CN112816615A - Chloride ion detector and chloride ion detection method - Google Patents
Chloride ion detector and chloride ion detection method Download PDFInfo
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- CN112816615A CN112816615A CN202110017041.1A CN202110017041A CN112816615A CN 112816615 A CN112816615 A CN 112816615A CN 202110017041 A CN202110017041 A CN 202110017041A CN 112816615 A CN112816615 A CN 112816615A
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 50
- 238000001514 detection method Methods 0.000 title claims abstract description 48
- 238000004448 titration Methods 0.000 claims abstract description 141
- 239000007788 liquid Substances 0.000 claims abstract description 96
- 238000005070 sampling Methods 0.000 claims abstract description 46
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000012806 monitoring device Methods 0.000 claims abstract description 12
- 238000004891 communication Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 105
- 238000000034 method Methods 0.000 claims description 65
- 239000000523 sample Substances 0.000 claims description 44
- 239000008213 purified water Substances 0.000 claims description 15
- 239000012895 dilution Substances 0.000 claims description 9
- 238000010790 dilution Methods 0.000 claims description 9
- 230000005611 electricity Effects 0.000 claims description 9
- 239000012470 diluted sample Substances 0.000 claims description 8
- 238000007865 diluting Methods 0.000 claims description 2
- 238000012544 monitoring process Methods 0.000 claims description 2
- 238000003113 dilution method Methods 0.000 claims 1
- ORMNPSYMZOGSSV-UHFFFAOYSA-N mercury(II) nitrate Inorganic materials [Hg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ORMNPSYMZOGSSV-UHFFFAOYSA-N 0.000 description 17
- 239000012488 sample solution Substances 0.000 description 15
- 238000003756 stirring Methods 0.000 description 13
- 238000005086 pumping Methods 0.000 description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 9
- 229910017604 nitric acid Inorganic materials 0.000 description 9
- 238000004140 cleaning Methods 0.000 description 7
- 238000002835 absorbance Methods 0.000 description 4
- 238000004164 analytical calibration Methods 0.000 description 3
- 239000003085 diluting agent Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910001987 mercury nitrate Inorganic materials 0.000 description 1
- DRXYRSRECMWYAV-UHFFFAOYSA-N nitrooxymercury Chemical compound [Hg+].[O-][N+]([O-])=O DRXYRSRECMWYAV-UHFFFAOYSA-N 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001960 triggered effect Effects 0.000 description 1
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N1/14—Suction devices, e.g. pumps; Ejector devices
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention discloses a chloride ion detector and a chloride ion detection method, and relates to the field of water quality detection equipment, wherein the chloride ion detector comprises a sampling tank, a communication device, a titration cell, a dropping liquid mechanism, a solution storage device, a water supply device, a reagent supply device and a controller; the reagent supply device is used for containing related reagents; the sampling tank is used for acquiring and outputting liquid; the titration cell is communicated with a dropping mechanism, the dropping mechanism is used for dropping a titration solution into the titration cell, and a titration monitoring device is arranged outside the titration cell; the communicating device is connected with the sampling tank, the titration cell, the water supply device, the solution storage device and the reagent supply device; the controller is electrically connected with the sampling tank, the communicating device, the titration cell and the dropping liquid mechanism, and the controller respectively controls the on-off of the sampling tank, the titration cell, the solution storage device and the on-off of the reagent supply device and the communicating device. The chloride ion detector and the chloride ion detection method provided by the invention can be used for detecting the concentration of a high-concentration chloride ion solution, and improving the detection precision and the detection efficiency.
Description
Technical Field
The invention relates to the field of water quality detection equipment, in particular to a chloride ion detector and a chloride ion detection method.
Background
Chloride ion detection is widely applied to industries such as building, medicine, environmental protection, electric power, petrochemical industry, heating and the like, and the existing chloride ion detection technology is mainly a semi-automatic detector developed on the basis of silver nitrate artificial titration method or electrode method as terminal judgment; the manual titration method has the characteristics of poor consistency in the detection process and large error of a detection result due to the artificial participation of the manual titration method, and a semi-automatic detector developed on the basis of taking an electrode method as an end point judgment has the defects of poor consistency and error in each measurement due to slow reaction of chemical potential and interference of a detection environment and impurity ions.
