CN104713876B - The assay method of free oxalic acid in a kind of single Lithium bis (oxalate) borate - Google Patents
The assay method of free oxalic acid in a kind of single Lithium bis (oxalate) borate Download PDFInfo
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- CN104713876B CN104713876B CN201510138938.4A CN201510138938A CN104713876B CN 104713876 B CN104713876 B CN 104713876B CN 201510138938 A CN201510138938 A CN 201510138938A CN 104713876 B CN104713876 B CN 104713876B
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- borate
- oxalate
- oxalic acid
- lithium bis
- titrant
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 235000006408 oxalic acid Nutrition 0.000 title claims abstract description 26
- DEUISMFZZMAAOJ-UHFFFAOYSA-N lithium dihydrogen borate oxalic acid Chemical compound B([O-])(O)O.C(C(=O)O)(=O)O.C(C(=O)O)(=O)O.[Li+] DEUISMFZZMAAOJ-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000003556 assay Methods 0.000 title claims abstract description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 22
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000004448 titration Methods 0.000 claims abstract description 10
- KVYRCBOUKXJXDK-UHFFFAOYSA-N 3,4-dimethylphenazine-1,2-diamine hydrochloride Chemical compound Cl.C1=CC=CC2=NC3=C(C)C(C)=C(N)C(N)=C3N=C21 KVYRCBOUKXJXDK-UHFFFAOYSA-N 0.000 claims abstract description 8
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 244000061458 Solanum melongena Species 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims description 5
- SIXOAUAWLZKQKX-UHFFFAOYSA-N carbonic acid;prop-1-ene Chemical compound CC=C.OC(O)=O SIXOAUAWLZKQKX-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000010812 external standard method Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- FCRDQIPCKDSOCE-UHFFFAOYSA-N C(C(=O)O)(=O)O.B([O-])(O)O.C(C(=O)O)(=O)O.C(C(=O)O)(=O)O.[Li+] Chemical compound C(C(=O)O)(=O)O.B([O-])(O)O.C(C(=O)O)(=O)O.C(C(=O)O)(=O)O.[Li+] FCRDQIPCKDSOCE-UHFFFAOYSA-N 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000002696 acid base indicator Substances 0.000 description 1
- 238000002479 acid--base titration Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- RIUWBIIVUYSTCN-UHFFFAOYSA-N trilithium borate Chemical compound [Li+].[Li+].[Li+].[O-]B([O-])[O-] RIUWBIIVUYSTCN-UHFFFAOYSA-N 0.000 description 1
Abstract
The present invention relates to a kind of assay method for determining the oxalic acid that dissociates in single Lithium bis (oxalate) borate, it dissolves single Lithium bis (oxalate) borate in glove box with acetonitrile as solvents, given instruction with the mixed solution of dimethyl diaminophenazine chloride and methylene blue agent, drop in aubergine, stir, volumetric titrimetry is carried out as titrant with diethylamine solution, the amount that titrant is consumed under green postscript is titrated to, the beneficial effects of the invention are as follows：By the present invention in that giving instruction agent with the mixed solution of dimethyl diaminophenazine chloride and methylene blue and diethylamine solution makees titrant, and by strictly controlling the ratio and moisture content of each component in indicator and titrant, so that color change is obvious in titration process, titration end-point, the convenient amount for calculating free oxalic acid can accurately be found.
Description
Technical field
The present invention relates to a kind of assay method for determining the oxalic acid that dissociates in single Lithium bis (oxalate) borate.
Background technology
Oxalic acid is one of raw material of the single Lithium bis (oxalate) borate of synthesis, the height of single Lithium bis (oxalate) borate medium-height grass acid content, it will straight
The single Lithium bis (oxalate) borate quality of influence is connect, so as to influence containing single Lithium bis (oxalate) borate electrolyte product quality, oxalic acid is to evaluate single oxalic acid
One important indicator of lithium borate quality.
Single Lithium bis (oxalate) borate chemical property is very active, easily with water and lower alcohol reaction generation oxalic acid, in conventional outdoor bar
Under part, acid base titration is carried out from common acid-base indicator and usual vehicle, because indicator discoloration does not take off substantially and quickly
Color, it is impossible to be exactly found titration end-point, it is impossible to be directly used in the measure of single Lithium bis (oxalate) borate medium-height grass acid content.
The content of the invention
The goal of the invention of the present invention is to contain in view of the above-mentioned problems, providing a kind of oxalic acid that in single Lithium bis (oxalate) borate dissociates that determines
The method of amount, by the present invention in that giving instruction agent with the mixed solution of dimethyl diaminophenazine chloride and methylene blue and diethylamine solution is titrated
Agent, and by strictly controlling the ratio and moisture content of each component in indicator and titrant so that color change in titration process
Substantially, titration end-point, the convenient amount for calculating free oxalic acid can accurately be found.
