CN114280117A - Method for measuring free fluorine content in 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer - Google Patents
Method for measuring free fluorine content in 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer Download PDFInfo
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- 239000011737 fluorine Substances 0.000 title claims abstract description 67
- 229920001577 copolymer Polymers 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 52
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims description 50
- 238000001514 detection method Methods 0.000 claims abstract description 28
- 239000000243 solution Substances 0.000 claims description 67
- -1 methyl 2-fluoroacrylate-pentaerythritol Chemical compound 0.000 claims description 34
- 239000012086 standard solution Substances 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 15
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 11
- 239000006228 supernatant Substances 0.000 claims description 10
- 238000005259 measurement Methods 0.000 claims description 9
- 239000007974 sodium acetate buffer Substances 0.000 claims description 9
- 238000003260 vortexing Methods 0.000 claims description 6
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- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 abstract 3
- 229940079593 drug Drugs 0.000 abstract 1
- 239000011550 stock solution Substances 0.000 description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 11
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
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- FYRWKWGEFZTOQI-UHFFFAOYSA-N 3-prop-2-enoxy-2,2-bis(prop-2-enoxymethyl)propan-1-ol Chemical compound C=CCOCC(CO)(COCC=C)COCC=C FYRWKWGEFZTOQI-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
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- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 208000002682 Hyperkalemia Diseases 0.000 description 1
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to the field of medicine quality control, in particular to a method for measuring the content of free fluorine in a 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer. The determination method comprises the following steps: and detecting the content of free fluorine in the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer by using an electrode method. The method can efficiently and specifically detect the content of free fluorine in the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer so as to meet the requirement of controlling the quality of 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer medicines and produce high-quality qualified products. The method is simple to operate, low in detection cost, high in sensitivity and high in accuracy.
Description
Technical Field
The invention relates to the field of medicine quality control, in particular to a method for measuring the content of free fluorine in a 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer.
Background
The 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer is a novel oral potassium ion binding agent and is used for treating adult patients with hyperkalemia. The 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer contains fluorine structurally, the medicine belongs to non-absorbable cation exchange polymer, but a trace amount of fluorine exists in a free state, and the free fluorine enters a digestive system along with the medicine.
Soluble fluorine is almost completely absorbed in the digestive tract, can quickly reach blood circulation, is combined with plasma albumin to inhibit enzyme activity, enters various tissues through capillary walls, and causes kidney injury, influences liver metabolism and causes skeletal lesion. The content of free fluorine in the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer directly affects the safety of the medicine, so that it is very important to accurately measure the content of free fluorine in the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer.
At present, no relevant literature and no patent report about a method for detecting the content of free fluorine in a 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer, and therefore, a method for detecting the content of free fluorine in the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer needs to be designed.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention provides a method for measuring the content of free fluorine in a 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer, which can efficiently and specifically detect the content of the free fluorine in the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer, and has the advantages of simple operation, low detection cost, high sensitivity and high accuracy.
The invention is realized by the following steps:
in a first aspect, an embodiment of the present invention provides a method for determining a free fluorine content in a 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer, including: and detecting the content of free fluorine in the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer by using an electrode method.
Further, in a preferred embodiment of the present invention, the method comprises: mixing the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer with water, taking supernatant, and adding an ionic strength regulator to form a solution to be tested;
then, detecting the solution to be detected by using an electrode method, and obtaining the content of free fluorine in the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer according to the detection result;
preferably, the volume ratio of the ionic strength modifier to the supernatant is 1: 1.2 to 1.2: 1, preferably 1: 1.
further, in a preferred embodiment of the present invention, the method comprises: inserting an electrode into the solution to be detected, reading the concentration of the fluorine ions in the solution to be detected, and calculating according to the following formula to obtain the content of the fluorine ions;
in the formula: w is the content of free fluorine in the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer, ug/ml;
m is the weighing sample amount of the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer, g;
c is the concentration of the fluorine ions in the solution to be detected, ug/ml;
v is the volume of the solution to be detected, and ml.
Further, in a preferred embodiment of the present invention, the ionic strength regulator is a sodium acetate buffer solution with a pH value of 5.0-5.5, preferably a sodium acetate buffer solution with a pH value of 5.5.
Further, in a preferred embodiment of the present invention, the concentration of the fluorine ions in the solution to be tested is 1ug/ml to 10ug/ml, preferably 5 ug/ml.
Further, in a preferred embodiment of the present invention, in the detection process, the time for inserting the electrode into the solution to be detected before reading the detection result is at least 10s, preferably 30 s.
