A fully automatic rapid silicate detector

Abstract

The utility model relates to a kind of full-automatic quick silicate detector, comprising: sample introduction system, by sample introduction cup (1) and heating device (11) are constituted, sample introduction cup (1) is connected with heating device (11), for accommodating water sample to be measured, heating device (11) is connected with sample introduction cup (1) and luminescence dish (10) respectively;Reaction detection system, by luminescence dish (10) and photomultiplier (2) are constituted, luminescence dish (10) is connected with heating device (11), flow path device (3) and photomultiplier (2) respectively;Flow path control device (3), by micro diaphragm pump, solenoid valve and metering sensor are constituted;Electronic control system, by control panel (7) and acquisition board (9) are constituted;Control panel (7) is used for flow path time sequence control and temperature PID adjustment;Acquisition board (9) is used for converting photomultiplier current into voltage, 24 bit ADC sampling and calculating silicate concentration, realize automatic dosing and stirring process, automatically complete the detection of silicate ion in water sample.

Description

Technical Field

[0001] This utility model relates to the field of calibration technology for analytical instruments, and in particular to a fully automatic rapid silicate detector. Background Technology

[0002] The treatment and monitoring of boiler water in thermal power plants is a crucial aspect, directly impacting boiler safety, energy efficiency, and the overall economic benefits of the power plant. The silicate content in boiler water is a key indicator of boiler water quality. Currently, most thermal power plants and the semiconductor industry use silicate analyzers based on the molybdenum blue colorimetric principle as the primary method for detecting silicate ion concentration. This process requires manual addition of reagents, followed by a chemical colorimetric reaction, and measurement using the analyzer. This process has low automation, long detection times, and significant human influence. Chemiluminescence (silicomolybdenum heteropolyacid spectrophotometry) utilizes the reaction of silicon and molybdate to produce silicomolybdenum heteropolyacid, which reacts with luminol to generate strong chemiluminescence. By detecting the intensity of the chemiluminescence, the concentration of the reactants can be directly determined. The luminescence reaction is completed within tens of seconds, making it a rapid and effective method for measuring trace amounts of silicate. The outstanding advantages of chemiluminescence are high sensitivity, no need for an external excitation light source, avoidance of interference from background light and stray light, and reduced noise. However, its measurement repeatability is poor and its measurement accuracy is low.

[0003] Therefore, the existing technology has the following technical defects:

[0004] (1) The reaction time is long, and each sample needs to be tested for more than ten minutes;

[0005] (2) The operation is complex and the degree of automation is low. The traditional silicon molybdenum blue colorimetric method involves multiple chemical processing steps, which increases the possibility of human error.

[0006] (3) The test results have low repeatability and poor accuracy. Utility Model Content

[0007] The purpose of this invention is to provide a fully automatic rapid silicate detector, solving the problem of rapid detection of silicate concentration in water in the laboratory. It is an intelligent silicate detector, primarily targeting trace and micro-scale silicate ions in water. The device uses chemiluminescence immunoassay, and the detection time for each sample is no more than 2 minutes. The fully automatic rapid silicate detector has a detection range of 0-50 μg / L, specifically designed for detecting trace silicate ions in water. The detector has a built-in heating device that automatically heats the water sample when the temperature is below 21°C, ensuring a constant temperature and guaranteeing accurate results. Furthermore, this detector is highly automated. The luminescent dish has a built-in drain pump, allowing for self-cleaning after the user pours the water sample into the sample cup, eliminating the need for manual cleaning. It automatically adds reagents and stirs, automatically completing the detection of silicate ions in the water sample.

[0008] This utility model provides a fully automatic rapid silicate detector, comprising:

[0009] The sample introduction system consists of a sample introduction cup (1) and a heating device (11). The sample introduction cup (1) is connected to the heating device (11) through a silicone tube and is used to hold the water sample to be tested. The heating device (11) is connected to the sample introduction cup (1) and the luminescent dish (10) respectively. The heating device (11) includes a PTC ceramic and a temperature sensor. The PTC ceramic is used to heat the water sample to 25±0.5℃ when the water sample temperature is <21℃, thereby eliminating the influence of temperature on color development. The temperature sensor is used to measure the real-time temperature of the water sample and perform feedback control.