Disclosure of Invention
The invention aims to provide a chloride ion detector and a chloride ion detection method, which are used for solving the problems in the prior art, can detect the concentration of a high-concentration chloride ion solution and improve the detection precision and the detection efficiency.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a chloride ion detector, which comprises a sampling tank, a communication device, a titration cell, a dropping liquid mechanism, a solution storage device, a water supply device, a reagent supply device and a controller, wherein the sampling tank is connected with the titration cell; the reagent supply device is used for containing related reagents; the sampling tank is used for acquiring and outputting liquid and can meter the dosage of the liquid; the titration cell is communicated with the dropping mechanism, the dropping mechanism is used for dropping a titration solution into the titration cell, a titration monitoring device is arranged on the outer side of the titration cell, and the titration monitoring device is used for monitoring the reaction degree of the solution in the titration cell; the communicating device is connected with the sampling tank, the titration cell, the solution storage device, the water supply device and the reagent supply device; the controller with sample jar, intercommunication device, titration cell and dropping liquid mechanism electricity are connected, the controller is used for controlling respectively the sample jar the titration cell solution storage device and reagent feeding device with the break-make of intercommunication device.
Preferably, the sampling device further comprises a liquid level sensor, wherein the liquid level sensor is arranged on the sampling tank; the number of the liquid level sensors is at least two, and each liquid level sensor is respectively arranged at different heights of the sampling tank; the level sensor is electrically connected to the controller, the level sensor being configured to meter a dose of liquid.
Preferably, the device further comprises a magnetic stirrer, wherein the magnetic stirrer is arranged at the bottom of the titration cell and is electrically connected with the controller.
Preferably, the titration monitoring device comprises a light emitting diode and a photoelectric sensor, and the light emitting diode and the photoelectric sensor are electrically connected with the controller.
Preferably, the titration apparatus further comprises a liquid discharge pump, the liquid discharge pump is communicated with a liquid discharge valve at the bottom of the titration cell, and the liquid discharge pump is electrically connected with the controller.
Preferably, the dropping liquid mechanism includes plunger pump, step motor, two three-way valves and reagent jar, two three-way valves are used for communicateing alone the plunger pump with reagent jar or communicateing alone the plunger pump with the titration cell, step motor is used for the drive the plunger pump, step motor with the controller electricity is connected, automatically controlled two three-way valves with the controller electricity is connected.
The chloride ion detector of claim 5, wherein: the plunger pump is characterized by further comprising a limit sensor, wherein the limit sensor is arranged at the bottom of the plunger pump and electrically connected with the controller.
The invention also provides a chloride ion detection method based on any one of the chloride ion detectors, which is characterized in that: the method can be used for detecting the chloride ions in the high-concentration chloride ion solution, and comprises the following steps:
the method comprises the following steps: respectively carrying out N times of dilution on a plurality of standard samples to respectively obtain a plurality of diluted standard samples, wherein N is more than or equal to 2, and the initial concentration Ci (i is more than or equal to 2) of each standard sample is known;
step two: titrating a plurality of diluted standard samples through the dropping mechanism respectively, and recording respective titrating liquid dosage Vi (i is more than or equal to 2) when the titration monitoring device detects that the titration reaction is finished;
step three: acquiring a linear relation V between the concentration C of the chloride ion solution and the dosage V of the titration solution as kC + b according to a plurality of groups Ci and Vi;
step four: diluting a sample to be tested for N times to obtain a diluted sample to be tested;
step five: titrating the diluted sample to be measured through the dropping mechanism until the titration monitoring device detects that the titration reaction is finished, recording the dosage of the titration solution, and calculating the concentration of the sample to be measured according to the linear relation V (kC + b) of the concentration C of the chloride ion solution and the dosage V of the titration solution;
wherein, to standard sample, the dilution of the sample that awaits measuring each time all includes:
s1: initial dilution step on the sample: the controller is used for respectively controlling the connection and disconnection of the sampling tank, the water supply device, the titration cell and the communication device; measuring a first dose of purified water to the titration cell and a second dose of sample to the titration cell to obtain an initially diluted sample;
s2: the dilution procedure was repeated on the samples: the controller is used for respectively controlling the quantity of the sampling tank, the water supply device, the solution storage device and the communication device to be switched on and off, so that the solution in the second dose titration cell is measured and delivered to the solution storage device, and the residual solution in the titration cell is discharged; measuring a first dose of purified water to a titration cell, and measuring a solution in a second dose of solution storage device to the titration cell to obtain a repeatedly diluted sample;
s3: repeat N-2 times S2.