The assay method of free oxalic acid in a kind of single Lithium bis (oxalate) borate, it is characterised in that：Make molten with acetonitrile in glove box
The single Lithium bis (oxalate) borate of agent dissolving, agent of being given instruction with the mixed solution of dimethyl diaminophenazine chloride and methylene blue is dropped in aubergine, stirring is equal
It is even, volumetric titrimetry is carried out as titrant with diethylamine solution, the amount that titrant is consumed under green postscript is titrated to.
The mg/kg of water content in above-mentioned glove box≤30.
The mg/kg of water content in above-mentioned acetonitrile≤20.
The mass ratio of above-mentioned dimethyl diaminophenazine chloride and methylene blue is 2.5：1.
The solvent of above-mentioned indicator is GBL, and the concentration of indicator is 0.1-0.5%.
The solvent of above-mentioned diethylamine solution is propene carbonate and ethylene carbonate, the propene carbonate and ethylene carbonate
The mass ratio of ester is 2：1, the mg/kg of water content in the solvent≤20.
The concentration of above-mentioned diethylamine solution is 0.1mg/kg.
The moisture content of above-mentioned diethylamine solution is less than 600 mg/kg.
The beneficial effects of the invention are as follows：By the present invention in that given instruction with the mixed solution of dimethyl diaminophenazine chloride and methylene blue agent with
And diethylamine solution makees titrant, and by strictly controlling the ratio and moisture content of each component in indicator and titrant so that
Color change substantially, can accurately find titration end-point, the convenient amount for calculating free oxalic acid in titration process.
Brief description of the drawings
Fig. 1 is curve maps of the list Lithium bis (oxalate) borate oxalic acid content Y with adding oxalic acid quality X.
Embodiment
With reference to embodiment, the invention will be further described, so that those skilled in the art can be more preferable
The understanding present invention, but and be not so limited the present invention.
First, instrument and reagent：
1st, magnetic agitation
2nd, diethylamine（Analysis is pure）（Moisture content is less than 600 mg/kg）
3rd, acetonitrile（Purity >=99%, moisture content≤20mg/kg）
4th, solid oxalic acid（Analysis is pure, 110 DEG C of dryings 4 hours）
2nd, experimental procedure：
1st, oxalic acid standard liquid is prepared：It is accurate to weigh 0.1 gram of oxalic acid, 150 grams of acetonitriles are added, oxalic acid content 0.067% is obtained.
2nd, titrant solution
Prepare：10 milli diethylamine are weighed, are added（Propene carbonate：Ethylene carbonate=2:1 mass ratio）Solution is to 1.0kg.
Demarcation：20 grams of standard liquids 1 are weighed, 4-5 drop mixed indicators is added, in aubergine, is placed on magnetic stirring apparatus,
Stir, green is titrated to diethylamine solution, write down the quality of the diethylamine solution of consumption.Diethylamine can so be obtained
The A of solution【I.e. 1 gram diethylamine solution is equivalent to A microgram oxalic acid】.
3rd, sample preparation：Claim 2 grams of single Lithium bis (oxalate) borate samples in glove box, 250 milliliters are dissolved in 150 grams of acetonitriles and is gathered
In tetrafluoro bottle, fully rock, dissolve it.
4th, sample is determined：A certain amount of sample 3 is weighed, 4-5 drop mixed indicators is added, in aubergine, is placed on magnetic agitation
On device, stir, green is titrated to diethylamine solution, write down the mass M of the diethylamine solution of consumption, according to following public affairs
Formula can calculate the free oxalic acid content X obtained in testing sample.
M1:Single Lithium bis (oxalate) borate quality（g）
M2:The acetonitrile quality of the single Lithium bis (oxalate) borate of dissolving（g）
M3:Weigh the quality of single Lithium bis (oxalate) borate/acetonitrile solution（g）
M:The quality of titrant consumption（g）
5th, the 4 parts 30 grams samples prepared by step 3 are taken（Wherein, single Lithium bis (oxalate) borate quality be 30 × 2/152=
0.3947g）, 0.2 gram, 0.5 gram, 1.0 grams, 1.5 grams is separately added into thereto and prepares oxalic acid standard liquid by step 1, is measured mixed
The free oxalic acid content of solution is closed, what is obtained the results are shown in Table 1.
In addition, the measurement result in table 1, makes single Lithium bis (oxalate) borate oxalic acid content Y with adding oxalic acid quality X song
Line chart, and calculate with external standard method the moisture content of testing sample.Compare external standard method result of calculation and direct measurement result.By comparing
Understand, in x=0, oxalic acid=1407mg/kg that external standard method is obtained, the result 1393mg/kg obtained with direct measurement is approached.By
This understands, oxalic acid content of dissociating in single Lithium bis (oxalate) borate is determined with method of the present invention, its result is accurately and reliably.
