CN112345691B - Method for detecting content of chloride ions in electrolyte solute of aluminum electrolytic capacitor - Google Patents
Method for detecting content of chloride ions in electrolyte solute of aluminum electrolytic capacitor Download PDFInfo
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- CN112345691B CN112345691B CN202011419509.1A CN202011419509A CN112345691B CN 112345691 B CN112345691 B CN 112345691B CN 202011419509 A CN202011419509 A CN 202011419509A CN 112345691 B CN112345691 B CN 112345691B
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000003792 electrolyte Substances 0.000 title claims abstract description 30
- 239000003990 capacitor Substances 0.000 title claims abstract description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 47
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000001514 detection method Methods 0.000 claims abstract description 37
- 239000012086 standard solution Substances 0.000 claims abstract description 24
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 23
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003729 cation exchange resin Substances 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 17
- 238000004448 titration Methods 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 9
- -1 ammonium ions Chemical class 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 3
- 239000000523 sample Substances 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 14
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 150000002576 ketones Chemical class 0.000 claims description 4
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical group COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000005342 ion exchange Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000012488 sample solution Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical group COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 2
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 claims description 2
- 239000008151 electrolyte solution Substances 0.000 claims 3
- 150000007942 carboxylates Chemical class 0.000 claims 2
- 230000020477 pH reduction Effects 0.000 abstract description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract 1
- 229910052709 silver Inorganic materials 0.000 abstract 1
- 239000004332 silver Substances 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 12
- 238000011084 recovery Methods 0.000 description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 230000029087 digestion Effects 0.000 description 4
- 238000004255 ion exchange chromatography Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000004454 trace mineral analysis Methods 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 150000001733 carboxylic acid esters Chemical class 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000003918 potentiometric titration Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910052946 acanthite Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 1
- 229940056910 silver sulfide Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004879 turbidimetry Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
- G01N31/164—Determining the equivalent point by means of a discontinuity by electrical or electrochemical means
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for detecting the content of chloride ions in electrolyte solute for an aluminum electrolytic capacitor, which adopts a nonaqueous potential titration method for detection: the method comprises the steps of taking a non-aqueous silver nitrate standard solution as a titrant, taking a silver sulfide-plated electrode (composite electrode) as a measuring electrode, preparing a to-be-measured sample into a to-be-measured solution by taking ethanol as a solvent, removing ammonium ions from the to-be-measured solution after acidification by a cation exchange resin column, titrating the to-be-measured solution to a terminal point by using the non-aqueous silver nitrate standard solution, and calculating the content of chloride ions according to a corresponding formula after titration is finished. The method applies the nonaqueous potential titration method to the detection of trace chloride ions in the electrolyte of the aluminum electrolytic capacitor for the first time, and pretreats the electrolyte diluted by ethanol through the cation exchange resin, thereby avoiding the influence of ammonium ions on the detection of the chloride ions by the nonaqueous potential titration method, and having the advantages of convenience, high efficiency, stability, good detection accuracy and the like.
Description
Technical Field
The invention relates to the field of chemical analysis, in particular to a method for detecting the content of chloride ions in electrolyte solute for an aluminum electrolytic capacitor.
Background
The electrolyte of the aluminum electrolytic capacitor mainly comprises the following components: more than 80% of main solvent (generally ethylene glycol), 5-10% of main electrolyte and a small amount of other additives. The performance of the main electrolyte determines the performance of the electrolyte, and is also a key factor for the final performance of the capacitor.
Because chloride ions can corrode an oxide film on the surface of the capacitor aluminum foil, the capacitor is scrapped, so that the content of the chloride ions is the most important control index of the main electrolyte, and the industrial requirement is less than 1 ppm.
