Device and method for detecting content of silicon in water

Abstract

The invention discloses a device and a method for detecting silicon content in water, belongs to the field of detection of components in water, and aims to solve the problem that the existing manual operation error of the silicon content in water is large. N placing grooves for placing colorimetric tubes are uniformly distributed around a bottom fixing frame on a test bed, a clear water adding assembly is used for pumping pure water into the colorimetric tubes from a pure water sample storage bottle through a pair of channels of a ten-way valve, and the pure water is cleaned through an oscillator and a timer; the wastewater discharge assembly is used for discharging wastewater after cleaning; the four reagent adding assemblies sequentially pump corresponding reagents into the colorimetric tube from the four reagent storage bottles through four pairs of channels of the ten-way valve, test reagents are added into a silicon dioxide solution in the colorimetric tube, and the solutions are mixed through the oscillator and the timer; the mixed sample taking and placing assembly is used for pumping the mixed solution in the colorimetric tube into the cuvette, a light source of the spectrophotometer irradiates the solution in the cuvette, and the absorbance sensor arranged in the cuvette placing groove detects the absorbance of the solution so as to obtain the silicon content.

Description

Technical Field

[0001] The invention relates to a technology for efficiently and accurately detecting silicon content in water, belonging to the field of water component detection. Background Art

[0002] The silica content in water not only affects the amount of scale generated, but also increases the hardness of the scale. When the silica concentration in the circulating cooling water is higher than the limit, the calcium ions and magnesium ions in the water are easy to react with the high concentration of silicon to form CaCO3·SiO2 precipitation and magnesium silicate scale, which has a low heat transfer coefficient, reduces the heat transfer efficiency of the heat exchanger, and causes pipe blockage. When the silica content in the boiler water is too high to form scale, the heat transfer performance of the heating surface deteriorates, and the heat released during fuel combustion cannot be quickly transferred to the boiler water, resulting in a large amount of heat being taken away by the flue gas, causing the exhaust temperature to rise, increasing the exhaust heat loss, and reducing the thermal efficiency of the boiler. Not only does it waste a lot of fuel, it can also cause metal overheating, reduce strength, and endanger safety. Standard GB / T12149-2017 "Determination of Silicon in Industrial Circulating Cooling Water and Boiler Water" is a traditional pure manual analysis method with large relative errors and cumbersome operation processes. Large power plants require that the detection of silicon content in industrial circulating cooling water and boiler water quality meet higher requirements of low content, high accuracy, and high precision. Therefore, effective detection of silicon content in industrial circulating cooling water and boiler water is crucial to effectively utilize fuel thermal efficiency, reduce scale generation, and ensure personal and equipment safety. Summary of the invention

[0003] In view of the technical problems that the existing method for determining silicon content in water is a purely manual chemical analysis method with large relative errors and complicated operations, the present invention provides a device and method for detecting silicon content in water.

[0004] In one aspect, the present invention provides a device for detecting silicon content in water, comprising a test bench, a bottom fixing frame, a vertical fixing rod, four reagent adding components, a clean water adding component, a waste water discharge component, a mixed sample taking and placing component, N colorimetric tubes, N oscillators, N timers, a colorimetric vessel placement slot, a spectrophotometer, an absorbance sensor, four reagent storage bottles, a pure water storage bottle and a ten-way valve;

[0005] The bottom fixing frame is arranged on the test bench, the vertical fixing rod is connected to the bottom fixing frame, and the vertical fixing rod is provided with a longitudinal slideway; N placement slots for placing colorimetric tubes are evenly distributed around the bottom fixing frame on the test bench, and an oscillator and a timer are arranged in each placement slot; a colorimetric cell placement slot is arranged on the test bench, and an absorbance sensor is arranged in the colorimetric cell placement slot;

[0006] Four reagent adding components, a clean water adding component, a waste water discharging component and a mixed sample taking and placing component are mounted on the vertical fixed rod. Each component can be moved to any position along the longitudinal slideway, and each component can be rotated 360° circumferentially to the top of any colorimetric tube.

[0007] The clean water adding component is used to pump pure water from the pure water storage bottle into the colorimetric tube through a pair of channels of the ten-way valve, and clean it through an oscillator and a timer; the waste water discharging component is used to discharge the cleaned waste water;

[0008] Four reagent adding components sequentially pump corresponding reagents from four reagent storage bottles into colorimetric tubes through four pairs of channels of a ten-way valve, add test reagents to the silica solution in the colorimetric tube, and mix the solutions through an oscillator and a timer;

[0009] The mixed sample taking and placing assembly is used to pump the mixed solution in the colorimetric tube into the cuvette. The light source of the spectrophotometer irradiates the solution in the cuvette. The absorbance sensor arranged in the cuvette placement slot detects the absorbance of the solution to obtain the silicon content.

[0010] Preferably, the reagent adding assembly comprises a rotatable and liftable mechanical rod, a solenoid valve and a volume sensor quantitative tube, the tail end of the rotatable and liftable mechanical rod is set on the vertical fixed rod through a rotatable connecting piece sleeve, the rotatable connecting piece sleeve drives the rotatable and liftable mechanical rod to move up and down to any position along the longitudinal slideway, the rotatable and liftable mechanical rod can be rotated 360° circumferentially to the top of any colorimetric tube through the rotatable connecting piece sleeve, the head end of the rotatable and liftable mechanical rod is provided with a solenoid valve, the input ends of the four solenoid valves are respectively connected to four reagent storage bottles, and the output ends of the four solenoid valves are respectively connected to a volume sensor quantitative tube;

[0011] The clean water adding component includes a rotatable and liftable mechanical rod, a solenoid valve and a volume sensor quantitative tube. The tail end of the rotatable and liftable mechanical rod is mounted on a vertical fixed rod through a rotatable connecting sleeve. The rotatable connecting sleeve drives the rotatable and liftable mechanical rod to move up and down along a longitudinal slide to any position. The rotatable and liftable mechanical rod is rotated 360° circumferentially to above any colorimetric tube through the rotatable connecting sleeve. A solenoid valve is arranged at the head end of the rotatable and liftable mechanical rod. The input end of the solenoid valve is connected to a pure water sample storage bottle, and the output end of the solenoid valve is connected to a volume sensor quantitative tube.

