CN112834688A - Calcium hardness detector and calcium hardness detection method - Google Patents
Calcium hardness detector and calcium hardness detection method Download PDFInfo
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- CN112834688A CN112834688A CN202110016805.5A CN202110016805A CN112834688A CN 112834688 A CN112834688 A CN 112834688A CN 202110016805 A CN202110016805 A CN 202110016805A CN 112834688 A CN112834688 A CN 112834688A
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- 238000001514 detection method Methods 0.000 title claims abstract description 55
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 47
- 239000011575 calcium Substances 0.000 title claims abstract description 47
- 238000004448 titration Methods 0.000 claims abstract description 142
- 239000007788 liquid Substances 0.000 claims abstract description 103
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 50
- 238000005070 sampling Methods 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000012806 monitoring device Methods 0.000 claims abstract description 18
- 238000004891 communication Methods 0.000 claims abstract description 6
- 238000012544 monitoring process Methods 0.000 claims abstract description 5
- 239000000523 sample Substances 0.000 claims description 59
- 239000000243 solution Substances 0.000 claims description 54
- 238000000034 method Methods 0.000 claims description 38
- 239000008213 purified water Substances 0.000 claims description 14
- 230000005611 electricity Effects 0.000 claims description 10
- 239000012470 diluted sample Substances 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- 238000004164 analytical calibration Methods 0.000 description 7
- DEGAKNSWVGKMLS-UHFFFAOYSA-N calcein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC(CN(CC(O)=O)CC(O)=O)=C(O)C=C1OC1=C2C=C(CN(CC(O)=O)CC(=O)O)C(O)=C1 DEGAKNSWVGKMLS-UHFFFAOYSA-N 0.000 description 7
- 229960002378 oftasceine Drugs 0.000 description 7
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 6
- 239000012266 salt solution Substances 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000001960 triggered effect Effects 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 1
- IBVDXHNTFWKXQE-UHFFFAOYSA-N [acetyloxy-[2-(diacetyloxyamino)ethyl]amino] acetate;sodium Chemical compound [Na].[Na].CC(=O)ON(OC(C)=O)CCN(OC(C)=O)OC(C)=O IBVDXHNTFWKXQE-UHFFFAOYSA-N 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000005406 washing Methods 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
-
- 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
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a calcium hardness detector and a calcium hardness detection method, and relates to the field of water quality detection, wherein the calcium hardness detector comprises a sampling tank, a communication device, a titration cell, a dropping liquid mechanism, a reagent supply device and a controller; the reagent supply device is used for containing a reagent required by detection; the sampling tank is used for metering, obtaining and outputting liquid; the titration cell is communicated with the dropping mechanism, a titration monitoring device is arranged on the outer side of the titration cell and used for monitoring the reaction degree of the solution in the titration cell, the monitoring device comprises a light source and a light sensing device, and the light sensing device is not directly irradiated by light of the light source; the communicating device is connected with the sampling tank, the titration cell 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 is used for respectively controlling the on-off of the sampling tank, the titration cell and the on-off of the reagent supply device and the communicating device. The calcium hardness detector and the calcium hardness detection method can improve the calcium hardness detection precision and improve the detection efficiency.
Description
Technical Field
The invention relates to the field of water quality detection equipment, in particular to a calcium hardness detector and a calcium hardness detection method.
Background
Calcium hardness means the content of calcium ions in water, the detection of calcium hardness is widely applied to industries such as beer brewing, environmental protection and the like, and the current technology for detecting calcium hardness mainly adopts an artificial titration method, and the problem of poor detection consistency is inevitably caused by artificial titration, so that the detection precision is influenced.
Disclosure of Invention
The invention aims to provide a calcium hardness detector and a calcium hardness detection method, which are used for solving the problems in the prior art and improving the calcium hardness detection precision.