At present, the whole aluminum electrolytic capacitor industry trace chloride ion detection method mainly comprises a turbidimetry method, an ion chromatography method and a halogen analyzer method. The general method for measuring the chemical reagent chloride GB/T9729-2007 is mainly characterized in that the qualitative detection is carried out on trace chloride ions by a turbidimetric method, and the accurate quantification cannot be carried out; the ion chromatography can quantitatively detect the content of trace chloride ions, but a sample must be subjected to strict pretreatment, namely high-temperature acid addition digestion and then filtration to obtain a clear and transparent aqueous solution, and the pretreatment operation is relatively troublesome; the halogen analyzer mainly measures the content of organic halogen according to the detection principle, and inorganic chlorine cannot be accurately measured.
In the CN103063726A patent, a potentiometric titration method is used to determine the content of chloride ions in the lithium ion battery electrolyte, although the method can detect the content of trace chloride ions, if ammonium ions exist in a sample, the interference on the detection result is serious, which results in poor sample recovery rate (about 10%), and the solute of the electrolyte in the whole aluminum electrolytic capacitor industry is mostly ethylene glycol solution of organic carboxylic acid ammonium salt, which results in that the detection cannot be performed by the electrotitration method.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for detecting the content of chloride ions in electrolyte solute of an aluminum electrolytic capacitor, aiming at overcoming the defects that the detection of trace chloride ions in the electrolyte of the aluminum electrolytic capacitor in the prior art can not be quantitatively detected or complex pretreatment is required when the detection can be conveniently carried out, and simultaneously solving the defect that the detection by an electrotitration method can not be adopted due to ammonium salt in the electrolyte solute of the aluminum electrolytic capacitor.
The technical scheme for solving the technical problems is as follows: a method for detecting the content of chloride ions in electrolyte solute for an aluminum electrolytic capacitor adopts a nonaqueous potential titration method to detect: taking a non-aqueous silver nitrate standard solution as a titrant, taking a composite electrode (a silver sulfide plating electrode) as a measuring electrode, preparing a to-be-measured sample into a to-be-measured solution by taking ethanol as a solvent, removing ammonium ions from the to-be-measured solution by a cation exchange resin column after the to-be-measured solution is acidified, then titrating the to-be-measured solution to a terminal point by using the non-aqueous silver nitrate standard solution, and calculating according to the following formula after titration is completed to obtain the content of chloride ions:
W＝C×(V-V 0 )×35.45×10 3 /m
w-chloride ion content, μ g/g;
c is the concentration of the non-aqueous silver nitrate standard solution, mol/L;
v is the volume of the non-aqueous silver nitrate standard solution consumed by titration of the sample solution, mL;
v0-volume of consumption of non-aqueous silver nitrate standard solution, mL, by blank ethanol titration;
m-mass of sample, g.
On the basis of the technical scheme, the invention can further specifically select as follows.
Preferably, the cation exchange resin used in the cation exchange resin column is D001H type macroporous resin.
Specifically, before the treatment of the ammonium ion in the solution to be detected, the cation exchange resin is fully soaked in dilute sulfuric acid, then is loaded into an ion exchange column, and is washed by deionized water until the effluent liquid is neutral.
Specifically, the liquid outlet speed of the liquid to be detected when the liquid passes through the cation exchange resin column is controlled to be 2-4 mL/min.
Specifically, the solvent of the non-aqueous silver nitrate standard solution is alcohols, ketones, carbonates or carboxylic acid esters.
Preferably, the alcohol is methanol, ethanol, propanol, propylene glycol or isopropanol.
Preferably, the ketone is acetone or butanone.
Preferably, the carbonate is dimethyl carbonate, diethyl carbonate, propylene carbonate or ethyl methyl carbonate.
Preferably, the carboxylic ester is methyl formate, ethyl formate or ethyl acetate.
Compared with the prior art, the invention has the beneficial effects that:
the method applies the nonaqueous potential titration method to the detection of trace chloride ions in the electrolyte of the aluminum electrolytic capacitor for the first time, and pretreats the electrolyte diluted by ethanol through cation exchange resin, thereby avoiding the influence of ammonium ions on the detection of chloride ions by the nonaqueous potential titration method, and having the advantages of convenience, high efficiency, stability, good detection accuracy and the like.