[0012] Preferably, the wastewater discharge assembly includes a rotatable and liftable mechanical rod, a peristaltic pump and a volume sensor quantitative tube, the tail end of the rotatable and liftable mechanical rod is mounted on the vertical fixed rod through a rotatable connecting piece, the rotatable connecting piece drives the rotatable and liftable mechanical rod to move up and down to any position along the longitudinal slideway, the rotatable and liftable mechanical rod is rotated 360° circumferentially to the top of any colorimetric tube through the rotatable connecting piece, a peristaltic pump is arranged at the head end of the rotatable and liftable mechanical rod, the input end of the peristaltic pump is connected to the volume sensor quantitative tube, and the output end of the peristaltic pump is connected to an external waste liquid bottle;

[0013] The mixed sample taking and placing assembly includes a rotatable and liftable mechanical rod, a peristaltic pump and a volume sensor quantitative tube. The tail end of the rotatable and liftable mechanical rod is mounted on a vertical fixed rod through a rotatable connecting piece sleeve. The rotatable connecting piece sleeve drives the rotatable and liftable mechanical rod to move up and down along a longitudinal slide to any position. The rotatable and liftable mechanical rod is rotated 360° circumferentially to the top of any colorimetric tube through the rotatable connecting piece sleeve. A peristaltic pump is arranged at the head end of the rotatable and liftable mechanical rod. The input and output ends of the peristaltic pump are connected to the volume sensor quantitative tube.

[0014] Preferably, the test reagents respectively placed in the four reagent storage bottles are hydrochloric acid solution, ammonium molybdate solution, oxalic acid solution and 1-amino-2-naphthol-4-sulfonic acid solution.

[0015] Preferably, the light source of the spectrophotometer 47 is an ultraviolet light source or a visible light source.

[0016] Preferably, a computer is also included, and the absorbance data is sent to the computer, and the silicon content is calculated in the computer.

[0017] Preferably, the tilt angle and oscillation amplitude of the oscillator are set on the computer side; and the timing time is set on the computer side.

[0018] Preferably, the colorimetric tube, the pure water storage bottle and the four reagent storage bottles are all made of polytetrafluoroethylene.

[0019] Another aspect of the present invention provides a method for detecting silicon content in water, which is implemented based on the device for detecting silicon content in water, and the method comprises the following steps:

[0020] Step 1: Obtaining a silicon content-absorbance calibration curve: Conducting an experiment using a plurality of standard solutions with known silicon dioxide concentrations to obtain a silicon content-absorbance calibration curve;

[0021] Step 2: Clean a colorimetric tube;

[0022] Step 3, adding a silica solution of unknown concentration to be tested into a colorimetric tube;

[0023] Step 4: Add the four reagents required for silicon concentration test into the colorimetric tube in sequence. After each addition of the reagent, shake the colorimetric tube with an oscillator to mix the liquid inside and start timing.

[0024] Step 5, extracting the mixed solution in the colorimetric tube into a cuvette, irradiating the solution in the cuvette with the light source of the spectrophotometer, and obtaining the absorbance of the solution using an absorbance detector;

[0025] Step 6, sending the absorbance measured after adding the test reagent to the silica solution to be tested to the computer;

[0026] Step 7: The computer obtains the silicon content corresponding to the absorbance in step 6 according to the silicon content-absorbance calibration curve obtained in step 1.

[0027] Preferably, the step of obtaining the silicon content-absorbance calibration curve in step 1 comprises:

[0028] Step 11, cleaning N colorimetric tubes;

[0029] Step 1 and 2: adding silicon dioxide standard solutions of different concentrations into N colorimetric tubes;

[0030] Step 13: Add the four reagents required for silicon concentration test to each colorimetric tube in turn. After each addition of reagent, shake the colorimetric tube with an oscillator to mix the liquid inside and start timing.

[0031] Step 14: extract the mixed solution in the colorimetric tube into a cuvette, illuminate the solution in the cuvette with the light source of the spectrophotometer, and obtain the absorbance of the solution using an absorbance detector;

[0032] Step 15: The absorbances measured after adding the test reagent to N silica standard solutions of different concentrations are sent to a computer;

[0033] Step 16: Use absorbance as the ordinate and silicon dioxide concentration as the abscissa to draw a silicon content-absorbance calibration curve using N sets of data.

[0034] Beneficial effects of the present invention: The present invention overcomes the defects of manual operation. The test device of the present invention can realize the steps of automatic cleaning and adding experimental reagents, freeing hands and making the experimental process cleaner and pollution-free, and the experimental results more accurate. At the same time, the device of the present invention has the advantage of simple operation. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 It is a structural schematic diagram of a device for detecting silicon content in water according to the present invention;

[0036] Figure 2 This is a flow chart of a method for detecting silicon content in water according to the present invention.