In order to achieve the purpose, the invention provides the following scheme:
the invention provides a calcium hardness detector which comprises a sampling tank, a communication device, a titration cell, a dropping liquid mechanism, 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 reagents required by the experiment; 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 used for monitoring the reaction degree of the solution in the titration cell, the monitoring device comprises a light source and a light sensing device, and the light sensing device is not directly irradiated by light of the light source; the communicating device is connected with the sampling tank, the titration cell and the reagent supply device; the controller with sample jar, intercommunication device, titration cell, dropping liquid mechanism electricity are connected, the controller is used for controlling respectively the sample jar titration cell 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;
preferably, 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 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.
Preferably, the plunger pump further comprises a limit sensor, the limit sensor is arranged at the bottom of the plunger pump, and the limit sensor is electrically connected with the controller.
A calcium hardness detection method based on the calcium hardness detector can be used for calcium hardness detection of a solution, and comprises the following steps:
the method comprises the following steps: adding a standard sample into a titration cell, wherein the concentration Ci of the standard sample is known;
step two: titrating the standard samples through the dropping mechanism respectively until the titration monitoring device detects that the titration reaction is finished, and recording respective titration liquid consumption Vi;
step three: repeating the first step and the second step for multiple times, titrating standard samples with different concentrations, and obtaining a linear relation V (kC + b) of the solution concentration C and the titration solution dosage V according to multiple groups of Ci and Vi (i is not less than 2);
step four: adding a sample to be detected into a titration cell;
step five: through dropping liquid mechanism titrates the sample that awaits measuring, extremely titrate monitoring devices and detect that titration reaction ends, record titration liquid quantity, according to solution concentration C and titration liquid quantity V's linear relation V ═ kC + b, calculate the concentration of the sample that awaits measuring
A calcium hardness detection method based on the calcium hardness detector can be used for calcium hardness detection of high-concentration solution, and comprises the following steps:
the method comprises the following steps: respectively diluting a plurality of standard samples to respectively obtain a plurality of diluted standard samples, wherein 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 solution concentration C and the titration solution dosage V as kC + b according to a plurality of groups of Ci and Vi;
step four: diluting a sample to be tested 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 solution concentration C and the dosage V of the titration solution;
wherein, the dilution to the standard sample and the sample to be measured comprises the following steps:
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; the method is characterized in that a first dose of purified water is measured to the titration cell, a second dose of sample is measured to the titration cell, and a diluted sample is obtained.
According to the calcium hardness detector and the calcium hardness detection method provided by the invention, the detection range can be increased and the detection precision can be improved by diluting the sample to be detected in the detection process, 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, the magneton 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 calcium hardness detection method 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 calcium hardness detector according to a first embodiment of the present invention;
fig. 2 is a schematic diagram illustrating a positional relationship between a light emitting diode and a photosensor 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 multi-position valve; 6-reagent tank; 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-step motor 15-two-position three-way valve;
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 calcium hardness detector and a calcium hardness 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
This embodiment provides a calcium hardness detector, as shown in FIGS. 1-2,
comprises a sampling tank, a communicating device, a titration cell, a dropping liquid mechanism, a reagent supply device and a controller; the reagent supply device is used for containing a reagent required by detection; the sampling tank is used for acquiring and outputting liquid and can meter the dosage of the liquid; the titration cell is communicated with a 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 used for monitoring the reaction degree of the solution in the titration cell, the monitoring device comprises a light source and a light sensing device, and the light sensing device is not directly irradiated by light of the light source; the communicating device is connected with the sampling tank, the titration cell 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 is used for respectively controlling the on-off of the sampling tank, the titration cell and the on-off of the reagent supply device and the communicating device. All the measurement and reaction work are controlled by the controller, no interference is considered in the detection process, and the detection precision and efficiency are improved.