Compared with the prior art, the invention has the following technical effects:
according to the chloride ion detector and the chloride ion detection method provided by the invention, the detection process can dilute a sample to be detected through the solution storage device, so that the detection range is increased, the detection of a high-concentration solution is realized, the detection precision is improved, the whole detection process is automatically controlled by the controller, the taking of the solution and the reagent is controlled by the liquid level sensor, the error of manual taking is avoided, and the precision of titration detection is improved.
Furthermore, a magnetic stirrer is arranged in the titration cell, so that the solution in the titration cell can be mixed more uniformly, and the titration detection result is more accurate.
Furthermore, the method for detecting the chloride ions can improve the measuring range of the detector by reducing the concentration of the solution to be detected, so that the practicability of the detector is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a chloride ion detector according to a first embodiment of the present invention.
Wherein: 1-a power pump; 2-a sampling tank; 3-a high level liquid level sensor; 4-a low level liquid level sensor; 5-a communication device; 6-liquid storage bottle; 7-a titration cell; 8-a photosensor; 9-a light emitting diode; 10-magnetic stirrer; 11-a stirrer driver; 12-a drain pump; 13-a plunger pump; 14-a stepper motor; 15-two-position three-way valve; 16-mercuric nitrate solution.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a chloride ion detector and a chloride ion detection method, which are used for solving the problems in the prior art and improving the accuracy of a detection result.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example one
The present embodiment provides a chloride ion detector, as shown in fig. 1, including a sampling tank 2, a communication device, a titration cell 7, a dropping mechanism, a solution storage device 6, a reagent supply device and a controller;
the reagent supply device comprises a reagent supply device A and a reagent supply device B which are respectively used for containing a nitric acid solution and a carbine dioctylhydrazone solution which need to be added into the titration cell before titration;
the sampling tank 2 is used for metering the liquid dosage and obtaining and outputting liquid, the upper part of the sampling tank 2 is communicated with the power pump 1, a liquid level sensor is arranged in the sampling tank 2, the power pump 1 pumps the liquid into the sampling tank 2, and when the liquid level reaches the set liquid level sensor, the power pump 1 is closed by the controller, so that the accurate control of the liquid dosage is realized, and the detection precision is improved;
in this embodiment, the intercommunication device is many valves 5, and many valves 5 are used for communicateing sample jar 2, titration cell 7, solution storage device 6 and reagent feeding device, and the controller is used for controlling the break-make of sample jar 2, titration cell 7, solution storage 6 device and reagent feeding device and intercommunication device respectively, wherein: f1, F2, F3, F4, F5, F6, F7, F8 are one to eight-position valves of the multi-position valve 5, the bottom of the sampling tank 2 communicates with the side of the multi-position valve 5, wherein: the F1 valve is communicated with the titration cell through a pipeline extending into the titration cell from the upper part of the titration cell, the F2 valve is communicated with the reagent supply device A, the F3 valve is communicated with the reagent supply device B, the F4 valve is communicated with the diluent, the diluent is purified water in the embodiment, the F5 valve is communicated with the bottom of the solution storage device, the F6 valve is a standby valve, the F7 valve is communicated with the F8 valve and a sampling channel, each valve is an electric control valve, all the electric control valves are electrically connected with the controller and are controlled by the controller, and the automation degree and the detection precision are further improved.
The titration cell 7 is communicated with the dripping mechanism, the dripping mechanism is used for dripping a titration solution into the titration cell 7, a titration monitoring device is arranged outside the titration cell 7 and consists of a photoelectric sensor 8 and a light-emitting diode 9, a connecting line of the photoelectric sensor 8 and the light-emitting diode 9 passes through the center of the titration cell 7, and the wavelength of the light-emitting diode 9 is 450 nm-550 nm; the titration process is monitored by the photoelectric sensor, so that the stage of titration can be accurately judged, and the detection precision is further improved.
The liquid level sensor is arranged at two different heights in the sampling tank 2, the liquid level sensor at the high position is a high-level liquid level sensor 3, the liquid level sensor at the low position is a low-level liquid level sensor 4, and the sampling tank 2 realizes the function of metering the dosage of the solution through the liquid level sensors; the sensor is used for automatic metering, so that errors caused by manual metering are avoided, and the precision of subsequent detection can be improved.
The high level liquid level sensor 3 corresponds to a first dose and the low level liquid level sensor 4 corresponds to a second dose.
