and lower ends of the light source system are in a specific ratio, thereby ensuring that during detection, the observation area of ​​the transverse light inlet 3 is always located within the ion emission region.

[0046] At the same time, the ejection volume of the sample 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 ejection volume of the sample, and is easier to be detected, thereby expanding the detection range. Embodiment 3

[0047] In the technical solution of the second embodiment, the height position of the ion emission area can be automatically adjusted according to the argon gas flow rate, so that it automatically corresponds to the horizontal light inlet 3, ensuring vertical observation at the best observation position at all times. However, when the light source system is raised or lowered, due to the limited thickness of the top plate of the adjustment box 15, the light source system will tilt to a certain extent when it is raised or lowered, and it is impossible to ensure that the ion emission area accurately corresponds to the horizontal light inlet 3.

[0048] 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 at the lower part of the adjustment box 15. The lower part 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 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 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 abuts against the lifting sleeve 19.

[0049] 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. Embodiment 4

[0050] A method for detecting total phosphorus in a water sample comprises the following steps: 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 causes the analysis system to detect the phosphorus concentration c2. The spectroscope 4 continues to rotate at a uniform speed and detects 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 injection 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 and c0 in step S4 to calculate the total phosphorus content of the water sample;

[0051] 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.

[0052] 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 .

[0053] The above are only preferred specific implementation modes of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical solutions and inventive concepts of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope 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 optical splitter system is also included, 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, and the optical splitter 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 arranged on the bottom surface of the vertical chamber (101), and the longitudinal light inlet (2) is arranged coaxially with the light source system; a transverse light inlet (3) is arranged 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 beam splitter (4) which is tilted and rotatably arranged at one end of the horizontal chamber (102) close to the light source system, the reflector having a plurality of hollow areas evenly distributed around its circumference, and 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), wherein the first reflector (5) and the second reflector (6) are both fixedly arranged on the top of the vertical chamber (101), and 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) 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.

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), and the 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 outside 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 3, characterized in that: The injection system comprises: An atomizer (14) for atomizing the sample, wherein the atomizer outlet of the atomizer (14) is fixedly connected to the lower end of the sample injection tube (10); A peristaltic pump is used to deliver the sample to the nebulizer (14).

5. A water sample total phosphorus detection device according to claim 4, characterized in that: Also included is an adjustment component, which is used to adjust the height position of the light source system, and the adjustment component includes: 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 part of the auxiliary air pipe (11) and located in the regulating box (15), and 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).

6. A water sample total phosphorus detection device according to claim 5, characterized in that: The auxiliary air pipe (11) comprises an upper guide section (1101) and a lower jet section (1102); the lower portion of the guide section (1101) is longitudinally slidably disposed on the top surface of the regulating box (15); the jet section (1102) is located on the lower side of the top surface of the regulating box (15); 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).

7. A water sample total phosphorus detection device according to claim 5, characterized in that: The adjustment assembly also includes a guide mechanism, and the guide mechanism includes: An orientation sleeve (18), the orientation sleeve (18) being vertically fixedly disposed at the lower part of the adjustment 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) abuts against the lifting sleeve (19).

8. A water sample total phosphorus detection device according to claim 7, characterized in that: A partition (20) is transversely arranged in the middle of the regulating box (15), the directional sleeve (18) is fixedly arranged on the upper side of the partition (20), and 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 outlet of the atomizer (14).

9. 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 8, 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 sample introduction 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), causing 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 injection 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 and c0 in step S4 to calculate the total phosphorus content of the water sample; 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.

10. A method for detecting total phosphorus in water samples according to claim 9, 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 .

Images