The reagent supply device comprises a water supply device, a reagent bottle A and a reagent bottle B which are respectively used for containing water, a calcein solution and an acid solution; 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 outside 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 communication device is a multi-position valve 5, the multi-position valve 5 is used for communicating the sampling tank 2, the titration cell 7, the reagent bottle a, the reagent bottle B, the sampling channel and the water supply device, and the controller is used for respectively controlling the on-off of the sampling tank 2, the titration cell 7, the reagent bottle a, the reagent bottle B, the sampling channel and the water supply device and the communication device, wherein F1, F2, F3, F4 and F5 are one-to-five-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 through stretching into the inside pipeline and the titration cell intercommunication of titration cell from titration cell upper portion, F2 valve and reagent bottle A intercommunication, F3 valve and reagent bottle B intercommunication, F4 valve and water feeding device intercommunication, the water feeding device is the pure water in this embodiment, F5 valve and sample access intercommunication, each valve is the electrically controlled valve, all electrically controlled valves all are connected with the controller electricity, by the control of controller, degree of automation and detection precision have further been improved, the required reagent of experiment includes water feeding device, the reagent in reagent bottle A and the reagent bottle B, the required reagent of experiment is used for adding in the titration cell 7 before the titration begins and carries out the preliminary treatment and is used for belt cleaning device to the solution in the titration cell 7.
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 used for monitoring a titration process, the monitoring device comprises a light source and a light sensing device, the light sensing device is a photoelectric sensor 8, the light source is a light emitting diode 9, the light receiving direction of the photoelectric sensor 8 and the light angle emitted by the light emitting diode 9 are 10-160 degrees, and the angle is 90 degrees in the embodiment; the wavelength of the light emitting diode 9 is 360 nm-600 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 control system is electrically connected with the power pump 1, the liquid level sensor, the multi-position valve 5, the photoelectric sensor 8, the light emitting diode 9 and the liquid dropping mechanism, the operation of each electric device is accurately controlled according to a set program, manual errors are avoided, and the detection precision is improved.
The liquid level sensor is respectively arranged at two different heights of 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, the high-level liquid level sensor 3 corresponds to a first dosage, the low-level liquid level sensor 4 corresponds to a second dosage, and the sampling tank 2 realizes the function of metering the dosage of the solution through the liquid level sensor; 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.
In this embodiment, titration cell 7 bottom is equipped with magnetic stirrers, and magnetic stirrers includes magnetic stirrers 10 and stirring driver 11, stirs 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 6, and the solution that holds in the reagent tank 6 is ethylenediamine tetraacetic acid disodium salt solution, and two three-way valves 15 are used for communicateing plunger pump 13 and reagent tank 6 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
In this embodiment, a method for detecting calcium hardness can detect the concentration of a solution with a first concentration;
the first step is as follows: instrument calibration process
Firstly, cleaning with purified water:
1. taking purified water to a titration cell 7: the control system firstly controls the power pump 1 to start pumping work, then controls the F4 valve of the multi-position valve 5 to be opened, other valves are all in a closed state at the moment, the power pump 1 is started firstly, then the F4 valve is opened, liquid can be directly pumped after the F4 valve is opened, and a purified water taking pipeline of the F4 valve is inserted into a purified water container; purified water is pumped into a high-level liquid level sensor 3 of a sampling tank 2, the high-level liquid level sensor 3 sends a signal to a control system after detecting liquid, the control system controls a power pump 1 to stop pumping the liquid, then the control system controls an F4 valve of a multi-position valve 5 to be closed and an F1 valve to be opened, the control system controls the power pump 1 to pump the liquid into a titration tank 7, and the process of taking the purified water into the titration tank 7 is completed;
2. liquid drainage: the control system controls to turn on the liquid discharge pump 12, discharge the purified water in the titration tank 7 and then turn off the liquid discharge pump 12.
Completing the purified water cleaning process;
II, sampling: the concentration of the sample is known, the control system firstly controls the power pump 1 to start pumping work, then the control system controls the F5 valve of the multi-position valve 5 to be opened, at the moment, other valves are in a closed state, the power pump 1 is started firstly, then the F5 valve is opened, liquid can be directly pumped after the F5 valve is opened, the sampling channel of the F5 valve is inserted into the sample with the known concentration, the sample with the known concentration is pumped into the high-position liquid level sensor 3 of the sampling tank 2, the high-position liquid level sensor 3 sends a signal to the control system after detecting the liquid, the control system controls the power pump 1 to stop pumping, then the control system controls the F5 valve of the multi-position valve 5 to be closed, the F1 valve is opened, the control system controls the power pump 1 to pump the sample with the known concentration into the titration cell 7.