Detailed Description
The present invention is further described in detail with reference to the following specific embodiments, which are provided for illustration only and are not intended to limit the scope of the present invention.
For the sake of brevity, the drugs, auxiliary devices, etc. used in the following examples are all commercially available products unless otherwise specified, and the methods used are all conventional methods unless otherwise specified.
Example 1
A method for detecting the content of chloride ions in electrolyte solute for an aluminum electrolytic capacitor adopts a nonaqueous potential titration method for detection, and specifically comprises the following steps:
(1) preparation of 0.001mol/L silver nitrate standard solution:
about 0.0846g of silver nitrate is weighed out, dissolved in 500mL of ethanol and shaken up for use.
(2) Preparing and calibrating a 0.001mol/L silver nitrate standard solution:
1g (accurate to 0.0001g) of 100ppm chloride standard solution is weighed, mixed evenly with 60g absolute ethyl alcohol (analytically pure) and calibrated by an automatic potentiometric titrator.
(3) Pretreatment of D001H type cation exchange resin
Soaking the resin in 1-2 wt% dilute sulfuric acid solution for 1-1.5 hr, soaking the resin in 4-5 wt% dilute sulfuric acid solution in the volume ratio of 2 to 1 for 1-1.5 hr, loading into ion exchange column, and washing with deionized water until the effluent is neutral.
(4) Detecting chloride ions in electrolyte solute:
60g (accurate to 0.01g) of electrolyte solute is weighed, 10mL of 25% nitric acid (acidification) and 60g of absolute ethyl alcohol (analytically pure) are added and uniformly mixed, then the mixture passes through the cation exchange resin column (the liquid outlet speed is controlled to be 2-4mL/min), and the solution passing through the resin column is measured by an automatic potentiometric titrator.
(5) Detection of chloride ions in blank ethanol:
60g of absolute ethyl alcohol (analytically pure) is weighed, 10mL of 25% nitric acid is added for acidification, then the solution passes through the cation exchange resin column (the liquid outlet speed is controlled to be 2-4mL/min), and the solution passing through the resin column is measured by an automatic potentiometric titrator.
(6) And (3) detecting the recovery rate of the added standard:
adding 0.6g (accurate to 0.0001g) of 100ppm chloride standard solution into the solution before resin treatment in the step (4), uniformly mixing, then passing through the cation exchange resin (the liquid outlet speed is controlled to be 2-4mL/min), and measuring the solution after resin treatment by using an automatic potentiometric titrator.
(7) After the detection is finished, calculating the result according to the following formula:
W＝C×(V-V 0 )×35.45×10 3 /m
w is the content of chloride ions, mu g/g;
c is the concentration of the non-aqueous silver nitrate standard solution, mol/L;
v is the volume of the non-aqueous silver nitrate standard solution consumed by titration of the sample solution, mL;
v0-volume of the standard solution of silver nitrate non-aqueous solution consumed by blank ethanol titration, mL;
m-mass of sample, g.
(8) The sample detection results are as follows:
the repeatability RSD value is 7.97%, and the repeatability of sample detection meets the requirement.
(9) The results of the detection of the recovery rate of the added standard are as follows:
the average recovery rate is 83.3% > 80%, and for trace analysis, the measurement requirements are met.
Example 2
Referring to the experimental procedure of example 1, the solvent ethanol of the silver nitrate standard solution was changed to propylene glycol, and other procedures were the same.
The detection results of the samples are as follows:
the RSD value is 8.16%, and the repeatability of sample detection meets the requirement.
The results of the detection of the recovery rate of the added standard are as follows:
the average recovery was 83.0%, which for trace analysis met the measurement requirements.
Example 3
Referring to the experimental procedure of example 1, the solvent ethanol of the silver nitrate standard solution was changed to diethyl carbonate, and other procedures were the same.
The detection results of the samples are as follows:
the RSD value is 8.39%, and the repeatability of sample detection meets the requirement.
