CN110824101B - Method for measuring functional groups on surface of carbon fiber - Google Patents
Method for measuring functional groups on surface of carbon fiber Download PDFInfo
- Publication number
- CN110824101B CN110824101B CN201911112531.9A CN201911112531A CN110824101B CN 110824101 B CN110824101 B CN 110824101B CN 201911112531 A CN201911112531 A CN 201911112531A CN 110824101 B CN110824101 B CN 110824101B
- Authority
- CN
- China
- Prior art keywords
- sample
- solution
- bottle
- water
- weight
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 34
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 34
- 125000000524 functional group Chemical group 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 28
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000000523 sample Substances 0.000 claims abstract description 126
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 57
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000012496 blank sample Substances 0.000 claims abstract description 20
- 239000000835 fiber Substances 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 91
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 60
- 238000005303 weighing Methods 0.000 claims description 24
- 238000004140 cleaning Methods 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 17
- 238000004448 titration Methods 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 13
- 238000007789 sealing Methods 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 13
- 239000012488 sample solution Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000011521 glass Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000012670 alkaline solution Substances 0.000 claims description 3
- 238000012544 monitoring process Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000460 chlorine Substances 0.000 abstract description 5
- 229910052801 chlorine Inorganic materials 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000002791 soaking Methods 0.000 abstract 1
- 238000005259 measurement Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000010079 rubber tapping Methods 0.000 description 2
- 239000008231 carbon dioxide-free water Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for measuring functional groups on the surface of carbon fibers in the field of carbon fibers. The method for measuring the functional groups on the surface of the carbon fiber comprises the steps of soaking a sample to be measured by using an excessive hydrochloric acid solution to convert the sample to be measured into chlorine-containing groups, adding a certain amount of sodium hydroxide solution with known concentration after the reaction is completed, titrating sodium hydroxide which does not react with the chlorine-containing groups by using hydrochloric acid, and simultaneously preparing a blank sample. Thereby calculating the concentration of functional groups on the surface of the fiber. The method has the advantages of short determination time, low cost and strong operability, and can meet the requirements of factory production.
Description
Technical Field
The invention relates to the field of carbon fibers, and in particular relates to a method for determining functional groups on the surface of carbon fibers.
Background
The carbon fiber is subjected to carbonization treatment in high-temperature inert gas at 1300-1600 ℃, and along with the escape of non-carbon elements and the enrichment of carbon elements, the activity of the surface of the carbon fiber is reduced, the surface tension is reduced, the wettability of the carbon fiber with matrix resin is reduced, the interlayer shear of the composite material is reduced, the surface of the carbon fiber is lyophobic, and the excellent performance of the carbon fiber is seriously affected. In order to convert the lyophobicity of the fiber surface to lyophilicity, the surface of the fiber needs to be treated. The chemical composition and the structural characteristics of the fiber surface determine the size of the free energy of the fiber surface, so that the wettability and the affinity between the fiber and resin are determined, and polar surface functional groups are commonly used for representing the surface characteristics of the carbon fiber.
The existing method for measuring the functional groups mainly comprises X-ray photoelectron spectroscopy (XPS), and the method has the defects of long processing time and high cost for measuring samples and can not meet the requirements of factory production.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for measuring functional groups on the surface of carbon fibers. The method has the advantages of short determination time, low cost and strong operability, and can meet the requirements of factory production.
According to the method for determining the functional groups on the surface of the carbon fiber, a sample to be measured is soaked by using an excessive hydrochloric acid solution to be converted into chlorine-containing groups, after the reaction is completed, a certain amount of sodium hydroxide solution with known concentration is added, sodium hydroxide which does not react with the chlorine-containing groups is titrated by using hydrochloric acid, and meanwhile, a blank sample is made. Thereby calculating the concentration of functional groups on the surface of the fiber.
One of the objectives of the present application is to provide a method for determining functional groups on the surface of carbon fibers, which may include the following steps:
1) weighing the weight of a carbon fiber sample to be measured, and reacting with an excessive acid solution;
2) cleaning samples with CO-free2Water replacement;
3) adding an alkaline solution;
4) weighing liquid, titrating a sample to be tested and a blank sample, and calculating a result.
Wherein,
the step 1) can comprise the following steps:
a) accurately weighing the weight of the sample, and placing the sample in a sample bottle; the weight of the sample is 5-15 g, and preferably 8-12 g;
b) adding acid, immersing the sample, stirring uniformly, sealing and standing.