[0037] 1. Colorimetric tube No. 1, 2. Colorimetric tube No. 2, 3. Colorimetric tube No. 3, 4. Colorimetric tube No. 4, 5. Colorimetric tube No. 5, 6. Colorimetric tube No. 6, 7. Hole for colorimetric tube No. 1, 8. Hole for colorimetric tube No. 2, 9. Hole for colorimetric tube No. 3, 10. Hole for colorimetric tube No. 4, 11. Hole for colorimetric tube No. 5, 12. Hole for colorimetric tube No. 6, 13. Bottom fixing frame, 14. Vertical fixing rod, 15. Quantitative tube for volume sensor No. 1, 16. Hole for colorimetric tube No. 1 Solenoid valve, 17, No. 1 rotatable and liftable mechanical rod, 18, No. 2 volume sensor quantitative tube, 19, No. 2 solenoid valve, 20, No. 2 rotatable and liftable mechanical rod, 21, No. 3 rotatable and liftable mechanical rod, 22, No. 3 solenoid valve, 23, No. 3 volume sensor quantitative tube, 24, No. 4 solenoid valve, 25, No. 4 rotatable and liftable mechanical rod, 26, No. 5 rotatable and liftable mechanical rod, 27, No. 4 volume sensor quantitative tube, 28, No. 5 solenoid valve, Magnetic valve, 29, No. 5 volume sensor quantitative tube, 30, ten-way valve, 31, No. 1 peristaltic pump, 32, No. 2 peristaltic pump, 33, No. 3 peristaltic pump, 34, No. 4 peristaltic pump, 35, No. 5 peristaltic pump, 36, pure water storage bottle, 37, No. 6 volume sensor quantitative tube, 38, hydrochloric acid solution storage bottle, 39, No. 7 volume sensor quantitative tube, 40, ammonium molybdate solution storage bottle, 41, No. 8 volume sensor quantitative tube, 42, oxalic acid solution storage bottle, 43. No. 9 volume sensor quantitative tube, 44. 1-amino-2-naphthol-4-sulfonic acid solution storage bottle, 45. No. 10 volume sensor quantitative tube, 46. Cuvette placement slot, 47. Spectrophotometer, 48. No. 6 rotatable and liftable mechanical rod, 49. No. 6 peristaltic pump, 50. No. 11 volume sensor quantitative tube, 51. No. 7 rotatable and liftable mechanical rod, 52. No. 7 peristaltic pump, 53. No. 12 volume sensor quantitative tube, 54. Test bench. DETAILED DESCRIPTION

[0038] 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 ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0039] It should be noted that, in the absence of conflict, the embodiments of the present invention and the features in the embodiments may be combined with each other.

[0040] The present invention will be further described below in conjunction with the accompanying drawings and specific embodiments, but they are not intended to limit the present invention.

[0041] Specific implementation method 1: The following is combined Figure 1The present embodiment is described. The present embodiment is a device for detecting silicon content in water, comprising a test bench, a bottom fixing frame, a vertical fixing rod, four reagent adding components, a clean water adding component, a waste water discharge component, a mixed sample taking and placing component, N colorimetric tubes, N oscillators, N timers, a colorimetric vessel placement slot, a spectrophotometer, an absorbance sensor, four reagent storage bottles, a pure water storage bottle and a ten-way valve;

[0042] The bottom fixing frame is arranged on the test bench, the vertical fixing rod is connected to the bottom fixing frame, and the vertical fixing rod is provided with a longitudinal slideway; N placement slots for placing colorimetric tubes are evenly distributed around the bottom fixing frame on the test bench, and an oscillator and a timer are arranged in each placement slot; a colorimetric cell placement slot is arranged on the test bench, and an absorbance sensor is arranged in the colorimetric cell placement slot;

[0043] Four reagent adding components, a clean water adding component, a waste water discharging component and a mixed sample taking and placing component are mounted on the vertical fixed rod. Each component can be moved to any position along the longitudinal slideway, and each component can be rotated 360° circumferentially to the top of any colorimetric tube.

[0044] The clean water adding component is used to pump pure water from the pure water storage bottle into the colorimetric tube through a pair of channels of the ten-way valve, and clean it through an oscillator and a timer; the waste water discharging component is used to discharge the cleaned waste water;

[0045] Four reagent adding components sequentially pump corresponding reagents from four reagent storage bottles into colorimetric tubes through four pairs of channels of a ten-way valve, add test reagents to the silica solution in the colorimetric tube, and mix the solutions through an oscillator and a timer;

[0046] The mixed sample taking and placing assembly is used to pump the mixed solution in the colorimetric tube into the cuvette. The light source of the spectrophotometer irradiates the solution in the cuvette. The absorbance sensor arranged in the cuvette placement slot detects the absorbance of the solution to obtain the silicon content.

[0047] The reagent adding component includes a rotatable and liftable mechanical rod, a solenoid valve and a volume sensor quantitative tube. The tail end of the rotatable and liftable mechanical rod is set on the vertical fixed rod through a rotatable connecting piece sleeve. The rotatable connecting piece sleeve drives the rotatable and liftable mechanical rod to move up and down to any position along the longitudinal slide. The rotatable and liftable mechanical rod rotates 360 degrees in the circumferential direction to the top of any colorimetric tube through the rotatable connecting piece sleeve. The head end of the rotatable and liftable mechanical rod is provided with a solenoid valve. The input ends of the four solenoid valves are respectively connected to four reagent storage bottles, and the output ends of the four solenoid valves are respectively connected to a volume sensor quantitative tube.

[0048] The clean water adding component includes a rotatable and liftable mechanical rod, a solenoid valve and a volume sensor quantitative tube. The tail end of the rotatable and liftable mechanical rod is mounted on a vertical fixed rod through a rotatable connecting sleeve. The rotatable connecting sleeve drives the rotatable and liftable mechanical rod to move up and down along a longitudinal slide to any position. The rotatable and liftable mechanical rod is rotated 360° circumferentially to above any colorimetric tube through the rotatable connecting sleeve. A solenoid valve is arranged at the head end of the rotatable and liftable mechanical rod. The input end of the solenoid valve is connected to a pure water sample storage bottle, and the output end of the solenoid valve is connected to a volume sensor quantitative tube.

[0049] The wastewater discharge assembly includes a rotatable and liftable mechanical rod, a peristaltic pump and a volume sensor quantitative tube. The tail end of the rotatable and liftable mechanical rod is set on the vertical fixed rod through a rotatable connecting piece sleeve. The rotatable connecting piece sleeve drives the rotatable and liftable mechanical rod to move up and down to any position along the longitudinal slideway. The rotatable and liftable mechanical rod is rotated 360 degrees in the circumferential direction to the top of any colorimetric tube through the rotatable connecting piece sleeve. A peristaltic pump is set at the head end of the rotatable and liftable mechanical rod. The input end of the peristaltic pump is connected to the volume sensor quantitative tube, and the output end of the peristaltic pump is connected to an external waste liquid bottle.