The detection result of the standard recovery rate is as follows:
the average recovery was 84.8%, which for trace analysis met the measurement requirements.
Example 4
Referring to the experimental procedure of example 1, the solvent ethanol of the silver nitrate standard solution was changed to ethyl formate, and the other procedures were the same.
The sample detection results are as follows:
the RSD value is 9.07 percent, and the repeatability of sample detection meets the requirement.
The results of the detection of the recovery rate of the added standard are as follows:
the average recovery was 90.2%, which for trace analysis met the measurement requirements.
Comparative example 1:
the electrolyte solute of step (4) of example 1 was measured and the labeled sample was detected using prior art ion chromatography.
Weighing 1g of sample, accurately obtaining the sample to be 0.1mg, adding nitric acid into a 10mL digestion tank for high-temperature digestion, and transferring the sample into a 10mL volumetric flask for constant volume after digestion.
The sample detection results are as follows:
the results of the detection of the recovery rate of the added standard are as follows:
as can be seen from the above examples and comparative examples, the method provided by the invention can be applied to detection of trace chloride ions in the electrolyte of an aluminum electrolytic capacitor by a nonaqueous potentiometric titration method, and the detection result has stability and accuracy equivalent to those of detection by an ion chromatography method in the prior art, but the detection equipment is relatively cheaper, and the pretreatment method for detecting a sample is simpler, so that the method has better popularization and use values.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.
Claims (9)
1. A method for detecting the content of chloride ions in electrolyte solute for an aluminum electrolytic capacitor is characterized by adopting a nonaqueous potential titration method for detection: taking a non-aqueous silver nitrate standard solution as a titrant, taking a composite electrode as a measuring electrode, preparing a to-be-measured liquid by taking ethanol as a solvent for a to-be-measured sample, removing ammonium ions from the to-be-measured liquid after the to-be-measured liquid is acidified by a cation exchange resin column, titrating the to-be-measured liquid to a terminal point by using the non-aqueous silver nitrate standard solution, and calculating according to the following formula after the titration is completed to obtain the chloride ion content:
W＝C×(V-V 0 )×35.45×10 3 /m
w-chloride ion content, μ g/g;
c is the concentration of the non-aqueous silver nitrate standard solution, mol/L;
v is the volume of the sample solution titrating the consumed non-aqueous silver nitrate standard solution, mL;
V 0 blank ethanol titration consumes volume, mL, of the non-aqueous silver nitrate standard solution;
m-mass of sample, g.
2. The method for detecting the chloride ion content of the solute in electrolyte for aluminum electrolytic capacitors as claimed in claim 1, wherein cation exchange resin adopted by the cation exchange resin column is D001H type macroporous resin.
3. The method for detecting the content of chloride ions in solute in electrolyte solution for aluminum electrolytic capacitor as claimed in claim 2, wherein the cation exchange resin is fully soaked in dilute sulfuric acid before ammonium ions in the solution to be detected are removed, and then is loaded into ion exchange column, and then is washed with deionized water until the effluent liquid is neutral.
4. The method for detecting the content of chloride ions in solute of electrolyte for the aluminum electrolytic capacitor as recited in claim 3, wherein a liquid outlet speed of a liquid to be detected passing through the cation exchange resin column is controlled to be 2-4 mL/min.
5. The method for detecting the content of chloride ions in solute in electrolyte for the aluminum electrolytic capacitor as recited in any one of claims 1 to 4, wherein a solvent of the non-aqueous silver nitrate standard solution is alcohol, ketone, carbonate or carboxylate.
6. The method for detecting the content of the chloride ions in the solute of the electrolyte solution for the aluminum electrolytic capacitor as recited in claim 5, wherein the alcohol is methanol, ethanol, propylene glycol, propanol or isopropanol.
7. The method for detecting the content of chloride ions in solute of electrolyte for aluminum electrolytic capacitors as recited in claim 5, wherein said ketone is acetone or butanone.