[0010] The reaction detection system consists of the light-emitting dish (10) and the photomultiplier tube (2). The light-emitting dish (10) is connected to the heating device (11), the flow path device (3), and the photomultiplier tube (2). The light-emitting dish (10) includes a quartz optical path cell, which provides a 10mm path for optical transmission. The photomultiplier tube (2) is used to detect the absorbance of molybdenum blue at 810nm wavelength, convert photons into electrons, and output current signals.

[0011] The flow path control device (3) consists of 3 micro diaphragm pumps, 6 solenoid valves and 3 metering sensors; the 3 micro diaphragm pumps are used to drive reagent A, reagent B and reagent C respectively; the 6 solenoid valves are used to switch the flow path; the 3 metering sensors are used to control the dosage volume.

[0012] The electronic control system consists of a control board (7) and a data acquisition board (9); the control board (7) is used for flow path timing control and temperature PID adjustment; the data acquisition board (9) is used to convert the photomultiplier tube current into voltage, perform 24-bit ADC sampling, and calculate silicate concentration.

[0013] Preferably, the inner wall of the sample inlet cup (1) is coated with polytetrafluoroethylene to prevent adsorption.

[0014] Preferably, the flow path control device (3) further includes a built-in magnetic stirrer for stirring the mixture formed by the added reagents A, B and C with the sample water.

[0015] Preferably, the fully automatic rapid silicate detector further includes:

[0016] The human-computer interaction system consists of a screen (6) and a switch button (12); wherein the screen (6) is used to display one or more of the real-time concentration, voltage value and temperature curve; and the switch button (12) is used to trigger the system to start self-test.

[0017] Preferably, the screen (6) is a 5-inch LCD touch screen.

[0018] Preferably, the switch button (12) is a waterproof button.

[0019] Preferably, the fully automatic rapid silicate detector further includes:

[0020] The main unit (5) and the side panel; wherein the side panel includes a right side panel (4) and a left side panel (8), wherein the right side panel (4) and the left side panel (8) are combined to form an integrated heat dissipation duct, and the inside of the right side panel (4) and the left side panel (8) is provided with metal wiring grooves to suppress EMI interference.

[0021] Preferably, the host (5) has an aluminum-magnesium alloy shell with dimensions of 400×300×200mm.

[0022] Preferably, the fully automatic rapid silicate detector further includes:

[0023] The power supply module (13) has an input of 220V±10% AC signal and outputs including +5V voltage for logic circuits, ±12V voltage for photomultiplier tube high voltage and +24V voltage for pump valve drive.

[0024] Preferably, the power supply module (13) includes an overvoltage protection unit for automatically cutting off power when the output is >26V.

[0025] The fully automatic rapid silicate detector of this invention has the following beneficial effects:

[0026] (1) The chemiluminescence method is used, which has a shorter measurement time and a lower detection limit compared with the traditional silicon molybdenum blue colorimetric method. The measurement time for each sample is no more than two minutes.

[0027] (2) It has a heating device to eliminate the influence of temperature changes between different water samples on the measurement results. The key is to solve the problem that the reaction rate of samples below 20℃ is so low that they cannot be detected.

[0028] (3) Unique flow path design and metering method to complete the rinsing of the luminescent dish and the metering of the water sample to be tested;

[0029] (4) It has a quantitative dosing function to ensure the stability of experimental results;

[0030] (5) It has a high degree of automation and features automatic rinsing, automatic dosing and automatic stirring functions. Attached Figure Description

[0031] To more clearly illustrate the technical solutions in the specific embodiments or related technologies of this utility model, the drawings used in the description of the specific embodiments or related technologies will be briefly introduced below. Obviously, the drawings described below are some embodiments of this utility model. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0032] Figure 1 Exploded view of the structure of the fully automatic rapid silicate detector provided in this embodiment of the utility model;

[0033] Figure 2 A general structural diagram of the fully automatic rapid silicate detector provided in this embodiment of the utility model;

[0034] Figure 3 The working principle diagram of the fully automatic rapid silicate detector provided in the embodiment of this utility model. Detailed Implementation

[0035] The technical solution of this utility model will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this utility model. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this utility model.

