CN113916965A - Method for detecting content of magnetic substance in lithium ion battery positive electrode material - Google Patents
Method for detecting content of magnetic substance in lithium ion battery positive electrode material Download PDFInfo
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- CN113916965A CN113916965A CN202111188392.5A CN202111188392A CN113916965A CN 113916965 A CN113916965 A CN 113916965A CN 202111188392 A CN202111188392 A CN 202111188392A CN 113916965 A CN113916965 A CN 113916965A
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 27
- 239000000126 substance Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000007774 positive electrode material Substances 0.000 title claims description 7
- 239000012086 standard solution Substances 0.000 claims abstract description 29
- 239000010405 anode material Substances 0.000 claims abstract description 20
- 238000012360 testing method Methods 0.000 claims abstract description 17
- 239000011248 coating agent Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 10
- 239000000725 suspension Substances 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 229910021397 glassy carbon Inorganic materials 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 12
- 239000007853 buffer solution Substances 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- 229920006395 saturated elastomer Polymers 0.000 claims description 12
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 12
- 239000012488 sample solution Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 239000003755 preservative agent Substances 0.000 claims description 8
- 230000002335 preservative effect Effects 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 238000003795 desorption Methods 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 239000000872 buffer Substances 0.000 claims description 2
- 239000000523 sample Substances 0.000 claims description 2
- 238000001514 detection method Methods 0.000 abstract description 6
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 238000007865 diluting Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229960002089 ferrous chloride Drugs 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005498 polishing 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
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention provides a method for detecting the content of magnetic substances in a lithium ion battery anode material, which is characterized in that carbon is used for coating nano Fe3O4Coating glassy carbon electrode on composite material suspension liquid as working electrode, and respectively testing Fe under different concentration gradients in a three-electrode system2+Standard solution, Co2+Standard solution, Ni2+Respectively constructing Fe by taking the concentration as an abscissa and the current value of a peak as an ordinate according to a voltage-current curve of the standard solution2+Standard solution, Co2+Standard solution, Ni2+A standard curve of the standard solution is used as a basis for testing the content of the magnetic substance in the lithium ion battery anode material; compared with the prior art, the detection method provided by the invention has high sensitivity, can reach the level of trace detection, can eliminate the interference of other metal ions, and has low cost and simple operation.
Description
Technical Field
The invention belongs to the technical field of detection, and particularly relates to a method for detecting the content of a magnetic substance in a lithium ion battery anode material.
Background
In recent years, with the wide application of lithium ion batteries in the fields of power batteries and energy storage, high energy density, high potential and high safety performance have become major development trends in the future, and the safety performance is a key performance index of the lithium ion batteries.
In the manufacturing process of the lithium ion battery anode material, magnetic substances are often mixed, and the lithium ion battery anode material is generally formed by single or mixed metal elements such as Fe, Co, Ni and the like. The presence of such magnetic impurity particles can lead to a reduction in the service life, consistency and safety of the battery. The magnetic substance impurities in the lithium ion battery anode material also have direct influence on the self-discharge of the battery, and the content of the magnetic substance impurities is in direct proportion to the self-discharge rate of the battery, namely, the higher the content of the magnetic substance is, the higher the self-discharge rate of the battery formed by the anode material is.
If the content of magnetic impurity particles in the lithium ion battery anode material can not be effectively detected and the magnetic substance is further controlled in the production link of the anode material, the performance of the battery can be seriously influenced. However, no method for detecting magnetic substances in the positive electrode material of the lithium ion battery exists in the prior art.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for detecting the content of magnetic substances in a lithium ion battery anode material, which can reach the level of trace detection and has low cost and simple operation.
The technical scheme adopted by the invention is as follows:
a method for detecting the content of magnetic substances in a lithium ion battery positive electrode material, which comprises the following steps:
(1) placing the lithium ion battery anode material and the magnet wrapped by the preservative film into the dispersion liquid, and ultrasonically stirring;
(2) placing the magnet wrapped by the preservative film into a container, adding dilute sulfuric acid and dilute nitric acid into the container at one time, and heating and ultrasonically stirring the mixture;
(3) centrifuging the solution obtained in the step (2), diluting the solution with dilute hydrochloric acid until the solution is weakly acidic, and then fixing the volume to obtain a sample solution;
(4) coating carbon with nano Fe3O4Ultrasonically dissolving the composite material in deionized water to obtain a suspension;
(5) uniformly coating the suspension on the polished glassy carbon electrode, and drying to obtain working electrodes A, B, C, D respectively;
(6) putting the working electrode A into NH3-NH4In Cl buffer solution, and consists of a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrodeThree-electrode system to which Fe was added dropwise2+Standard solution, test to obtain different Fe2+Voltage-current curve at concentration and in Fe2+The concentration is abscissa, Fe2+Constructing a standard curve by taking the current value of the peak as a vertical coordinate to obtain a linear equation A;
(7) putting working electrode B into NH3-NH4Adding Co dropwise into Cl buffer solution, forming a three-electrode system by taking a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode2+Standard solution, tested to obtain different Co2+Voltage-current curve at concentration and with Co2+Concentration is abscissa, Co2+Constructing a standard curve by taking the current value of the peak as a vertical coordinate to obtain a linear equation B;
(8) putting working electrode C into NH3-NH4In the mixed solution of Cl buffer solution, a platinum wire electrode is used as a counter electrode, a saturated Ag/AgCl electrode is used as a reference electrode to form a three-electrode system, and Ni is dropwise added into the three-electrode system2+Standard solution, tested to give different Ni2+Voltage-current curve at concentration and in Ni2+Concentration is abscissa, Ni2+Constructing a standard curve by taking the current value of the peak as a vertical coordinate to obtain a linear equation C;
(9) putting working electrode E into NH3-NH4In Cl buffer solution, a platinum wire electrode is used as a counter electrode, a saturated Ag/AgCl electrode is used as a reference electrode to form a three-electrode system, the sample solution in the step (3) is added, a voltage-current curve of the sample is obtained through testing, and Fe on the voltage-current curve is used2+Peak current value, Co2+Peak current value, Ni2+The peak current values are respectively substituted into the linear equation A, B, C to obtain Fe in the sample solution2+、Co2+、Ni2+The concentration of (c); and then the contents of Fe, Co and Ni in the lithium ion battery anode material can be calculated.
In the step (1), the dispersion liquid is deionized water.
In the step (2), the volume fractions of the dilute nitric acid and the dilute sulfuric acid are both 30-38%; the volume ratio of the dilute nitric acid to the dilute sulfuric acid is 1: 2-5.
In the step (3), diluted hydrochloric acid is used for diluting until the pH value of the solution is 6-7.
In steps (6) to (9), the NH3-NH4The amount of Cl buffer was 20mL, the concentration was 0.1M, and the pH was 5.0.
In the steps (6) to (9), the concentration gradient of each standard solution added is 30, 60, 90, 120, 150, 180, 210, 240, 270 and 300 ppb.
In the steps (6) to (9), after the test is finished, a desorption voltage of 0.6V needs to be applied under the condition of stirring, and the desorption lasts for 60 s.
In the testing method provided by the invention, carbon is used for coating nano Fe3O4Coating glassy carbon electrode on composite material suspension liquid as working electrode, and respectively testing Fe under different concentration gradients in a three-electrode system2+Standard solution, Co2+Standard solution, Ni2+Respectively constructing Fe by taking the concentration as an abscissa and the current value of a peak as an ordinate according to a voltage-current curve of the standard solution2+Standard solution, Co2+Standard solution, Ni2+And (5) testing the content of the magnetic substance in the lithium ion battery positive electrode material on the basis of a standard curve of the standard solution.
When the sample solution is prepared, firstly, the lithium ion battery anode material and the magnet wrapped by the preservative film are placed in dispersion liquid, and the magnetic substance in the lithium ion battery anode material is screened out through ultrasonic stirring; then dissolving the magnetic substance by dilute nitric acid and dilute sulfuric acid, centrifuging the solution obtained by dissolving, diluting the solution to pH 6-7 by dilute hydrochloric acid, and then fixing the volume.
Compared with the prior art, the detection method provided by the invention has high sensitivity, can reach the level of trace detection, can eliminate the interference of other metal ions, and has low cost and simple operation.
Drawings
FIG. 1 shows the different Fe values in example 12+Voltage-current curve at concentration and with Fe2+The concentration is abscissa, Fe2+Constructing a standard curve A by taking the current value of the peak as a vertical coordinate;
FIG. 2 is a schematic view ofDifferent Co in example 12+Voltage-current curve at concentration and with Co2+Concentration is abscissa, Co2+Constructing a standard curve B by taking the current value of the peak as a vertical coordinate;
FIG. 3 shows the different Ni in example 12+Voltage-current curve at concentration and with Ni2+Concentration is abscissa, Ni2+Constructing a standard curve C by taking the current value of the peak as a vertical coordinate;
FIG. 4 is a voltage-current curve of the sample solution in example 2 without addition.
