CN116008197A - Nickel and cobalt ion concentration online analysis instrument and analysis method thereof - Google Patents
Nickel and cobalt ion concentration online analysis instrument and analysis method thereof Download PDFInfo
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- CN116008197A CN116008197A CN202310309211.2A CN202310309211A CN116008197A CN 116008197 A CN116008197 A CN 116008197A CN 202310309211 A CN202310309211 A CN 202310309211A CN 116008197 A CN116008197 A CN 116008197A
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Abstract
The invention provides an online analysis instrument for nickel and cobalt ion concentration and an analysis method thereof, which relate to the technical field of online measurement instruments for wet smelting, and a nonlinear regression model of the proportion of the nickel and cobalt ion concentration to R, G, B component of solution color and the total content of nickel and cobalt is established before measurement; the method is characterized in that a sample solution to be measured is extracted on line at a process sampling point, color measurement is carried out on the initial sample solution, the proportion value of nickel and cobalt ions in the initial sample solution is regressed according to a color measurement model, the total content of cobalt and nickel is measured by using an EDTA complexation titration method, the concentration of nickel and cobalt ions is calculated based on the total content of nickel and cobalt ions respectively, and the technical problems that the on-line detection technology and instrument in the prior art can not simultaneously measure the concentration of nickel and cobalt ions in the nickel and cobalt solvent extraction process, and the EDTA titration method can only measure the total concentration of nickel and cobalt ions and can not simultaneously realize the detection of the respective concentrations of nickel and cobalt ions are solved.
Description
Technical Field
The invention relates to the technical field of wet smelting online measuring instruments, in particular to an online nickel and cobalt ion concentration analyzing instrument and an analyzing method thereof.
Background
Nickel and cobalt are widely applied in the fields of aviation, aerospace, electronics, batteries and the like, and occupy an important place in industry; due to the similar chemical properties of nickel and cobalt, which are often co-produced or semi-produced in ore deposits, the current solvent extraction technology is the main method for smelting and separating nickel and cobalt. In the nickel and cobalt solvent extraction process, the nickel and cobalt raw materials are different in source, the components of leaching liquid in the preamble process are complex, and the concentrations of main elements nickel, cobalt ions and impurity metal ions in the solution in the extraction process are required to be frequently analyzed and detected, so that indexes of the extraction production process are mastered in real time and process adjustment is performed in time.
In the prior art, nickel and cobalt ions have high concentration and wide range in the nickel and cobalt extraction process, the concentration range of the nickel and cobalt ions is generally 0.01g/L-100g/L, and the online detection technology and instrument in the prior art cannot simultaneously measure the nickel and cobalt ion concentrations in the process, so that the analysis and detection of the nickel and cobalt ion concentrations are realized through the off-line analysis of a laboratory, the workload of manual sampling and testing is high, and the hysteresis is large and cannot meet the requirements of automation and flow optimization control; in addition, in the prior art, EDTA titration is generally adopted for detecting the concentration of nickel and cobalt ions in a laboratory, but the EDTA titration in the prior art can only measure the total concentration of nickel and cobalt ions, and cannot simultaneously detect the concentrations of nickel and cobalt ions.
Disclosure of Invention
The invention aims to provide an online analysis instrument and an online analysis method for nickel and cobalt ion concentration, which are used for solving the technical problems that an online detection technology and an online analysis instrument in the prior art cannot simultaneously measure the nickel and cobalt ion concentration in a nickel and cobalt solvent extraction process, and an EDTA titration method can only measure the total concentration of nickel and cobalt ions, so that the detection of the respective concentrations of nickel and cobalt ions cannot be simultaneously realized.
The invention provides an online analysis method for nickel and cobalt ion concentration, which comprises the following steps:
establishing a color measurement model, and establishing a nonlinear regression model of the concentration ratio of nickel and cobalt ions to the component proportion of the color R, G, B of the solution and the total content of nickel and cobalt by utilizing data according to the RGB proportion of the color components of nickel and cobalt ions in the solution and the total content of nickel and cobalt;
extracting a sample solution to be measured on line at a process sampling point;
quantitatively sampling the extracted sample to be measured to form an initial sample solution;
carrying out color measurement on the initial sample solution, and regressing the proportion value of nickel and cobalt ions in the initial sample solution according to a color measurement model;
adding a shielding buffer reagent to the initial sample to form a first sample solution;
Adding a solid indicator to the first sample solution to form a second sample solution, wherein the solid indicator comprises an ammonium purple urea indicator;
titrating the second sample solution by adopting the EDTA standard solution, measuring the ratio information of the R, G, B component of the color in the solution in real time in the titration process, stopping the titration when the color information has a color variation point, and recording the volume of the consumed EDTA standard solution;
calculating the total content of nickel and cobalt ions based on an EDTA complexometric titration formula;
the concentration of nickel and cobalt ions is calculated based on the total content of nickel and cobalt ions.
In a preferred embodiment of the present invention, the step of establishing a color measurement model includes:
determining the proportion of the components of the combined color R, G, B based on the ion concentration proportion when nickel and cobalt ions coexist, and sequentially preparing nickel and cobalt mixed solutions with different concentration proportions according to gradients under the condition of fixed light sources;
and measuring the nickel and cobalt mixed solution with each concentration ratio to obtain the color R, G, B component ratio of the nickel and cobalt mixed solution with the corresponding concentration ratio, and modeling by using data to obtain a nonlinear regression model of the nickel and cobalt ion concentration ratio and the solution color R, G, B component ratio and the total nickel and cobalt ion content.
In a preferred embodiment of the present invention, the method further comprises the steps of:
storing an initial sample solution in a titration cup;
color information measurement is carried out on the water solution stored in the titration cup, and a reference background value of the titration cup is obtained;
and subtracting the reference background value from the ratio information of the components of the color R, G, B in the solution when the color information appears in the color variation point, and obtaining the respective ratio information of the three components of the color R, G, B of the sample.
In a preferred embodiment of the present invention, the method further comprises the steps of:
and (3) adding water to dilute the initial sample solution, and adding a shielding buffer reagent to the diluted initial sample solution to form a first sample solution.
In a preferred embodiment of the present invention, the step of formulating the shielding buffer comprises:
preparing an ammonia-ammonium chloride buffer solution with the pH range of 9-11;
fluoride, sodium thiosulfate and tartaric acid are sequentially added to the ammonia-ammonium chloride buffer solution corresponding to the impurity components of the initial sample solution.