[0036] In the description of this utility model, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the accompanying drawings and are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0037] In the description of this utility model, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "joining" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0038] like Figure 1-2 As shown, this utility model provides a fully automatic rapid silicate detector, comprising:

[0039] (I) The sample introduction system consists of a sample introduction cup (1) and a heating device (11). The sample introduction cup (1) is connected to the heating device (11) through a silicone tube and is used to hold the water sample to be tested (5-50mL). The inner wall of the sample introduction cup (1) is coated with polytetrafluoroethylene for anti-adsorption. The heating device (11) is connected to the sample introduction cup (1) and the luminescent dish (10) respectively. The heating device (11) includes a PTC ceramic and a temperature sensor. The PTC ceramic is used to heat the water sample to 25±0.5℃ when the water sample temperature is <21℃, thereby eliminating the influence of temperature on color development. The temperature sensor is used to measure the real-time temperature of the water sample and perform feedback control (accuracy ±0.1℃).

[0040] (II) The reaction detection system consists of the light-emitting dish (10) and the photomultiplier tube (2). The light-emitting dish (10) is connected to the heating device (11), the flow path device (3), and the photomultiplier tube (2) respectively. It includes a quartz optical path cell, which provides a 10mm path for the optical path. When the detector is working, the light-emitting dish (10) needs to be rinsed with water (three times with deionized water), and then 5mL of water sample is retained before adding the drug for reaction in steps. The photomultiplier tube (2) is a Hamamatsu H7827 (spectral response 300-850nm), which is used to detect the absorbance of molybdenum blue at a wavelength of 810nm and convert photons into electrons. The gain is 10. 6 And the output current signal is 0.1-10μA (corresponding to 0-200μg / L);

[0041] (III) Flow path control device (3), consisting of 3 micro diaphragm pumps, 6 solenoid valves and 3 metering sensors; the 3 micro diaphragm pumps are used to drive reagent A, reagent B and reagent C respectively, and the flow rate is set to 0.5-3 mL / s in this embodiment; the 6 solenoid valves are used to switch the flow path (in this embodiment, the response time of all 6 solenoid valves is <50ms); the 3 metering sensors are used to control the dosage volume (accuracy ±1%).

[0042] In a preferred embodiment, the flow path control device (3) further includes a built-in magnetic stirrer for stirring the mixture formed by the added reagents A, B, and C with the sample water. In this embodiment, the built-in magnetic stirrer can mix at 300 rpm for 10 seconds. Its working process includes:

[0043] 1. Add reagent A (ammonium molybdate): 0.5-2 mL → Silicomolybdate yellow is formed;

[0044] 2. Add reagent B (dilute sulfuric acid): 0.5-2 mL → adjust pH to 1.2 ± 0.1;

[0045] 3. Add reagent C (luminescent agent): 1-3 mL → reduce to silicomolybdenum blue;

[0046] 4. Magnetic stir bar (built-in): Mix at 300 rpm for 10 seconds.

[0047] (iv) Electronic control system, consisting of control board (7) and acquisition board (9); the core component of control board (7) is STM32H743VI (ARM Cortex-M7), used for flow path timing control (accurate to millisecond level) and temperature PID regulation, control board (7) executes ASTM D859 test protocol; acquisition board (9) is used to convert photomultiplier tube current to voltage (I / V conversion), perform 24-bit ADC sampling (TI ADS1256) and calculate silicate concentration, the formula for calculating silicate concentration is as follows (1):

[0048]

[0049] Where A represents absorbance, and a and b are calibration parameters;

[0050] In a preferred embodiment, the fully automatic rapid silicate detector further includes:

[0051] The human-computer interaction system consists of a screen (6) and a switch button (12); wherein the screen (6) is a 5-inch LCD touch screen (resolution 800×480) used to display one or more of the real-time concentration, voltage value and temperature curve; the switch button (12) is a waterproof button (IP67) used to trigger the system to start self-test.

