CN116008264A - Method for detecting impurities in lithium tetrafluoroborate - Google Patents
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- CN116008264A CN116008264A CN202310080018.6A CN202310080018A CN116008264A CN 116008264 A CN116008264 A CN 116008264A CN 202310080018 A CN202310080018 A CN 202310080018A CN 116008264 A CN116008264 A CN 116008264A
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- -1 lithium tetrafluoroborate Chemical compound 0.000 title claims abstract description 55
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 title claims abstract description 53
- 239000012535 impurity Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 111
- 239000000243 solution Substances 0.000 claims abstract description 66
- 238000004448 titration Methods 0.000 claims abstract description 44
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000005457 ice water Substances 0.000 claims abstract description 17
- ZPLCXHWYPWVJDL-UHFFFAOYSA-N 4-[(4-hydroxyphenyl)methyl]-1,3-oxazolidin-2-one Chemical compound C1=CC(O)=CC=C1CC1NC(=O)OC1 ZPLCXHWYPWVJDL-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 10
- 239000012085 test solution Substances 0.000 claims abstract description 9
- 238000005303 weighing Methods 0.000 claims abstract description 6
- 239000000523 sample Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 7
- 229910052796 boron Inorganic materials 0.000 claims description 7
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 6
- CEQFOVLGLXCDCX-WUKNDPDISA-N methyl red Chemical compound C1=CC(N(C)C)=CC=C1\N=N\C1=CC=CC=C1C(O)=O CEQFOVLGLXCDCX-WUKNDPDISA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 4
- 239000012086 standard solution Substances 0.000 claims description 4
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 3
- 229930195725 Mannitol Natural products 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 230000003301 hydrolyzing effect Effects 0.000 claims description 3
- 239000000594 mannitol Substances 0.000 claims description 3
- 235000010355 mannitol Nutrition 0.000 claims description 3
- 239000012496 blank sample Substances 0.000 claims description 2
- 238000005562 fading Methods 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- 238000001514 detection method Methods 0.000 description 10
- 230000006872 improvement Effects 0.000 description 8
- 238000000354 decomposition reaction Methods 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 229910013063 LiBF 4 Inorganic materials 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 229910003002 lithium salt Inorganic materials 0.000 description 2
- 159000000002 lithium salts Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 235000002639 sodium chloride Nutrition 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000000010 aprotic solvent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000001301 oxygen Chemical group 0.000 description 1
- 229910052760 oxygen Chemical group 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229960002668 sodium chloride Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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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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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides a method for detecting impurities in lithium tetrafluoroborate, which comprises the following steps: s1, preparing a sodium hydroxide standard titration solution and a bromothymol blue indicator solution; s2, weighing a lithium tetrafluoroborate sample into ice water to be dissolved, wherein the temperature of the ice water is 0-6 ℃; s3, dropwise adding the bromothymol blue indicator solution, and titrating by using the sodium hydroxide standard titration solution until the indicator changes from yellow green to light blue, namely, the end point is obtained, wherein the content of free acid in impurities in lithium tetrafluoroborate is obtained: omega= (V-V) 0 ）*C*M/(m*10 ‑3 ) Wherein V is the volume of sodium hydroxide standard titration solution consumed by titration of the test solution, and the unit is milliliter; v (V) 0 The volume of the sodium hydroxide standard titration solution consumed for titration of the blank test solution is in milliliters; c is hydrogenSodium oxide standard titration solution concentration in moles per liter; m is the mass of the sample in grams; m is the molar mass of hydrofluoric acid in grams per mole.
Description
Technical Field
The invention relates to a method for detecting impurities in lithium tetrafluoroborate.
Background
Currently, lithium tetrafluoroborate, molecular formula LiBF 4 The molecular weight is 93.74, and the lithium salt is mainly used as electrolyte lithium salt for lithium ion battery electrolyte. The classical electrolyte system used in lithium ion secondary batteries is that electrolyte salts are dissolved in organic aprotic solvents. And lithium tetrafluoroborate (LiBF 4) has better chemical stability and thermal stability, is sensitive to environmental water distribution, and is hopefully developed into an excellent electrolyte system widely used in the fields of energy storage and power lithium ion batteries. At present, the preparation method of lithium tetrafluoroborate comprises an aqueous solution method, wherein hydrofluoric acid, boric acid and lithium carbonate are generally adopted as raw materials in the aqueous solution method, the process conditions are mild, and impurities in the method generally contain higher impurities, such as free hydrofluoric acid and the like, so that the impurities need to be detected.