[0050] The mixed sample taking and placing assembly includes a rotatable and liftable mechanical rod, a peristaltic pump and a volume sensor quantitative tube. The tail end of the rotatable and liftable mechanical rod is mounted on a vertical fixed rod through a rotatable connecting piece sleeve. The rotatable connecting piece sleeve drives the rotatable and liftable mechanical rod to move up and down along a longitudinal slide to any position. The rotatable and liftable mechanical rod is rotated 360° circumferentially to the top of any colorimetric tube through the rotatable connecting piece sleeve. A peristaltic pump is arranged at the head end of the rotatable and liftable mechanical rod. The input and output ends of the peristaltic pump are connected to the volume sensor quantitative tube.

[0051] The test reagents placed in the four reagent storage bottles are hydrochloric acid solution, ammonium molybdate solution, oxalic acid solution and 1-amino-2-naphthol-4-sulfonic acid solution.

[0052] The absorbance data is sent to a computer where the silicon content is calculated.

[0053] The tilt angle and oscillation amplitude of the oscillator are set on the computer side; the timing time is set on the computer side.

[0054] The colorimetric tube, pure water storage bottle, four reagent storage bottles and connecting tubes are all made of polytetrafluoroethylene.

[0055] The following is an example of N=6. Figure 1The device comprises 6 colorimetric tubes (1, 2, 3, 4, 5, 6), 6 colorimetric tube placement holes (6, 7, 8, 9, 10, 11, 12), a bottom fixing frame 13, a vertical fixing rod 14, 7 rotatable and liftable mechanical rods (17, 20, 21, 26, 25, 48, 51), 5 solenoid valves (16, 19, 22, 24, 28), 12 volume sensor quantitative tubes (15, 18, 23, 27, 29, 45, 43, 41, 39, 37, 50, 53), a pure water storage bottle 36, a hydrochloric acid solution storage bottle 38, an ammonium molybdate solution storage bottle 40, an oxalic acid solution storage bottle 42, 1-amino-2-naphthol-4 -sulfonic acid solution storage bottle 44, 7 peristaltic pumps (31, 32, 33, 34, 35, 49, 52), a ten-way valve 30, a spectrophotometer 47, and a cuvette placement slot 46; the materials of the 12 volume sensor quantitative tubes (15, 18, 23, 27, 29, 45, 43, 41, 39, 37, 50, 53), the pure water storage bottle 36, the hydrochloric acid solution storage bottle 38, the ammonium molybdate solution storage bottle 40, the oxalic acid solution storage bottle 42, and the 1-amino-2-naphthol-4-sulfonic acid solution storage bottle 44 are all polytetrafluoroethylene; the materials of the 6 colorimetric tubes (1, 2, 3, 4, 5, 6) are all high-temperature resistant polytetrafluoroethylene.

[0056] The six colorimetric tubes (1, 2, 3, 4, 5, 6) have scale lines and are equipped with matching sealing covers. After being taken out of the device and covered with sealing covers, they can be heated in a 100°C water bath without deformation, and can be taken out at will, which is convenient for adding liquid and cleaning; the 12 volume sensor quantitative tubes (15, 18, 23, 27, 29, 45, 43, 41, 39, 37, 50, 53) have scale lines and can quantitatively measure the volume of liquid; the bottom fixing frame 13 can fix the vertical fixing The vertical fixed rod 14 is provided with a longitudinal slideway, and 7 rotatable and liftable mechanical rods (17, 20, 21, 26, 25, 48) are respectively equipped with position sensors, and each rotatable and liftable mechanical rod is sleeved on the vertical fixed rod 14 through a rotatable connecting piece, and the rotatable connecting piece can move up and down along the longitudinal slideway. After reaching the specified position, the rotatable and liftable mechanical rod can rotate 360° along the rotatable connecting piece to position and identify 6 colorimetric tube placement holes (6, 7, 8, 9, 10, 11, 12) and the position of the cuvette placement slot 46; the rotatable connecting piece is nested inside and outside, the inner layer moves along the longitudinal slideway of the vertical fixed rod 14, and the outer layer can rotate circumferentially along the inner layer, driving the rotatable and liftable mechanical rod (17, 20, 21, 26, 25, 48) to rotate circumferentially; the pure water storage bottle 36, the hydrochloric acid solution storage bottle 38, the ammonium molybdate solution storage bottle 40, the oxalic acid solution storage bottle 42, the 1-amino-2-naphthol-4-sulfonic acid solution storage bottle The bottles 44 can be taken out at will, which is convenient for adding liquid and cleaning; the bottom of the six colorimetric tube placement holes (6, 7, 8, 9, 10, 11, 12) is equipped with a timing sensor and an oscillator; the colorimetric cell placement slot 46 can be replaced with colorimetric cells of different sizes as required, and the inner wall of the slot is also equipped with an absorbance detector. The light source of the spectrophotometer 47 is an ultraviolet light source or a visible light source, which irradiates the solution in the colorimetric cell, and the absorbance detector detects its absorbance and transmits the detected value to the computer.

[0057] The pure water sample storage bottle 36, hydrochloric acid solution sample storage bottle 38, ammonium molybdate solution sample storage bottle 40, oxalic acid solution sample storage bottle 42, and 1-amino-2-naphthol-4-sulfonic acid solution sample storage bottle 44 are all equipped with two matching covers, one of which has a hole in the middle connected to the volume sensor quantitative tube (45, 43, 41, 39, 37) and is used during the experiment, and the other cover is a hole-free sealing cover and is used after the experiment.

[0058] One end of the No. 10 volume sensor quantitative tube 45 passes through the perforated lid of the 1-amino-2-naphthol-4-sulfonic acid solution storage bottle 44 and is inserted into the bottom of the 1-amino-2-naphthol-4-sulfonic acid solution storage bottle 44, and the other end is connected to the access end of the No. 5 peristaltic pump 35 through a connecting tube. The output end of the No. 5 peristaltic pump 35 enters the channel 1 of the ten-way valve 30 through the connecting tube. After the channel 10 of the ten-way valve 30 is output, it is connected to one end of the No. 1 solenoid valve 16 through the connecting tube, and the other end of the No. 1 solenoid valve 16 is connected to the No. 1 volume sensor quantitative tube 15.

