CN110658183A - Method for measuring electrolyte content in nickel-hydrogen electrolyte - Google Patents
Method for measuring electrolyte content in nickel-hydrogen electrolyte Download PDFInfo
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- CN110658183A CN110658183A CN201810686255.6A CN201810686255A CN110658183A CN 110658183 A CN110658183 A CN 110658183A CN 201810686255 A CN201810686255 A CN 201810686255A CN 110658183 A CN110658183 A CN 110658183A
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- 239000003792 electrolyte Substances 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 26
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 23
- 239000001257 hydrogen Substances 0.000 title claims abstract description 23
- 239000012086 standard solution Substances 0.000 claims abstract description 55
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 42
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 28
- 239000012488 sample solution Substances 0.000 claims abstract description 24
- 239000012470 diluted sample Substances 0.000 claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 16
- 239000012452 mother liquor Substances 0.000 claims abstract description 14
- 239000003085 diluting agent Substances 0.000 claims abstract description 13
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 10
- 238000007865 diluting Methods 0.000 claims abstract description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 239000012895 dilution Substances 0.000 claims description 11
- 238000010790 dilution Methods 0.000 claims description 11
- 239000007864 aqueous solution Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052987 metal hydride Inorganic materials 0.000 claims description 5
- 239000010413 mother solution Substances 0.000 claims description 4
- 238000005259 measurement Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 238000003556 assay Methods 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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Abstract
The invention discloses a method for measuring the electrolyte content in nickel-hydrogen electrolyte, which comprises the following steps: preparing standard mother liquor, wherein the deviation between the theoretical concentration values of KOH, NaOH and LiOH in the standard mother liquor and the theoretical concentration value of the corresponding electrolyte in the sample solution to be detected is less than or equal to 3 percent of the theoretical concentration value of the sample solution to be detected; diluting at least three parts of standard mother liquor to form at least three gradient standard solutions, wherein the linearity of K, Na and Li in the standard solutions is respectively more than or equal to 0.995, and taking the standard solution with the intermediate gradient as a correction standard solution; diluting the sample solution to be detected with a diluent to obtain a diluted sample solution to be detected; and fourthly, preparing a standard curve by adopting an inductively coupled plasma emission spectrometer, measuring the diluted sample solution to be detected and the correction standard solution, and correcting by using the measured value and the theoretical value of the correction standard solution to obtain the content of the electrolyte in the sample solution to be detected. The invention has the advantages that: the stability and accuracy are good.
Description
Technical Field
The invention relates to the technical field of determination of electrolyte in nickel-hydrogen electrolyte.
Background
The nickel-hydrogen electrolyte mainly comprises KOH, NaOH, LiOH and H2And O, accurately detecting the contents of KOH, NaOH and LiOH serving as electrolytes, which is a precondition for ensuring the quality of the nickel-hydrogen electrolyte.
At present, the electrolyte content in the nickel-hydrogen electrolyte is generally measured by an inductively coupled plasma spectrometer. In long-term assay work it was found that: K. na and Li belong to IA elements, and have similar structural properties, and can generate mutual interference in the measurement process, thereby influencing the accuracy of the measured value.
Disclosure of Invention
The purpose of the invention is: the method for measuring the electrolyte content in the nickel-hydrogen electrolyte can avoid the mutual interference among K, Na and Li, thereby effectively improving the measurement accuracy.
In order to achieve the purpose, the invention adopts the technical scheme that: the method for measuring the electrolyte content in the nickel-hydrogen electrolyte comprises the following steps: the method for measuring the content of KOH, NaOH and LiOH electrolytes comprises the following steps: preparing standard mother liquor, wherein the deviation between the theoretical concentration values of KOH, NaOH and LiOH in the standard mother liquor and the theoretical concentration values of KOH, NaOH and LiOH in a sample solution to be detected is less than or equal to 3 percent of the theoretical concentration value of the sample solution to be detected; at least three standard mother solutions are taken and respectively diluted by diluents to form at least three gradient standard solutions, the linearity of K, Na and Li in all the gradient standard solutions is respectively more than or equal to 0.995, and one intermediate gradient standard solution is selected as a correction standard solution; thirdly, pretreating the sample solution to be detected, comprising the following steps: taking a sample solution to be measured, and diluting the sample solution with a diluent, wherein the dilution multiple is (1 +/-0.05) of the dilution multiple when the calibration standard solution is prepared in the second step, so as to obtain a diluted sample solution to be measured; fourthly, an inductively coupled plasma emission spectrometer is adopted, a standard curve is prepared from the standard solutions with a plurality of gradients in the second step, the diluted sample solution to be detected is measured, the measured value of the electrolyte in the diluted sample solution to be detected is obtained, the calibration standard solution is measured, the measured value of the electrolyte in the calibration standard solution is obtained, the measured value of the electrolyte in the diluted sample solution to be detected is corrected by the measured value and the theoretical value of the electrolyte in the calibration standard solution, and the content of the electrolyte in the sample solution to be detected is obtained through calculation.