Taking the disodium ethylene diamine tetraacetate solution in the reagent tank 6: when the control system executes the process of taking a sample with a known concentration, the control system simultaneously executes the process of taking the solution in the reagent tank 6: the control system sends a signal to a stepping motor 14 of a plunger pump 13, the plunger pump 13 is controlled to move downwards, when the plunger pump 13 moves to the bottom, a limit sensor at the bottom of the plunger pump 13 sends a signal to the control system, the control system controls the stepping motor 14 of the plunger pump 13 to stop moving, the control system adjusts a two-position three-way valve 15, a pipe at the lower end of the plunger pump 13 is communicated with a pipe inserted into a reagent tank 6, the control system sends a signal to the stepping motor 14 of the plunger pump and controls the plunger pump 13 to move upwards, when the plunger pump 13 is filled with an ethylene diamine tetraacetic acid disodium salt solution, the control system controls the stepping motor 14 of the plunger pump 13 to stop moving, and therefore the disodium ethylenediamine tetraacetate salt solution is taken, and the ethylene diamine tetraacetic acid disodium salt solution;
fourthly, taking a calcein solution: the control system firstly controls the power pump 1 to start pumping work, then controls the F2 valve of the multi-position valve 5 to be opened, at the moment, other valves are in a closed state, the power pump 1 is started firstly, then the F2 valve is opened, the F2 valve is communicated with the reagent bottle A, the reagent bottle A contains calcein solution, the calcein solution is pumped into the low-position liquid level sensor 4 of the sampling tank 2, the low-position liquid level sensor 4 sends a signal to the control system after detecting the liquid, the control system controls the power pump 1 to stop pumping, then controls the F2 valve of the multi-position valve 5 to be closed, the F1 valve is opened, the control system controls the power pump 1 to pump the calcein solution into the titration cell 7, and therefore the calcein solution pumping is completed.
Fifthly, titration: the control system controls the stirrer driver 11 to rotate, the magnet on the stirrer driver 11 drives the stirring magnet 10 to rotate through magnetic field force, the stirring magnet stirs the mixed liquid in the titration cell 7, meanwhile, the light emitting diode 9 of the titration cell 7 is turned on, the wavelength of the light emitting diode 9 is 360 nm-600 nm, before the titration end point is not reached, the mixed liquid in the titration cell 7 is triggered to generate fluorescence when the light emitted by the light emitting diode 9 irradiates the liquid in the titration cell 7, the fluorescence generated by the liquid is converted into an electric signal U by the photoelectric sensor 8 of the titration cell 7, the electric signal is transmitted to the control system, the included angle phi between the photoelectric sensor 8 of the titration cell 7 and the installation position of the light emitting diode 9 is 10-160 degrees, the optimal selection is 90 degrees in the embodiment, before the plunger pump is started to titrate, the control system records that the electric signal of the photoelectric0Then the control system adjusts the two-position three-way valve 15, the pipeline at the lower end of the plunger pump 13 is communicated with the titration cell 7, then the stepping motor 14 of the plunger pump 13 is controlled to start to move, the plunger of the plunger pump 13 moves downwards, the ethylene diamine tetraacetic acid disodium salt solution 6 in the plunger pump is dripped into the titration cell 7, meanwhile, the control system records the electric signal U of the photoelectric sensor 8, and simultaneously, the control system also records the pulse number N of the stepping motor 14 of the plunger pump 13 sent by the control system when the electric signal is U0When the electrical signal U of the photoelectric sensor 8 is changed into eU0When e is 0.1-0.8, recording the corresponding control system directional plungerThe pulse number N is sent by the stepping motor 14 of the pump 13, then the control system sends a signal to the plunger pump 13 to stop moving, then the control system sends a signal to the stirring sub driver 11 to stop moving, and the system carries out liquid discharge, so that the titration is completed.