In this embodiment, titration cell 7 bottom is equipped with magnetic stirrers, and magnetic stirrers includes magnetic stirrers 10 and stirring driver 11, acts on the solution in titration cell 7 through magnetic stirrers 10, is favorable to titrating going on of reaction, further improves and detects the precision.
In this embodiment, the titration cell 7 further includes a liquid discharge pump 12, the liquid discharge pump 12 is communicated with a liquid discharge port at the bottom of the titration cell 7, the liquid discharge pump 12 is electrically connected to the controller, and the liquid discharge pump 12 can accelerate the discharge of the solution in the titration cell 7, thereby increasing the detection speed.
The dropping liquid mechanism in this embodiment includes plunger pump 13, step motor 14, two three-way valves 15 and reagent tank 16, and the solution that holds in the reagent tank 16 is the mercuric nitrate solution, and two three-way valves 15 are used for communicateing plunger pump 13 and reagent tank 16 alone or communicateing plunger pump 13 and titration cell 7 alone, and step motor 14 is used for the drive plunger pump 13, step motor 14 with the controller electricity is connected, two three-way valves 15 with the controller electricity is connected.
In this embodiment, the bottom of the plunger pump 13 is provided with a limit sensor, the limit sensor is electrically connected with the controller, when the stepping motor 14 drives the plunger pump 13 to move to the bottom of the plunger pump 13, the limit sensor is triggered, the controller stops the stepping motor 14, and the plunger pump 13 is prevented from exceeding the stroke and causing failure.
Example two
The embodiment provides a chloride ion detection method, which can detect the concentration of a low-concentration solution, wherein the dosage measured by a high-level liquid level sensor 3 is a first dosage, and the dosage measured by a low-level liquid level sensor 4 is a second dosage;
the first step is as follows: instrument calibration process
Firstly, a cleaning process:
1. taking purified water to a titration cell 7: the power pump 1 is started to pump liquid firstly through the controller, then the F4 valve is opened, the purified water is communicated with the sampling tank 2 and is pumped into the sampling tank 2, when the liquid level of the purified water triggers the high-level liquid level sensor, the F4 valve is closed, and the power pump 1 stops pumping liquid; opening an F1 valve, starting a power pump 1 to inject water, and injecting purified water into a titration cell 7 to finish the process of taking the purified water into the titration cell 7;
2. liquid drainage: the drain pump 12 is turned on, and the liquid in the titration flask 7 is drained, and then the drain pump 12 is turned off.
Completing the cleaning process;
starting low concentration sampling after completing' cleaning process
Secondly, the process of taking purified water to the titration cell 7 is executed;
thirdly, sampling a sample solution to a titration cell 7: when the concentration of the sample solution is known, the controller controls the starting force pump 1 to start liquid pumping firstly, then controls the F7 valve to be opened, a sample solution container with known concentration is communicated with the sampling tank 2 to pump the sample solution into the sampling tank 2, and when the liquid level triggers the low level liquid level sensor 4, the F7 valve is closed, and the power pump 1 is closed; and opening an F1 valve, starting the power pump 1 to inject the sample solution with the known concentration into the titration cell 7, and finishing the process of taking the sample solution with the known concentration into the titration cell 7.
Fourthly, stirring and mixing the samples: starting a stirrer driver 11, driving a magnetic stirrer 10 in the titration cell 7 through a magnetic field, uniformly stirring the liquid in the titration cell 7, and then closing the stirrer driver 11 to finish the process of stirring and mixing the sample;
thus completing the low degree sampling
Fifthly, taking a nitric acid solution: opening an F2 valve after starting a power pump 1, pumping the nitric acid solution to a sampling tank 2, closing the power pump 1 after a liquid level triggers a low level liquid level sensor 4, closing an F2 valve, opening an F1 valve, starting the power pump 1 to inject the nitric acid solution into a titration cell 7, and finishing the process of taking the nitric acid solution;
sixthly, taking a carbobenzene dioctahydrazone solution: opening an F3 valve after starting a power pump 1, pumping nitric acid solution to a sampling tank 2, closing the power pump 1 after a liquid level triggers a low level liquid level sensor 4, closing an F3 valve, opening an F1 valve, starting the power pump 1, and injecting carbonzene dioctahydrazone into a titration cell 7 to finish the process of taking the carbobenzene dioctahydrazone solution;
seventhly, completing the process of stirring and mixing the sample again;
eighthly, taking a mercuric nitrate solution 16: and (3) turning on the stepping motor 14 to enable the stepping motor 14 to drive the plunger pump 13 to move downwards, stopping the stepping motor 14 after the plunger pump 13 touches the bottom limit sensor, adjusting the two-position three-way valve 15 to only communicate the plunger pump 13 with the reagent tank, wherein the reagent tank is filled with the mercuric nitrate solution 16, turning on the stepping motor 14 to drive the plunger pump 13 to pump, fully pumping the mercuric nitrate solution 16 in the plunger pump 13, turning off the stepping motor 14, and completing the process of taking the mercuric nitrate solution 16.