Further, in the method for determining the electrolyte content in the nickel-hydrogen electrolyte, the diluent is a high-grade pure nitric acid aqueous solution, wherein the volume ratio of nitric acid to water is 1: 19.
Further, in the method for determining the electrolyte content in the nickel-hydrogen electrolyte, the wavelength condition selected in the inductively coupled plasma emission spectrometer is as follows: k: 766.491nm, Na: 589.592nm, Li: 670.783 nm.
Further, in the method for determining the electrolyte content in the nickel-hydrogen electrolyte, in the second step, three portions of the standard mother liquor are respectively diluted by the diluent to form three gradient standard solutions, and the linear average of K, Na and Li in the three gradient standard solutions is respectively greater than or equal to 0.995.
Furthermore, in the method for determining the electrolyte content in the nickel-hydrogen electrolyte solution, the standard solution with the second gradient is taken as a calibration standard solution.
The invention has the advantages that: the method for measuring the electrolyte content in the nickel-hydrogen electrolyte has good stability and accuracy, and can effectively eliminate the influence on the measurement result caused by the mutual interference of K, Na and Li, thereby providing effective guarantee for ensuring the quality of the nickel-hydrogen electrolyte.
Drawings
FIG. 1 is a graph showing the linear distribution of K, Na, and Li concentrations in a standard solution.
Detailed Description
The method for measuring the electrolyte content in the nickel-metal hydride electrolyte will be described in detail below.
The method for measuring the electrolyte content in the nickel-hydrogen electrolyte comprises the following steps: KOH, NaOH, LiOH. The electrolyte determination method comprises the following steps:
preparing standard mother liquor, wherein the deviation between the theoretical concentration values of KOH, NaOH and LiOH in the standard mother liquor and the theoretical concentration values of KOH, NaOH and LiOH in the sample solution to be detected is less than or equal to 3 percent of the theoretical concentration value of the sample solution to be detected. Preparing standard mother liquor according to a theoretical concentration value of a sample solution to be detected, and aiming at: eliminating the influence of mutual interference of K, Na and Li on the measurement result. The concentration theoretical value of the standard mother liquor is as close as possible to the theoretical value of the sample solution to be measured, and the influence of the mutual interference among K, Na and Li on the measurement result can be eliminated as much as possible.
Secondly, for convenience, in this example, three standard mother solutions are taken and diluted with a diluent, i.e., a superior pure nitric acid aqueous solution, wherein the volume ratio of nitric acid to water is 1:19, to form three gradient standard solutions. The linearity of K, Na and Li in the standard solution of three gradients is respectively more than or equal to 0.995. The calibration standard solution is the standard solution of the second gradient. In general, an odd-numbered gradient of standard solution may be used as a calibration standard solution, and an even-numbered gradient of standard solution may be used as a calibration standard solution.
Thirdly, pretreating the sample solution to be detected, comprising the following steps: and (3) taking a sample solution to be detected, diluting with a diluent, namely a superior pure nitric acid aqueous solution, wherein the volume ratio of nitric acid to water is 1:19, the dilution multiple is (1 +/-0.05) of the dilution multiple when the calibration standard solution is prepared in the second step, and the dilution multiple is as close as possible to the dilution multiple when the calibration standard solution is prepared in the second step, so as to obtain the diluted sample solution to be detected.
And fourthly, adopting an inductively coupled plasma emission spectrometer (ICP), wherein the selected wavelength conditions are as follows: k: 766.491nm, Na: 589.592nm, Li: 670.783 nm. A calibration curve was prepared from the three gradients of the standard solution in the second step. Measuring the diluted sample solution to be measured to obtain the measured value of the electrolyte in the diluted sample solution to be measured; and measuring the calibration standard solution to obtain the measured value of the electrolyte of the calibration standard solution. And correcting the measured value of the electrolyte of the diluted sample solution to be detected by using the measured value and the theoretical value of the electrolyte of the correction standard solution, and calculating to obtain the content of the electrolyte in the sample solution to be detected.
The method for measuring the electrolyte content in the nickel-metal hydride electrolyte will be described in further detail with reference to the following examples.
Four batches of the nickel-hydrogen electrolyte produced by this company will be described as an example. The four batches of nickel-hydrogen electrolytes are respectively as follows: HB-3005ET0117001, HB-3005ET0117002, HB-3005ET0117003 and HB-3005ET 0117004. The theoretical values of the electrolyte mass fractions of the above four batches were as follows:
KOH：24％；
NaOH：2.76％；
LiOH：0.92％。
the concentration theoretical values of KOH, NaOH and LiOH in the prepared standard mother liquor are as follows: 23.92%, 2.69% and 0.893%.