Sixthly, acid washing: the control system firstly controls the power pump 1 to start pumping work, then controls the F3 valve of the multi-position valve 5 to be opened, does not open the F3 valve at the moment, firstly starts the power pump 1, then opens the F3 valve, and can directly pump liquid after opening the F3 valve; the F3 valve is communicated with a reagent bottle B, the reagent bottle B contains an acid solution which is sulfuric acid or hydrochloric acid, the acid solution is pumped into the low level liquid level sensor 4 of the sampling tank 2, the low level liquid level sensor 4 sends a signal to the control system after detecting the liquid, the control system controls the power pump 1 to stop pumping, then the control system controls the F3 valve of the multi-level valve 5 to be closed, the F4 valve is opened, the control system controls the power pump 1 to pump the liquid into the sampling tank 2, purified water is pumped into the sampling tank 2, when the liquid reaches the upper sensor 3 of the sampling tank 2, the control system controls the power pump 1 to stop pumping, then the control system controls the F4 valve of the multi-level valve 5 to be closed, the F1 valve is opened, the control system controls the power pump 1 to pump the liquid into the titration tank 7, the control system controls the stirring sub driver 11 to rotate, a magnet on the stirring sub driver 11 drives the stirring magnet 10 to rotate through magnetic field force, and (3) uniformly mixing the sample in the titration cell 7 with the purified water, and performing the action of draining liquid by the system so as to finish pickling.
And finishing the titration process after finishing the first to sixth processes.
Seventhly, calibration: after the above-mentioned process is completed, the control system records the standard sample concentration C and the number of pulses N sent by the control system corresponding to the titration end point of the standard sample to the stepping motor 14 of the plunger pump 13, hereinafter referred to as the number of pulses N, selects two or more standard samples to calibrate, and according to the concentrations C and the number of pulses N of different standard samples, may find N ═ kC + b, which is the linear relationship between the sample concentration C and the titration end point number of pulses N, so as to complete the calibration process.
Under the condition that the calcein solution, the acid solution, the ethylenediaminetetraacetic acid disodium salt solution 6 and the purified water are not replaced, the first step of the instrument calibration process only needs to be operated once.
The second step is that: concentration detection process
The difference between the concentration detection process and the instrument calibration process is that the process II in the instrument calibration process is as follows: the sample with known concentration in the 'sampling sample' is replaced by the sample to be detected.
And (3) calibrating the instrument according to a second flow: and after the known concentration sample in the known concentration sample is replaced by the sample to be detected, the steps are executed to finish the titration process, the control system records the pulse number N of the titration end point of the sample, and the linear relation N between the concentration C of the sample and the pulse number N of the titration end point of the sample, which is solved according to the instrument calibration process, is kC + b, so that the concentration C of the sample to be detected can be obtained, and the concentration detection process of the first concentration solution is finished for the first time.
EXAMPLE III
The embodiment provides a calcium hardness detection method, which comprises the steps of detecting the concentration of a solution with a second concentration, wherein the second concentration is greater than the first concentration, and the method comprises the following steps:
the difference between this embodiment and the second embodiment is that the first step: a second procedure in the instrument calibration procedure: samples of known concentration were taken.