Detailed Description
The following detailed description is made with reference to the accompanying drawings.
Carbon-coated nano Fe used in the invention3O4The preparation method of the composite material is disclosed in example 1 in Chinese patent CN 101728526A.
Fe2+Standard solution, Co2+Standard solution, Ni2+The preparation method of the standard solution comprises the following steps: respectively dissolving a ferrous chloride standard substance, a cobalt chloride standard substance and a nickel chloride standard substance in deionized water, and gradually diluting the mixture by the deionized water until the concentration of the mixture is 10 ppb.
The conditions of the electrochemical workstation were: frequency 25Hz, amplitude 25mV, incremental potential 4 mV.
After the test of each test system is completed, a desorption voltage of 0.6V is applied under the condition of stirring, and desorption is carried out for 60s, so that residual metal on the electrode is eliminated.
Example 1
The construction of each standard curve is as follows:
s1, coating 0.25mg of carbon with nano Fe3O4Ultrasonically dissolving the composite material in 20mL of deionized water to obtain a suspension;
s2, polishing the glassy carbon electrode by using 0.3 mu m aluminum oxide, uniformly coating 5 mu L of suspension on the polished glassy carbon electrode, and naturally drying to obtain working electrodes A, B, C, D respectively;
s3, using the working electrode A, the platinum wire electrode as the counter electrode and the saturated Ag/AgCl electrode as the reference electrodeThe three-electrode system is placed in 20mL of 0.1M NH with pH of 5.03-NH4Adding Fe dropwise into the mixed solution A by connecting an electrochemical workstation in a Cl buffer solution2+Standard solution, added Fe2+The concentration gradient of the standard solution is 30, 60, 90, 120, 150, 180, 210 and 240 ppb; different Fe is obtained by testing2+Voltage-current curve at concentration and in Fe2+The concentration is abscissa, Fe2+The peak current values are plotted on the ordinate to form a standard curve a, as shown in fig. 1, resulting in a linear equation a: y is-0.7839 +41.93X, linear correlation coefficient R20.993 where Y is the current value in μ a; x is Fe2+In ppb;
s4, putting a three-electrode system consisting of a working electrode B, a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode into 20mL of 0.1M NH with pH of 5.03-NH4Adding Co dropwise into the mixed solution B by connecting an electrochemical workstation in a Cl buffer solution2+Standard solution, added Co2+The concentration gradient of the standard solution is 30, 60, 90, 120, 150, 180, 210 and 240 ppb; testing to obtain different Co2+Voltage-current curve at concentration and with Co2+Concentration is abscissa, Co2+The peak current value is plotted on the ordinate to form a standard curve B, as shown in fig. 2, which yields a linear equation B: -7.6088+30.27X, coefficient of linear correlation R20.999 where Y is the current value in μ a; x is Co2+In ppb;
s5, putting a three-electrode system consisting of a working electrode C, a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode into 20mL of 0.1M NH with pH of 5.03-NH4Adding Ni into the mixed solution C dropwise by connecting an electrochemical workstation in a Cl buffer solution2+Standard solution, added Ni2+The concentration gradient of the standard solution is 30, 60, 90, 120, 150, 180, 210 and 240 ppb; testing to obtain different Ni2+Voltage-current curve at concentration and in Ni2+Concentration is abscissa, Ni2+The peak current values are plotted on the ordinate to form a standard curve C, as shown in fig. 3, resulting in the linear equation C:y ═ 7.21+29.47X, linear correlation coefficient R20.998 where Y is the current value in μ a; x is Ni2+The concentration of (b) is in ppb.
Example 2
The method for detecting the content of the magnetic substance in the lithium ion battery anode material comprises the following steps:
(1) placing 10mg of a cherry-shaped magnet wrapped by the lithium ion battery anode material and the preservative film in deionized water, and ultrasonically stirring for 30 min; thus, the magnetic substance in the lithium ion battery anode material can be adsorbed on the surface of the magnet wrapped by the preservative film;
(2) placing the magnet wrapped by the preservative film taken out from the step (1) in a beaker, sequentially adding 20mL of 38% dilute sulfuric acid and 30mL of 38% dilute nitric acid, heating, stirring and ultrasonically stirring for 2 h;
(3) centrifuging, decompressing, concentrating and drying the solution obtained in the step (2), and then adding deionized water to a constant volume of 5mL to obtain a sample solution;
(4) putting a three-electrode system consisting of a working electrode E, a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode into 20mL of 0.1M NH with pH of 53-NH4Adding 5mL of the sample solution obtained in the step (3) into the Cl buffer solution, and testing to obtain a voltage-current curve, wherein the voltage-current curve is shown in FIG. 4;
(5) fe on the voltage-current curve in step (4)2+Substitution of peak current values into linear equation A, Co2+Substitution of peak current values into linear equation B, Ni2+Substituting the peak current value into the linear equation C to calculate Fe in the sample solution2 +、Co2+、Ni2+The concentration of (c); and then the contents of Fe, Co and Ni in the lithium ion battery anode material can be calculated.