[0052] In a preferred embodiment, the fully automatic rapid silicate detector further includes:

[0053] The host (5) and the side panel; wherein the host (5) is an aluminum-magnesium alloy shell with dimensions of 400×300×200mm; the side panel includes a right side panel (4) and a left side panel (8), wherein the right side panel (4) and the left side panel (8) are combined to form an integrated heat dissipation duct (the heat dissipation duct can control the temperature to <40℃), and the inside of the right side panel (4) and the left side panel (8) are provided with metal wiring grooves to suppress EMI interference.

[0054] The right side plate (4) and the left side plate (8) are metal plates, and the internal metal wiring channels suppress EMI interference through the following principle:

[0055] Shielding effect: The aluminum-magnesium alloy tank forms a Faraday cage, reflecting / absorbing external electromagnetic waves (30dB attenuation @ 1GHz);

[0056] Path isolation: Separate high-frequency and low-frequency cables (power / signal line spacing ≥15mm) to reduce crosstalk;

[0057] Grounding discharge: The tank is connected to the host grounding layer at multiple points to conduct interference current into the ground;

[0058] Eddy current loss: The alternating magnetic field induces eddy currents on the tank wall, which are converted into heat energy and consumed (enhanced by μ metal coating).

[0059] In a preferred embodiment, the fully automatic rapid silicate detector further includes:

[0060] The power supply module (13) has an input of 220V±10% AC signal and outputs including +5V voltage for logic circuits, ±12V voltage for photomultiplier tube high voltage and +24V voltage for pump valve drive.

[0061] In a preferred embodiment, the power supply module (13) includes an overvoltage protection unit for automatically cutting off power when the output is >26V.

[0062] like Figure 3 As shown, the working principle is as follows:

[0063] After turning on switch button 12, power supply module 13 supplies power to the instrument, and the fully automatic rapid silicate detector is turned on. The water sample to be tested is added to sample cup 1, flows through heating device 11 (automatically heated when the water sample temperature is below 21℃), and enters luminescent dish 10. The drain pump operates, continuously rinsing the luminescent dish 10 with the incoming water sample. Only the last 5 ml of water sample is retained for testing. After ensuring the water sample is measured, control board 7 controls the pump and valve in flow path control device 3 to add different reagents to luminescent dish 10. First, 0.5-2 mL of reagent A (ammonium molybdate) is added, followed by 0.5-2 mL of reagent B (sulfuric acid). After stirring and reacting for several tens of seconds, 1-3 mL of reagent C (luminescent agent) is added. At this time, an instantaneous oxidation-luminescence reaction is completed in luminescent dish 10. The emitted light is amplified by photomultiplier tube 2 and converted into a voltage value. After being acquired and processed by acquisition board 9, a digital signal is obtained, and the concentration of silicate ions and the measurement voltage in the water sample are displayed on screen 6, completing the detection.

[0064] Drug preparation plan:

[0065] Reagent A: 2% ammonium molybdate. In a 1000mL volumetric flask, add 800mL of silica-free water, then add 20g of analytical grade ammonium molybdate. Dissolve completely, then add water to bring the volume to 1000mL.

[0066] Reagent B: 4% dilute sulfuric acid. In a 1000mL volumetric flask, first add 800mL of silica-free water, then add 27mL of analytical grade concentrated sulfuric acid, and dilute to 1000mL with water.

[0067] Reagent C: Alkaline luminescent agent. Using a graduated polyethylene reagent bottle, first pour in 800 mL of silica-free water, then add 40 g of analytical grade NaOH granules and 0.2 g of luminescent agent. After fully dissolving, add water to a final volume of 1000 mL.

[0068] Technical parameters of application examples

[0069] Detection range 0.1-200 μg / L Detection limit 0.05 μg / L (3σ) Repeatability RSD ≤ 1.5% (20 μg / L) Single test time ≤3 minutes Reagent consumption <5mL / sample Temperature stability ±0.1℃

[0070] Through the above description of the embodiments, those skilled in the art can clearly understand that the above embodiments can be implemented by software, or by using software plus necessary general-purpose hardware platforms. Based on this understanding, the technical solutions of the above embodiments can be embodied in the form of a software product, which can be stored in a non-volatile storage medium (such as a CD-ROM, USB flash drive, mobile hard drive, etc.), including several instructions to cause a computer device (such as a personal computer, server, or network device, etc.) to execute the methods described in the various embodiments of this utility model.