Claims (1)
1. a kind of assay method for the oxalic acid that dissociates in single Lithium bis (oxalate) borate, it is characterised in that：Acetonitrile as solvents is used in glove box
The single Lithium bis (oxalate) borate of dissolving, agent of being given instruction with the mixed solution of dimethyl diaminophenazine chloride and methylene blue is dropped in aubergine, stirred,
Volumetric titrimetry is carried out as titrant with diethylamine solution, the amount that titrant is consumed under green postscript is titrated to；
The mg/kg of water content in the glove box≤30；
The mg/kg of water content in the acetonitrile≤20；
The mass ratio of the dimethyl diaminophenazine chloride and methylene blue is 2.5：1；
The solvent of the indicator is GBL, and the concentration of indicator is 0.1-0.5%；
The solvent of the diethylamine solution be propene carbonate and ethylene carbonate, the propene carbonate and ethylene carbonate
Mass ratio is 2：1, the mg/kg of water content in the solvent≤20；
The concentration of the diethylamine solution is 0.1mg/kg；
The moisture content of the diethylamine solution is less than 600 mg/kg.
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| CN201510138938.4A CN104713876B (en) | 2015-03-27 | 2015-03-27 | The assay method of free oxalic acid in a kind of single Lithium bis (oxalate) borate |
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| CN201510138938.4A CN104713876B (en) | 2015-03-27 | 2015-03-27 | The assay method of free oxalic acid in a kind of single Lithium bis (oxalate) borate |
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| CN108241036A (en) * | 2016-12-23 | 2018-07-03 | 九江天赐高新材料有限公司 | A kind of assay method of di-oxalate lithium borate purity and its impurity content |
| CN108226374A (en) * | 2017-12-21 | 2018-06-29 | 珠海市赛纬电子材料股份有限公司 | A kind of assay method of the free acid content of the electrolyte containing special additive |
| CN112255222B (en) * | 2020-10-19 | 2022-03-29 | 厦门海辰新能源科技有限公司 | Composition, application thereof and screening method of electrolyte |
| CN116148416A (en) * | 2022-12-15 | 2023-05-23 | 福建德尔科技股份有限公司 | Method for detecting free acid in difluoro bis (lithium oxalate) phosphate |
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| CN104215740B (en) * | 2014-09-25 | 2016-08-17 | 河南工信环保科技有限公司 | A kind of acidity assaying method of cupric ferrum sulfuric acid solution |
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Inventor after: Zhao Zhihua Inventor after: Ren Hai Inventor after: Li Lifei Inventor after: Liu Yong Inventor after: Song Pengbin Inventor before: Zhao Zhihua Inventor before: Ren Hai Inventor before: Wang Jifeng Inventor before: Li Lifei Inventor before: Liu Yong Inventor before: Song Pengbin |
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Free format text: CORRECT: INVENTOR; FROM: ZHAO ZHIHUA REN HAI WANG JIFENG LI LIFEI LIU YONG SONG PENGBIN TO: ZHAO ZHIHUA REN HAI LI LIFEI LIU YONG SONG PENGBIN |
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Address after: 256800, No. six, Qingfeng Road, Chengbei Industrial Zone, Zhanhua District, Shandong, Binzhou, 7 Patentee after: Shandong Hairong power materials Limited by Share Ltd Address before: 256899 Qingfeng No. six road, City North Industrial Park, Zhanhua County, Shandong Province, No. 7 Patentee before: SHANDONG HIRONG POWER SUPPLY MATERIAL CO., LTD. |
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Effective date of registration: 20200601 Address after: 257100 Room 102, building 5, accelerator of science and technology enterprise, No. 17, Xinghua River, Dongying District, Dongying City, Shandong Province Patentee after: Dongying gurun special new energy Co., Ltd Address before: 256800, No. six, Qingfeng Road, Chengbei Industrial Zone, Zhanhua District, Shandong, Binzhou, 7 Patentee before: SHANDONG HIRONG POWER SUPPLY MATERIAL Co.,Ltd. |
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Effective date of registration: 20211126 Address after: 256800 No. 7 Qingfeng six road, Chengbei Industrial Park, Zhanhua District, Binzhou, Shandong. Patentee after: SHANDONG HIRONG POWER SUPPLY MATERIAL Co.,Ltd. Address before: Room 102, building 5, science and technology enterprise accelerator, 17 xinghuahe, Dongying District, Dongying City, Shandong Province 257100 Patentee before: Dongying gurun special new energy Co., Ltd |