8. The method for detecting the chloride ion content of the solute in the electrolyte solution for aluminum electrolytic capacitors as claimed in claim 5, wherein the carbonate is dimethyl carbonate, diethyl carbonate, propylene carbonate or ethyl methyl carbonate.
9. The method for detecting the content of chloride ions in solute in electrolyte for the aluminum electrolytic capacitor as recited in claim 5, wherein said carboxylate is methyl formate, ethyl formate or ethyl acetate.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3862892A (en) * | 1972-01-25 | 1975-01-28 | Max Planck Gesellschaft | Aluminium object with anodic oxide surface |
| AU8245675A (en) * | 1974-06-25 | 1977-01-06 | Mitsui Mining & Smelting Co., Ltd | Method and apparatus for purification of aqueous zinc sulphate solution used in electrolytical production of zinc |
| CN104781647A (en) * | 2012-09-14 | 2015-07-15 | 雷诺两合公司 | Method for detecting and measuring hydrofluoric acid in electrolyte solution containing lithium hexafluorophosphate LiPF6 of lithium battery |
| CN105006366A (en) * | 2015-06-17 | 2015-10-28 | 武汉海斯普林科技发展有限公司 | High-voltage aluminum electrolytic capacitor electrolyte |
| CN105017091A (en) * | 2015-06-17 | 2015-11-04 | 武汉海斯普林科技发展有限公司 | High-purity iron p-toluenesulfonate solution synthesis method |
| CN109300693A (en) * | 2018-09-20 | 2019-02-01 | 武汉海斯普林科技发展有限公司 | A kind of electrolysis additive and preparation method thereof and aluminum electrolytic capacitor electrolyte |
| CN110887888A (en) * | 2019-11-15 | 2020-03-17 | 超威电源集团有限公司 | Method for detecting content of chloride ions in lead-acid storage battery electrolyte |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103063726B (en) * | 2013-01-10 | 2015-01-07 | 广州天赐高新材料股份有限公司 | Detection method for chlorine ion content in lithium-ion battery electrolyte |
| CN108152443A (en) * | 2017-12-15 | 2018-06-12 | 青岛科技大学 | A kind of chloride ion conductor method in aniline-nitrobenzene condensation reaction recycling catalyst feed liquid |
| CN110231435A (en) * | 2019-07-26 | 2019-09-13 | 黄河三角洲京博化工研究院有限公司 | A kind of method of chloride content determination in aluminium wastewater |
-
2020
- 2020-12-07 CN CN202011419509.1A patent/CN112345691B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3862892A (en) * | 1972-01-25 | 1975-01-28 | Max Planck Gesellschaft | Aluminium object with anodic oxide surface |
| AU8245675A (en) * | 1974-06-25 | 1977-01-06 | Mitsui Mining & Smelting Co., Ltd | Method and apparatus for purification of aqueous zinc sulphate solution used in electrolytical production of zinc |
| CN104781647A (en) * | 2012-09-14 | 2015-07-15 | 雷诺两合公司 | Method for detecting and measuring hydrofluoric acid in electrolyte solution containing lithium hexafluorophosphate LiPF6 of lithium battery |
| CN105006366A (en) * | 2015-06-17 | 2015-10-28 | 武汉海斯普林科技发展有限公司 | High-voltage aluminum electrolytic capacitor electrolyte |
| CN105017091A (en) * | 2015-06-17 | 2015-11-04 | 武汉海斯普林科技发展有限公司 | High-purity iron p-toluenesulfonate solution synthesis method |
| CN109300693A (en) * | 2018-09-20 | 2019-02-01 | 武汉海斯普林科技发展有限公司 | A kind of electrolysis additive and preparation method thereof and aluminum electrolytic capacitor electrolyte |
| CN110887888A (en) * | 2019-11-15 | 2020-03-17 | 超威电源集团有限公司 | Method for detecting content of chloride ions in lead-acid storage battery electrolyte |
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