[0059] One end of the No. 9 volume sensor quantitative tube 43 passes through the perforated lid of the oxalic acid solution storage bottle 42 and is inserted into the bottom of the oxalic acid solution storage bottle 42, and the other end is connected to the access end of the No. 4 peristaltic pump 34 through a connecting tube. The output end of the No. 4 peristaltic pump 34 enters the channel 2 of the ten-way valve 30 through the connecting tube. After the output of the channel 9 of the ten-way valve 30, it is connected to one end of the No. 2 solenoid valve 19 through the connecting tube, and the other end of the No. 2 solenoid valve 19 is connected to the No. 2 volume sensor quantitative tube 18.

[0060] One end of the No. 8 volume sensor quantitative tube 41 passes through the perforated lid of the ammonium molybdate solution storage bottle 40 and is inserted into the bottom of the ammonium molybdate solution storage bottle 40, and the other end is connected to the access end of the No. 3 peristaltic pump 33 through a connecting tube, and the output end of the No. 3 peristaltic pump 33 enters the channel 3 of the ten-way valve 30 through the connecting tube. After the channel 8 of the ten-way valve 30 is output, it is connected to one end of the No. 3 solenoid valve 22 through the connecting tube, and the other end of the No. 3 solenoid valve 22 is connected to the No. 3 volume sensor quantitative tube 23.

[0061] One end of the No. 7 volume sensor quantitative tube 39 passes through the perforated lid of the hydrochloric acid solution storage bottle 38 and is inserted into the bottom of the hydrochloric acid solution storage bottle 38, and the other end is connected to the access end of the No. 2 peristaltic pump 32 through a connecting tube, and the output end of the No. 2 peristaltic pump 32 enters the channel 4 of the ten-way valve 30 through the connecting tube. After the output of the channel 7 of the ten-way valve 30, it is connected to one end of the No. 4 solenoid valve 24 through the connecting tube, and the other end of the No. 4 solenoid valve 24 is connected to the No. 4 volume sensor quantitative tube 27.

[0062] One end of the No. 6 volume sensor quantitative tube 37 passes through the perforated lid of the water sample storage bottle 36 and is inserted into the bottom of the water sample storage bottle 36, and the other end is connected to the access end of the No. 1 peristaltic pump 31 through a connecting tube. The output end of the No. 1 peristaltic pump 31 enters the channel 5 of the ten-way valve 30 through the connecting tube. After the channel 6 of the ten-way valve 30 is output, it is connected to one end of the No. 5 solenoid valve 28 through the connecting tube, and the other end of the No. 5 solenoid valve 28 is connected to the No. 5 volume sensor quantitative tube 29.

[0063] The eleventh volume sensor quantitative tube 50 is connected to the access end of the sixth peristaltic pump 49, and the output end of the sixth peristaltic pump 49 is connected to the waste liquid bottle through a connecting tube.

[0064] Specific implementation method 2: The following is combined Figure 1 and Figure 2 This embodiment describes a method for detecting silicon content in water described in this embodiment, which is implemented based on the device for detecting silicon content in water described in the first embodiment. The method includes the following steps:

[0065] Step 1: Obtaining a silicon content-absorbance calibration curve: Conducting an experiment using a plurality of standard solutions with known silicon dioxide concentrations to obtain a silicon content-absorbance calibration curve;

[0066] Step 2: Clean a colorimetric tube;

[0067] Step 3, adding a silica solution of unknown concentration to be tested into a colorimetric tube;

[0068] Step 4: Add the four reagents required for silicon concentration test into the colorimetric tube in sequence. After each addition of the reagent, shake the colorimetric tube with an oscillator to mix the liquid inside and start timing.

[0069] Step 5: extract the mixed solution in the colorimetric tube into a cuvette, illuminate the solution in the cuvette with the light source of the spectrophotometer, and obtain the absorbance of the solution using an absorbance detector;

[0070] Step 6, sending the absorbance measured after adding the test reagent to the silica solution to be tested to the computer;

[0071] Step 7: The computer obtains the silicon content corresponding to the absorbance in step 6 according to the silicon content-absorbance calibration curve obtained in step 1.

[0072] The steps for obtaining the silicon content-absorbance calibration curve in step 1 include:

[0073] Step 11, cleaning N colorimetric tubes;

[0074] Step 1 and 2: adding silicon dioxide standard solutions of different concentrations into N colorimetric tubes;

[0075] Step 13: Add the four reagents required for silicon concentration test to each colorimetric tube in turn. After each addition of reagent, shake the colorimetric tube with an oscillator to mix the liquid inside and start timing.

[0076] Step 14: extract the mixed solution in the colorimetric tube into a cuvette, illuminate the solution in the cuvette with the light source of the spectrophotometer, and obtain the absorbance of the solution using an absorbance detector;

[0077] Step 15: The absorbances measured after adding the test reagent to N silica standard solutions of different concentrations are sent to a computer;

[0078] Step 16: Use absorbance as the ordinate and silicon dioxide concentration as the abscissa to draw a silicon content-absorbance calibration curve using N sets of data.

[0079] The detection method is explained by taking N=6 as an example.