The acid in the step b) is hydrochloric acid solution; the concentration of the hydrochloric acid solution can be 0.05-0.25 mol/L;
the standing time in the step b) can be 8-16 h.
The step 2) can comprise the following steps:
a) pouring out acid in the sample bottle, adding desalted water into the sample bottle to wash the sample, continuously stirring, measuring the pH value of the cleaning solution, pouring out the cleaning solution, and repeating for multiple times until the pH value of the cleaning solution is consistent with that of the desalted water;
b) adding CO-free2And (3) immersing the sample in water, standing for 0.5-1.5 h, and pouring out the liquid for later use.
The effect of this step is to control the CO content entering the filaments2Water was replaced to reduce titration error.
The step 3) can comprise the following steps:
a) accurately adding a certain amount of CO-free liquid into a sample bottle2Water, submerging the sample, and then adding a certain amount of NaOH solution; the added alkaline solution participates in the reaction and reacts with the chlorine-containing functional groups on the fibers; wherein the dosage of the NaOH solution can be 0.5-1.5 mL, and the concentration of the NaOH solution can be 0.05-0.25 mol/L;
b) uniformly stirring the liquid, sealing the sample bottle, and heating the sealed sample bottle in a water bath; a blank control was also prepared: the same amount of desalted water as in a) was added to another identical sample bottle and placed in a water bath, and the temperature of the desalted water in the sample bottle was monitored. The temperature of the water bath can be 53-63 ℃, the heating time can be 30-60 min, the specific set temperature range can be different due to different water baths, the temperature of the water bath can be adjusted according to actual conditions so as to control the temperature in the sample bottle not to exceed 55 ℃, and meanwhile, the temperature in the sample bottle is kept constant so as to ensure better reaction activity.
The step 4) may comprise the following steps:
a) cooling the heated sample bottle to room temperature, accurately weighing the sample bottle filled with the sample and the solution, and accurately recording the weight of the solution in the sample bottle to be titrated;
b) adding CO-free solution into a sample bottle needing titration2Water, sealing and carrying out titration;
c) the blank sample in the step 4) is as follows: will not have CO2Water was added to a sample bottle without CO2The amount of water used was the same as the CO-free amount in the sample bottle obtained in step b) of step 4)2The total content of water is the same; accurately adding NaOH solution with the same concentration and the same dosage as those in the step a) of the step 3), sealing, and titrating the blank sample.
In the step 4), the step of processing the first and second images,
and the titration is to titrate the sample solution and the blank sample by using 0.005-0.05 mol/L HCl solution, and record the volume number of the consumed HCl solution.
Preferably, the first and second electrodes are formed of a metal,
the step 1) comprises the following specific steps:
a) accurately weighing the 250mL sample bottles, recording the weights respectively, weighing 10 +/-1 g of sample after returning to zero, and recording the accurate weight of the sample;
b) 125mL of 0.1mol/L HCl solution is added to the measuring cylinder, the liquid must be used to immerse the sample, the mixture is stirred uniformly, sealed and kept stand overnight.
The step 2) may specifically include the following steps:
a) and (3) clamping the sample by using tweezers to pour out the hydrochloric acid solution, pouring desalted water into the bottle to wash the bottle, continuously stirring the bottle, measuring the pH value of the cleaning solution, pouring out the cleaning solution, adding new desalted water, and repeating the operation until the pH value of the cleaning solution is consistent with that of the desalted water.
b) 150mL of CO-free solution was added to the flask with a measuring cylinder2The sample was immersed and left for 1h, and the liquid was poured off after 1 h.
The step 3) may specifically include the following steps:
a) accurately pipette 120mL of CO-free solution into the vial2Water, over the sample, and exactly 1mL of 0.1mol/L NaOH solution (slow bleed) was added.
b) Stirring the liquid uniformly, sealing the sample bottle, putting the sealed sample bottle into a water bath at 58 ℃ for heating for 45min, and preparing a blank sample: while 120mL of desalted water was added to another identical sample bottle and placed in a water bath, the temperature of the desalted water in the sample bottle was measured by monitoring with a thermometer (the temperature in the sample bottle was controlled not to exceed 55 ℃).