Disclosure of Invention
The invention provides a method for detecting impurities in lithium tetrafluoroborate, which can effectively solve the problems.
The invention is realized in the following way:
the method for detecting the impurities in the lithium tetrafluoroborate comprises the following steps:
s1, preparing a sodium hydroxide standard titration solution and a bromothymol blue indicator solution;
s2, weighing a lithium tetrafluoroborate sample into ice water to be dissolved, wherein the temperature of the ice water is 0-6 ℃;
s3, dropwise adding the bromothymol blue indicator solution, and titrating by using the sodium hydroxide standard titration solution until the indicator changes from yellow green to light blue, namely, the end point is obtained, wherein the content of free acid in impurities in lithium tetrafluoroborate is obtained: omega= (V-V) 0 ）*C*M/(m*10 -3 ) Wherein V is hydrogen and oxygen consumed by titration of the test solutionThe volume of the sodium-chloride standard titration solution is in milliliters; v (V) 0 The volume of the sodium hydroxide standard titration solution consumed for titration of the blank test solution is in milliliters; c is the concentration of a sodium hydroxide standard titration solution, and the unit is mol per liter; m is the mass of the sample in grams; m is the molar mass of hydrofluoric acid in grams per mole.
The beneficial effects of the invention are as follows: according to the invention, the lithium tetrafluoroborate solution is titrated by a sodium hydroxide standard titration solution, and bromothymol blue is used as an indicator, so that the method is simple in operation, high in accuracy, convenient and quick in detection. Furthermore, the lithium tetrafluoroborate sample is dissolved into ice water, so that the decomposition of the lithium tetrafluoroborate in the water can be inhibited, and the detection accuracy is remarkably improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a flowchart of a method for detecting impurities in lithium tetrafluoroborate according to an embodiment of the present invention.
Fig. 2 is a flowchart of a method for detecting impurities in lithium tetrafluoroborate according to another embodiment of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention. Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, based on the embodiments of the invention, which are apparent to those of ordinary skill in the art without inventive faculty, are intended to be within the scope of the invention.
In the description of the present invention, the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
Referring to fig. 1, an embodiment of the present invention provides a method for detecting impurities in lithium tetrafluoroborate, including the following steps:
s1, preparing a sodium hydroxide standard titration solution and a bromothymol blue indicator solution;
s2, weighing a lithium tetrafluoroborate sample into ice water to be dissolved, wherein the temperature of the ice water is 0-6 ℃;
s3, dropwise adding the bromothymol blue indicator solution, and titrating by using the sodium hydroxide standard titration solution until the indicator changes from yellow green to light blue, namely, the end point is obtained, wherein the content of free acid in impurities in lithium tetrafluoroborate is obtained: omega= (V-V) 0 ）*C*M/(m*10 -3 ) Wherein V is the volume of sodium hydroxide standard titration solution consumed by titration of the test solution, and the unit is milliliter; v (V) 0 The volume of the sodium hydroxide standard titration solution consumed for titration of the blank test solution is in milliliters; c is the concentration of a sodium hydroxide standard titration solution, and the unit is mol per liter; m is the mass of the sample in grams; m is the molar mass of hydrofluoric acid in grams per mole.
As a further improvement, the concentration of the sodium hydroxide standard titration solution is 0.005-0.02 mol/L. In one example, the concentration of the sodium hydroxide standard titration solution is 0.01mol/L. Because of the low content of impurity acids in lithium tetrafluoroborate, it is necessary to use a standard titration solution of sodium hydroxide with a low concentration for titration, otherwise, the solution is easy to be excessive and exceeds the titration endpoint.
As a further improvement, the concentration of the bromothymol blue indicator solution is 0.5 g-5 g/L.
As a further improvement, the concentration of the lithium tetrafluoroborate sample in ice water is 20-50 g/L.
The lithium tetrafluoroborate sample is stable in dry air and is decomposed in wet air, when the lithium tetrafluoroborate sample is dissolved in water at normal temperature, the aqueous solution is slowly decomposed, and when acid is added, the lithium tetrafluoroborate sample is more severely decomposed, and the reaction equation is as follows:
LiBH 4 + 4H 2 O —→ Li[B(OH) 4 ] + 4H 2 ↑
2LiBH 4 + 2HF —→ 2LiF + B 2 H 6 + 2H 2 ↑。
since lithium tetrafluoroborate itself contains a trace amount of hydrofluoric acid, it accelerates the decomposition of lithium tetrafluoroborate when dissolved in water, and is disadvantageous for the final detection result. In order to suppress the accelerated decomposition of lithium tetrafluoroborate by hydrofluoric acid without affecting the detection of hydrofluoric acid, it is preferable to dissolve a lithium tetrafluoroborate sample in ice water, so that the decomposition of lithium tetrafluoroborate in water can be suppressed. As a further improvement, preferably, the temperature of the ice water is 1-2 ℃.
