CN109470796A - The detection method of dicarboxylic acids content in a kind of aluminum electrolytic capacitor electrolyte - Google Patents
The detection method of dicarboxylic acids content in a kind of aluminum electrolytic capacitor electrolyte Download PDFInfo
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- CN109470796A CN109470796A CN201811618786.8A CN201811618786A CN109470796A CN 109470796 A CN109470796 A CN 109470796A CN 201811618786 A CN201811618786 A CN 201811618786A CN 109470796 A CN109470796 A CN 109470796A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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Abstract
The present invention relates to a kind of detection methods of dicarboxylic acids content in aluminum electrolytic capacitor electrolyte, it is detected using high performance liquid chromatography, mobile phase A is phosphoric acid-potassium dihydrogen phosphate buffer solution of pH3~4,40~60mmol/L, and the solvent of mobile phase A is the first alcohol and water that volume ratio is 1:1~2；Mobile phase B is the trifluoroacetic acid solution that volumn concentration is 0.1~0.3%, and the solvent of Mobile phase B is the methanol, acetonitrile and water that volume ratio is 10~20:1:2~6；Elution program are as follows: when sample injection time is 0 to 15 minute, mobile phase is mobile phase A；At 15.01 to 45 minutes, mobile phase is the mixed liquor of the mobile phase A that volume ratio is 1:0.9~1.1 and Mobile phase B；At 45.01 to 60 minutes, mobile phase is mobile phase A.The present invention can be such that 6~16 dicarboxylic acids efficiently separate, and meet the requirement of qualitative and quantitative analysis.
Description
Technical field
The invention belongs to analysis method technical fields, and in particular to dicarboxylic acids contains in a kind of aluminum electrolytic capacitor electrolyte
The detection method of amount.
Background technique
Aluminium electrolutic capacitor has the characteristics that function admirable, capacity are big, price is low, easy processing, is widely used in information
In the electronic system products such as electronic equipment, household electrical appliances, electromechanics, at present since the electrolyte of Dicarboxylic Acids series is because of oxidation efficiency
High and good high-temperature stability, is commonly used as the Working electrolyte of aluminium electrolutic capacitor.Thus to aluminium electrolutic capacitor electricity
Dicarboxylic acids in solution liquid carries out qualitative and quantitatively has very big necessity, and organic carboxylic that Dicarboxylic Acids especially carbochain is high
Acid has the characteristics that the features such as not soluble in water, conductivity is low, uses the ion chromatography based on water phase to be analyzed and dissolves first
It is exactly problem, furthermore responsiveness is low, can not be effectively detected.And using liquid-phase chromatography method be it is effective and feasible, with
The type of dicarboxylic acids used in the development of industry is more and more, and being no lack of has the dicarboxylic acids of Long carbon chain to be applied to this row
Industry, and have the dicarboxylic acids of low carbon chain and high carbon chain and deposit situation, and have the influence of solvent He other organic additives.And it is existing
The phenomenon that can not being measured simultaneously in technology there are low carbon chain dicarboxylic acids and high carbon chain dicarboxylic acids, in previous analysis method
Apply in general to the analysis method of low carbon chain dicarboxylic acids, the dicarboxylic acids of high carbon chain can not appearance, and be suitable for high carbon chain
The analysis method of dicarboxylic acids, low carbon chain can not be completely isolated.
Therefore, the method for dicarboxylic acids seems outstanding in a kind of measurement aluminum electrolytic capacitor electrolyte quickly, easy of demand
Be it is important, realize that low carbon chain and high carbon chain dicarboxylic acids while detect, increase the popularity of detection method, increase each component
Separating degree reduces the interference of other organic components.
Summary of the invention
The purpose of the present invention is to provide it is a kind of can be realized low carbon chain and high carbon chain dicarboxylic acids while the aluminium that detects
The detection method of dicarboxylic acids content in electrolytic capacitor electrolyte.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
The detection method of dicarboxylic acids content, is detected using high performance liquid chromatography in a kind of aluminum electrolytic capacitor electrolyte
The content of dicarboxylic acids in the aluminum electrolytic capacitor electrolyte, mobile phase include mobile phase A and Mobile phase B；The stream
Dynamic phase A is phosphoric acid-potassium dihydrogen phosphate buffer solution of pH3~4,40~60mmol/L, and the solvent of the mobile phase A is volume
Than the first alcohol and water for 1:1~2；The Mobile phase B is the trifluoroacetic acid solution that volumn concentration is 0.1~0.3%, institute
The solvent for the Mobile phase B stated is the methanol, acetonitrile and water that volume ratio is 10~20:1:2~6；The elution program of gradient elution are as follows:
When sample injection time is 0 to 15 minute, mobile phase is mobile phase A；When sample injection time is 15.01 to 45 minutes, mobile phase is volume
Than the mixed liquor of mobile phase A and Mobile phase B for 1:0.9~1.1；When sample injection time is 45.01 to 60 minutes, mobile phase is stream
Dynamic phase A.
Preferably, the analysis instrument that the high performance liquid chromatography uses is high performance liquid chromatograph；Chromatographic column is C18
Column.