Further, in a preferred embodiment of the present invention, the detection temperature is in the range of 0 ℃ to 80 ℃, preferably 25 ℃.
Further, in a preferred embodiment of the present invention, the level of the electrode reference solution during the detection is at least 2.5cm, preferably 5cm, higher than the level of the solution to be detected.
Further, in a preferred embodiment of the present invention, the method comprises: before detecting the solution to be detected, correcting the electrode;
preferably, the correcting the electrode comprises: carrying out multi-point correction on the electrode by using standard solutions with various known concentrations;
preferably, the correction slope should be between 90% and 110%, preferably between 95% and 105%.
Further, in a preferred embodiment of the present invention, the mixing of the methyl 2-fluoroacrylate-pentaerythritol triallyl ether copolymer with water comprises: any one of vortexing, sonication, and shaking, preferably vortexing; preferably, the mixing time is from 10min to 30min, preferably 20 min.
The invention has the beneficial effects that: the embodiment of the invention adopts an electrode method to efficiently and specifically detect the content of free fluorine in the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer so as to meet the requirement of controlling the quality of the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer medicine and produce high-quality qualified products. The method is simple to operate, low in detection cost, high in sensitivity and high in accuracy.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following examples provide specific illustrations of the method for determining the free fluorine content of a 2-fluoroacrylate-pentaerythritol triallyl ether copolymer.
The embodiment of the invention provides a method for measuring the content of free fluorine in a 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer, which comprises the following steps:
s1, correcting electrodes;
the electrode is subjected to multipoint correction, specifically, the electrode is subjected to multipoint correction by using various standard solutions with known concentrations, and the correction slope is 90-110%, preferably 95-105%. For example, the correction slope is any value between 90% and 110%, such as 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99%, 100%, 101%, 102%, 103%, 104%, 105%, 106%, 107%, 108%, 109%, and 110%.
It should be noted that, as long as the standard solution is a standard solution whose fluoride ion concentration is known and whose corrected slope satisfies the above requirements, the examples of the present invention are merely illustrative of the concentration and preparation method of the standard solution, and do not mean that only a plurality of standard solutions provided by the examples of the present invention can be used.
Specifically, the present example uses five standard solutions of known concentration for multi-point calibration of the electrodes.
First, a stock solution of standard solution was prepared: diluting 1000ug/ml of fluoride ion solution with deionized water to obtain stock solutions with fluoride ion concentrations of 2ug/ml, 4ug/ml, 10ug/ml, 16ug/ml and 20 ug/ml.
Then, a standard solution was prepared: the stock solutions of the five standard solutions are respectively mixed with an ionic strength regulator in equal amount to form standard solutions, and the fluorine ion concentrations of the five standard solutions are respectively 1ug/ml, 2ug/ml, 5ug/ml, 8ug/ml and 10 ug/ml.
Then, a correction is made, the correction slope being between 90% and 110%, preferably between 95% and 105%.
S2, preparing a solution to be detected;
weighing the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer, mixing the copolymer with water for extraction, standing, taking supernatant, adding an ionic strength regulator, and uniformly mixing to form a solution to be detected. Wherein the volume ratio of the ionic strength regulator to the supernatant is 1: 1.2 to 1.2: 1, preferably 1: 1, preferably adding an equal amount of the ionic strength regulator.
The water extraction can ensure that fluorine on the structure of the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer does not fall off, thereby achieving the purpose of specifically detecting the content of free fluorine. The ionic strength regulator is used for complexing metal ions in the solution, and improves the detection sensitivity of fluorine.
Further, in order to promote that free fluorine in the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer can be fully dissolved and ensure the accuracy of the detection effect, the mixing mode comprises the following steps: any one of vortexing, sonication, and shaking, preferably vortexing; preferably, the mixing time is from 10min to 30min, preferably 20 min. For example, the mixing time is 10-30min such as 10min, 12min, 15min, 18min, 20min, 23min, 25min, 27min and 30 min.
Further, the ionic strength regulator is sodium acetate buffer solution with pH value of 5.0-5.5, preferably sodium acetate buffer solution with pH value of 5.5. The selection of the ionic strength regulator has a significant influence on the detection of the fluoride ions in the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer, the change of the pH of the ionic strength regulator or the change of the pH of a sodium acetate buffer solution may cause that the fluoride ions in the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer cannot be detected or the accuracy of the detection result is influenced, and the content of the fluoride ions in the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer can be efficiently and accurately detected by using the ionic strength regulator.