The step 4) may specifically include the following steps:
a) and cooling the heated sample bottle to room temperature, accurately weighing the sample bottle filled with the sample and the solution by using an analytical balance, recording an accurate result, and accurately recording the weight of the solution in the sample bottle to be titrated.
b) Adding CO-free solution into a sample bottle needing titration2Water to 200mL, sealed and titrated with a titrator.
c) The blank sample in the step 4) is as follows: 200mL of CO-free2Water was added to the sample bottle, 1mL of 0.1mol/L NaOH solution (slow tapping) was added, the flask was sealed, and the blank was titrated with a titrator.
The sample solution and the blank sample were titrated separately with 0.01mol/L HCl solution using a titrator (pH electrode calibrated beforehand), and the number of volumes of HCl solution consumed was recorded separately.
Wherein,
the calculation in the step 4) comprises:
1. total weight of sample solution MS:
MS＝M1-M2
in the formula: m is a group of1-wet container, weight of lid + sample + solution + wet glass rod, g;
M2-dry container, weight with lid + sample + dry glass rod, g;
2. total HCl volume consumed VGeneral (1)：
In the formula: MS-weight of all solutions to be titrated in the container, g;
VHCl, titration-weighing a portion of titratable solution, the number of volumes of acid consumed in the titration (obtained directly from the titrator);
m-exact weight of solution weighed, g;
(weigh out a portion of titratable solution because we cannot titrate all of it, always a portion of it will stick to the vessel walls and fibers, we cannot titrate it in its entirety, we only titrate the volume of acid consumed by a portion of titratable solution, and thus derive the total volume of acid consumed in titrating the weight of all of the titratable solution in the vessel.)
3. Carbon fiber surface functional group:
in the formula: vBlank spaceVolume number of blank HCl solution consumed, mL;
cHClthe exact concentration of the HCl solution used, mol/L, is titrated;
m-exact weight of sample, g.
The method has the advantages of short determination time, low cost of used determination instruments, strong operability due to common reagents, basic operations of weighing and pipetting, and small personnel error, thereby meeting the requirements of factory production.
Detailed Description
The present invention will be further described with reference to the following examples. However, the present invention is not limited to these examples.
Example 1
The functional groups on the surface of the carbon fiber are measured according to the following method, which comprises the following steps:
1) weighing the weight of a carbon fiber sample to be detected, and reacting with excessive hydrochloric acid;
2) cleaning the sample, and replacing with carbon dioxide-free water;
3) adding sodium hydroxide solution;
4) weighing liquid, titrating a sample to be measured and a blank sample, and calculating a result.
The step 1) comprises the following specific steps:
a) accurately weighing the 250mL sample bottles, recording the weights respectively, weighing 10 +/-1 g of sample after returning to zero, and recording the accurate weight of the sample;
b) 125mL of 0.1mol/L HCl solution is added to the measuring cylinder, the liquid must be used to immerse the sample, the mixture is stirred uniformly, sealed and kept stand overnight.
The step 2) specifically comprises the following steps:
a) clamping the sample by using a pair of tweezers to pour out the hydrochloric acid solution, pouring desalted water into the bottle to wash the bottle, continuously stirring the bottle, measuring the pH value of the cleaning solution, pouring out the cleaning solution, adding new desalted water, and repeating the operation until the pH value of the cleaning solution is consistent with that of the desalted water;
b) 150mL of CO-free solution was added to the flask with a measuring cylinder2Water, submerge the sample and leave for 1h, and pour out the liquid after 1 h.
The step 3) may specifically include the following steps:
a) accurately pipette 120mL of CO-free solution into the vial2Water, submerging the sample, and then accurately adding 1mL of 0.1mol/L NaOH solution (slowly discharging liquid);
b) stirring the liquid uniformly, sealing the sample bottle, putting the sealed sample bottle into a water bath at 58 ℃ for heating for 45min, adding 120mL of desalted water into the same sample bottle, putting the desalted water into the water bath, and measuring the temperature of the desalted water in the sample bottle by using a thermometer (controlling the temperature in the sample bottle not to exceed 55 ℃). The step 4) may specifically include the following steps:
a) and cooling the heated sample bottle to room temperature, accurately weighing the sample bottle filled with the sample and the solution by using an analytical balance, recording an accurate result, and accurately recording the weight of the solution in the sample bottle to be titrated.
b) Adding CO-free solution into a sample bottle needing titration2Water to 200mL, sealed and titrated with a titrator.
c) The blank sample in the step 4) is as follows: 200mL of CO-free2Water was added to the sample bottle, 1mL of 0.1mol/L NaOH solution (slow tapping) was added, the flask was sealed, and the blank was titrated with a titrator.