[0080] First, after the corresponding liquids are filled in the pure water storage bottle 36, the hydrochloric acid solution storage bottle 38, the ammonium molybdate solution storage bottle 40, the oxalic acid solution storage bottle 42, and the 1-amino-2-naphthol-4-sulfonic acid solution storage bottle 44, the lids having holes in the middle for connecting with the volume sensor quantitative tubes (45, 43, 41, 39, 37) are replaced, and the volume sensor quantitative tubes (45, 43, 41, 39, 37) are connected to them respectively. No liquid is added when the colorimetric tube is cleaned. A required size is placed in the colorimetric cell slot 46. inch colorimetric cuvette, turn on the device switch and the computer host, set the corresponding program, parameters, time, and volume of pure water required for cleaning on the computer, and enter the pipeline cleaning stage before the experiment. The fourth rotatable and liftable mechanical rod 25 moves up and down on the longitudinal slide of the vertical fixed rod 14 to the set position and then rotates to the top of the No. 1 colorimetric tube 1. The No. 5 volume sensor quantitative tube 29 enters the upper part of the No. 1 colorimetric tube 1, the No. 1 peristaltic pump 31 is turned on, and the No. 6 volume sensor quantitative tube 37 extracts a certain volume from the pure water storage bottle 36. The accumulated pure water enters the channel 5 of the ten-way valve 30, flows out from the channel 6 of the ten-way valve 30 and enters the No. 5 solenoid valve 28. After the No. 5 solenoid valve 28 is started, the pure water enters the No. 1 colorimetric tube 1 through the No. 5 volume sensor quantitative tube 29. After the oscillator shakes the No. 1 colorimetric tube 1 to mix the internal liquid, the timing starts automatically. When the timing ends, the No. 6 rotatable and liftable mechanical rod 48 moves up and down along the longitudinal slide of the vertical fixed rod 14 to the set position and then rotates to the top of the No. 1 colorimetric tube 1. The No. 11 volume sensor quantitative tube 5 0 enters the bottom of colorimetric tube No. 1, peristaltic pump No. 6 is started, and the water after cleaning in colorimetric tube No. 1 is drawn from volume sensor quantitative tube No. 11 50 and discharged into the waste liquid bottle, and rotatable and liftable mechanical rod No. 6 moves to the original position along the longitudinal slide of vertical fixed rod 14 and then rotates to the relative position of colorimetric tube No. 2, colorimetric tube No. 3, colorimetric tube No. 4, colorimetric tube No. 5, colorimetric tube No. 6, and the cuvette in cuvette slot 46, and repeats the cleaning steps of colorimetric tube No. 1 to complete all cleaning steps.

[0081] After the cleaning step is completed, colorimetric tube No. 1, colorimetric tube No. 2, colorimetric tube No. 3, colorimetric tube No. 4, colorimetric tube No. 5, and colorimetric tube No. 6 are taken out of the device respectively, and the prepared silica standard solution diluted to a fixed scale is added respectively. The concentrations of the standard solutions C1, C2, C3, C4, C5, and C6 are 0.00 mg / L, 0.01 mg / L, 0.02 mg / L, and 0.04 mg / L respectively. , 0.06mg / L, 0.08mg / L, and the concentration values ​​of the standard solution C1, C2, C3, C4, C5, and C6 are respectively input into the computer. After the solution is loaded, colorimetric tube No. 1, colorimetric tube No. 2, colorimetric tube No. 3, colorimetric tube No. 4, colorimetric tube No. 5, and colorimetric tube No. 6 are respectively placed in 6 colorimetric tube placement holes (6, 7, 8, 9, 10, 11, 12), and the reagent adding step is entered.

[0082] The No. 2 peristaltic pump 32 is turned on, and the No. 7 volume sensor quantitative tube 39 draws a certain volume of hydrochloric acid solution from the hydrochloric acid storage bottle 38 and enters the channel 4 of the ten-way valve 30, and then flows out from the channel 7 of the ten-way valve 30 and enters the No. 4 solenoid valve 24. After the No. 4 solenoid valve 24 is started, the hydrochloric acid solution enters the No. 1 colorimetric tube 1 through the No. 4 volume sensor quantitative tube 27. The No. 5 rotatable and liftable mechanical rod 26 moves up and down along the longitudinal slide of the vertical fixed rod 14 to the set position and then rotates to the top of the No. 1 colorimetric tube 1, so that the No. 4 volume sensor quantitative tube 27 enters the upper part of the No. 1 colorimetric tube 1, and the quantitative volume of hydrochloric acid solution is added to the No. 1 colorimetric tube 1; the No. 3 peristaltic pump 33 is turned on, and the No. 8 volume sensor quantitative tube 41 draws a certain volume of hydrochloric acid solution from the ammonium molybdate storage bottle 38. The volume of ammonium molybdate solution enters the channel 3 of the ten-way valve 30, flows out from the channel 8 of the ten-way valve 30 and enters the No. 3 solenoid valve 22. After the No. 3 solenoid valve 22 is started, the ammonium molybdate enters the No. 1 colorimetric tube 1 through the No. 3 volume sensor quantitative tube 23. The No. 3 rotatable and liftable mechanical rod 21 moves up and down along the longitudinal slide of the vertical fixed rod 14 to the set position and then rotates to the top of the No. 1 colorimetric tube 1, so that the No. 3 volume sensor quantitative tube 23 enters the upper part of the No. 1 colorimetric tube 1, and the quantitative volume of ammonium molybdate solution is added to the No. 1 colorimetric tube 1. After the oscillator shakes the No. 1 colorimetric tube 1 to mix the internal liquid, the timing of 5 minutes starts automatically and the timing ends; the No. 4 peristaltic pump 34 is turned on, and the No. 9 volume sensor quantitative tube 43 extracts a certain volume from the oxalic acid storage bottle 42. The accumulated oxalic acid solution enters the channel 2 of the ten-way valve 30, flows out from the channel 9 of the ten-way valve 30 and enters the second solenoid valve 19. After the second solenoid valve 19 is started, the oxalic acid solution enters the first colorimetric tube 1 through the second volume sensor quantitative tube 18. The second rotatable and liftable mechanical rod 20 moves up and down along the longitudinal slide of the vertical fixed rod 14 to the set position and then rotates to the top of the first colorimetric tube 1, so that the second volume sensor quantitative tube 18 enters the upper part of the first colorimetric tube 1, and the quantitative volume of oxalic acid solution is added to the first colorimetric tube 1. After the oscillator shakes the first colorimetric tube 1 to mix the internal liquid, the timing of 1 minute starts automatically and the timing ends; the fifth peristaltic pump 35 is turned on, and the tenth volume sensor quantitative tube 45 is moved from 1-amino-2-naphthol-4-sulfonic acid A certain volume of 1-amino-2-naphthol-4-sulfonic acid solution is drawn from the solution storage bottle 44 and enters the channel 1 of the ten-way valve 30. After flowing out from the channel 10 of the ten-way valve 30, it enters the No. 1 solenoid valve 16. After the No. 1 solenoid valve 16 is started, the 1-amino-2-naphthol-4-sulfonic acid solution enters the No. 1 colorimetric tube 1 through the No. 1 volume sensor quantitative tube 15. The No. 1 rotatable and liftable mechanical rod 17 moves up and down along the longitudinal slide of the vertical fixed rod 14 to a set position and then rotates to the top of the No. 1 colorimetric tube 1. The No. 1 volume sensor quantitative tube 15 enters the upper part of the No. 1 colorimetric tube 1, and a quantitative volume of oxalic acid solution is added to the No. 1 colorimetric tube 1. After the oscillator shakes the No. 1 colorimetric tube 1 to mix the internal liquid, the timing of 10 minutes starts automatically and the timing ends.Repeat the above steps to complete the reagent addition and timing steps of colorimetric tube No. 2, colorimetric tube No. 3, colorimetric tube No. 4, colorimetric tube No. 5, and colorimetric tube No. 6, respectively.

