CN112858572A - High-turbidity water chloride ion online measurement system and method based on molar method - Google Patents

High-turbidity water chloride ion online measurement system and method based on molar method Download PDF

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CN112858572A
CN112858572A CN202110082986.1A CN202110082986A CN112858572A CN 112858572 A CN112858572 A CN 112858572A CN 202110082986 A CN202110082986 A CN 202110082986A CN 112858572 A CN112858572 A CN 112858572A
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silver nitrate
water
reaction chamber
constant volume
potassium chromate
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刘玮
黄茜
龙国军
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Xian Thermal Power Research Institute Co Ltd
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Xian Thermal Power Research Institute Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
    • G01N31/162—Determining the equivalent point by means of a discontinuity
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • G01N21/79—Photometric titration
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/02—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using precipitation

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Abstract

The invention discloses a high turbidity water chloride ion online measurement system and method based on a molar method.A water sample input pipeline is communicated with an inlet of a water sample pretreatment device, an outlet of the water sample pretreatment device is connected with an inlet of a pH adjusting device, and an outlet of the pH adjusting device is communicated with a water inlet of a constant volume reaction chamber; a dosing system, a sensitive color detector and a liquid level detector are arranged on the constant volume reaction chamber, and a stirrer is arranged at the bottom of the constant volume reaction chamber; the controller is connected with the water sample pretreatment device, the pH adjusting device, the liquid drop counter, the sensitive color detector, the liquid level detector, the dosing system and the constant volume reaction chamber, and the system and the method can realize the on-line measurement of the high turbidity water chloride ions.