The first to seventh processes and the eighth process are operated simultaneously.
Ninthly, a titration process:
starting a stirrer driver 11, driving a magnetic stirrer 10 in a titration cell 7 through a magnetic force field, stirring mixed liquid in the titration cell 7, simultaneously turning on a light-emitting diode 9, converting light penetrating through the titration cell 7 into a voltage signal by a photoelectric sensor 8, transmitting the voltage signal to a controller, after the diode is turned on for T1 seconds, setting T1 to be 10-50, and recording the voltage average value U of the photoelectric sensor 8 in T1 seconds by the controller0Adjusting a two-position three-way valve 15 to only communicate the plunger pump 13 with the titration tank 7, starting a stepping motor 14, and dropwise adding a mercury nitrate solution 16 in the plunger pump 13 into the titration tank 7;
and simultaneously, the controller records a voltage signal U of the photoelectric sensor 8 and calculates the absorbance, wherein the absorbance A is log (U)0U) and the controller records the number of pulses N sent by the corresponding controller to the stepper motor 14 at the corresponding absorbance a0When the absorbance A is larger than or equal to A0When the stepping motor 14 stops moving, A0And the number of pulses N sent to the stepping motor 14 by the corresponding controller is recorded by the controller to be 0.1-0.5, namely the number of pulses N corresponding to the first calibration dosage, and the liquid discharge pump 12 is started to complete the liquid discharge process.
Tenthly, calibrating: after the titration of the sample solution, which is a solution with a known concentration, is completed, the controller records the concentration C of the sample solution and the number N of pulses sent to the stepping motor 14 by the controller corresponding to the time when the titration of the sample solution is completed, selects two or more solutions with different concentrations and known concentrations for titration, can obtain N corresponding to the solutions with different concentrations C, and can determine that the linear relation between N and C is N ═ kC + b according to different concentrations C and N.
And finishing the instrument calibration process.
The second step is that: detection of solutions of unknown concentration
Step 1: sequentially performing the cleaning process and the process of taking purified water to the titration cell 7
Step 2: starting the power pump 1 to start liquid pumping, controlling to open the F7 valve, communicating a container containing a sample solution to be detected with the sampling tank 2, pumping the sample solution to be detected into the sampling tank 2, and when the liquid level triggers the low-level page sensor, closing the F7 valve and closing the power pump 1; and opening an F1 valve, starting the power pump 1 to inject the sample solution to be detected into the titration cell 7, and finishing the process of taking the sample solution to be detected into the titration cell 7.
And step 3: the process of stirring and mixing the sample, the process of taking the nitric acid solution, the process of taking the carbine dioctahydrazone solution, the process of stirring and mixing the sample, the process of taking the mercuric nitrate solution 16 and the process of titration are sequentially executed.
After the above steps are completed, the controller records the pulse number N sent to the stepping motor 14 by the controller when the titration of the sample is finished, that is, the pulse number N corresponding to the first titration dose, and according to the linear relationship between the concentration C and the pulse number N in the instrument calibration process, the concentration C of the sample to be detected can be obtained.
The process used in the embodiment is controlled and completed by the controller, errors caused by human intervention are avoided, the detection precision is high, and the detection efficiency is high.