[0083] The 11th rotatable and liftable mechanical rod 51 moves along the longitudinal slide of the vertical fixed rod 14 to the specified position and then rotates to the top of the No. 1 colorimetric tube 1. The 11th rotatable and liftable mechanical rod 51 continues to move downward along the longitudinal slide of the vertical fixed rod 14 to the lower end of the No. 12 volume sensor quantitative tube 53 and enters the liquid in the No. 1 colorimetric tube 1. The No. 7 peristaltic pump 52 is started, and the No. 12 volume sensor quantitative tube 53 extracts a quantitative volume of liquid from the liquid in the No. 1 colorimetric tube 1. The 11th rotatable and liftable mechanical rod 51 moves upward along the longitudinal slide of the vertical fixed rod 14 to the original position. The 11th rotatable and liftable mechanical rod 5 1 moves along the longitudinal slide of the vertical fixed rod 14 and rotates to the top of the cuvette of the cuvette slot 46, releases the solution just extracted into the cuvette, and after being irradiated by the light source of the spectrophotometer 47, the absorbance A1 detected by the spectrophotometer detector is transmitted to the computer terminal; repeat the above steps, respectively detect the absorbance A2, A3, A4, A5, A6 of the liquid in the No. 2 colorimetric tube 2, the No. 3 colorimetric tube 3, the No. 4 colorimetric tube 4, the No. 5 colorimetric tube 5, and the No. 6 colorimetric tube 6, and transmit them to the computer terminal; with the measured absorbance A as the ordinate and the concentration value C of the silica solution as the abscissa, draw a calibration curve or calculate the regression equation.

[0084] After drawing the curve or calculating the regression equation, the cleaning step at the end of the experiment is carried out. The cleaning process is exactly the same as the cleaning process before the experiment. The number of cleaning times is set on the computer as needed. After the cleaning is completed, the six colorimetric tubes (1, 2, 3, 4, 5, 6) are all clean colorimetric tubes. The colorimetric tubes can also be taken out of the device and manually cleaned. A corresponding volume of pure water is added to the clean colorimetric tube No. 1 as a blank. A quantitative volume of the water sample to be tested is placed in the other five clean colorimetric tubes (2, 3, 4, 5, 6) as needed. The above steps of adding reagents, timing, shaking, and detecting are repeated to obtain the absorbance of the blank and the water sample to be tested.

[0085] The computer automatically calculates the concentration values ​​of the blank and the water sample to be tested based on the drawn calibration curve or calculated regression equation. The method process refers to steps 2 to 7. The calibration curve range can be adjusted according to the calcium dioxide content in the water sample to be tested.

[0086] After the experiment, the cleaning steps are carried out. The specific cleaning process is exactly the same as the cleaning process before the experiment. The number of cleaning times can be set on the computer as needed. After the cleaning is completed, turn off the device switch.

[0087] The computer terminal in the present invention can control the entire test process and can display the result value of the final silica concentration calculated according to the formula in the standard GB / T12149-2017 "Determination of silicon in industrial circulating cooling water and boiler water".

[0088] Although the present invention is described herein with reference to specific embodiments, it should be understood that these embodiments are merely examples of the principles and applications of the present invention. It should therefore be understood that many modifications may be made to the exemplary embodiments and that other arrangements may be devised without departing from the spirit and scope of the present invention as defined by the appended claims. It should be understood that the various dependent claims and features described herein may be combined in a manner different from that described in the original claims. It should also be understood that the features described in conjunction with a single embodiment may be used in other described embodiments.

Claims

1. A device for detecting silicon content in water, characterized in that: It includes a test bench, a bottom fixing frame, a vertical fixing rod, 4 reagent adding components, a clean water adding component, a waste water discharge component, a mixed sample taking and placing component, N colorimetric tubes, N oscillators, N timers, a colorimetric vessel placement slot, a spectrophotometer, an absorbance sensor, four reagent storage bottles, a pure water storage bottle and a ten-way valve; The bottom fixing frame is arranged on the test bench, the vertical fixing rod is connected to the bottom fixing frame, and the vertical fixing rod is provided with a longitudinal slideway; N placement slots for placing colorimetric tubes are evenly distributed around the bottom fixing frame on the test bench, and an oscillator and a timer are arranged in each placement slot; a colorimetric cell placement slot is arranged on the test bench, and an absorbance sensor is arranged in the colorimetric cell placement slot; Four reagent adding components, a clean water adding component, a waste water discharging component and a mixed sample taking and placing component are mounted on the vertical fixed rod. Each component can be moved to any position along the longitudinal slideway, and each component can be rotated 360° circumferentially to the top of any colorimetric tube. The clean water adding component is used to pump pure water from the pure water storage bottle into the colorimetric tube through a pair of channels of the ten-way valve, and clean it through an oscillator and a timer; the waste water discharging component is used to discharge the cleaned waste water; Four reagent adding components sequentially pump corresponding reagents from four reagent storage bottles into colorimetric tubes through four pairs of channels of a ten-way valve, add test reagents to the silica solution in the colorimetric tube, and mix the solutions through an oscillator and a timer; The mixed sample taking and placing assembly is used to pump the mixed solution in the colorimetric tube into the cuvette. The light source of the spectrophotometer irradiates the solution in the cuvette. The absorbance sensor arranged in the cuvette placement slot detects the absorbance of the solution to obtain the silicon content.