S3, measuring the content of free fluorine;
and detecting the solution to be detected by using an electrode method, and obtaining the content of free fluorine in the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer according to the detection result. Specifically, inserting an electrode into the solution to be detected, reading the concentration of fluorine ions in the solution to be detected, and calculating according to the following formula to obtain the content of the fluorine ions;
in the formula: w is the middle stream of the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer
Free fluorine content, ug/ml;
m is the weighed amount of the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer, g;
c is the concentration of the fluorine ions in the solution to be detected, ug/ml;
v is the volume of the solution to be detected, and ml.
Furthermore, the concentration of the fluorine ions in the solution to be detected is 1ug/ml to 10ug/ml, preferably 5 ug/ml. For example, the fluoride ion concentration is 1ug/ml, 2ug/ml, 3ug/ml, 4ug/ml, 5ug/ml, 6ug/ml, 7ug/ml, 8ug/ml, 9ug/ml, 10ug/ml, etc., and any value between 1 and 10 ug/ml.
Further, the electrode fill hole should be kept open during the measurement, so that the level of the electrode reference solution is at least 2.5cm, preferably 5cm, above the level of the solution to be measured.
Further, the detection temperature is in the range of 0 ℃ to 80 ℃, and the preferred temperature is 25 ℃. For example, the temperature is 0 ℃, 10 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃ and 80 ℃, etc., and any value between 0 ℃ and 80 ℃.
Further, the solution to be detected and the standard solution should be at the same temperature to ensure the accuracy of the detection result.
Further, in order to ensure the accuracy of the detected result, the electrode needs a sufficient stabilization time, and the time for inserting the electrode into the solution to be detected before the measurement is at least 10s, preferably 30 s.
Further, the measuring process should use a teflon container to contain the solution to be measured.
The following will specifically describe the method for determining the free fluorine content in the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer provided by the present invention with reference to specific examples.
Example 1
This example provides a method for determining a free fluorine content in a 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer, including:
s1, correcting electrodes;
diluting 1000ug/ml of fluoride ion solution with deionized water to obtain stock solutions with fluoride ion concentrations of 2ug/ml, 4ug/ml, 10ug/ml, 16ug/ml and 20 ug/ml.
Then, a standard solution was prepared: the stock solutions of the five standard solutions are respectively mixed with an ionic strength regulator in equal amount to form standard solutions, and the fluorine ion concentrations of the five standard solutions are respectively 1ug/ml, 2ug/ml, 5ug/ml, 8ug/ml and 10 ug/ml.
The five standard solutions with known concentrations are used for carrying out multi-point correction on the electrode, and the correction slope is 99%.
S2, preparing a solution to be detected;
weighing 2 g of methyl fluoroacrylate-pentaerythritol triallyl ether copolymer (the preparation process comprises the steps of preparing a uniform oil phase from 2-methyl fluoroacrylate, pentaerythritol triallyl ether and benzoyl peroxide, preparing a water phase from a solution of ethanol and sodium chloride in a reaction kettle, adding the oil phase into the water phase under stirring, gradually heating for polymerization), placing the mixture into a centrifuge tube, adding 20ml of deionized water, performing vortex extraction for 20min, standing, taking 8ml of supernatant, placing the supernatant into a beaker, adding an equivalent amount of ionic strength regulator, uniformly mixing to obtain a solution to be measured, and preparing 6 parts in parallel. Wherein the ionic strength regulator is sodium acetate buffer solution with pH of 5.5.
S3, measuring the content of free fluorine;
inserting an electrode into the solution to be detected, reading the concentration of the fluorine ions in the solution to be detected, and calculating according to the following formula to obtain the content of the fluorine ions;
in the formula: w is the content of free fluorine in the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer, ug/ml;
m is the weighed amount of the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer, g;
c is the concentration of the fluorine ions in the solution to be detected, ug/ml;
v is the volume of the solution to be detected, and ml.
The amount of free fluorine in the methyl 2-fluoroacrylate-pentaerythritol triallyl ether copolymer of this example was calculated to be 61 ppm.
Wherein the liquid level of the electrode reference solution is 5cm higher than that of the solution to be detected, the solution to be detected and the standard solution are at the same temperature, the detection temperature is 25 ℃, the electrode is inserted into the solution to be detected for 30s, and a polytetrafluoroethylene container is used for containing the solution to be detected.
Verification example
The specificity, sensitivity, linearity, repeatability and accuracy of the method for measuring the content of free fluorine in the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer provided by the embodiment of the invention are verified, the method is as shown in the embodiment 1, and only the detection solutions are different, specifically as follows;
blank solution: 8ml of deionized water was mixed with an equal amount of ionic strength adjuster.