In this example, the process of taking a sample with a known concentration is as follows: the system executes ' 1 ' in the first procedure of the instrument calibration procedure in the first procedure in the embodiment II, and pure water is taken to the titration cell 7 '; the control system firstly controls the power pump 1 to start pumping work, then controls the F5 valve of the multi-position valve 5 to be opened, at the moment, the F5 valve is not opened, the power pump 1 is started firstly, then the F5 valve is opened, liquid can be directly pumped after the F5 valve is opened, the pipeline of the sampling product channel 1 of the F5 is inserted into a sample, the sample is pumped into the low-position liquid level sensor 4 of the sampling tank 2, the low-position liquid level sensor 4 sends a signal to the control system after detecting the liquid, the control system controls the power pump 1 to stop pumping liquid, then controls the F5 valve of the multi-position valve 5 to be closed, the F1 valve is opened, and the control system controls the power pump 1 to pump the sample into the titration cell 7; the control system controls the stirring sub driver 11 to rotate, the magnet on the stirring sub driver 11 drives the stirring magnet 10 to rotate through magnetic field force, and the sample in the titration cell 7 is uniformly mixed with the purified water, so that the extraction and dilution of the known sample are completed.
In this embodiment, the sample with the known concentration and the sample to be detected are further diluted, so that the detection range of the detector is further increased, the solution with the actual concentration exceeding the range of the first embodiment can be detected, and the practicability is improved.
The detection method using the first concentration or the second concentration during detection comprises the following steps: determining an 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 first concentration or a detection method of the second concentration; or when the concentration of the sample to be detected can not be detected by the first concentration detection method, the detection is carried out by the second concentration detection method.
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 calcium hardness detector is characterized in that: comprises a sampling tank, a communicating device, a titration cell, a dropping liquid mechanism, a reagent supply device and a controller; the reagent supply device is used for containing a reagent required by detection; 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 used for monitoring the reaction degree of the solution in the titration cell, the monitoring device comprises a light source and a light sensing device, and the light sensing device is not directly irradiated by light of the light source; the communicating device is connected with the sampling tank, the titration cell and the reagent supply device; the controller with sample jar, intercommunication device, titration cell, dropping liquid mechanism electricity are connected, the controller is used for controlling respectively the sample jar titration cell and reagent feeding device with the break-make of intercommunication device.
2. The calcium hardness tester according to claim 1, wherein: still include level sensor, level sensor sets up on the sample jar.
3. The calcium hardness tester according to claim 2, wherein: 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.
4. The calcium hardness tester according to claim 1, wherein: still include magnetic stirrers, magnetic stirrers sets up titration cell bottom, magnetic stirrers with the controller electricity is connected.
5. The calcium hardness tester according to 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 calcium hardness tester according to 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 calcium hardness tester according to claim 6, 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 calcium hardness detection method based on the calcium hardness detector according to any one of claims 1 to 7, characterized in that: can be used for calcium hardness detection of a solution, comprising the following steps:
the method comprises the following steps: adding a standard sample into a titration cell, wherein the concentration Ci of the standard sample is known;
step two: titrating the standard samples through the dropping mechanism respectively until the titration monitoring device detects that the titration reaction is finished, and recording respective titration liquid consumption Vi;
step three: repeating the first step and the second step for multiple times, titrating standard samples with different concentrations, and obtaining a linear relation V (kC + b) of the solution concentration C and the titration solution dosage V according to multiple groups of Ci and Vi (i is not less than 2);
step four: adding a sample to be detected into a titration cell;
step five: through dropping liquid mechanism titrates the sample that awaits measuring, extremely titrate monitoring devices and detect that the titration reaction is ended, record titration liquid quantity, according to solution concentration C and titration liquid quantity V's linear relation V kC + b, calculate the concentration of the sample that awaits measuring.
9. A calcium hardness detection method based on the calcium hardness detector according to any one of claims 1 to 7, characterized in that: can be used for calcium hardness detection of high concentration solution, and comprises the following steps:
the method comprises the following steps: respectively diluting a plurality of standard samples to respectively obtain a plurality of diluted standard samples, wherein 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 solution concentration C and the titration solution dosage V as kC + b according to a plurality of groups of Ci and Vi;
step four: diluting a sample to be tested 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 solution concentration C and the dosage V of the titration solution;
wherein, the dilution to the standard sample and the sample to be measured comprises the following steps:
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; the method is characterized in that a first dose of purified water is measured to the titration cell, a second dose of sample is measured to the titration cell, and a diluted sample is obtained.
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Cited By (1)
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