2. A device for detecting silicon content in water according to claim 1, characterized in that: The reagent adding component includes a rotatable and liftable mechanical rod, a solenoid valve and a volume sensor quantitative tube. The tail end of the rotatable and liftable mechanical rod is set on the vertical fixed rod through a rotatable connecting piece sleeve. The rotatable connecting piece sleeve drives the rotatable and liftable mechanical rod to move up and down to any position along the longitudinal slide. The rotatable and liftable mechanical rod rotates 360 degrees in the circumferential direction to the top of any colorimetric tube through the rotatable connecting piece sleeve. The head end of the rotatable and liftable mechanical rod is provided with a solenoid valve. The input ends of the four solenoid valves are respectively connected to four reagent storage bottles, and the output ends of the four solenoid valves are respectively connected to a volume sensor quantitative tube. The clean water adding component includes a rotatable and liftable mechanical rod, a solenoid valve and a volume sensor quantitative tube. The tail end of the rotatable and liftable mechanical rod is mounted on a vertical fixed rod through a rotatable connecting sleeve. The rotatable connecting sleeve drives the rotatable and liftable mechanical rod to move up and down along a longitudinal slide to any position. The rotatable and liftable mechanical rod is rotated 360° circumferentially to above any colorimetric tube through the rotatable connecting sleeve. A solenoid valve is arranged at the head end of the rotatable and liftable mechanical rod. The input end of the solenoid valve is connected to a pure water sample storage bottle, and the output end of the solenoid valve is connected to a volume sensor quantitative tube.

3. A device for detecting silicon content in water according to claim 1, characterized in that: The wastewater discharge assembly includes a rotatable and liftable mechanical rod, a peristaltic pump and a volume sensor quantitative tube. The tail end of the rotatable and liftable mechanical rod is set on the vertical fixed rod through a rotatable connecting piece sleeve. The rotatable connecting piece sleeve drives the rotatable and liftable mechanical rod to move up and down to any position along the longitudinal slideway. The rotatable and liftable mechanical rod is rotated 360 degrees in the circumferential direction to the top of any colorimetric tube through the rotatable connecting piece sleeve. A peristaltic pump is set at the head end of the rotatable and liftable mechanical rod. The input end of the peristaltic pump is connected to the volume sensor quantitative tube, and the output end of the peristaltic pump is connected to an external waste liquid bottle. The mixed sample taking and placing assembly includes a rotatable and liftable mechanical rod, a peristaltic pump and a volume sensor quantitative tube. The tail end of the rotatable and liftable mechanical rod is mounted on a vertical fixed rod through a rotatable connecting piece sleeve. The rotatable connecting piece sleeve drives the rotatable and liftable mechanical rod to move up and down along a longitudinal slide to any position. The rotatable and liftable mechanical rod is rotated 360° circumferentially to the top of any colorimetric tube through the rotatable connecting piece sleeve. A peristaltic pump is arranged at the head end of the rotatable and liftable mechanical rod. The input and output ends of the peristaltic pump are connected to the volume sensor quantitative tube.

4. A device for detecting silicon content in water according to claim 1, characterized in that: The test reagents placed in the four reagent storage bottles are hydrochloric acid solution, ammonium molybdate solution, oxalic acid solution and 1-amino-2-naphthol-4-sulfonic acid solution.

5. A device for detecting silicon content in water according to claim 1, characterized in that: The light source of the spectrophotometer 47 is an ultraviolet light source or a visible light source.

6. A device for detecting silicon content in water according to claim 1, characterized in that: Also included is a computer to which the absorbance data is sent and in which the silicon content is calculated.

7. A device for detecting silicon content in water according to claim 6, characterized in that: The tilt angle and oscillation amplitude of the oscillator are set on the computer side; the timing time is set on the computer side.

8. A device for detecting silicon content in water according to claim 1, characterized in that: The colorimetric tubes, pure water storage bottles and four reagent storage bottles are all made of polytetrafluoroethylene.

9. A method for detecting silicon content in water, implemented based on the device for detecting silicon content in water according to any one of claims 1 to 8, characterized in that: The method comprises the following steps: Step 1: Obtaining a silicon content-absorbance calibration curve: Conducting an experiment using a plurality of standard solutions with known silicon dioxide concentrations to obtain a silicon content-absorbance calibration curve; Step 2: Clean a colorimetric tube; Step 3, adding a silica solution of unknown concentration to be tested into a colorimetric tube; Step 4: Add the four reagents required for silicon concentration test into the colorimetric tube in sequence. After each addition of the reagent, shake the colorimetric tube with an oscillator to mix the liquid inside and start timing. Step 5: extract the mixed solution in the colorimetric tube into a cuvette, illuminate the solution in the cuvette with the light source of the spectrophotometer, and obtain the absorbance of the solution using an absorbance detector; Step 6, sending the absorbance measured after adding the test reagent to the silica solution to be tested to the computer; Step 7: The computer obtains the silicon content corresponding to the absorbance in step 6 according to the silicon content-absorbance calibration curve obtained in step 1.

10. A method for detecting silicon content in water according to claim 9, characterized in that: The steps for obtaining the silicon content-absorbance calibration curve in step 1 include: Step 11, cleaning N colorimetric tubes; Step 1 and 2: adding silicon dioxide standard solutions of different concentrations into N colorimetric tubes; Step 13: Add the four reagents required for silicon concentration test to each colorimetric tube in turn. After each addition of reagent, shake the colorimetric tube with an oscillator to mix the liquid inside and start timing. Step 14: extract the mixed solution in the colorimetric tube into a cuvette, illuminate the solution in the cuvette with the light source of the spectrophotometer, and obtain the absorbance of the solution using an absorbance detector; Step 15: The absorbances measured after adding the test reagent to N silica standard solutions of different concentrations are sent to a computer; Step 16: Use absorbance as the ordinate and silicon dioxide concentration as the abscissa to draw a silicon content-absorbance calibration curve using N sets of data.

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