Detection limiting solution: diluting 1000ug/ml of fluoride ion solution with deionized water to obtain 0.6ug/ml stock solution, and mixing the stock solution with ionic strength regulator to obtain 0.3ug/ml detection limit solution.
Quantitative limiting solution: diluting 1000ug/ml of fluoride ion solution with deionized water to obtain 1.8ug/ml stock solution, and mixing the stock solution with ionic strength regulator to obtain 0.9ug/ml limit solution.
Recovery of stock solution: a stock solution having a concentration of 3ug/ml was prepared by diluting 1000ug/ml of the fluoride ion solution with deionized water.
Accuracy test solution: placing 1g of 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer in a centrifuge tube, adding 20ml of recovery rate stock solution, performing vortex extraction for 20min, standing, taking 8ml of supernatant, placing in a beaker, adding an equivalent amount of ionic strength regulator, uniformly mixing, and preparing 6 parts serving as a solution to be detected in parallel.
The results are shown in tables 1 to 4.
TABLE 1 specificity and sensitivity
| Sample name | Fluorine concentration (ug/ml) |
| Blank solution | 0.02 |
| Detection limit | 0.3 |
| Limit of quantification | 0.9 |
TABLE 2 method linearity
TABLE 3 method repeatability
TABLE 4 method accuracy
| Sample name | Background volume (ug) | Adding scalar quantity (ug) | Measurement (ug) | Recovery rate |
| Sample 1 | 63 | 60 | 126 | 105％ |
| Sample 2 | 62 | 60 | 124 | 103％ |
| Sample 3 | 61 | 60 | 125 | 107％ |
| Sample No. 4 | 64 | 60 | 127 | 105％ |
| Sample No. 5 | 64 | 60 | 125 | 102％ |
| Sample No. 6 | 65 | 60 | 128 | 105％ |
As can be seen from tables 1 to 4, the detection limit of the method for determining the content of free fluorine in the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer provided by the embodiment of the invention is 0.3ug/ml, the blank solution does not interfere with the detection (the measured value of the blank solution is less than the measured value of the detection limit solution), and the method has high specificity and sensitivity; the linearity is judged by the electrode correction slope, the slope is 99 percent, the range of 90 percent to 110 percent of the electrode correction slope requirement can be met, and the method has good linearity; judging the repeatability by using RSD, wherein the repeatability meets the requirement that the RSD with the content of more than 10ppm in Chinese pharmacopoeia is less than 6 percent; the accuracy is judged by the recovery rate, the recovery rate can meet the requirement that the recovery rate range with the content of more than 100ppm in Chinese pharmacopoeia is 85-110 percent, and the method is proved to have high accuracy.
Comparative example 1: the measurement was carried out with reference to the method for measuring the content of free fluorine in the copolymer of methyl 2-fluoroacrylate-pentaerythritol triallylether provided in example 1, except that the ionic strength adjusting agent was a sodium acetate buffer solution having a pH of 2.5.
The detection accuracy is 62-65%, and the comparison and analysis with the result of example 1 shows that the reduction of the pH of the ionic strength regulator has a direct influence on the accuracy of the result.
The specific results are shown in table 5 below:
TABLE 5 accuracy
| Sample name | Background volume (ug) | Adding scalar quantity (ug) | Measurement (ug) | Recovery rate |
| Sample 1 | 59 | 60 | 98 | 65％ |
| Sample 2 | 58 | 60 | 95 | 62％ |
| Sample 3 | 62 | 60 | 99 | 62％ |
| Sample No. 4 | 63 | 60 | 101 | 63％ |
| Sample No. 5 | 61 | 60 | 100 | 65％ |
| Sample No. 6 | 62 | 60 | 101 | 65％ |
Comparative example 2: the measurement was performed with reference to the method for measuring the content of free fluorine in the 2-fluoroacrylate-pentaerythritol triallyl ether copolymer provided in example 1, except that the ratio of the ionic strength modifier to the supernatant was 1: 3.
the detection accuracy is 70-75%, and the comparison and analysis with the result of example 1 shows that the reduction of the addition amount of the ionic strength regulator has a direct influence on the accuracy of the result.
Specific results are shown in table 6 below:
TABLE 6 accuracy
| Sample name | Background volume (ug) | Adding scalar quantity (ug) | Measurement (ug) | Recovery rate |
| Sample 1 | 62 | 60 | 106 | 73％ |
| Sample 2 | 64 | 60 | 107 | 72％ |
| Sample 3 | 58 | 60 | 103 | 75％ |
| Sample No. 4 | 60 | 60 | 103 | 72％ |
| Sample No. 5 | 62 | 60 | 104 | 70％ |
| Sample No. 6 | 63 | 60 | 106 | 72％ |
Comparative example 3: the measurement was carried out with reference to the method for measuring the free fluorine content in the copolymer of methyl 2-fluoroacrylate-pentaerythritol triallylether provided in example 1, except that the substance to be measured was calcium chloride.