In a preferred embodiment of the present invention, the method further comprises the steps of:
and (5) draining and flushing the equipment for completing the detection and analysis of the sample solution.
The invention provides a nickel and cobalt ion concentration online analysis instrument applied to the nickel and cobalt ion concentration online analysis method, which comprises the following components: the device comprises a sampling mechanism, a measuring mechanism and a control main body;
The sampling mechanism comprises a sample chamber, the sampling mechanism is used for being arranged at a process sampling point, and the sampling mechanism can extract a sample solution to be measured on line and convey the sample solution to the sample chamber;
the measuring mechanism is communicated with the sample chamber and is used for quantitatively extracting a sample solution from the sample chamber to form an initial sample solution, and the measuring mechanism is used for measuring the total content of nickel and cobalt ions in the initial sample solution based on an EDTA complexometric titration method;
the control main body is in electrical signal connection with the measuring mechanism, a color measuring model is pre-established in the control main body, and the control main body is used for returning the proportion values of nickel and cobalt ions in the initial sample solution according to the color measuring model corresponding to the total content of nickel and cobalt ions in the initial sample solution so as to calculate the concentration of nickel and cobalt ions respectively.
In a preferred embodiment of the invention, the sampling mechanism comprises a sampling pump, a first control valve and a liquid level gauge;
the sampling pump is communicated with a process sampling point through a first pipeline, the sampling pump is communicated with the sample chamber through a first control valve, the sampling pump is used for pumping a sample solution to be measured in the process sampling point and conveying the sample solution to the sample chamber, and the first control valve is used for controlling the communication or closing of the sampling pump and the sample chamber;
The liquid level meter is positioned inside the sample chamber, the liquid level meter, the first control valve and the sampling pump are all in electrical signal connection with the control main body, the liquid level meter is used for detecting liquid level information in the sample chamber and conveying the liquid level information to the control main body, and the control main body correspondingly controls the opening and closing of the sampling pump and the first control valve.
In a preferred embodiment of the invention, the sampling mechanism further comprises a second control valve and an evacuation valve;
the sampling pump is communicated with the process sampling point through a second pipeline, the second pipeline is communicated with the first pipeline, the end part of the second pipeline is positioned between the sampling pump and the first control valve, the second control valve is positioned on the second pipeline, and the second control valve is used for communicating or closing the second pipeline so as to adjust the solution pumped by the sampling pump through the first pipeline to flow back to the process sampling point through the second pipeline;
the evacuation valve is arranged on the sample chamber and is used for controlling the discharge of the sample solution in the sample chamber.
In a preferred embodiment of the invention, the measuring mechanism comprises a first syringe pump, a color sensor, a titration cup, a first dosing pump, a doser and a second syringe pump;
The titration cup is communicated with the sample chamber through the first injection pump, the color sensor, the first dosing pump, the quantitative feeder and the second injection pump are all in electrical signal connection with the control main body, and the control main body is used for controlling the first injection pump to quantitatively extract a sample solution from the sample chamber;
the titration cup is communicated with the shielding buffer reagent storage mechanism through the first metering pump, and the control main body is used for controlling the first metering pump to add the shielding buffer reagent into the titration cup;
the quantitative feeder is pre-stored with a solid indicator, and is communicated with the titration cup, and is used for quantitatively adding the solid indicator into the titration cup;
the titration cup is communicated with the EDTA standard solution storage mechanism through the second injection pump, and the control main body is used for controlling the second injection pump to titrate and add the EDTA standard solution into the titration cup;
the color sensor is positioned on one side of the titration cup, and is used for acquiring the ratio information of the R, G, B component of the color in the sample solution in the titration cup and transmitting the information to the control main body.
In a preferred embodiment of the present invention, the doser includes a drive body, a feed bin, a feed shaft, a limiting sleeve, and a blanking collector;
the feeding box is internally pre-stored with a solid indicator, and the solid indicator comprises solid powder prepared by mixing ammonium purple urea and sodium chloride;
the driving main body and the blanking material collector are respectively positioned at two opposite sides of the feeding box body, the feeding shaft is positioned in the feeding box body, the feeding shaft penetrates through the feeding box body and is in transmission connection with the driving main body, a discharging hole is formed in one side, close to the blanking material collector, of the feeding box body, the limiting shaft sleeve is in sealing connection with the discharging hole, a quantitative through hole is formed in the feeding shaft, the feeding shaft is in matched connection with the limiting shaft sleeve, the limiting shaft sleeve can be sleeved outside the feeding shaft, and the quantitative through hole is positioned outside the limiting shaft sleeve;
the driving main body is used for driving the feeding shaft to reciprocate along the feeding box body, the feeding shaft is used for accommodating quantitative solid indicators into the limiting shaft sleeve through the quantitative through holes, the driving main body can drive the feeding shaft to extend out of the feeding box body so that the quantitative through holes extend out of the limiting shaft sleeve, the quantitative solid indicators accommodated by the quantitative through holes fall into the discharging collector, and the discharging collector is communicated with the titration cup so as to convey the received solid indicators into the titration cup.
In a preferred embodiment of the invention, the measuring mechanism further comprises a second dosing pump, a liquid discharge pump and a stirrer;
the titration cup is communicated with an external water source through the second metering pump, the second metering pump is in electric signal connection with the control main body, and the control main body is used for controlling the second metering pump to dilute the titration cup by adding water;
the liquid discharging pump is communicated with the titration cup, and the liquid discharging pump and the second dosing pump are used for discharging liquid and flushing the titration cup for completing detection and analysis of the sample solution.
According to the nickel and cobalt ion concentration online analysis method provided by the invention, a color measurement model is established before measurement, and a nonlinear regression model of the nickel and cobalt ion concentration and solution color R, G, B component proportion and the total content of nickel and cobalt is established according to the principle that the component proportion of the combined color R, G, B is determined in advance according to the ion concentration proportion when nickel and cobalt ions coexist in a color soft measurement mode; the method has the advantages that the sample solution to be measured is extracted on line through the process sampling point, the color measurement is carried out on the initial sample solution, the proportion value of nickel and cobalt ions in the initial sample solution is regressed according to the color measurement model, the total content of cobalt and nickel is measured by using the EDTA complexation titration method, the concentration of nickel and cobalt ions is calculated based on the total content of nickel and cobalt ions, and the technical problems that the on-line detection technology and the instrument in the prior art can not simultaneously measure the concentration of nickel and cobalt ions in the nickel and cobalt solvent extraction process, and the EDTA titration method can only measure the total concentration of nickel and cobalt ions, and can not simultaneously realize the detection of the respective concentrations of nickel and cobalt ions are solved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the overall structure of an on-line analysis instrument for nickel and cobalt ion concentration provided by an embodiment of the invention;
FIG. 2 is a schematic diagram of the structure of a quantitative feeder of an on-line analysis instrument for nickel and cobalt ion concentration according to an embodiment of the present invention;
FIG. 3 is a schematic diagram of the structure of the quantitative feeder of the nickel and cobalt ion concentration online analysis instrument provided by the embodiment of the invention during feeding;
fig. 4 is a schematic structural diagram of a quantitative feeder of the nickel and cobalt ion concentration online analysis instrument in discharging.