As a further improvement, during titration, a class A glass clip-on micro-titer tube was used, with a minimum index of 0.01ml.
As a further improvement, in order to prevent the decomposition of lithium tetrafluoroborate from ultimately affecting the detection result, it is necessary to complete the titration as soon as possible. The titration time is controlled to be completed within 2-5min, and the deviation of the detection result (the deviation from the mean value) can be controlled to be within 5%. More preferably, the titration time is controlled within 2min, and can be controlled within 2%. The time exceeds 5 minutes, and the deviation of the detection result is more than 10%.
Embodiment one:
100ml ice water was added to the flask and 3-4 pieces of small ice were added to control the temperature to 1.+ -. 1 ℃ and 10 drops of bromothymol blue indicator were added to the ice water. About 3g of the sample was weighed in 4 portions by the decrement method (as shown in Table 1) to an accuracy of 0.0001g, and the sample was rapidly poured into a flask containing ice water, and the flask was shaken to rapidly dissolve the sample. And (3) rapidly titrating by using sodium hydroxide standard titration solution (0.01 mol/L), and shaking the triangular flask while dripping until the indicator changes from yellow-green to light blue (completed within 5 minutes), wherein the end point is the end point, and the temperature of the solution at the end point is still kept at 1+/-1 ℃.
Blank tests were performed simultaneously. The blank test solution is the same as the test solution in the types and amounts of other reagents added except for the absence of the test sample.
By calculation, the content omega of the free acid is about 170 mg/Kg; the average value was 167.88mg/Kg and the standard deviation was 3.15.
| Sample numbering | Sample mass (g) | Sample consumption NaOH (mL) | Results (mg/Kg) |
| Blank space | 0.00 | 0.03 | —— |
| 1 | 3.1059 | 2.58 | 164.29 |
| 2 | 3.1147 | 2.64 | 167.67 |
| 3 | 3.1885 | 2.70 | 167.57 |
| 4 | 3.1996 | 2.78 | 171.98 |
Referring to fig. 2, in an embodiment of the present invention, as a further improvement, the method for detecting an impurity in lithium tetrafluoroborate may further include a method for detecting boron in an impurity in lithium tetrafluoroborate, which specifically includes:
s4, accurately weighing a lithium tetrafluoroborate sample; 25mL of 20wt% calcium nitrate solution and 25mL of water are added, and a methyl red indicator is added dropwise;
s5, titrating with 1mol/L sodium hydroxide solution, and changing the solution from red to yellow;
s6, boiling, heating, hydrolyzing, taking out and cooling to room temperature in a constant-temperature water bath kettle;
s7, dropwise adding a methyl red indicator, and neutralizing with 1mol/L sodium hydroxide solution until the color of the solution turns light yellow;
s8, titrating with 0.1mol/L hydrochloric acid until the solution becomes red;
s9, adding 5 drops of phenolphthalein and 2g of mannitol, and titrating with 0.1mol/L sodium hydroxide solution to change the solution from red to light yellow and then to reddish, wherein the end point is the red without fading, and the content of boron in impurities in lithium tetrafluoroborate is as follows: omega 1 =（V 1 -V 2 ）*C 1 *M 1 /(m 1 *1000)*100%，V 1 The volume of the sodium hydroxide standard solution consumed by the solution is in milliliters; v (V) 2 The volume of the sodium hydroxide standard solution consumed for the blank sample is in milliliters; c (C) 1 The molar concentration of the standard titration solution is expressed in mol per liter; m is M 1 Is the molar mass of boron in grams per mole; m is m 1 The mass of the sample is given in grams.
In the step S4, the calcium nitrate solution is added to form a precipitate with impurities in the lithium tetrafluoroborate sample, so that the effect of removing impurities is achieved, and the interference of other impurities on the detection result is prevented.
Further, in step S4, a methyl red indicator is added, the color change range of the methyl red is PH4.4-6.2, the color change range is orange when the PH value is in the range of 4.4-6.2, the color change range is red when the PH value is < = 4.4, and the color change range is yellow when the PH value is > = 6.2. In step S5, the pH is titrated to 6.2 or higher by sodium hydroxide solution, i.e., to weak acidity or neutrality. The purpose of titration to weakly acidic or neutral is to first exclude interference from other acidic species in the solution.
In the step S6, the action of boiling, heating, hydrolyzing, taking out and cooling to the room temperature in the constant-temperature water bath kettle is that the fluoboric acid is relatively stable in the concentrated solution and can be mixed with water or alcohol. Thus, it is rapidly decomposed in an aqueous solution by heating to form hydroxyfluoroboric acid (HBF) 3 OH) for subsequent detection. That is, the content of the hydroxy fluoroboric acid is detected subsequently, thereby indirectly obtaining the hydroxy fluoroboric acid.
In step S9, since boric acid is an extremely weak acid, it cannot be titrated directly with strong alkali sodium hydroxide, and mannitol is needed to strengthen boric acid, so that the apparent dissociation constant is increased, and thus the accuracy of detection can be improved.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, and various modifications and variations may be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The method for detecting the impurities in the lithium tetrafluoroborate is characterized by comprising the following steps of:
s1, preparing a sodium hydroxide standard titration solution and a bromothymol blue indicator solution;
s2, weighing a lithium tetrafluoroborate sample into ice water to be dissolved, wherein the temperature of the ice water is 0-6 ℃;
s3, dropwise adding the bromothymol blue indicator solution, and titrating by using the sodium hydroxide standard titration solution until the indicator changes from yellow green to light blue, namely, the end point is obtained, wherein the content of free acid in impurities in lithium tetrafluoroborate is obtained: omega= (V-V) 0 ）*C*M/(m*10 -3 ) Wherein V is the volume of sodium hydroxide standard titration solution consumed by titration of the test solution, and the unit is milliliter; v (V) 0 The volume of the sodium hydroxide standard titration solution consumed for titration of the blank test solution is in milliliters; c is the concentration of a sodium hydroxide standard titration solution, and the unit is mol per liter; m is the mass of the sample in grams; m is the molar mass of hydrofluoric acid in grams per mole.
2. The method for detecting impurities in lithium tetrafluoroborate as claimed in claim 1, wherein the concentration of the sodium hydroxide standard titration solution is 0.005-0.02 mol/L.
3. The method for detecting impurities in lithium tetrafluoroborate as claimed in claim 1, wherein the concentration of the bromothymol blue indicator solution is 0.5g to 5g/L.
4. The method for detecting impurities in lithium tetrafluoroborate according to claim 1, wherein the concentration of the lithium tetrafluoroborate sample in ice water is 20-50 g/L.
5. The method for detecting impurities in lithium tetrafluoroborate as claimed in claim 1, wherein the temperature of the ice water is 1-2 ℃.
6. The method for detecting impurities in lithium tetrafluoroborate as claimed in claim 1, further comprising: a class A glass clip-on micro-titer tube was used, with a minimum index of 0.01ml.
7. The method for detecting impurities in lithium tetrafluoroborate as claimed in claim 1, wherein the titration time is controlled to be completed within 2 to 5 minutes.
8. The method for detecting impurities in lithium tetrafluoroborate as claimed in claim 1, further comprising: and detecting boron in impurities in the lithium tetrafluoroborate.
9. The method for detecting impurities in lithium tetrafluoroborate as claimed in claim 1, wherein the step of detecting boron in impurities in lithium tetrafluoroborate comprises:
s4, accurately weighing a lithium tetrafluoroborate sample; 25mL of 20wt% calcium nitrate solution and 25mL of water are added, and a methyl red indicator is added dropwise;
s5, titrating with 1mol/L sodium hydroxide solution, and changing the solution from red to yellow;
s6, boiling, heating, hydrolyzing, taking out and cooling to room temperature in a constant-temperature water bath kettle;
s7, dropwise adding a methyl red indicator, and neutralizing with 1mol/L sodium hydroxide solution until the color of the solution turns light yellow;
s8, titrating with 0.1mol/L hydrochloric acid until the solution becomes red;
s9, adding 5 drops of phenolphthalein and 2g of mannitol, and titrating with 0.1mol/L sodium hydroxide solution to change the solution from red to light yellow and then to reddish, wherein the end point is the red without fading, and the content of boron in impurities in lithium tetrafluoroborate is as follows: omega 1 =（V 1 -V 2 ）*C 1 *M 1 /(m 1 *1000)*100%，V 1 The volume of the sodium hydroxide standard solution consumed by the solution is in milliliters; v (V) 2 The volume of the sodium hydroxide standard solution consumed for the blank sample is in milliliters; c (C) 1 Is the molar concentration of the standard titration solution, unitIn moles per liter; m is M 1 Is the molar mass of boron in grams per mole; m is m 1 The mass of the sample is given in grams.
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