The sample solution and the blank sample were titrated separately with 0.01mol/L HCl solution using a titrator (pH electrode calibrated beforehand), and the number of volumes of HCl solution consumed was recorded separately.
Wherein,
the calculation in the step 4) comprises:
1. total weight of sample solution MS:
MS＝M1-M2
in the formula: m1-wet container, weight of lid + sample + solution + wet glass rod, g;
M2-dry container, weight with lid + sample + dry glass rod, g;
2. total HCl volume consumed VGeneral (1)：
In the formula: MS-weight of all solutions to be titrated in the container, g;
VHCl, titration-weighing a portion of the titratable solution, the number of volumes of acid consumed during titration (obtained directly from the titrator);
m-exact weight of a portion of the solution weighed, g;
3. carbon fiber surface functional group:
in the formula: vBlank spaceVolume number of blank HCl solution consumed, mL;
cHClthe exact concentration of the HCl solution used, mol/L, is titrated;
m-exact weight of sample, g.
Carbon fiber (24K) samples produced at different time periods using the method described above were tested using this method for less than 24 hours with the results shown in table 1 below:
TABLE 1
As can be seen from Table 1, the results of the parallel samples of the same sample are slightly different from each other, and the measured results are better in parallelism.
Example 2
Using the same bundle of factory-produced 24K carbon fibers, a plurality of persons A to J performed the measurement of the surface functional groups by the method of the present invention, and the results are shown in the following Table 2:
TABLE 2
(Note: calculation of relative deviation using average of all results 1.480 as true value.)
As can be seen from Table 2, in the same sample, different persons have smaller difference of results, smaller deviation of sample results and better reproducibility when the method is used for measurement.
The method for measuring the functional groups on the surface of the carbon fiber is simple and easy to implement, has low requirements on instruments, can measure results in a short time, and has accurate and stable measurement results of the same sample, good reproducibility of different personnel for measuring the same sample and small difference among the personnel. A large amount of experimental measurement data can accurately reflect the surface functional group performance of the fiber sample, and the fiber sample can be well served for practical production.
Claims (8)
1. A method for determining functional groups on the surface of carbon fibers is characterized by comprising the following steps:
1) weighing the weight of a carbon fiber sample to be measured, and reacting with excessive acid;
2) cleaning samples with CO-free2Water replacement;
3) adding an alkaline solution;
4) weighing liquid, titrating a sample to be tested and a blank sample, and calculating a result;
the step 1) comprises the following steps:
a) accurately weighing the weight of the sample, and placing the sample in a sample bottle; the weight of the sample is 5-15 g;
b) adding acid, immersing the sample, stirring uniformly, sealing and standing;
the acid in the step 1) is hydrochloric acid solution;
the step 2) comprises the following steps:
a) pouring out acid in the sample bottle, adding desalted water to wash the sample, continuously stirring, measuring the pH value of the cleaning solution, pouring out the cleaning solution, and repeating for multiple times until the pH value of the cleaning solution is consistent with that of the desalted water;
b) adding CO-free2Immersing the sample in water, standing, and pouring out the liquid for later use; wherein the standing time is 0.5-1.5 h;
the step 3) comprises the following steps:
a) adding CO-free into bottle2Water, submerging the sample, and then adding NaOH solution;
b) and uniformly stirring the liquid, sealing the sample bottle, and heating the sealed sample bottle in water bath.
2. The method for determining functional groups on the surface of carbon fibers according to claim 1, wherein:
the step 1) comprises the following steps:
a) accurately weighing the weight of the sample, and placing the sample in a sample bottle; the weight of the sample is 8-12 g.
3. The method for determining functional groups on the surface of carbon fibers according to claim 1, wherein:
in the step 1) described above, the step of,
the concentration of the hydrochloric acid solution is 0.05-0.25 mol/L;
the standing time is 8-16 h.
4. The method for determining functional groups on the surface of carbon fibers according to claim 1, wherein:
in the step 3), the step of the method comprises the following steps,
in the step a), the using amount of the NaOH solution is 0.5-1.5 mL, and the concentration of the NaOH solution is 0.05-0.25 mol/L;
in the step b), the temperature of the water bath is 53-63 ℃, and the heating time is 30-60 min.