Taking three standard mother solutions, and respectively diluting with a diluent, namely a superior pure nitric acid aqueous solution, wherein the volume ratio of nitric acid to water is 1:19, and the dilution times are respectively as follows: 1290. 2580 and 3870 to obtain a first standard solution, a second standard solution and a third standard solution. The linearity of K, Na and Li in the standard solution of three gradients is respectively more than or equal to 0.995, as shown in figure 1. The second standard solution was taken as a calibration standard solution.
Taking a sample solution to be measured, diluting with a diluent, namely a superior-superior pure nitric acid aqueous solution, wherein the volume ratio of nitric acid to water is 1:19, and the dilution times are (2580 +/-129) times of the dilution times when the second standard solution is prepared, so as to obtain the diluted sample solution to be measured.
An inductively coupled plasma emission spectrometer (ICP) is adopted, and the selected wavelength conditions are as follows: k: 766.491nm, Na: 589.592nm, Li: 670.783 nm.
And (4) measuring the diluted sample solution to be measured and the second standard solution. The results were as in examples 1 and 2,
Tables in example 3 and example 4 show.
Example 1: the sample to be detected is nickel-hydrogen electrolyte (HB-3005ET 0117001).
Example 1 analysis of results:
example 2: the sample to be detected is nickel-hydrogen electrolyte (HB-3005ET 0117002).
Example 2 analysis of results:
example 3: the sample to be detected is nickel-hydrogen electrolyte (HB-3005ET 0117003).
Example 3 analysis of results:
example 4: the sample to be detected is nickel-hydrogen electrolyte (HB-3005ET 0117003).
Example 4 analysis of results:
the embodiment shows that the method for measuring the electrolyte content in the nickel-metal hydride electrolyte has good stability and accuracy, and can effectively eliminate the influence on the measurement result caused by the mutual interference of K, Na and Li, thereby providing effective guarantee for ensuring the quality of the nickel-metal hydride electrolyte.
Claims (5)
1. The method for measuring the electrolyte content in the nickel-hydrogen electrolyte comprises the following steps: the method for measuring the content of KOH, NaOH and LiOH electrolytes comprises the following steps: preparing standard mother liquor, wherein the deviation between the theoretical concentration values of KOH, NaOH and LiOH in the standard mother liquor and the theoretical concentration values of KOH, NaOH and LiOH in a sample solution to be detected is less than or equal to 3 percent of the theoretical concentration value of the sample solution to be detected; at least three standard mother solutions are taken and respectively diluted by diluents to form at least three gradient standard solutions, the linearity of K, Na and Li in all the gradient standard solutions is respectively more than or equal to 0.995, and one intermediate gradient standard solution is selected as a correction standard solution; thirdly, pretreating the sample solution to be detected, comprising the following steps: taking a sample solution to be measured, and diluting the sample solution with a diluent, wherein the dilution multiple is (1 +/-0.05) of the dilution multiple when the calibration standard solution is prepared in the second step, so as to obtain a diluted sample solution to be measured; fourthly, an inductively coupled plasma emission spectrometer is adopted, a standard curve is prepared from the standard solutions with a plurality of gradients in the second step, the diluted sample solution to be detected is measured, the measured value of the electrolyte in the diluted sample solution to be detected is obtained, the calibration standard solution is measured, the measured value of the electrolyte in the calibration standard solution is obtained, the measured value of the electrolyte in the diluted sample solution to be detected is corrected by the measured value and the theoretical value of the electrolyte in the calibration standard solution, and the content of the electrolyte in the sample solution to be detected is obtained through calculation.
2. The method according to claim 1, wherein the method further comprises: the diluent is a superior pure nitric acid aqueous solution, wherein the volume ratio of nitric acid to water is 1: 19.
3. The method according to claim 1, wherein the method further comprises: the wavelength conditions selected in the inductively coupled plasma emission spectrometer are as follows: k: 766.491nm, Na: 589.592nm, Li: 670.783 nm.
4. The method for determining the electrolyte content in a nickel-metal hydride electrolyte as claimed in claim 1, 2 or 3, wherein: in the second step, three portions of standard mother liquor are taken and respectively diluted by diluent to form three gradient standard solutions, and the linearity of K, Na and Li in the three gradient standard solutions is respectively more than or equal to 0.995.
5. The method according to claim 4, wherein the method further comprises: taking the standard solution of the second gradient as a correction standard solution.
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Application publication date: 20200107 |