[0071] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this utility model, and are not intended to limit it. Although the utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this utility model.

Claims

1. A fully automatic rapid silicate detector, characterized in that, include: The sample introduction system consists of a sample introduction cup (1) and a heating device (11). The sample introduction cup (1) is connected to the heating device (11) through a silicone tube and is used to hold the water sample to be tested. The heating device (11) is connected to the sample introduction cup (1) and the luminescent dish (10) respectively. The heating device (11) includes a PTC ceramic and a temperature sensor. The PTC ceramic is used to heat the water sample to 25±0.5℃ when the water sample temperature is <21℃, thereby eliminating the influence of temperature on color development. The temperature sensor is used to measure the real-time temperature of the water sample and perform feedback control. The reaction detection system consists of the light-emitting dish (10) and the photomultiplier tube (2). The light-emitting dish (10) is connected to the heating device (11), the flow path control device (3), and the photomultiplier tube (2). The light-emitting dish (10) includes a quartz optical path cell, which provides a 10mm path for optical transmission. The photomultiplier tube (2) is used to detect the absorbance of molybdenum blue at 810nm wavelength, convert photons into electrons, and output current signals. The flow path control device (3) consists of 3 micro diaphragm pumps, 6 solenoid valves and 3 metering sensors; the 3 micro diaphragm pumps are used to drive reagent A, reagent B and reagent C respectively; the 6 solenoid valves are used to switch the flow path; the 3 metering sensors are used to control the dosage volume. The electronic control system consists of a control board (7) and a data acquisition board (9); the control board (7) is used for flow path timing control and temperature PID adjustment; the data acquisition board (9) is used to convert the photomultiplier tube current into voltage, perform 24-bit ADC sampling, and calculate silicate concentration.

2. The fully automatic rapid silicate detector according to claim 1, characterized in that, The inner wall of the sample inlet cup (1) is coated with polytetrafluoroethylene.

3. The fully automatic rapid silicate detector according to claim 2, characterized in that, The flow path control device (3) also includes a built-in magnetic stirrer for stirring the mixture formed by the added reagents A, B and C with the sample water.

4. The fully automatic rapid silicate detector according to claim 3, characterized in that, The fully automated rapid silicate detector also includes: The human-computer interaction system consists of a screen (6) and a switch button (12); wherein the screen (6) is used to display one or more of the real-time concentration, voltage value and temperature curve; and the switch button (12) is used to trigger the system to start self-test.

5. The fully automatic rapid silicate detector according to claim 4, characterized in that, The screen (6) is a 5-inch LCD touchscreen.

6. The fully automatic rapid silicate detector according to claim 5, characterized in that, The switch button (12) is a waterproof button.

7. The fully automatic rapid silicate detector according to claim 6, characterized in that, The fully automated rapid silicate detector also includes: The main unit (5) and the side panel; wherein the side panel includes a right side panel (4) and a left side panel (8), wherein the right side panel (4) and the left side panel (8) are combined to form an integrated heat dissipation duct, and the inside of the right side panel (4) and the left side panel (8) is provided with metal wiring grooves to suppress EMI interference.

8. The fully automatic rapid silicate detector according to claim 7, characterized in that, The host (5) has an aluminum-magnesium alloy shell with dimensions of 400×300×200mm.

9. The fully automatic rapid silicate detector according to claim 8, characterized in that, The fully automated rapid silicate detector also includes: The power supply module (13) has an input of 220V±10% AC signal and outputs including +5V voltage for logic circuits, ±12V voltage for photomultiplier tube high voltage and +24V voltage for pump valve drive.

10. A fully automatic rapid silicate detector according to claim 9, characterized in that, The power supply module (13) includes an overvoltage protection unit for automatically cutting off power when the output is >26V.

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