5. The method for determining functional groups on the surface of carbon fibers according to claim 1, wherein:
the step 4) comprises the following steps:
a) cooling the heated sample bottle to room temperature, accurately weighing the sample bottle filled with the sample and the solution, and accurately recording the weight of the sample solution to be titrated;
b) adding CO-free solution into a sample bottle needing titration2Water, sealing and carrying out titration;
c) blank sample preparation described in step 4): will not have CO2Water was added to a sample bottle without CO2The amount of water used was the same as the CO-free amount in the sample bottle obtained in step b) of step 4)2The total content of water is the same; accurately adding NaOH solution with the same concentration and the same dosage as those in the step a) of the step 3), sealing, titrating the blank sample, and calculating the concentration of the functional groups on the surface of the fiber.
6. The method for determining functional groups on the surface of carbon fibers according to claim 5, wherein: in the step 4), the step of processing the first and second images,
and the titration is to titrate the sample solution and the blank sample by using 0.005-0.05 mol/L HCl solution, and record the volume number of the consumed HCl solution.
7. The method for determining functional groups on the surface of carbon fibers according to claim 5, wherein: the calculation in the step 4) comprises:
1. total weight of sample solution MS:
MS＝M1-M2
in the formula: m1-wet container, weight of lid + sample + solution + wet glass rod, g;
M2-dry container, weight with lid + sample + dry glass rod, g;
2. total HCl volume consumed VGeneral assembly：
In the formula: MS-weight of all sample solutions to be titrated in the container, g;
VHCl，titration-weighing a portion of titratable sample solution, the volume of acid consumed in the titration;
m-exact weight of sample solution weighed, g;
3. carbon fiber surface functional group:
in the formula: vBlank spaceThe number of volumes of HCl solution consumed for the blank sample, mL;
cHClthe exact concentration of the HCl solution used, mol/L, is titrated;
m-exact weight of sample, g.
8. The method for measuring functional groups on the surface of carbon fibers according to any one of claims 1 to 7, wherein:
the step 1) comprises the following steps:
a) accurately weighing 250mL of sample bottles, weighing 10 +/-1 g of samples after returning to zero, and recording the accurate weight of the samples;
b) adding 125mL of 0.1mol/L HCl solution, enabling the sample to be immersed in the solution, uniformly stirring, sealing and standing;
the step 2) comprises the following steps:
a) pouring the HCl solution in the sample bottle, pouring desalted water into the sample bottle for washing, continuously stirring, measuring the pH value of the cleaning solution, pouring the cleaning solution, and repeating the operation until the pH value of the cleaning solution is consistent with that of the desalted water;
b) adding 100-180 mL of CO-free solution into a bottle2Immersing the sample in water, standing for 0.5-1.5 h, and pouring off the liquid;
the step 3) comprises the following steps:
a) accurately add 120mL of CO-free solution to the bottle2Water, submerging the sample, and then accurately adding 1mL of 0.1mol/L NaOH solution;
b) uniformly stirring the liquid, sealing the sample bottle, putting the sealed sample bottle into a water bath at 53-63 ℃ for heating for 45min, and preparing a blank sample: adding 120mL of desalted water into another identical sample bottle, putting the sample bottle into a water bath, and monitoring and determining that the temperature of the desalted water in the sample bottle does not exceed 55 ℃;
the step 4) comprises the following steps:
a) cooling the heated sample bottle to room temperature, accurately weighing the sample bottle filled with the sample and the solution by using an analytical balance, recording an accurate result, and accurately recording the weight of the solution in the sample bottle to be titrated;
b) adding CO-free solution into a sample bottle needing titration2Water is added to 200mL, sealed and titrated by a titrator;