Description

High-turbidity water chloride ion online measurement system and method based on molar method
Technical Field
The invention belongs to the field of chemical analysis of industrial production water quality, and relates to a high turbidity water chloride ion online measurement system and method based on a molar method.
Background
In recent years, with the increasing attention of our country on environmental protection, flue gas desulfurization and zero discharge of wastewater, and water saving effect and pollution discharge of industrial circulating cooling water are always the focus of the concerns of pollutant discharge, energy conservation and consumption reduction of various large production enterprises. The chlorine ion is a key index in monitoring industrial circulating water, desulfurization slurry and desulfurization wastewater, and the monitoring means and method of the content of the chlorine ion become research hotspots of various large instrument manufacturers at home and abroad.
At present, chlorine ions in industrial circulating water, desulfurization slurry and desulfurization wastewater are periodically sampled every day by a laboratory worker and are measured by a manual analysis method. The manual analysis not only has complex operation, increases the workload of the laboratory staff, is restricted by the technical level of the laboratory staff, and the measurement accuracy is difficult to ensure. When the measured value is lower, the problem that the chloride ions exceed the standard cannot be found, the corrosion of the circulating cooling water heat exchange pipe, the desulfurization equipment and related equipment is caused, the working efficiency of the equipment is reduced, and the service life of the equipment is prolonged. When the measured value is on the high side, the actual control value is on the low side, and for the circulating cooling water system, the concentration ratio of circulating water can be reduced, and the water-saving benefit and the economic benefit are reduced. If an online measurement system can be constructed, the online continuous monitoring of the chloride ion concentration of high-turbidity water such as industrial circulating water, desulfurization slurry, desulfurization wastewater and the like can be realized, the workload of chemical examination personnel is greatly reduced, the measurement accuracy of chloride ions is improved, the chloride ion concentration is ensured to be always controlled within a standard requirement range, and no chloride ion corrosion risk is ensured when related equipment runs, but similar disclosure is absent in the prior art.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the online measurement system and the online measurement method for the high turbidity water chloride ions based on the Moore method.
In order to achieve the aim, the online measuring system for the high turbidity water chloride ions based on the molar method comprises a water sample input pipeline, a water sample pretreatment device, a pH adjusting device, a constant volume reaction chamber, a dosing assembly, a sensitive color detector, a liquid level detector, a sewage discharge pipeline and a controller;
the water sample input pipeline is communicated with an inlet of the water sample pretreatment device, an outlet of the water sample pretreatment device is connected with an inlet of the pH adjusting device, and an outlet of the pH adjusting device is communicated with a water inlet of the constant volume reaction chamber;
a dosing assembly, a sensitive color detector and a liquid level detector are arranged on the constant volume reaction chamber, and a stirrer is arranged at the bottom of the constant volume reaction chamber;
the controller is connected with the water sample pretreatment device, the pH adjusting device, the sensitive color detector, the liquid level detector, the dosing assembly and the constant volume reaction chamber.
The outlet of the water sample pretreatment device is connected with the inlet of the pH adjusting device through a #1 electromagnetic valve, and the controller is connected with the #1 electromagnetic valve.
The drug adding component comprises a potassium chromate drug adding component and a silver nitrate drug adding component, and the potassium chromate drug adding component and the silver nitrate drug adding component are both connected with the constant volume reaction chamber and the controller.
The potassium chromate dosing assembly comprises a potassium chromate medicine tank and a potassium chromate dosing device, the potassium chromate medicine tank is communicated with the constant volume reaction chamber through the potassium chromate dosing device, and the controller is connected with the potassium chromate dosing device.
The silver nitrate dosing assembly comprises a silver nitrate dosing tank, a silver nitrate dosing device and a liquid drop counter, wherein the silver nitrate dosing tank is communicated with the constant volume reaction chamber through the silver nitrate dosing device and the liquid drop counter, and the controller is connected with the liquid drop counter and the silver nitrate dosing device.
The potassium chromate dosing device and the silver nitrate dosing device are both piston pumps or peristaltic pumps.
And a sewage discharge pipeline is arranged at the bottom of the constant volume reaction chamber.
A #2 electromagnetic valve is arranged on the sewage discharge pipeline, and the controller is connected with the #2 electromagnetic valve.
A method for online measurement of chloride ions in high-turbidity water based on a molar method comprises the following steps:
and (3) taking potassium chromate as an indicator, titrating the high turbid water by a silver nitrate standard titration solution within the pH range of 5-9.5, reacting the silver nitrate with chloride in the high turbid water to generate silver chloride precipitate, and reacting with the potassium chromate indicator to generate brick red silver nitrate when excessive silver nitrate exists, wherein the brick red silver nitrate indicates that the reaction reaches the end point, so as to test the chloride ion concentration of the high turbid water.
The invention has the following beneficial effects:
according to the high turbid water chloride ion online measurement system and method based on the Moore method, during specific operation, potassium chromate is used as an indicator, high turbid water is titrated by a silver nitrate standard titration solution within the pH range of 5-9.5, silver chloride precipitates are generated under the action of silver nitrate and chlorides in the high turbid water, and therefore the chloride ion concentration of the high turbid water is measured online.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Wherein, 1 is the water sample input pipeline, 2 is water sample preprocessing device, 3 is #1 solenoid valve, 4 is pH adjusting device, 5 is constant volume reaction chamber, 6 is the stirring, 7 is the potassium chromate medicinal cupping, 8 is the potassium chromate charge device, 9 is the silver nitrate medicinal cupping, 10 is the silver nitrate medicine device, 11 is the drop counter, 12 is sensitive color detector, 13 is the liquid level detector, 14 is #2 solenoid valve, 15 is the blowdown pipeline, 16 is the controller.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