Icon: 100-process sampling points; 200-a sampling mechanism; 201-sample chamber; 202-a sampling pump; 212-a first line; 222-a second line; 203-a first control valve; 204-level gauge; 205-a second control valve; 206-an evacuation valve; 300-measuring mechanism; 301-a first syringe pump; 302-a color sensor; 303-titration cup; 304-a first metering pump; 305-a doser; 315-driving the body; 325-feeding box body; 335-a feed shaft; 3351-quantitative through-hole; 345-limited bushing; 355-blanking collector; 306-a second syringe pump; 307-a second metering pump; 308-a liquid discharge pump; 309-stirrer.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
As shown in fig. 1 to 4, the method for on-line analysis of nickel and cobalt ion concentration provided in this embodiment includes the following steps: establishing a color measurement model, and establishing a nonlinear regression model of the concentration ratio of nickel and cobalt ions to the component proportion of the color R, G, B of the solution and the total content of nickel and cobalt by utilizing data according to the RGB proportion of the color components of nickel and cobalt ions in the solution and the total content of nickel and cobalt; extracting a sample solution to be measured on line at a process sampling point 100; carrying out color measurement on the initial sample solution, and regressing the proportion value of nickel and cobalt ions in the initial sample solution according to a color measurement model; quantitatively sampling the extracted sample to be measured to form an initial sample solution; adding a shielding buffer reagent to the initial sample to form a first sample solution; adding a solid indicator to the first sample solution to form a second sample solution, wherein the solid indicator comprises an ammonium purple urea indicator; titrating the second sample solution by adopting the EDTA standard solution, measuring the ratio information of the R, G, B component of the color in the solution in real time in the titration process, stopping the titration when the color information has a color variation point, and recording the volume of the consumed EDTA standard solution; the concentration of nickel and cobalt ions is calculated based on the total content of nickel and cobalt ions.
It should be noted that, the online analysis method for nickel and cobalt ion concentration provided in this embodiment can combine the EDTA complexometric titration method (also referred to as "ethylenediamine tetraacetic acid titration method", EDTA, ethylenediamine tetraacetic acid) with the color soft measurement, and obtain the nickel and cobalt ion concentration in the sample solution online through modeling calculation, so as to realize the synchronous online detection of the nickel and cobalt ion concentration in the nickel and cobalt extraction production process; specifically, since nickel and cobalt ions have respective colors in a solution (the color of nickel ions in water is green, and the color of cobalt ions in an aqueous solution is pink), when nickel and cobalt ions form a solution with different ion concentrations, the color of the solution is a combined color of the two colors, and the component ratio of the combined color R, G, B is determined by the concentration ratio of the two ions, and by pre-proportioning nickel and cobalt ion solutions with different concentration ratios and performing color measurement on the nickel and cobalt ion solutions with different concentration ratios, a nonlinear regression model of the concentration ratio of nickel and cobalt ions to the solution color R, G, B and the total content of nickel and cobalt is established in a computer according to corresponding data; further, the following nickel and cobalt ion concentration online analysis instrument is installed near the process sampling point 100, the sample solution to be measured is extracted online from the process sampling point 100, the sample solution to be measured is extracted quantitatively according to the instrument measurement standard, an initial sample solution is formed, namely, the total volume of the initial sample solution is known at the moment, the color measurement is carried out on the initial sample solution, and the proportion value of nickel and cobalt ions in the initial sample solution is regressed according to the color measurement model; the shielding buffer reagent and the solid indicator are sequentially added into the initial sample solution, wherein the shielding buffer reagent can form shielding for Ca, mg, cu, fe plasma existing in the sample solution, and meanwhile, the pH value in the titration process is stabilized, so that the color change in the EDTA titration process is more obvious; the solid indicator comprises an ammonium purple urea indicator which improves the color development effect in the EDTA titration process; finally, through carrying out EDTA standard solution titration on the second sample solution, when the color is mutated in the titration process, namely the titration end point, the total content of nickel and cobalt ions can be automatically calculated through inputting an EDTA complexation titration formula in advance in a computer; the independent concentrations of the nickel ions and the cobalt ions are calculated by multiplying the total content of the nickel ions and the cobalt ions by the corresponding proportion of the nickel ions and the cobalt ions respectively, so that the limitation that the properties of the nickel ions and the cobalt ions are similar and cannot be synchronously measured is solved, and a foundation is laid for process monitoring and automatic control of the nickel and cobalt extraction production flow.
Calculating the total content of nickel and cobalt ions based on an EDTA complexometric titration formula;
the calculation formula is as follows:
；
wherein X: the sum (wt%) of the nickel and cobalt contents in the sample; v (V) 1 : titration experiments consume the volume (mL) of EDTA standard solution; v (V) 0 : blank runs consumed the volume (mL) of EDTA standard solution; c: actual concentration (mol/L) of EDTA standard titration solution; m: the weight (g) of the sample contained in the second sample solution; m: theoretical molar mass (g/mol) of nickel cobalt; e: total sample solution volume (mL) of the initial sample solution; f: sample solution volume (mL) of the second sample solution.
Wherein V is 1 Can be known at the titration end point, V 0 And the values of C can be found experimentally before measurement, M and M can be found prior to sampling from the sample solution, and E and F can be found separately after sampling from the sample solution.
According to the nickel and cobalt ion concentration online analysis method provided by the embodiment, a color measurement model is established before measurement, a nonlinear regression model of nickel and cobalt ion concentration and solution color R, G, B component proportion and total nickel and cobalt content is established according to the principle that the proportion of the combined color R, G, B component is determined in advance according to the ion concentration proportion when nickel and cobalt ions coexist in a color soft measurement mode; the sample solution to be measured is extracted on line through the process sampling point 100, the color measurement is carried out on the initial sample solution, the proportion value of nickel and cobalt ions in the initial sample solution is regressed according to the color measurement model, the total content of cobalt and nickel is measured by utilizing the EDTA complexometric titration method, the concentration of nickel and cobalt ions is calculated based on the total content of nickel and cobalt ions respectively, and the technical problems that the on-line detection technology and the instrument in the prior art can not simultaneously measure the concentration of nickel and cobalt ions in the nickel and cobalt solvent extraction process, and the EDTA titration method can only measure the total concentration of nickel and cobalt ions and can not simultaneously realize the detection of the respective concentrations of nickel and cobalt ions are solved.
Further, in a preferred embodiment of the present invention, the step of establishing a color measurement model includes: the proportion of the components of the combined color R, G, B is determined based on the proportion of the ion concentration when nickel and cobalt ions coexist, the ratio is influenced R, G, B by the color measurement principle, and the ratio is influenced by the color shade, namely the total concentration of the ions, and nickel and cobalt mixed solutions with different concentration proportions are sequentially prepared according to gradients under the condition of fixed light sources; and measuring the nickel and cobalt mixed solution with each concentration ratio to obtain the color R, G, B component ratio of the nickel and cobalt mixed solution with corresponding concentration ratio and different ion contents, and obtaining a nonlinear regression model of the nickel and cobalt ion concentration ratio and the solution color R, G, B component ratio and the total ion content of the nickel and cobalt by utilizing data modeling.
In this embodiment, in order to ensure accuracy of modeling, under the condition of a fixed light source, nickel and cobalt mixed solutions with different concentration ratios are sequentially prepared according to gradients, each concentration ratio of nickel and cobalt mixed solution is correspondingly measured with a color R, G, B component ratio, data modeling can be performed on a computer through a large number of supports to obtain a proportional relationship between the concentration ratio of nickel and cobalt ions and the solution color R, G, B component ratio, and further a nonlinear regression model of the concentration ratio of nickel and cobalt ions and the solution color R, G, B component ratio and total content of nickel and cobalt is obtained, namely, on the basis that the solution color R, G, B component ratio is known, the corresponding concentration ratio of nickel and cobalt ions is obtained through the nonlinear regression model.
In a preferred embodiment of the present invention, the method further comprises the steps of: the initial sample solution is stored in a titration cup 303; color information measurement is carried out on the water solution stored in the titration cup 303, and a reference background value of the titration cup 303 is obtained; and subtracting the reference background value from the ratio information of the components of the color R, G, B in the solution when the color information appears in the color variation point, and obtaining the respective ratio information of the three components of the color R, G, B of the sample.
In this embodiment, the titration cup 303 is used as a storage container for a sample solution, the titration cup 303 can be made of a material with high light transmittance, before the sample solution is measured, the ratio of R, G, B components of the color when the aqueous solution is stored in the titration cup 303 is measured, that is, the color information of the aqueous solution of the titration cup 303 is obtained and used as a reference background value, when the ratio of R, G, B components of the color at the end point of titration is measured, the reference background value is subtracted, and then the non-linear regression model is input, so that errors caused by the reference background value of the titration cup 303 can be better avoided, and the accuracy of calculating the concentration of nickel and cobalt ions can be better improved.
In a preferred embodiment of the present invention, the method further comprises the steps of: and (3) adding water to dilute the initial sample solution, and adding a shielding buffer reagent to the diluted initial sample solution to form a first sample solution.
In this embodiment, after the sample solution is quantitatively pumped into the titration cup 303, the initial sample solution may be diluted with water, the dilution factor may be 50-100 times, and the reaction speed in the EDTA titration process in the subsequent step may be increased by diluting the initial sample.
In a preferred embodiment of the present invention, the step of formulating the shielding buffer comprises: preparing an ammonia-ammonium chloride buffer solution with the pH range of 9-11; fluoride, sodium thiosulfate and tartaric acid are sequentially added to the ammonia-ammonium chloride buffer solution corresponding to the impurity components of the initial sample solution.
In this embodiment, 5-10ml of shielding buffer reagent can be added to shield Ca, mg, cu, fe plasma in the sample solution, and stabilize the pH value in the titration process, so that the color change in the EDTA titration process is more obvious. The shielding buffer reagent is generally prepared into an ammonia-ammonium chloride buffer solution with the pH value of 10, and the shielding buffer reagent is used for avoiding the increase of acidity of a titration solution, reducing a condition constant, reducing the reaction completeness, influencing the color changing point of an indicator and the self color, leading to the increase of an end point error, then, shielding reagents such as fluoride, sodium thiosulfate, tartaric acid and the like can be added, and the specific selection of the shielding reagent can be determined and added according to the actual impurity ion components in a sample solution.
In a preferred embodiment of the present invention, the method further comprises the steps of: and (5) draining and flushing the equipment for completing the detection and analysis of the sample solution.
In this embodiment, after the measurement and analysis of the sample solution are completed, the titration cup 303 is cleaned by clean water to wait for the next measurement, so that the service life of the whole device is ensured.
As shown in fig. 1 to 4, the nickel and cobalt ion concentration online analysis instrument applied to the nickel and cobalt ion concentration online analysis method provided in this embodiment includes: a sampling mechanism 200, a measuring mechanism 300, and a control body; the sampling mechanism 200 comprises a sample chamber 201, the sampling mechanism 200 is used for being installed at the process sampling point 100, and the sampling mechanism 200 can extract a sample solution to be measured on line and convey the sample solution into the sample chamber 201; the measuring mechanism 300 is communicated with the sample chamber 201, the measuring mechanism 300 is used for quantitatively extracting the sample solution from the sample chamber 201 to form an initial sample solution, and the measuring mechanism 300 is used for measuring the total content of nickel and cobalt ions in the initial sample solution based on an EDTA complexometric titration method; the control main body is in electric signal connection with the measuring mechanism 300, the control main body is pre-established with a color measuring model, and the control main body is used for returning the proportion value of the nickel and cobalt ions in the initial sample solution according to the color measuring model corresponding to the total content of the nickel and cobalt ions in the initial sample solution so as to calculate the concentration of the nickel and cobalt ions respectively.
Alternatively, the control body may be various, for example: a single chip microcomputer, a computer or a PLC, etc., preferably, the control main body may be a computer with a display screen, and the computer may have a plurality of buttons thereon, and the various components of the sampling mechanism 200 and the measuring mechanism 300 are controlled by controlling the different buttons.
In this embodiment, the sampling mechanism 200 may pump the sample solution at the process sampling point 100 through a pipeline, so as to convey the sample solution in the process flow into the sample chamber 201; the measuring device can quantitatively extract the sample solution from the sample chamber 201, the color R, G, B component proportion measurement is carried out on the extracted sample solution, the titration measurement on the sample solution is completed through the EDTA complexometric titration method, the control main body can receive the data of the measuring device in the color measurement and titration process, the total content of nickel and cobalt ions is calculated according to the EDTA complexometric titration formula, the proportion of nickel and cobalt ions in the sample solution is regressed according to the color R, G, B component proportion, and finally the concentration values of the nickel ions and the cobalt ions in the sample solution are obtained through automatic calculation.
In the preferred embodiment of the present invention, sampling mechanism 200 includes a sampling pump 202, a first control valve 203, and a level gauge 204; the sampling pump 202 is communicated with the process sampling point 100 through a first pipeline 212, the sampling pump 202 is communicated with the sample chamber 201 through a first control valve 203, the sampling pump 202 is used for pumping a sample solution to be measured in the process sampling point 100 and delivering the sample solution to the sample chamber 201, and the first control valve 203 is used for controlling the communication or closing of the sampling pump 202 and the sample chamber 201; the liquid level meter 204 is located inside the sample chamber 201, the liquid level meter 204, the first control valve 203 and the sampling pump 202 are all connected with the control main body through electric signals, the liquid level meter 204 is used for detecting liquid level information in the sample chamber 201 and conveying the liquid level information to the control main body, and the control main body correspondingly controls the opening and closing of the sampling pump 202 and the first control valve 203.
In this embodiment, the sampling pump 202 is installed near the process sampling point 100, and the sampling pump 202 may be a hose pump, and the flow rate range of the hose pump may be 1-2L/Min; the sampling pump 202 is communicated with the process sampling point 100 through the first pipeline 212, the first control valve 203 can adopt a gas control valve lined with tetrafluoro, when sampling detection analysis is required to be carried out on the solution discharged from the process sampling point 100, the sampling pump 202 sucks sample solution into the sample chamber 201 through the first pipeline 212 by opening the sampling pump 202 and the first control valve 203, the liquid level meter 204 can carry out liquid level detection on the sample solution in the sample chamber 201, namely, after the liquid level meter 204 detects that the liquid level in the sample chamber 201 reaches the position of the liquid level meter 204, the control main body correspondingly controls the sampling pump 202 and the first control valve 203 to be closed, and the sampling of the sample solution is completed.
In a preferred embodiment of the present invention, the sampling mechanism 200 further comprises a second control valve 205 and an evacuation valve 206; the sampling pump 202 is communicated with the process sampling point 100 through a second pipeline 222, the second pipeline 222 is communicated with the first pipeline 212, the end part of the second pipeline 222 is positioned between the sampling pump 202 and the first control valve 203, the second control valve 205 is positioned on the second pipeline 222, and the second control valve 205 is used for communicating or closing the second pipeline 222 so as to regulate the solution pumped by the sampling pump 202 through the first pipeline 212 to flow back to the process sampling point 100 through the second pipeline 222; an evacuation valve 206 is mounted on the sample chamber 201, the evacuation valve 206 being used to control the evacuation of the sample solution from the sample chamber 201.
In this embodiment, the second control valve 205 may also be a gas-controlled valve lined with tetrafluoro, where the second control valve 205 may control the sampling pump 202 to pump the sample solution back, i.e. the sampling pump 202 is in circulation communication with the process sampling point 100 through the first pipeline 212 and the second pipeline 222, respectively, and the second control valve 205 is located between the sampling pump 202 and the first control valve 203, when the analyzer opens the sampling flow, the sampling pump 202 and the second control valve 205 are opened, the first control valve 203 is closed, and when the process sample solution is pumped by the sampling pump 202 and then returned to the process flow through the second control valve 205, after waiting for fresh solution in the process flow to be delivered to the process sampling point 100, the second control valve 205 is closed, the first control valve 203 is opened, and the sampling pump 202 delivers the sample to be detected to the sample chamber 201.
Further, the evacuation valve 206 can also be a gas-controlled valve lined with tetrafluoro, the sample chamber 201 can be designed with a lower port, the evacuation valve 206 is positioned at the bottom of the sample chamber 201, and the evacuation valve 206 can control the discharge of the sample solution in the sample chamber 201; the liquid level meter 204 may be a tuning fork type liquid level meter 204, the tuning fork switch is made of 316L material and is coated with ECTFE (ethylene chlorotrifluoroethylene copolymer) coating, the sampling pump 202 and the first control valve 203 are always in an open state in the sampling process, when the liquid level meter 204 detects a liquid level signal for the first time, the sampling pump 202 and the first control valve 203 are closed, at this time, the control main body opens the evacuation valve 206, fresh sample solution can drain old sample remained in the sample chamber 201 in the last measurement, and then the sampling pump 202 and the first control valve 203 are opened again until the sampling pump 202 and the first control valve 203 are closed after the liquid level meter 204 detects the liquid level signal again, and sampling of the sample solution is completed; when the measurement is finally completed, the evacuation valve 206 is opened to completely evacuate the remaining solution from the sample chamber 201.
In the preferred embodiment of the present invention, the measurement mechanism 300 includes a first syringe pump 301, a color sensor 302, a titration cup 303, a first dosing pump 304, a doser 305, and a second syringe pump 306; the titration cup 303 is communicated with the sample chamber 201 through a first syringe pump 301, and the first syringe pump 301, the color sensor 302, the first dosing pump 304, the quantitative feeder 305 and the second syringe pump 306 are all electrically connected with a control main body, wherein the control main body is used for controlling the first syringe pump 301 to quantitatively extract the sample solution from the sample chamber 201 in a quantitative manner; the titration cup 303 is communicated with the shielding buffer reagent storage mechanism through a first dosing pump 304, and the control main body is used for controlling the first dosing pump 304 to add shielding buffer reagent into the titration cup 303; the solid indicator is pre-stored in the quantitative feeder 305, the quantitative feeder 305 is communicated with the titration cup 303, and the quantitative feeder 305 is used for quantitatively adding the solid indicator into the titration cup 303; the titration cup 303 is communicated with the EDTA standard solution storage mechanism through a second injection pump 306, and the control main body is used for controlling the second injection pump 306 to titrate and add the EDTA standard solution into the titration cup 303; the color sensor 302 is located on one side of the titration cup 303, and the color sensor 302 is used for acquiring the ratio information of the color R, G, B component in the sample solution in the titration cup 303 and transmitting the information to the control main body.