c) the blank sample in step 4) is: another 250mL sample bottle was prepared, and 200mL of CO-free sample bottle was filled with2Adding water into a sample bottle, accurately adding 1mL of 0.1mol/L NaOH solution, sealing, and titrating a blank sample by using a titrator;
the titration was performed using a 0.01mol/L HCl solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911112531.9A CN110824101B (en) | 2019-11-14 | 2019-11-14 | Method for measuring functional groups on surface of carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911112531.9A CN110824101B (en) | 2019-11-14 | 2019-11-14 | Method for measuring functional groups on surface of carbon fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110824101A CN110824101A (en) | 2020-02-21 |
| CN110824101B true CN110824101B (en) | 2022-05-13 |
Family
ID=69555113
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911112531.9A Active CN110824101B (en) | 2019-11-14 | 2019-11-14 | Method for measuring functional groups on surface of carbon fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110824101B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5304638A (en) * | 1989-06-08 | 1994-04-19 | Central Blood Laboratories Authority | Protein separation medium |
| US5466347A (en) * | 1992-12-10 | 1995-11-14 | Permelec Electrode, Ltd. | Method for electrolyzing aqueous solution of alkali chloride |
| JP2001083134A (en) * | 1999-09-10 | 2001-03-30 | Nippon Soda Co Ltd | Method for determining nitrogen in organic compound by kjeldahl method |
| WO2001046085A2 (en) * | 1999-12-23 | 2001-06-28 | Cosofret Sorin Cezar | Composition functioning as a binding agent and as a combat factor against ascensional humidity in building and method to apply |
| CN101805319A (en) * | 2010-04-21 | 2010-08-18 | 石药集团维生药业（石家庄）有限公司 | Method for directly converting and preparing sodium ascorbate by using sodium gulonic acid |
| EP2570384A1 (en) * | 2011-09-13 | 2013-03-20 | Atomic Energy Council - Institute of Nuclear Energy Research | Quantitative analysis of a functional group on the surface of a solid material |
| JP2018169318A (en) * | 2017-03-30 | 2018-11-01 | 日本製紙株式会社 | Method of measuring amounts of anionic functional groups in anion-modified cellulose-based materials |
| CN109324148A (en) * | 2017-08-01 | 2019-02-12 | 金华盛纸业（苏州工业园区）有限公司 | A kind of detection method of the substance with anhydride functional group |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102141562B (en) * | 2010-09-28 | 2012-11-07 | 上海师范大学 | Method for analyzing purity of 2,4,5-triamino-6-hydroxy pyrimidine sulfate sample by utilizing titration |
| US8492161B2 (en) * | 2011-08-25 | 2013-07-23 | Atomic Energy Council—Institute of Nuclear Energy Research | Quantitative analysis of a function group on the surface of a solid material |
| CN107002347A (en) * | 2014-12-09 | 2017-08-01 | 国立大学法人东京大学 | Surface processed carbon fiber, surface processed carbon fiber beam and their manufacture method |
| CN106018673A (en) * | 2016-07-21 | 2016-10-12 | 中国科学院山西煤炭化学研究所 | Quantitative analysis method for surface oxygenic functional groups of graphene materials |
| JP7172033B2 (en) * | 2017-03-01 | 2022-11-16 | 王子ホールディングス株式会社 | Fibrous Cellulose, Fibrous Cellulose-Containing Composition, Fibrous Cellulose Dispersion, and Method for Producing Fibrous Cellulose |
| CN107282025B (en) * | 2017-04-20 | 2018-09-21 | 浙江农林大学 | Nano-cellulose base is functionalized the preparation method of aerogel type heavy-metal adsorption material |
| CN107402167A (en) * | 2017-06-27 | 2017-11-28 | 兰州蓝星纤维有限公司 | A kind of polyacrylonitrile-radical polymer fluid, the assay method of protofilament inherent viscosity |
| CN107478545B (en) * | 2017-08-15 | 2020-10-23 | 兰州蓝星纤维有限公司 | Method for measuring adhesion number of carbon fiber precursors |
| CN108362824B (en) * | 2018-01-16 | 2020-07-14 | 中蓝长化工程科技有限公司 | Method for determining carbonate radical and bicarbonate radical in borate-containing brine |
| CN110031602A (en) * | 2019-04-26 | 2019-07-19 | 太原理工大学 | The measuring method of oxygen-containing functional group in a kind of lignite |
-
2019
- 2019-11-14 CN CN201911112531.9A patent/CN110824101B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5304638A (en) * | 1989-06-08 | 1994-04-19 | Central Blood Laboratories Authority | Protein separation medium |