referring to fig. 1, the online measurement system for chlorine ions in high turbidity water based on a molarity method comprises a water sample input pipeline 1, a water sample pretreatment device 2, #1 electromagnetic valve 3, a pH adjustment device 4, a constant volume reaction chamber 5, a dosing assembly, a sensitive color detector 12, a liquid level detector 13, a sewage discharge pipeline 15, #2 electromagnetic valve 14 and a controller 16;
the water sample input pipeline 1 is communicated with an inlet of a water sample pretreatment device 2, an outlet of the water sample pretreatment device 2 is connected with an inlet of a pH adjusting device 4 through a #1 electromagnetic valve 3, and an outlet of the pH adjusting device 4 is communicated with a water inlet of a constant volume reaction chamber 5;
be provided with on the constant volume reacting chamber 5 and add medicine subassembly, sensitive colour detector 12 and level detector 13, the bottom of constant volume reacting chamber 5 is provided with stirring 6 and sewage pipes 15, is provided with #2 solenoid valve 14 on the sewage pipes 15.
The drug adding assembly comprises a potassium chromate drug adding assembly and a silver nitrate drug adding assembly, the potassium chromate drug adding assembly comprises a potassium chromate drug tank 7 and a potassium chromate drug adding device 8, the silver nitrate drug adding assembly comprises a silver nitrate drug tank 9, a silver nitrate drug adding device 10 and a liquid drop counter 11, the silver nitrate drug tank 9 is communicated with the constant volume reaction chamber 5 through the silver nitrate drug adding device 10 and the liquid drop counter 11, the potassium chromate drug tank 7 is communicated with the constant volume reaction chamber 5 through the potassium chromate drug adding device 8, and the potassium chromate drug adding device 8 and the silver nitrate drug adding device 10 are piston pumps or peristaltic pumps.
The input end of the controller 16 is connected with the water sample pretreatment device 2, the pH adjusting device 4, the droplet counter 11, the sensitive color detector 12 and the liquid level detector 13, and the output end of the controller 16 is connected with the water sample pretreatment device 2, #1 electromagnetic valve 3, the pH adjusting device 4, the potassium chromate dosing device 8, the silver nitrate dosing device 10, the constant volume reaction chamber 5 and the #2 electromagnetic valve 14.
The invention discloses a high turbidity water chloride ion online measurement method based on a molar method, which comprises the following steps:
and (3) taking potassium chromate as an indicator, titrating the high turbidity water by using a silver nitrate standard titration solution within the pH range of 5-9.5, reacting the silver nitrate with chloride to generate silver chloride precipitate, and reacting with the potassium chromate indicator to generate brick red silver nitrate when excessive silver nitrate exists, wherein the brick red silver nitrate indicates that the reaction reaches the end point, so as to test the chloride ion concentration of the high turbidity water.
The specific operation process of the invention is as follows:
the high turbid water enters the water sample pretreatment device 2 through the water sample input pipeline 1, and the controller 16 controls the water sample pretreatment device 2 to carry out water sample pretreatment on the high turbid water so as to filter solid impurities in the high turbid water;
the controller 16 opens the solenoid valve 3 #1, the water sample enters the pH adjusting device 4, and the controller 16 controls the pH adjusting device 4 to adjust the pH value of the water sample to 5-9.5;
the water sample output by the pH adjusting device 4 flows into the constant volume reaction chamber 5, the inner wall of the constant volume reaction chamber 5 is washed by the water sample, after the washing is finished, the controller 16 closes the solenoid valve 3 #1, opens the solenoid valve 14 #2, discharges the solution in the constant volume reaction chamber 5 through the sewage discharge pipeline 15, and closes the solenoid valve 14 #2 by the controller 16;
the controller 16 opens the electromagnetic valve 3 #1, the controller 16 controls the water sample to continuously flow into the constant volume reaction chamber 5, the controller 16 enables the liquid level of the constant volume reaction chamber 5 to be increased to a preset value V according to the liquid level value fed back by the liquid level detector 13, the controller 16 closes the electromagnetic valve 3 #1, the controller 16 starts the stirrer 6 to stir, the controller 16 starts the potassium chromate dosing device 8, a potassium chromate reagent is added into the constant volume reaction chamber 5, the silver nitrate dosing device 10 is started later, a silver nitrate standard titration solution with a known concentration is added into the constant volume reaction chamber 5 drop by drop, the controller 16 records the consumed silver nitrate solution amount through the liquid drop counter 11, when the sensitive color detector 12 detects the occurrence of brick red precipitate in the reaction solution, the controller 16 turns off the silver nitrate dosing device 10, and the controller 16 records the volume V of the consumed silver nitrate standard titration solution.1Calculating the concentration rho of the chloride ions according to the concentration rho, and finally displaying the calculation result;
Figure BDA0002909761940000061
wherein, V1The volume of silver nitrate standard titration solution used for reaction consumption recorded by the controller 16; v0The volume of silver nitrate standard titration solution consumed for the blank test stored in the controller 16; v is the volume of the high turbidity water entering the constant volume reaction chamber 5; c is an accurate value of the concentration of the silver nitrate standard titration solution; m is the number of molar masses of chlorine, M being 35.45 g/mol.
Finally, the controller 16 opens the solenoid valve 14 #2 to discharge the solution in the constant volume reaction chamber 5 through the drain pipe 15.
The invention can realize the automatic on-line continuous monitoring of the concentration of the chloride ions in high-turbidity water such as industrial circulating water, desulfurization slurry, desulfurization wastewater and the like, can replace the working mode that an assay worker samples periodically to perform manual analysis, greatly lightens the workload of the assay worker, avoids the chloride ion pollution possibly occurring after the water sample is taken out and the measurement error caused by different operation levels of the worker in the manual analysis process, improves the accuracy of the measurement of the concentration of the chloride ions in high-turbidity water, and ensures the operation efficiency and the safety of related equipment such as a circulating water system, a desulfurization system and the like.
When the concentration of the chloride ions in the high turbid water such as industrial circulating water, the desulfurization slurry and the desulfurization wastewater is measured on line, the controller 16 can automatically and continuously monitor the concentration of the chloride ions only by introducing a water sample without any manual intervention or operation and displaying the concentration on the display screen, so the method is simple and convenient to use, has strong practicability, can be widely applied to the water quality monitoring and supervision of the high turbid water in industrial production in various industries such as electric power, chemical engineering and the like, and improves the working efficiency of chemical operators and chemical supervisors.