Preferably, the chromatographic condition of the high performance liquid chromatography are as follows: column temperature is 30~40 DEG C；Sample volume is 25~100 μ
L；Flow velocity is 1.0mL/min, Detection wavelength 210nm.
Preferably, sample solution is diluted aluminum electrolytic capacitor electrolyte by the Mobile phase B obtained.
Preferably, standard solution is diluted standard sample by the Mobile phase B obtained.
According to a kind of specific embodiment, the detection method includes the following steps:
(1) sample solution is subjected to efficient liquid phase chromatographic analysis, according in the appearance time judgement sample solution
The type of dicarboxylic acids；
(2) standard solution of the dicarboxylic acids judged in selection step (1) carries out efficient liquid phase chromatographic analysis, according to appearance
Time carries out the dicarboxylic acids in the sample solution qualitative；
(3) standard solution of the qualitative dicarboxylic acids of selection step (2), using external standard method in the sample solution
Dicarboxylic acids is quantified.
Due to the implementation of above technical scheme, the invention has the following advantages over the prior art:
The present invention passes through high performance liquid chromatography to dicarboxylic acids content in aluminium electricity electrolyte by the improvement to mobile phase
It is detected, 6~16 dicarboxylic acids can be made to efficiently separate, and dicarboxylic acids and other organic components can be distinguished well, made
The separating degree of sample is higher, improves the detection limit of test method, reduces the purpose of the interference of other organic matters, meets qualitative and fixed
The requirement of analysis is measured, analysis method is simple, quick, accurate, and the measurement for dicarboxylic acids in aluminum electrolytic capacitor electrolyte provides
Simple and reliable analysis method.
Detailed description of the invention
Fig. 1 is adipic acid, azelaic acid, decanedioic acid, eleven carbon diacids, 12 carbon that 1 concentration of embodiment is 1000ppm
The chromatogram for mixing sample of binary acid, 2- butyl octanoic acid.
Specific embodiment
The following examples are but not limit the invention to this for illustrating several specific embodiments of the invention
A little specific embodiments.One skilled in the art would recognize that present invention encompasses may wrap in Claims scope
All alternatives, improvement project and the equivalent scheme included.
Embodiment 1
Prepare mobile phase A: phosphoric acid-potassium dihydrogen phosphate buffer solution of pH 3.5,50mmol/L, methanol: the volume ratio of water
For 2:3；Mobile phase B: methanol: acetonitrile: the volume ratio of water is 75:5:20, and the volumn concentration of trifluoroacetic acid is 0.2%.
Analysis instrument used is LC-20AT type high performance liquid chromatograph；Chromatographic column is C18 column, 5 μm, 150 × 4.6mm
(I.D)；Column temperature is 40 DEG C；Sample volume is 25 μ L；Flow velocity is 1.0mL/min；Gradient program are as follows: sample injection time is 0 to 15 minute,
Mobile phase B accounting is 0% in mobile phase；15.01 to 45 minutes, Mobile phase B accounting was 50% in mobile phase, 45.01 to 60 points
Clock, the accounting of Mobile phase B are 0%.
The adipic acid, azelaic acid, decanedioic acid, 11 carbon binary that concentration is 1000ppm have been prepared with Mobile phase B dilution
Acid, dodecanedicarboxylic acid, dibutyl suberic acid mixed standard solution, analyzed into high performance liquid chromatography chromatograph, spectrogram
See Fig. 1.
Embodiment 2
Prepare containing 8% azelaic acid, 10% dibutyl suberic acid, 0.5% 3-nitroacetophenone, 0.5% boric acid,
The aluminum electrolytic capacitor electrolyte of 81% ethylene glycol.
Prepare mobile phase A: phosphoric acid-potassium dihydrogen phosphate buffer solution of pH 3.5,50mmol/L, methanol: the volume ratio of water
For 2:3；Mobile phase B: methanol: acetonitrile: the volume ratio of water is 75:5:20, and the volumn concentration of trifluoroacetic acid is 0.2%.
Analysis instrument used is LC-20AT type high performance liquid chromatograph；Chromatographic column is C18 column, 5 μm, 150 × 4.6mm
(I.D)；Column temperature is 40 DEG C；Sample volume is 25 μ L；Flow velocity is 1.0mL/min；Gradient program are as follows: sample injection time is 0 to 15 minute,
Mobile phase B accounting is 0% in mobile phase；15.01 to 45 minutes, Mobile phase B accounting was 50% in mobile phase, 45.01 to 60 points
Clock, the accounting of Mobile phase B are 0%.
It weighs above-mentioned aluminum electrolytic capacitor electrolyte sample 0.50g and is diluted to 50g with Mobile phase B, shake up dissolution completely, into
High performance liquid chromatograph is analyzed, and is azelaic acid and dibutyl suberic acid in qualitative matching sample according to appearance time.