In this embodiment, the first syringe pump 301 may be a high-precision syringe pump, the resolution and the measurement precision are better than 0.01ml, and the sample loading amount can be flexibly selected according to the sample concentration; the color sensor 302 can adopt a high-precision color sensor 302, the color sensor 302 can acquire the respective ratio information of the solution color R, G, B, the titration cup 303 can adopt a quartz material, and the characteristics of colorless and high light transmittance are achieved; the first dosing pump 304 may be a peristaltic pump, which can ensure that the amount of shielding buffer agent added in a single pass is 5-10ml; the second syringe pump 306 may sequentially titrate the EDTA standard solution; wherein, the shielding buffer reagent storage mechanism can contain the shielding buffer reagent prepared in advance, the EDTA standard solution storage mechanism can also contain the EDTA standard solution prepared in advance, and the preparation method of the EDTA standard solution belongs to the conventional mode in the field, and is not limited in this regard; the dosage of the sample solution is controlled by the high-precision injection pump and the dosage of the solid indicator is controlled by the quantitative feeder 305 to be matched for use, so that the concentration measuring range of nickel and cobalt ions is enlarged, and the industrial field applicability is strong.
In the preferred embodiment of the present invention, the doser 305 includes a drive body 315, a feed box 325, a feed shaft 335, a limiting sleeve 345, and a feed collector 355; the feed box 325 is pre-stored with a solid indicator, and the solid indicator comprises solid powder prepared by mixing ammonium purple urea and sodium chloride; the driving main body 315 and the blanking collector 355 are respectively positioned at two opposite sides of the feeding box body 325, the feeding shaft 335 is positioned in the feeding box body 325, the feeding shaft 335 penetrates through the feeding box body 325 and is in transmission connection with the driving main body 315, a discharging hole is formed in one side, close to the blanking collector 355, of the feeding box body 325, the limiting shaft sleeve 345 is in sealing connection with the discharging hole, the feeding shaft 335 is provided with a quantitative through hole 3351, the feeding shaft 335 is in matched connection with the limiting shaft sleeve 345, the limiting shaft sleeve 345 can be sleeved outside the feeding shaft 335, and the quantitative through hole 3351 is positioned outside the limiting shaft sleeve 345; the driving body 315 is used for driving the feeding shaft 335 to reciprocate along the feeding box 325, the feeding shaft 335 is used for accommodating a fixed amount of solid indicator through the fixed amount through hole 3351 and extending into the limiting shaft sleeve 345, the driving body 315 can drive the feeding shaft 335 to extend out of the feeding box 325, so that the fixed amount through hole 3351 extends out of the limiting shaft sleeve 345, the fixed amount of solid indicator accommodated by the fixed amount through hole 3351 falls into the blanking collector 355, and the blanking collector 355 is communicated with the titration cup 303 to convey the received solid indicator into the titration cup 303.
It should be noted that, the doser 305 may be a micro doser 305 to ensure that the ammonium violaceum indicator is added, because the ammonium violaceum solution is very easy to be destructed and lose efficacy in air, the traditional mode of adding the prepared reagent is not suitable for the requirement of an on-line instrument, and the accurate addition of the solid indicator can ensure that the ammonium violaceum indicator is added on line in real time, wherein the solid indicator can be a solid powder indicator prepared by mixing ammonium violaceum and sodium chloride, the doser 305 ensures that the solid powder is added, the single addition amount of the doser 305 can be 0.5g, and the addition accuracy is better than 5%.
In this embodiment, the pre-prepared solid indicator may be accommodated in the feed box 325, and the inside of the feed box 325 is in a sealed state, where the driving main body 315 may adopt a driving cylinder, and a limit shaft sleeve may be disposed in a sealing manner at one end of the feed shaft 335 penetrating through the feed box 325 and connected to the driving main body 315, the limit shaft sleeve may be connected to the feed box 325 in a sealing manner, the feed shaft 335 penetrates through the limit shaft sleeve, and the feed shaft 335 is connected to the limit shaft sleeve in a sliding manner in a matching manner, i.e. the feed shaft 335 may reciprocate relative to the limit shaft sleeve under the driving of the driving main body 315, and likewise, the limit shaft sleeve 345 penetrates through the discharge hole and the feed box 325 in a sealing manner, the feed shaft 335 penetrates through the limit shaft sleeve 345, and the feed shaft 335 and the limit shaft sleeve 345 are connected in a sliding manner in a matching manner, i.e. the feed shaft 335 may reciprocate relative to the limit shaft sleeve 345 under the driving of the driving main body 315, wherein a gap is arranged between the limiting shaft sleeve 345 and the limiting shaft sleeve, the gap range of the limiting shaft sleeve 345 and the limiting shaft sleeve is larger than the extension length of the quantitative through hole 3351, when the feeding shaft 335 is positioned in the feeding box 325, the quantitative through hole 3351 is used for accommodating the solid indicator, when the driving main body 315 drives the feeding shaft 335 to move towards one end extending out of the limiting shaft sleeve 345, the quantitative through hole 3351 enters into the limiting sleeve, namely, the quantitative through hole 3351 carries the solid indicator with the volume of the quantitative through hole 3351 into the limiting sleeve, when the driving main body 315 continuously drives the feeding shaft 335 to extend, after the quantitative through hole 3351 extends out of the limiting sleeve, the solid indicator in the quantitative through hole 3351 can fall into the blanking collector 355 under the action of gravity, and enters into the titration cup 303 through the conveying of the blanking collector 355 to finish the quantitative feeding of the solid indicator, meanwhile, the technical problem that the ammonium purple urea solution is easy to be deformed and invalid in the air can be avoided.