EXAMPLE III
The difference between the method for detecting chloride ions in this embodiment and the second embodiment is that the method for detecting chloride ions in this embodiment can detect the concentration of a high-concentration solution, increase the detection range of a detector, and measure a solution with a higher concentration, where a dose measured by the high level liquid level sensor 3 is a first dose, and a dose measured by the low level liquid level sensor 4 is a second dose, and the steps in this embodiment are as follows:
firstly, the method comprises the following steps: solution calibration
Executing the cleaning process;
sampling the solution:
executing the process of taking purified water to the titration cell 7;
after the process of 'sampling the solution to the titration cell 7' is executed, the process of 'stirring and mixing the sample' is executed;
and (3) executing the step of taking a sample in the titration cell to a solution storage device: the controller firstly controls the power pump 1 to start pumping work, at the moment, a valve is not opened, the power pump 1 is started firstly and then opened, liquid can be directly pumped after the valve is opened, then the controller controls the F1 valve of the multi-position valve 5 to be opened, a sample in the titration cell is pumped into the position of the low-position liquid level sensor 4 of the meter 2, the low-position liquid level sensor 4 sends a signal to the controller after detecting the liquid, the controller controls the power pump 1 to stop pumping the liquid, then the controller controls the F1 valve of the multi-position valve 5 to be closed, the F5 valve is opened, and the controller controls the power pump 1 to pump the sample into the liquid storage bottle 6;
performing a "drain" process, and then performing a "cleaning process";
executing' taking purified water to a titration cell;
and (3) taking a sample in the liquid storage bottle to a titration cell: the controller firstly controls the power pump 1 to start pumping work, the valve is not opened at the moment, the power pump 1 is firstly opened, the valve is opened afterwards, liquid can be directly pumped after the valve is opened, then the controller controls the F5 valve of the multi-position valve 5 to be opened, a sample in the liquid storage bottle 6 is pumped into the position of the low-position liquid level sensor 4 of the meter 2, the low-position liquid level sensor 4 sends a signal to the controller after detecting the liquid, the controller controls the power pump 1 to stop pumping the liquid, then the controller controls the F5 valve of the multi-position valve 5 to be closed, the F1 valve is opened, the controller controls the power pump 1 to pump the solution in the liquid storage bottle into the titration cell 7
Executing the process of stirring and mixing the sample;
this completes the "solution sampling".
The "taking a nitric acid solution", "taking a carbine dioctahydrazone solution", "stirring and mixing the sample process", "taking a mercuric nitrate solution 16", "titration process", and "calibration" in example two were performed to find that the relationship between the concentration C and the number of pulses N was N ═ kC + b.
And finishing the calibration of the solution.
Secondly, solution titration
And replacing the sample solution in the solution calibration with the solution to be detected, executing the solution calibration process to obtain the pulse number N corresponding to the titration dose used for titrating the solution to be detected, and obtaining the concentration of the solution to be detected according to the relation between the concentration C and the pulse number N.
In the embodiment, the steps can dilute the sample to be detected, so that the detection range of the detector is increased, and the practicability is improved.
Example four
This embodiment is different from the third embodiment in that the method for detecting chloride ions can detect the concentration of a solution with a higher concentration, and the steps in this embodiment are as follows:
performing a "solution sampling" process;
executing a 'liquid drainage' process after executing a 'process of taking a sample in a titration cell to a solution storage device', and then executing a 'cleaning process';
after the process of taking purified water to the titration cell 7 is carried out, the process of taking a sample in the liquid storage bottle to the titration cell is carried out "
Executing the process of stirring and mixing the sample;
the "taking a nitric acid solution", "taking a carbine dioctahydrazone solution", "stirring and mixing the sample process", "taking a mercuric nitrate solution 16", "titration process", and "calibration" in example two were performed to find that the relationship between the concentration C and the number of pulses N was N ═ kC + b.
After the sample solution in the solution calibration in the third embodiment is replaced by the solution to be measured with higher concentration, the solution calibration flow in the third embodiment is executed to obtain the number of pulses N corresponding to the dose of the titrating agent used for titrating the solution to be measured, and the concentration of the solution to be measured can be obtained according to the relationship between the concentration C and the number of pulses N.
In the embodiment, the step can further dilute the sample to be detected, so that the detection range of the detector is increased, and the practicability is improved.
The selection conditions of the detection method using the bottom concentration or the high concentration during detection are as follows: determining the approximate range of the concentration of the sample to be detected in advance according to the type of the sample to be detected, and then determining and selecting a detection method of the bottom concentration or a high-concentration detection method; or when the concentration of the sample to be detected can not be detected by the bottom concentration detection method, the high-concentration detection method is used for detection.