Azelaic acid is diluted with Mobile phase B and dibutyl suberic acid standard specimen has prepared azelaic acid and dibutyl suberic acid concentration is equal
It for the standard solution of 500ppm, 1000ppm and 2000ppm, is analyzed into high performance liquid chromatography, passes through the concentration of standard solution
The standard curve of standard specimen has been obtained with peak area, has been 7.85% by the content that azelaic acid is calculated in external standard curve, dibutyl
The content of suberic acid is 10.11%, is met with practical additive amount of preparing.
Experiment is tested using potassium dihydrogen phosphate buffer solution system leacheate, is only capable of out the peak and nitro acetyl of azelaic acid
The peak of benzene, dibutyl suberic acid not appearance, using the leacheate of trifluoroacetic acid system test azelaic acid and 3-nitroacetophenone without
Method separately causes azelaic acid without standard measure.
The present invention includes but is not limited to above embodiments, and those skilled in the art can become in the claims in the present invention
Get more embodiments in return.
Claims (6)
1. the detection method of dicarboxylic acids content in a kind of aluminum electrolytic capacitor electrolyte, it is characterised in that: use efficient liquid phase
The content of dicarboxylic acids in the chromatography detection aluminum electrolytic capacitor electrolyte, mobile phase includes mobile phase A and mobile phase
B；The mobile phase A is phosphoric acid-potassium dihydrogen phosphate buffer solution of pH3~4,40~60mmol/L, the mobile phase A
Solvent is the first alcohol and water that volume ratio is 1:1~2；The Mobile phase B is the trifluoro that volumn concentration is 0.1~0.3%
Acetic acid solution, the solvent of the Mobile phase B are the methanol, acetonitrile and water that volume ratio is 10~20:1:2~6；Gradient elution
Elution program are as follows: when sample injection time is 0 to 15 minute, mobile phase is mobile phase A；When sample injection time is 15.01 to 45 minutes, stream
Dynamic is mutually the mixed liquor of mobile phase A and Mobile phase B that volume ratio is 1:0.9~1.1；When sample injection time is 45.01 to 60 minutes,
Mobile phase is mobile phase A.
2. the detection method of dicarboxylic acids content, feature exist in aluminum electrolytic capacitor electrolyte according to claim 1
In: the analysis instrument that the high performance liquid chromatography uses is high performance liquid chromatograph；Chromatographic column is C18 column.
3. the detection method of dicarboxylic acids content, feature in aluminum electrolytic capacitor electrolyte according to claim 1 or 2
It is: the chromatographic condition of the high performance liquid chromatography are as follows: column temperature is 30~40 DEG C；Sample volume is 25~100 μ L；Flow velocity is
1.0mL/min, Detection wavelength 210nm.
4. the detection method of dicarboxylic acids content, feature exist in aluminum electrolytic capacitor electrolyte according to claim 1
By the Mobile phase B aluminum electrolytic capacitor electrolyte is diluted in: sample solution obtained.
5. the detection method of dicarboxylic acids content, feature exist in aluminum electrolytic capacitor electrolyte according to claim 1
By the Mobile phase B standard sample is diluted in: standard solution obtained.
6. the detection side of dicarboxylic acids content in aluminum electrolytic capacitor electrolyte according to any one of claim 1 to 5
Method, it is characterised in that: the detection method includes the following steps:
(1) sample solution is subjected to efficient liquid phase chromatographic analysis, according to the binary in the appearance time judgement sample solution
The type of carboxylic acid；
(2) standard solution of the dicarboxylic acids judged in selection step (1) carries out efficient liquid phase chromatographic analysis, according to appearance time
Dicarboxylic acids in the sample solution is carried out qualitative；
(3) standard solution of the qualitative dicarboxylic acids of selection step (2), using external standard method to the binary in the sample solution
Carboxylic acid is quantified.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111044639A (en) * | 2019-12-31 | 2020-04-21 | 河北中科同创科技发展有限公司 | Mobile phase for directly detecting sebacic acid and liquid phase direct detection method for sebacic acid |
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| EP1750126A1 (en) * | 2004-05-26 | 2007-02-07 | Ajinomoto Co., Inc. | Method and apparatus for analyzing aminofunctional compound |
| CN105467058A (en) * | 2016-01-25 | 2016-04-06 | 惠州市豪鹏科技有限公司 | Method for detecting carboxylic ester compounds in lithium ion battery electrolyte |
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2018
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| EP1750126A1 (en) * | 2004-05-26 | 2007-02-07 | Ajinomoto Co., Inc. | Method and apparatus for analyzing aminofunctional compound |
| CN105467058A (en) * | 2016-01-25 | 2016-04-06 | 惠州市豪鹏科技有限公司 | Method for detecting carboxylic ester compounds in lithium ion battery electrolyte |
| CN106525906A (en) * | 2016-09-29 | 2017-03-22 | 江苏国泰超威新材料有限公司 | Method for detecting content of fluorine ions in perfluoroalkyl sulfonyl imine salts |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111044639A (en) * | 2019-12-31 | 2020-04-21 | 河北中科同创科技发展有限公司 | Mobile phase for directly detecting sebacic acid and liquid phase direct detection method for sebacic acid |
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Application publication date: 20190315 |