Optionally, the quantitative feeder 305 may further include a stirring shaft, a vibrator and a heating plate, where the stirring shaft may be detachably connected with the feeding shaft 335, and the stirring shaft may be of a T-shaped structure, and the stirring shaft may stir the solid indicator in the feeding box 325 along with the reciprocating movement of the feeding shaft 335, so as to play a role in stirring and breaking an arch, and prevent the powder material from bridging the arch, where a position of the limiting sleeve corresponding to the stirring shaft may be provided with a groove, and the stirring shaft may reciprocate along the groove; the vibrator is connected with the blanking collector 355, the blanking collector 355 can be of a conical structure, the outlet end is positioned at the bottom of the conical structure, the outlet end is connected with the titration cup 303, and the blanking collector 355 can be formed by natural rubber; the vibrator is arranged on the side wall of the blanking collector 355, when the solid indicator falls into the blanking collector 355, the vibrator starts to vibrate with the blanking collector 355, so that materials are prevented from being stuck on the side wall of the blanking collector 355, the materials are ensured to fall into the titration cup 303 completely, and the materials are prevented from being stuck and blocked; the heating sheet can be fixedly arranged on the outer side wall of the feed box 325, and the solid indicator powder can be controlled to be at a temperature of about 70 ℃, so that the solid indicator powder is prevented from being adhered to the side wall in a wet manner under a severe industrial environment and the color development is reduced.
Optionally, the quantitative feeder 305 may further include an adjusting block, where the adjusting block can be connected to the quantitative through hole 3351, and is installed inside the quantitative through hole 3351 by the adjusting block, so as to adjust the volume of the quantitative through hole 3351, so as to adjust the content of the solid indicator contained in the quantitative through hole 3351 in a single time; for example, the quantitative through hole 3351 may be a square hole for aggregate and feeding, wherein an adjusting block with quantitative specification can be added to the inner side wall of the square hole, and the addition amount of the solid indicator can be controlled to be 0.5g and 1g by changing the volume of the square hole, so that the range of the concentration of the measured solution with larger span can be suitable.
In the preferred embodiment of the present invention, the measuring mechanism 300 further includes a second dosing pump 307, a liquid discharge pump 308, and a stirrer 309; the titration cup 303 is communicated with an external water source through a second dosing pump 307, the second dosing pump 307 is electrically connected with a control main body, and the control main body is used for controlling the second dosing pump 307 to dilute the titration cup 303 by adding water; a drainage pump 308 is in communication with the titration cup 303, and the drainage pump 308 and the second dosing pump 307 are used to drain and rinse the titration cup 303 that completes the sample solution detection analysis.
In this embodiment, a peristaltic pump may be used as the second dosing pump 307, tap water can be added into the titration cup 303 to dilute by using the second dosing pump 307, the water adding range of the second dosing pump 307 may be adjusted in advance according to the control main body, so that the dilution multiple may be 50-100 times, and the reaction speed in the EDTA titration process in the subsequent step may be accelerated by diluting the initial sample; the liquid discharge pump 308 can also adopt a peristaltic pump, wherein the liquid discharge pump 308 can be matched with the second metering pump 307 for use, and after the liquid discharge pump 308 is used for discharging the solution in the titration cup 303, the second metering pump 307 is used for flushing the interior of the titration cup 303 and waiting for the next measurement; wherein, the pump pipes of the first dosing pump 304, the second dosing pump 307 and the liquid discharge pump 308 can use chemical pipes, thereby prolonging the service life.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (12)
1. The on-line analysis method for the concentration of nickel and cobalt ions is characterized by comprising the following steps:
establishing a color measurement model, and establishing a nonlinear regression model of the concentration ratio of nickel and cobalt ions to the component proportion of the color R, G, B of the solution and the total content of nickel and cobalt by utilizing data according to the RGB proportion of the color components of nickel and cobalt ions in the solution and the total content of nickel and cobalt;
extracting a sample solution to be measured on line at a process sampling point (100);
quantitatively sampling the extracted sample to be measured to form an initial sample solution;
carrying out color measurement on the initial sample solution, and regressing the proportion value of nickel and cobalt ions in the initial sample solution according to a color measurement model;
Adding a shielding buffer reagent to the initial sample to form a first sample solution;
adding a solid indicator to the first sample solution to form a second sample solution, wherein the solid indicator comprises an ammonium purple urea indicator;
titrating the second sample solution by adopting the EDTA standard solution, measuring the ratio information of the R, G, B component of the color in the solution in real time in the titration process, stopping the titration when the color information has a color variation point, and recording the volume of the consumed EDTA standard solution;
calculating the total content of nickel and cobalt ions based on an EDTA complexometric titration formula;
the concentration of nickel and cobalt ions is calculated based on the total content of nickel and cobalt ions.
2. The method for online analysis of nickel and cobalt ion concentration according to claim 1, wherein the step of establishing a color measurement model comprises:
determining the proportion of the components of the combined color R, G, B based on the ion concentration proportion when nickel and cobalt ions coexist, and sequentially preparing nickel and cobalt mixed solutions with different concentration proportions according to gradients under the condition of fixed light sources;
and measuring the nickel and cobalt mixed solution with each concentration ratio to obtain the color R, G, B component ratio of the nickel and cobalt mixed solution with the corresponding concentration ratio, and modeling by using data to obtain a nonlinear regression model of the nickel and cobalt ion concentration ratio and the solution color R, G, B component ratio and the total nickel and cobalt ion content.
3. The method for on-line analysis of nickel and cobalt ion concentration according to claim 1, further comprising the steps of:
storing an initial sample solution in a titration cup (303);
performing color information measurement on the water solution stored in the titration cup (303) to obtain a reference background value of the titration cup (303);
and subtracting the reference background value from the ratio information of the components of the color R, G, B in the solution when the color information appears in the color variation point, and obtaining the respective ratio information of the three components of the color R, G, B of the sample.
4. The method for on-line analysis of nickel and cobalt ion concentration according to claim 2, further comprising the steps of:
and (3) adding water to dilute the initial sample solution, and adding a shielding buffer reagent to the diluted initial sample solution to form a first sample solution.
5. The method for on-line analysis of nickel and cobalt ion concentration according to claim 4, wherein the step of preparing a shielding buffer reagent comprises:
preparing an ammonia-ammonium chloride buffer solution with the pH range of 9-11;
fluoride, sodium thiosulfate and tartaric acid are sequentially added to the ammonia-ammonium chloride buffer solution corresponding to the impurity components of the initial sample solution.
6. The method for on-line analysis of nickel and cobalt ion concentration according to any one of claims 1 to 5, further comprising the steps of:
And (5) draining and flushing the equipment for completing the detection and analysis of the sample solution.
7. A nickel and cobalt ion concentration on-line analyzer applied to the nickel and cobalt ion concentration on-line analysis method according to any one of claims 1 to 6, comprising: a sampling mechanism (200), a measuring mechanism (300) and a control body;
the sampling mechanism (200) comprises a sample chamber (201), the sampling mechanism (200) is used for being installed at a process sampling point (100), and the sampling mechanism (200) can extract a sample solution to be measured on line and convey the sample solution into the sample chamber (201);
the measuring mechanism (300) is communicated with the sample chamber (201), the measuring mechanism (300) is used for quantitatively extracting a sample solution from the sample chamber (201) to form an initial sample solution, and the measuring mechanism (300) is used for measuring the total content of nickel and cobalt ions in the initial sample solution based on an EDTA complexometric titration method;
the control main body is in electrical signal connection with the measuring mechanism (300), a color measuring model is pre-established on the control main body, and the control main body is used for returning out the proportion values of nickel and cobalt ions in the initial sample solution according to the color measuring model corresponding to the total content of nickel and cobalt ions in the initial sample solution so as to respectively calculate the concentration of the nickel and cobalt ions.
8. The nickel and cobalt ion concentration online analysis instrument according to claim 7, wherein the sampling mechanism (200) comprises a sampling pump (202), a first control valve (203) and a liquid level meter (204);
the sampling pump (202) is communicated with a process sampling point (100) through a first pipeline (212), the sampling pump (202) is communicated with the sample chamber (201) through the first control valve (203), the sampling pump (202) is used for extracting a sample solution to be measured in the process sampling point (100) and conveying the sample solution to the sample chamber (201), and the first control valve (203) is used for controlling the communication or closing of the sampling pump (202) and the sample chamber (201);
the liquid level meter (204) is located inside the sample chamber (201), the liquid level meter (204), the first control valve (203) and the sampling pump (202) are all connected with the control main body through electric signals, the liquid level meter (204) is used for detecting liquid level information in the sample chamber (201) and conveying the liquid level information to the control main body, and the control main body correspondingly controls the opening and closing of the sampling pump (202) and the first control valve (203).
9. The nickel and cobalt ion concentration online analysis instrument according to claim 8, wherein the sampling mechanism (200) further comprises a second control valve (205) and an evacuation valve (206);
the sampling pump (202) is communicated with the process sampling point (100) through a second pipeline (222), the second pipeline (222) is communicated with the first pipeline (212), the end part of the second pipeline (222) is positioned between the sampling pump (202) and the first control valve (203), the second control valve (205) is positioned on the second pipeline (222), and the second control valve (205) is used for communicating or closing the second pipeline (222) so as to adjust the solution pumped by the sampling pump (202) through the first pipeline (212) to flow back to the process sampling point (100) through the second pipeline (222);
the evacuation valve (206) is mounted on the sample chamber (201), and the evacuation valve (206) is used for controlling the discharge of the sample solution in the sample chamber (201).
10. The nickel and cobalt ion concentration online analysis instrument according to any one of claims 7-9, wherein the measurement mechanism (300) comprises a first syringe pump (301), a color sensor (302), a titration cup (303), a first dosing pump (304), a doser (305), and a second syringe pump (306);
The titration cup (303) is communicated with the sample chamber (201) through the first injection pump (301), and the first injection pump (301), the color sensor (302), the first dosing pump (304), the quantitative feeder (305) and the second injection pump (306) are all electrically connected with the control main body, and the control main body is used for controlling the first injection pump (301) to quantitatively extract sample solution from the sample chamber (201);
the titration cup (303) is communicated with the shielding buffer reagent storage mechanism through the first dosing pump (304), and the control main body is used for controlling the first dosing pump (304) to add the shielding buffer reagent into the titration cup (303);
the quantitative feeder (305) is pre-stored with a solid indicator, the quantitative feeder (305) is communicated with the titration cup (303), and the quantitative feeder (305) is used for quantitatively adding the solid indicator into the titration cup (303);
the titration cup (303) is communicated with the EDTA standard solution storage mechanism through the second injection pump (306), and the control main body is used for controlling the second injection pump (306) to titrate and add the EDTA standard solution into the titration cup (303);
The color sensor (302) is located at one side of the titration cup (303), and the color sensor (302) is used for acquiring ratio information of the color R, G, B component in the sample solution in the titration cup (303) and transmitting the information to the control main body.
11. The nickel and cobalt ion concentration online analysis instrument according to claim 10, wherein the doser (305) comprises a drive body (315), a feed box (325), a feed shaft (335), a limiting sleeve (345), and a feed collector (355);
the feed box (325) is pre-stored with a solid indicator, and the solid indicator comprises solid powder prepared by mixing ammonium purple urea and sodium chloride;
the driving main body (315) and the discharging material collector (355) are respectively positioned at two opposite sides of the feeding box body (325), the feeding shaft (335) is positioned inside the feeding box body (325), the feeding shaft (335) penetrates through the feeding box body (325) to be in transmission connection with the driving main body (315), a discharging hole is formed in one side, close to the discharging material collector (355), of the feeding box body (325), the limiting shaft sleeve (345) is in sealing connection with the discharging hole, a quantitative through hole (3351) is formed in the feeding shaft (335), the feeding shaft (335) is in matched connection with the limiting shaft sleeve (345), the limiting shaft sleeve (345) can be sleeved outside the feeding shaft (335), and the quantitative through hole (3351) is positioned outside the limiting shaft sleeve (345);
The driving main body (315) is used for driving the feeding shaft (335) to move back and forth along the feeding box body (325), the feeding shaft (335) is used for enabling a quantitative solid indicator to be contained in the quantitative through hole (3351) to extend into the limiting shaft sleeve (345), the driving main body (315) can drive the feeding shaft (335) to extend out of the feeding box body (325), so that the quantitative through hole (3351) extends out of the limiting shaft sleeve (345), the quantitative solid indicator contained in the quantitative through hole (3351) falls into the blanking collector (355), and the blanking collector (355) is communicated with the titration cup (303) to convey the received solid indicator into the titration cup (303).
12. The nickel and cobalt ion concentration online analysis instrument according to claim 10, wherein the measurement mechanism (300) further comprises a second dosing pump (307), a liquid discharge pump (308), and a stirrer (309);
the titration cup (303) is communicated with an external water source through the second dosing pump (307), the second dosing pump (307) is electrically connected with the control main body, and the control main body is used for controlling the second dosing pump (307) to add water into the titration cup (303) for dilution;
The liquid discharge pump (308) is communicated with the titration cup (303), and the liquid discharge pump (308) and the second dosing pump (307) are used for performing liquid discharge flushing on the titration cup (303) which is used for completing sample solution detection analysis.
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