The principle and the implementation mode of the invention are explained by applying a specific example, and the description of the embodiment is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (9)
1. A chloride ion detector is characterized in that: comprises a sampling tank, a communicating device, a titration cell, a dropping liquid mechanism, a solution storage device, a water supply device, a reagent supply device and a controller; the reagent supply device is used for containing related reagents; the sampling tank is used for acquiring and outputting liquid and can meter the dosage of the liquid; the titration cell is communicated with the dropping mechanism, the dropping mechanism is used for dropping a titration solution into the titration cell, a titration monitoring device is arranged on the outer side of the titration cell, and the titration monitoring device is used for monitoring the reaction degree of the solution in the titration cell; the communicating device is connected with the sampling tank, the titration cell, the solution storage device, the water supply device and the reagent supply device; the controller with sample jar, intercommunication device, titration cell and dropping liquid mechanism electricity are connected, the controller is used for controlling respectively the sample jar the titration cell solution storage device and reagent feeding device with the break-make of intercommunication device.
2. The chloride ion detector of claim 1, wherein: the liquid level sensor is arranged on the sampling tank; the number of the liquid level sensors is at least two, and each liquid level sensor is respectively arranged at different heights of the sampling tank; the level sensor is electrically connected to the controller, the level sensor being configured to meter a dose of liquid.
3. The chloride ion detector of claim 1, wherein: still include magnetic stirrers, magnetic stirrers sets up titration cell bottom, magnetic stirrers with the controller electricity is connected.
4. The chloride ion detector of claim 1, wherein: the titration monitoring device comprises a light-emitting diode and a photoelectric sensor, and the light-emitting diode and the photoelectric sensor are electrically connected with the controller.
5. The chloride ion detector of claim 1, wherein: the titration apparatus further comprises a liquid discharge pump, the liquid discharge pump is communicated with a liquid discharge valve at the bottom of the titration cell, and the liquid discharge pump is electrically connected with the controller.
6. The chloride ion detector of claim 1, wherein: the dropping liquid mechanism includes plunger pump, step motor, two three-way valves and reagent jar, two three-way valves are used for communicateing alone the plunger pump with reagent jar or communicateing alone the plunger pump with the titration cell, step motor is used for the drive the plunger pump, step motor with the controller electricity is connected, automatically controlled two three-way valves with the controller electricity is connected.
7. The chloride ion detector of claim 5, wherein: the plunger pump is characterized by further comprising a limit sensor, wherein the limit sensor is arranged at the bottom of the plunger pump and electrically connected with the controller.
8. A chloride ion detection method based on the chloride ion detector of any one of claims 1 to 7, characterized in that: the method can be used for detecting the chloride ions in the high-concentration chloride ion solution, and comprises the following steps:
the method comprises the following steps: respectively carrying out N times of dilution on a plurality of standard samples to respectively obtain a plurality of diluted standard samples, wherein N is more than or equal to 2, and the initial concentration Ci (i is more than or equal to 2) of each standard sample is known;
step two: titrating a plurality of diluted standard samples through the dropping mechanism respectively, and recording respective titrating liquid dosage Vi (i is more than or equal to 2) when the titration monitoring device detects that the titration reaction is finished;
step three: acquiring a linear relation V between the concentration C of the chloride ion solution and the dosage V of the titration solution as kC + b according to a plurality of groups Ci and Vi;
step four: diluting a sample to be tested for N times to obtain a diluted sample to be tested;
step five: titrating the diluted sample to be measured through the dropping mechanism until the titration monitoring device detects that the titration reaction is finished, recording the dosage of the titration solution, and calculating the concentration of the sample to be measured according to the linear relation V (kC + b) of the concentration C of the chloride ion solution and the dosage V of the titration solution;
wherein, to standard sample, the dilution of the sample that awaits measuring each time all includes:
s1: initial dilution step on the sample: the controller is used for respectively controlling the connection and disconnection of the sampling tank, the water supply device, the titration cell and the communication device; measuring a first dose of purified water to the titration cell and a second dose of sample to the titration cell to obtain an initially diluted sample;
s2: the dilution procedure was repeated on the samples: the controller is used for respectively controlling the quantity of the sampling tank, the water supply device, the solution storage device and the communication device to be switched on and off, so that the solution in the second dose titration cell is measured and delivered to the solution storage device, and the residual solution in the titration cell is discharged; measuring a first dose of purified water to a titration cell, and measuring a solution in a second dose of solution storage device to the titration cell to obtain a repeatedly diluted sample;
s3: repeat N-2 times S2.