Claims (9)

1. A high turbid water chloride ion online measurement system based on a molar method is characterized by comprising a water sample input pipeline (1), a water sample pretreatment device (2), a pH adjusting device (4), a constant volume reaction chamber (5), a dosing assembly, a sensitive color detector (12), a liquid level detector (13), a sewage discharge pipeline (15) and a controller (16);
the water sample input pipeline (1) is communicated with an inlet of the water sample pretreatment device (2), an outlet of the water sample pretreatment device (2) is connected with an inlet of the pH adjusting device (4), and an outlet of the pH adjusting device (4) is communicated with a water inlet of the constant volume reaction chamber (5);
a dosing assembly, a sensitive color detector (12) and a liquid level detector (13) are arranged on the constant volume reaction chamber (5), and a stirrer (6) is arranged at the bottom of the constant volume reaction chamber (5);
the controller (16) is connected with the water sample pretreatment device (2), the pH adjusting device (4), the sensitive color detector (12), the liquid level detector (13), the dosing assembly and the constant volume reaction chamber (5).
2. A Moore method-based online measurement system for chloride ions in high turbidity water according to claim 1, characterized in that the outlet of the water sample pretreatment device (2) is connected with the inlet of the pH adjustment device (4) through a #1 electromagnetic valve (3), and the controller (16) is connected with the #1 electromagnetic valve (3).
3. The online measurement system for the chloride ions in the high turbidity water based on the molar method according to claim 1, wherein the medicine adding component comprises a potassium chromate medicine adding component and a silver nitrate medicine adding component, and both the potassium chromate medicine adding component and the silver nitrate medicine adding component are connected with the constant volume reaction chamber (5) and the controller (16).
4. The online measurement system for the chloride ions in the high-turbidity water based on the molar method according to claim 3, wherein the potassium chromate dosing assembly comprises a potassium chromate medicine tank (7) and a potassium chromate dosing device (8), the potassium chromate medicine tank (7) is communicated with the constant-volume reaction chamber (5) through the potassium chromate dosing device (8), and the controller (16) is connected with the potassium chromate dosing device (8).
5. The online measurement system for the chloride ions in the high turbidity water based on the Moore method according to claim 4, wherein the silver nitrate dosing assembly comprises a silver nitrate dosing tank (9), a silver nitrate dosing device (10) and a liquid drop counter (11), wherein the silver nitrate dosing tank (9) is communicated with the constant volume reaction chamber (5) through the silver nitrate dosing device (10) and the liquid drop counter (11), and the controller (16) is connected with the liquid drop counter (11) and the silver nitrate dosing device (10).
6. A Moore-method-based online measurement system for chloride ions in high turbidity water according to claim 5, wherein the potassium chromate dosing device (8) and the silver nitrate dosing device (10) are both piston pumps or peristaltic pumps.
7. The on-line measurement system for chlorine ions in high turbidity water based on the molar method according to claim 1, characterized in that a blowdown pipe (15) is provided at the bottom of the constant volume reaction chamber (5).
8. A molarity-based on-line measurement system for high turbidity water chloride ions according to claim 5, characterized in that the blowdown pipe (15) is provided with a #2 solenoid valve (14), and the controller (16) is connected with the #2 solenoid valve (14).
9. A high turbidity water chlorine ion online measurement method based on a molar method is characterized by comprising the following steps:
and (3) taking potassium chromate as an indicator, titrating the high turbid water by a silver nitrate standard titration solution within the pH range of 5-9.5, reacting the silver nitrate with chloride in the high turbid water to generate silver chloride precipitate, and reacting with the potassium chromate indicator to generate brick red silver nitrate when excessive silver nitrate exists, wherein the brick red silver nitrate indicates that the reaction reaches the end point, so as to test the chloride ion concentration of the high turbid water.
CN202110082986.1A 2021-01-21 2021-01-21 High-turbidity water chloride ion online measurement system and method based on molar method Pending CN112858572A (en)

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