The above detailed description of a method for detecting the content of a magnetic substance in a positive electrode material of a lithium ion battery with reference to examples is illustrative and not restrictive, and several examples may be cited within the scope of the present invention, and thus, variations and modifications may be made without departing from the general inventive concept within the scope of the present invention.
Claims (6)
1. A method for detecting the content of magnetic substances in a lithium ion battery positive electrode material is characterized by comprising the following steps:
(1) placing the lithium ion battery anode material and the magnet wrapped by the preservative film into the dispersion liquid, and ultrasonically stirring;
(2) placing the magnet wrapped by the preservative film into a container, sequentially adding dilute sulfuric acid and dilute nitric acid into the container, and ultrasonically stirring;
(3) centrifuging, decompressing, concentrating and drying the solution obtained in the step (2), and then adding deionized water to a constant volume to obtain a sample solution;
(4) coating carbon with nano Fe3O4Ultrasonically dissolving the composite material in deionized water to obtain a suspension;
(5) uniformly coating the suspension on the polished glassy carbon electrode, and drying to obtain working electrodes A, B, C, D respectively;
(6) putting the working electrode A into NH3-NH4Adding Fe dropwise into Cl buffer solution, forming a three-electrode system by taking a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode2+Standard solution, test to obtain different Fe2+Voltage-current curve at concentration and in Fe2+The concentration is abscissa, Fe2+Constructing a standard curve by taking the current value of the peak as a vertical coordinate to obtain a linear equation A;
(7) putting working electrode B into NH3-NH4Adding Co dropwise into Cl buffer solution, forming a three-electrode system by taking a platinum wire electrode as a counter electrode and a saturated Ag/AgCl electrode as a reference electrode2+Standard solution, tested to obtain different Co2+Voltage-current curve at concentration and with Co2+Concentration is abscissa, Co2+Constructing a standard curve by taking the current value of the peak as a vertical coordinate to obtain a linear equation B;
(8) putting working electrode C into NH3-NH4In the mixed solution of Cl buffer solution, a platinum wire electrode is used as a counter electrode, a saturated Ag/AgCl electrode is used as a reference electrode to form a three-electrode system, and Ni is dropwise added into the three-electrode system2+Standard solution, tested to give different Ni2+Voltage-current curve at concentration and in Ni2+Concentration is abscissa, Ni2+Constructing a standard curve by taking the current value of the peak as a vertical coordinate to obtain a linear equation C;
(9) putting working electrode E into NH3-NH4In Cl buffer solution, a platinum wire electrode is used as a counter electrode, a saturated Ag/AgCl electrode is used as a reference electrode to form a three-electrode system, the sample solution in the step (3) is added, a voltage-current curve of the sample is obtained through testing, and Fe on the voltage-current curve is used2+Peak current value, Co2+Peak current value, Ni2+The peak current values are respectively substituted into the linear equation A, B, C to obtain Fe in the sample solution2+、Co2+、Ni2+The concentration of (c); and then the contents of Fe, Co and Ni in the lithium ion battery anode material can be calculated.
2. The method of claim 1, wherein in step (1), the dispersion is deionized water.
3. The method according to claim 1, wherein in the step (2), the volume fractions of the dilute sulfuric acid and the dilute nitric acid are both 30-38%; the volume ratio of the dilute sulfuric acid to the dilute nitric acid is 1.5-5: 1.
4. The method of claim 1, wherein in steps (6) - (9), the NH is performed3-NH4The amount of Cl buffer was 20mL, the concentration was 0.1M, and the pH was 5.0.
5. The method according to claim 1, wherein in the steps (6) to (9), the concentration gradient of each standard solution added is 30, 60, 90, 120, 150, 180, 210, 240, 270, 300 ppb.
6. The method of claim 1, wherein in steps (6) - (9), a desorption voltage of 0.6V is applied under stirring for 60s after the test is completed.
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