9. Such dilution methods are not limited to the dilution of chloride ion solutions.
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Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5192509A (en) * | 1991-08-22 | 1993-03-09 | Halliburton Company | Apparatus for automatic titration |
| JP2004035031A (en) * | 2002-07-02 | 2004-02-05 | Saraya Kk | Dilution device |
| JP2005308679A (en) * | 2004-04-26 | 2005-11-04 | Asahi Life Sci Kk | Salinity concentration measuring method, unit water amount measuring method, and measuring instrument therefor |
| CN104007239A (en) * | 2014-06-12 | 2014-08-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Automatic online measurement system and method for high-concentration ions |
| CN105319206A (en) * | 2014-06-11 | 2016-02-10 | 肖巍 | Water quality purification detection device and water quality purification detection method |
| CN105806993A (en) * | 2016-04-08 | 2016-07-27 | 天津中水有限公司 | Method for detecting chloride in reclaimed water and titration apparatus |
| WO2016137431A1 (en) * | 2015-02-23 | 2016-09-01 | Nantpharma, Llc | Robust methods for determining heparin concentrations |
| CN109116043A (en) * | 2018-09-17 | 2019-01-01 | 沈阳汉威科技有限公司 | Monitoring water quality on line equipment and control method based on programmable controller |
| CN208705295U (en) * | 2018-07-23 | 2019-04-05 | 山东省科学院生物研究所 | The detection device of gluconic acid sodium content in a kind of fermentation liquid |
| CN110927329A (en) * | 2019-12-16 | 2020-03-27 | 国网四川省电力公司电力科学研究院 | Atmospheric environment chloride ion deposition rate testing device and method |
| CN110967309A (en) * | 2019-12-26 | 2020-04-07 | 苏州奥特福环境科技有限公司 | Online detection system and method for available chlorine in water quality disinfection process |
| CN111272751A (en) * | 2020-04-07 | 2020-06-12 | 南京力创环境科技有限公司 | Titration method water quality on-line automatic monitoring system and method |
| CN111735907A (en) * | 2020-08-04 | 2020-10-02 | 湖南航天磁电有限责任公司 | Method for measuring chloride ion content in industrial lanthanum oxide by potentiometric titration |
-
2021
- 2021-01-07 CN CN202110017041.1A patent/CN112816615B/en active Active
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5192509A (en) * | 1991-08-22 | 1993-03-09 | Halliburton Company | Apparatus for automatic titration |
| JP2004035031A (en) * | 2002-07-02 | 2004-02-05 | Saraya Kk | Dilution device |
| JP2005308679A (en) * | 2004-04-26 | 2005-11-04 | Asahi Life Sci Kk | Salinity concentration measuring method, unit water amount measuring method, and measuring instrument therefor |
| CN105319206A (en) * | 2014-06-11 | 2016-02-10 | 肖巍 | Water quality purification detection device and water quality purification detection method |
| CN104007239A (en) * | 2014-06-12 | 2014-08-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Automatic online measurement system and method for high-concentration ions |
| WO2016137431A1 (en) * | 2015-02-23 | 2016-09-01 | Nantpharma, Llc | Robust methods for determining heparin concentrations |
| CN105806993A (en) * | 2016-04-08 | 2016-07-27 | 天津中水有限公司 | Method for detecting chloride in reclaimed water and titration apparatus |
| CN208705295U (en) * | 2018-07-23 | 2019-04-05 | 山东省科学院生物研究所 | The detection device of gluconic acid sodium content in a kind of fermentation liquid |
| CN109116043A (en) * | 2018-09-17 | 2019-01-01 | 沈阳汉威科技有限公司 | Monitoring water quality on line equipment and control method based on programmable controller |
| CN110927329A (en) * | 2019-12-16 | 2020-03-27 | 国网四川省电力公司电力科学研究院 | Atmospheric environment chloride ion deposition rate testing device and method |
| CN110967309A (en) * | 2019-12-26 | 2020-04-07 | 苏州奥特福环境科技有限公司 | Online detection system and method for available chlorine in water quality disinfection process |
| CN111272751A (en) * | 2020-04-07 | 2020-06-12 | 南京力创环境科技有限公司 | Titration method water quality on-line automatic monitoring system and method |
| CN111735907A (en) * | 2020-08-04 | 2020-10-02 | 湖南航天磁电有限责任公司 | Method for measuring chloride ion content in industrial lanthanum oxide by potentiometric titration |
Non-Patent Citations (2)
| Title |
|---|
| 李红艳等: "离子色谱法标定盐酸标准滴定溶液浓度", 《福建分析测试》 * |
| 李红艳等: "离子色谱法标定盐酸标准滴定溶液浓度", 《福建分析测试》, no. 01, 15 January 2010 (2010-01-15), pages 68 - 72 * |
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