The detection accuracy is 12% -18%, and the comparison and analysis with the result of the example 1 show that the method has specific detection on the content of free fluorine in the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer.
The specific results are shown in table 7 below:
TABLE 7 accuracy
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for measuring the content of free fluorine in a 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer is characterized by comprising the following steps: and detecting the content of free fluorine in the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer by using an electrode method.
2. The method of claim 1 for determining the free fluorine content of a copolymer of methyl 2-fluoroacrylate-pentaerythritol triallyl ether, comprising: mixing the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer with water, then taking supernatant, then adding an ionic strength regulator to form a solution to be tested,
then, detecting the solution to be detected by using an electrode method, and obtaining the content of free fluorine in the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer according to the detection result;
preferably, the volume ratio of the ionic strength modifier to the supernatant is 1: 1.2 to 1.2: 1, preferably 1: 1.
3. the method of claim 2, wherein the method comprises: inserting an electrode into the solution to be detected, reading the concentration of the fluorine ions in the solution to be detected, and calculating according to the following formula to obtain the content of the fluorine ions;
in the formula: w is the content of free fluorine in the 2-methyl fluoroacrylate-pentaerythritol triallyl ether copolymer, ug/ml;
m is the weighing sample amount of the 2-fluoro methyl acrylate-pentaerythritol triallyl ether copolymer, g;
c is the concentration of the fluorine ions in the solution to be detected, ug/ml;
v is the volume of the solution to be detected, and ml.
4. The method for determining the content of free fluorine in a methyl 2-fluoroacrylate-pentaerythritol triallylether copolymer according to claim 2 or 3, wherein the ionic strength modifier is a sodium acetate buffer solution having a pH of 5.0 to 5.5, preferably a sodium acetate buffer solution having a pH of 5.5.
5. The method for determining the content of free fluorine in the copolymer of methyl 2-fluoroacrylate-pentaerythritol triallyl ether according to claim 2 or 3, wherein the concentration of the fluoride ions in the solution to be determined is 1ug/ml to 10ug/ml, preferably 5 ug/ml.
6. The method for determining the content of free fluorine in a copolymer of methyl 2-fluoroacrylate-pentaerythritol triallyl ether according to claim 2, wherein the time for inserting an electrode into the solution to be tested during the test is at least 10s, preferably 30s, before the test result is read.
7. The method for determining the content of free fluorine in a copolymer of methyl 2-fluoroacrylate-pentaerythritol triallyl ether according to claim 2, wherein the detection temperature is in the range of 0 ℃ to 80 ℃, preferably 25 ℃.
8. The method for determining the content of free fluorine in a copolymer of methyl 2-fluoroacrylate-pentaerythritol triallylether according to claim 2, wherein the level of the electrode reference solution during the measurement is at least 2.5cm, preferably 5cm, higher than the level of the solution to be measured.
9. The method for determining the free fluorine content in a methyl 2-fluoroacrylate-pentaerythritol triallyl ether copolymer according to any one of claims 6 to 8, comprising: before detecting the solution to be detected, correcting the electrode;
preferably, the correcting the electrode comprises: carrying out multi-point correction on the electrode by using standard solutions with various known concentrations;
preferably, the correction slope should be between 90% and 110%, preferably between 95% and 105%.
10. The method of claim 2, wherein the mixing of the methyl 2-fluoroacrylate-pentaerythritol triallyl ether copolymer with water comprises: any one of vortexing, sonication, and shaking, preferably vortexing; preferably, the mixing time is from 10min to 30min, preferably 20 min.
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| CN102937614A (en) * | 2012-11-14 | 2013-02-20 | 中国科学院青海盐湖研究所 | Method for analyzing content of free fluorin in lithium ion battery electrolyte salt LiBF4 |
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| CN102937614A (en) * | 2012-11-14 | 2013-02-20 | 中国科学院青海盐湖研究所 | Method for analyzing content of free fluorin in lithium ion battery electrolyte salt LiBF4 |
| CN107271530A (en) * | 2017-07-17 | 2017-10-20 | 云南云天化股份有限公司 | A kind of method of Oil repellent in fluorine-containing organic solvent of Accurate Determining |
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