| US5466347A (en) * | 1992-12-10 | 1995-11-14 | Permelec Electrode, Ltd. | Method for electrolyzing aqueous solution of alkali chloride |
| JP2001083134A (en) * | 1999-09-10 | 2001-03-30 | Nippon Soda Co Ltd | Method for determining nitrogen in organic compound by kjeldahl method |
| WO2001046085A2 (en) * | 1999-12-23 | 2001-06-28 | Cosofret Sorin Cezar | Composition functioning as a binding agent and as a combat factor against ascensional humidity in building and method to apply |
| CN101805319A (en) * | 2010-04-21 | 2010-08-18 | 石药集团维生药业（石家庄）有限公司 | Method for directly converting and preparing sodium ascorbate by using sodium gulonic acid |
| EP2570384A1 (en) * | 2011-09-13 | 2013-03-20 | Atomic Energy Council - Institute of Nuclear Energy Research | Quantitative analysis of a functional group on the surface of a solid material |
| JP2018169318A (en) * | 2017-03-30 | 2018-11-01 | 日本製紙株式会社 | Method of measuring amounts of anionic functional groups in anion-modified cellulose-based materials |
| CN109324148A (en) * | 2017-08-01 | 2019-02-12 | 金华盛纸业（苏州工业园区）有限公司 | A kind of detection method of the substance with anhydride functional group |
Non-Patent Citations (3)
| Title |
|---|
| Effects of Acid Modification on Pb(Ⅱ) and Cu(Ⅱ) Adsorption of Bamboo-based Activated Carbon;Chung, Jaewoo;《Jornal of Korea Organic Resource Recycling Association》;20161231;第24卷(第1期);第3-10页 * |
| 多壁碳纳米管表面修饰化学官能团的定量分析;李晓峰 等;《山东大学学报(理学版)》;20090131;第44卷(第1期);第17-23页 * |
| 活性炭表面结构及官能团的归一化实验研究;雷灿;《中国优秀博硕士学位论文全文数据库(硕士) 工程科技Ⅰ辑》;20140715(第7期);第B016-340页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110824101A (en) | 2020-02-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107621428B (en) | Cementitious material content assaying method suitable for limestone fine aggregate maturing | |
| CN110824101B (en) | Method for measuring functional groups on surface of carbon fiber | |
| CN113092510A (en) | X-fluorescence determination method for potassium nitrate as high-alumina glass raw material | |
| CN112730733A (en) | Method for detecting content of chloride ions in sea sand | |
| CN108956367A (en) | A kind of assessment method of anode oxide film sealing quality | |
| Dvořák et al. | A new method for the measurement of internal stress in electrodeposits | |
| CN105301194B (en) | The detection method of surface of positive electrode active material covered effect | |
| CN111638236A (en) | Quantitative analysis method for selenium in crude selenium | |
| CN109444198A (en) | Rapid assay methods suitable for bentonite, clay chemistry ingredient | |
| CN109030389A (en) | The measuring method of total sulfur in a kind of anode material for lithium-ion batteries | |
| JP7439645B2 (en) | Manufacturing method and management method for chemically strengthened glass | |
| IT9021284A1 (en) | GRAVIMETRIC DETERMINATION OF THE IODINE NUMBER OF THE BLACK SMOKE | |
| CN113155879A (en) | Method for measuring contents of silicon dioxide and calcium fluoride in fluorite | |
| CN109682870B (en) | Method and device for measuring concentration of metal ions in molten salt | |
| CN115372244A (en) | Evaluation device and method for sulfide stress corrosion cracking resistance of pipeline steel | |
| CN115932158A (en) | Method for testing content of residual chlorine element on surface of powder toughening material | |
| US2716596A (en) | Determination of tin on tinplate | |
| CN111239331A (en) | Method for detecting content of calcium oxide in quick lime | |
| CN109613237A (en) | A kind of cystatin C detection kit | |
| Covington | Procedures for testing pH responsive glass electrodes at 25, 37, 65 and 85 C and determination of alkaline errors up to 1 mol dm-3 Na+, K+, Li+ | |
| CN104792648A (en) | Method for measuring content of aluminum and iron in steel grit aluminum by combining weighing method and titration method | |
| CN104280333B (en) | Based on the method that glass column determines chemical durability of glass | |
| CN116183534B (en) | Detection method of electroplating solution brightening agent | |
| CN109696519B (en) | Method for testing oxidation reduction degree of graphene oxide | |
| CN117969493A (en) | Method for detecting high silicon content in aluminum alloy by ICP-AES method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |