CN112414998A - Method for determining impurity elements in polyacrylonitrile carbon fiber sample - Google Patents
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Abstract
The invention discloses a method for determining impurity elements in a polyacrylonitrile carbon fiber sample, which comprises the steps of ashing the carbon fiber sample, and treating ashing residues by adopting high-purity hydrofluoric acid and hydrochloric acid solution; and (3) measuring impurity elements in the ash by adopting an inductively coupled plasma atomic emission spectrometry. The invention adopts high-purity hydrofluoric acid and hydrochloric acid to dissolve the ignition residues, applies the inductively coupled plasma atomic emission spectrometer provided with the hydrofluoric acid resistant sampling system to prepare samples at one time, and the same sample solution can simultaneously determine a plurality of impurity elements in the polyacrylonitrile-based carbon fiber sample, thereby saving the test time and solving the problems of complexity, easy error introduction and the like of the existing method; the method is simple, convenient and rapid, and has high sensitivity and accuracy.
Description
Technical Field
The invention relates to the technical field of carbon fiber impurity element determination, in particular to a method for determining impurity elements in a polyacrylonitrile carbon fiber sample.
Background
Carbon Fiber (CF) is a new high-strength and high-modulus fiber material with a carbon content of more than 95%. The composite material has the advantages of 'outer flexibility and inner stiffness', lighter weight than metal aluminum, higher strength than steel, inherent intrinsic characteristics of carbon materials, soft processability of textile fibers, high strength, high modulus, low density, high temperature resistance, corrosion resistance, fatigue resistance, good electric and heat conductivity, electromagnetic shielding performance and the like, and is widely applied to civil fields of aerospace, national defense and military industries, sports goods, transportation, medical appliances, civil engineering and construction and the like. According to different production raw materials, the carbon fiber is divided into polyacrylonitrile-based carbon fiber, asphalt-based carbon fiber, viscose-based carbon fiber and the like. The polyacrylonitrile-based carbon fiber is a high-performance fiber material prepared by taking polyacrylonitrile as a raw material and carrying out spinning, pre-oxidation, carbonization and surface treatment, and has the advantages of excellent mechanical property, widest application range, largest dosage and quickest development. The analysis and detection of carbon fiber products, such as the measurement of indexes such as carbon fiber diameter, carbon fiber density, carbon fiber monofilament, multifilament tensile property, carbon fiber carbon content, ash content, sizing agent content and the like, have corresponding national standards or industrial standards, but no corresponding standard method has been provided for the measurement of introduced trace potassium, sodium, calcium, magnesium, iron, silicon and other impurities in the carbon fiber during the preparation process. The existence of these impurity elements can cause the internal defects of the fiber, and seriously affect the oxidation resistance, high-temperature tensile property and high-temperature mechanical property of the fiber. The invention aims to provide a sample pretreatment mode and a determination method for detecting impurity elements in a polyacrylonitrile-based carbon fiber (protofilament, oxidized fiber and carbon fiber) sample, which accurately determine and strictly control the content of the impurity elements in the polyacrylonitrile-based carbon fiber to guide industrial production.
Few reports are made at home and abroad for the determination of impurity elements in carbon fiber samples. Poplar and warong, etc. in research on a test method for mass fraction of impurity elements in carbon fibers (high-tech fibers and applications, volume 40, 6, 2015), the sample is ashed, and then is subjected to stepwise dissolution and stepwise test, namely, the sample is treated by an alkali fusion method, and the silicon content is measured by silicon-molybdenum blue colorimetry; digesting the sample by adopting an acid dissolution-filtration-ashing-redissolution mode, and measuring the contents of potassium, sodium, calcium and magnesium in the sample by using AAS or ICP-OES. The method is time-consuming and tedious, interference is easily introduced by the digestion mode, and the method is not suitable for measuring trace elements in the carbon fiber sample.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a sample pretreatment method and a sample determination method for determining the content of trace elements such as potassium, sodium, calcium, magnesium, iron, silicon and the like in a polyacrylonitrile-based carbon fiber sample by using an inductively coupled plasma atomic emission spectrometry, which are simple, convenient, rapid, high in sensitivity and good in accuracy.
For the determination of impurity elements of a polyacrylonitrile-based carbon fiber sample, because the impurity content is low and the sample has a large amount of stable carbon, if microwave digestion is adopted, the sample weighing amount is small, and the test requirements cannot be met; the sample weighing is large, and the digestion is incomplete. Therefore, it is proposed to perform pretreatment of a sample by a dry ashing method. The dry ashing method is simple and rapid, and is suitable for analysis and test of mass samples. However, if the ashing temperature is not properly selected, the low temperature elements (potassium, sodium, etc.) will be lost. According to the invention, after a polyacrylonitrile-based carbon fiber sample is incinerated at a proper temperature, HF + HCl is directly used for dissolving residues, and ICP-AES is used for determining the contents of trace elements such as potassium, sodium, calcium, magnesium, iron and silicon.
In order to achieve the purpose, the invention adopts the following technical scheme:
1. a method for determining impurity elements in a polyacrylonitrile-based carbon fiber sample is characterized in that the carbon fiber sample is ashed, and the ashed residues are treated by high-purity acid; measuring impurity elements in the ash by adopting an inductively coupled plasma atomic emission spectrometry; the method specifically comprises the following steps:
(1) ashing the carbon fiber sample;
(2) dissolving the ashing residues by using high-purity acid to prepare a sample solution;
(3) preparing a mixed standard use solution of potassium, sodium, calcium, magnesium and iron, and preparing a standard use solution of silicon;
(4) and the sample solution is used for measuring impurity elements in ash by an inductively coupled plasma atomic emission spectrometer provided with a hydrofluoric acid resistant sampling system.
Further, the carbon fiber sample is ashed in the step (1), specifically, the carbon fiber sample is placed in a quartz beaker and is placed in a muffle furnace, and the temperature is raised from room temperature to 600 ℃ within 60-90min in a temperature programming manner until the ashing is complete.
Furthermore, in the step (2), the sample solution is prepared by dissolving the high-purity acid, specifically, the ashing residue is prepared by dissolving the high-purity hydrofluoric acid and hydrochloric acid solution.
Further, the step (2) of dissolving the ashing residues with a high-purity hydrofluoric acid and hydrochloric acid solution to prepare a sample solution specifically comprises the following steps: absorbing the ashing residues (cotton floccules) in the quartz beaker by using a wet glass rod, transferring the ashing residues into a plastic centrifugal test tube, cleaning the glass rod by using deionized water, dropwise adding hydrofluoric acid into the plastic centrifugal test tube, completely dissolving the ashing residues, adding a hydrochloric acid solution into the quartz beaker to dissolve the ashing residues remained on the inner wall and the bottom of the quartz beaker, transferring the ashing residues into the plastic centrifugal test tube by using a polytetrafluoroethylene rod, cleaning the beaker by using deionized water, and fixing the volume to the scale of the plastic centrifugal test tube. The method is adopted to dissolve the ashing residues, so that potassium, sodium, calcium, magnesium, iron and silicon elements in the ashing residues are completely dissolved in hydrofluoric acid and hydrochloric acid solution, silicon dioxide in the ashing residues reacts with the hydrofluoric acid to generate fluosilicic acid, and all elements to be detected have no loss. Because of the low content of impurity elements in the carbon fiber, if the ashing residue is not completely dissolved or a part of the ashing residue is lost, the measurement data may be inaccurate.
Still further, the standard use solution for preparing potassium, sodium, calcium, magnesium and iron in the step (3) is specifically: preparing standard use solutions containing 0.00, 0.50, 1.00, 2.00, 4.00, 6.00, 8.00 and 10.0mg/L of potassium, sodium, calcium, magnesium and iron respectively; the preparation of the silicon standard use solution specifically comprises the following steps: preparing standard silicon use solutions with silicon contents of 0.00, 5.00, 10.0, 20.0, 30.0, 40.0, 50.0, 80.0 and 100.0mg/L respectively.
Still further, the impurity elements in the step (4) refer to potassium, sodium, calcium, magnesium, iron and silicon elements.
And (3) further, the sample solution in the step (4) is used for measuring the impurity elements in the sample solution by an inductively coupled plasma atomic emission spectrometer provided with a hydrofluoric acid resistant sampling system. When potassium, sodium, calcium, magnesium, iron and silicon elements are measured, the wavelengths of the inductively coupled plasma atomic emission spectrometer are 766.490nm, 589.592nm, 317.933nm, 279.553nm, 259.940nm and 212.412nm respectively. The specific test process is as follows:
(1) under the determined working condition of the inductively coupled plasma atomic emission spectrometer, drawing a standard curve:
standard curve of potassium, sodium, calcium, magnesium and iron: sucking potassium-sodium-calcium-magnesium-iron series standard solution, and drawing a standard curve of potassium-sodium-calcium-magnesium-iron element by taking the mass concentration (mg/L) of the potassium-sodium-calcium-magnesium-iron element as an abscissa and taking the emission intensity as an ordinate.
(2) Silicon standard curve: sucking silicon standard series solution, and drawing a standard curve of silicon element by taking silicon mass concentration (mg/L) as an abscissa and taking emission intensity as an ordinate.
(3) And under the determined working condition of the inductively coupled plasma atomic emission spectrometer, determining the contents of potassium, sodium, calcium, magnesium, iron and silicon elements in the sample solution.
(4) And (4) calculating a result: calculating the mass fractions (ug/g) of potassium, sodium, calcium, magnesium, iron and silicon in the carbon fiber sample according to the formula (1);
in the formula: x-content of element to be measured, ug g-1
Cx-concentration of corresponding element in sample solution to be tested, ug-mL-1
Cx0-concentration of corresponding element in blank solution, ug. mL-1
V-constant volume of sample solution, mL
m-mass of sample, g.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention adopts high-purity hydrofluoric acid and hydrochloric acid to dissolve the ignition residues, applies the inductively coupled plasma atomic emission spectrometer provided with the hydrofluoric acid resistant sampling system to prepare samples at one time, and the same sample solution can simultaneously determine a plurality of impurity elements in the polyacrylonitrile-based carbon fiber sample, thereby saving the test time and solving the problems of complexity, easy error introduction and the like of the existing method; the method is simple, convenient and rapid, and has high sensitivity and accuracy.
(2) The method has the advantages of high precision (the relative standard deviation of six measurements is less than 4%), good accuracy (the recovery rate of each element is more than 95%), simple process and convenient operation.
Drawings
Fig. 1 is a calcium standard curve with a correlation coefficient r of 0.9998 for ca317.933;
fig. 2 is an iron standard curve with a correlation coefficient r of 0.9998 for fe259.940;
fig. 3 is a potassium standard curve with a K766.490 correlation coefficient r of 0.9998;
fig. 4 is a magnesium standard curve for mg279.553 with a correlation coefficient r of 0.9995;
fig. 5 is a sodium standard curve with a correlation coefficient r of 0.9995 for na589.592;
fig. 6 is a silicon standard curve with a correlation coefficient of si212.412 of r 0.9997.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the attached table and the drawings in the embodiment of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
1. Instrumentation and reagents used in this example:
1.1 instruments
1) Electronic balance
2) Muffle furnace
3) Inductively coupled plasma atomic emission spectrometer (with anti-hydrofluoric acid sample system)
4)15mL or 10mL plastic centrifuge tubes (calibrated)
5)50mL, 100mL volumetric flask
6)5.0mL, 10.0mL pipette
Note: all utensils are soaked in nitric acid with the volume ratio of (1+1) for 24h, and cleaned for later use according to the program.
1.2 reagents
1) Hydrochloric acid, guaranteed purity (relative density 1.19), available from Merck, Germany
2) Hydrochloric acid solution with the volume ratio of (1+3)
3) Hydrofluoric acid, super pure (more than 40% by weight), purchased from the national pharmaceutical group
4) Standard stock solutions of potassium, sodium, calcium, magnesium and iron (all single standard solutions, element content all 1000mg/L) purchased from steel, Yannak
5) Silicon Standard stock solution (Single Standard solution, content 500.0mg/L) available from Steel, Minaku
6) The used water is secondary deionized water
2. Determination of trace potassium, sodium, calcium, magnesium, iron, silicon and other element content in polyacrylonitrile-based carbon fiber sample
2.1 preparation of Standard solution
2.1.1 preparation of Standard intermediate solution of Potassium, sodium, calcium, magnesium, iron mixture
10.0mL of the standard stock solution with single-mark potassium, sodium, calcium, magnesium and iron is respectively transferred into a 100mL volumetric flask and diluted to the scale with 5% HCl. The solution contains 100.0mg/L of potassium, sodium, calcium, magnesium and iron respectively.
2.1.2 preparation of Standard Mixed use solutions of Potassium, sodium, calcium, magnesium, iron
The mixed standard intermediate solutions 0.00, 0.50, 1.00, 2.00, 4.00, 6.00, 8.00mL and 10.0mL were transferred into a series of 100.0mL volumetric flasks and diluted to the mark with 0.5% HCl. Standard use solutions containing potassium, sodium, calcium, magnesium and iron of 0.00, 0.50, 1.00, 2.00, 4.00, 6.00, 8.00 and 10.0mg/L are obtained.
2.1.3 preparation of silicon Standard use solutions
0.00, 0.50, 1.00, 2.00, 3.00, 4.00, 5.00, 8.00 and 10.00mL of silicon standard stock solution (500mg/L) is transferred into a series of 50.0mL volumetric flasks to obtain silicon standard use solutions with silicon contents of 0.00, 5.00, 10.0, 20.0, 30.0, 40.0, 50.0, 80.0 and 100.0mg/L respectively.
2.2 preparation of sample solutions
2.2.1 sample preparation
And cutting the carbon fiber sample into small sections with the length less than 2cm for later use.
2.2.2 sample ashing
Weighing 2-3 g of carbon fiber sample in a 50mL quartz beaker, placing the quartz beaker in a muffle furnace, and heating the carbon fiber sample to 600 ℃ from room temperature within 60min in a temperature programming manner until ashing is complete.
In the sample ashing process, the carbon fiber sample can be completely ashed by heating from room temperature to 600 ℃ within 70min, 80min and 90min in a temperature programming mode.
2.2.3 preparation of sample solutions
Absorbing the ashing residues (cotton floccules) in the quartz beaker by using a wet glass rod, transferring the ashing residues into a plastic centrifugal test tube, cleaning the glass rod by using deionized water, controlling the volume to be 2mL, dropwise adding 0.25mL of hydrofluoric acid into the plastic centrifugal test tube, completely dissolving the ashing residues, adding 2mLHCl (1+3) into the original beaker, dissolving the ashing residues remained on the inner wall and the bottom of the quartz beaker, transferring the solution into the plastic centrifugal test tube by using a polytetrafluoroethylene rod, cleaning the beaker by using the deionized water, and fixing the volume to 10.0 mL.
And simultaneously blank.
2.3 testing of samples
2.3.1 Standard Curve plotting
Working condition of inductively coupled plasma atomic emission spectrometer and recommended spectral line of each element (see Table 1)
TABLE 1 Instrument operating conditions and recommended spectral lines for the elements
Under the instrument operating conditions identified in table 1, a standard curve is plotted:
2.3.1.1 standard curve of potassium sodium calcium magnesium iron: mixed standard use solutions containing 0.00, 0.50, 1.00, 2.00, 4.00, 6.00, 8.00 and 10.0mg/L of potassium, sodium, calcium, magnesium and iron which are prepared according to the method 2.1.2 are sequentially inhaled, and a standard curve of corresponding elements is drawn by taking the mass concentration (mg/L) of the elements measured in the standard series solutions as an abscissa and the emission intensity as an ordinate. The standard curve is shown in figures 1-5. The correlation coefficients of the standard curves are all larger than 0.999.
2.3.1.2 silicon standard curve: sucking silicon standard series solution, sequentially sucking silicon standard use solutions with silicon contents of 0.00, 5.00, 10.0, 20.0, 30.0, 40.0, 50.0, 80.0 and 100.0mg/L prepared according to 2.1.3, and drawing a standard curve of silicon element by taking the mass concentration (mg/L) of the silicon element in the standard series solution as an abscissa and taking the emission intensity as an ordinate. The standard curve is shown in figure 6. The correlation coefficient of the standard curve is larger than 0.999.
The method of the invention was tested for precision, method repeatability and method recovery as follows:
1. method for testing precision by using precursor as carbon fiber sample
3.0914g of a carbon fiber A (precursor) sample was accurately weighed in a 50mL quartz beaker, placed in a muffle furnace, and sample solutions were prepared in 2.2 and 2.3 and subjected to an analytical test. The same solution was assayed in six replicates. The relative standard deviation of all elemental determinations was less than 4% (see table 2).
TABLE 2 method precision test with precursor as carbon fiber sample
2. Method for testing precision by taking carbon filaments as carbon fiber samples
3.0422g of a sample of carbon fiber B (carbon filament) was accurately weighed into a 50mL quartz beaker, placed in a muffle furnace, and sample solutions were prepared at 2.2 and 2.3 and subjected to analytical testing. The same solution was assayed in six replicates. The relative standard deviation of all elemental determinations was less than 2% (see table 3).
TABLE 3 method precision test with carbon filament as carbon fiber sample
3. Method for repeatability test by taking precursor as carbon fiber sample
Six samples of 3.0. + -. 0.1g (accurately weighed to 0.0001g) of carbon fiber A (precursor) were accurately weighed in six 50mL quartz beakers, placed in muffle furnaces, and sample solutions were prepared in 2.2 and 2.3 and subjected to analytical testing. Six samples tested results and the relative standard deviation of all elemental determinations was less than 4% (see table 4).
TABLE 4 method repeatability test with protofilament as carbon fiber sample
4. Method for repeatability test by taking carbon filaments as carbon fiber sample
Six samples of 3.0 + -0.1 g (accurately weighed to 0.0001g) of carbon fiber B (carbon filament) were accurately weighed in six 50mL quartz beakers, placed in muffle furnaces, and sample solutions were prepared at 2.2 and 2.3 and subjected to analytical testing. Six samples tested results and the relative standard deviation of all elemental determinations was less than 5% (see table 5).
TABLE 5 method repeatability test with carbon filaments as carbon fiber samples
5. Method spiking recovery test
Spiking recovery is a common internal quality control means in laboratories. Weighing two samples with the same quantity, quantitatively adding the component to be measured into one of the two samples, and measuring the standard recovery rate according to the same sample test steps so as to examine the accuracy of the method.
5.1 potassium sodium calcium magnesium iron standard addition recovery test:
accurately weighing six samples of carbon fiber B with the same amount of 3.0 +/-0.1 g (accurately weighed to 0.0001g), respectively adding different amounts of standard solutions into six 50mL quartz beakers, respectively, placing the beakers in a muffle furnace, and raising the temperature from room temperature to 550 ℃, 600 ℃, 700 ℃ and 800 ℃ within 90min in a temperature programming manner until ashing is complete. After cooling, sample solutions were prepared as 2.2 and 2.3 and were tested analytically to investigate the process recovery. And (3) test results: at 600 ℃, the recovery rate of each element of potassium, sodium, calcium, magnesium and iron is more than 98 percent; the temperature is higher than 700 ℃, the low-temperature element K, Na has different escape losses (the recovery rates of potassium and sodium are 87.26% and 86.82% respectively at 700 ℃, and the recovery rates of potassium and sodium are reduced to 84.44% and 82.62% respectively at 800 ℃). The ashing temperature has little influence on the measurement of calcium, magnesium and iron. Taken together, 600 ℃ was determined to be the optimum ashing temperature (see table 6).
TABLE 6 ashing temperature selection and standard recovery test for polyacrylonitrile-based carbon fibers
5.2 silicon spiking recovery test
Accurately weighing A, B carbon fiber samples, respectively placing the samples in 50mL quartz beakers, weighing different amounts of spectral pure silicon dioxide which is burned to constant weight at 810 ℃ by a high-precision microbalance, adding the spectral pure silicon dioxide into the beakers, placing the beakers in a muffle furnace, cooling, preparing sample solutions according to 2.2 and 2.3, carrying out analytical test, and inspecting the recovery rate of the method. The recovery rates of silicon element are all more than 95% (see table 7).
TABLE 7 Polyacrylonitrile-based carbon fiber silicon standard addition recovery test
Claims (7)
1. A method for determining impurity elements in a polyacrylonitrile-based carbon fiber sample is characterized in that the carbon fiber sample is ashed, and the ashed residues are treated by high-purity acid; measuring impurity elements in the ash by adopting an inductively coupled plasma atomic emission spectrometry; the method specifically comprises the following steps:
(1) ashing the carbon fiber sample;
(2) dissolving the ashing residues by using high-purity acid to prepare a sample solution;
(3) preparing a mixed standard use solution of potassium, sodium, calcium, magnesium and iron, and preparing a standard use solution of silicon;
(4) and the sample solution is used for measuring impurity elements in the sample solution by an inductively coupled plasma atomic emission spectrometer provided with a hydrofluoric acid resistant sampling system.
2. The method for determining impurity elements in a polyacrylonitrile-based carbon fiber sample according to claim 1, wherein: and (2) ashing the carbon fiber sample in the step (1), specifically, putting the carbon fiber sample in a quartz beaker, putting the quartz beaker in a muffle furnace, and heating the carbon fiber sample from room temperature to 600 ℃ within 60-90min in a temperature programming manner until ashing is complete.
3. The method for determining impurity elements in a polyacrylonitrile-based carbon fiber sample according to claim 1, wherein: and (3) dissolving the sample solution in the step (2) by using high-purity acid, specifically dissolving the ashing residues by using high-purity hydrofluoric acid and hydrochloric acid solution to prepare the sample solution.
4. The method for determining impurity elements in a polyacrylonitrile-based carbon fiber sample according to claim 3, wherein: the step (2) of preparing the sample solution by dissolving the ashing residues with the high-purity hydrofluoric acid and hydrochloric acid solution comprises the following steps: sucking up the ashing residues in the quartz beaker by using a wet glass rod, transferring the ashing residues into a plastic centrifugal test tube, cleaning the glass rod by using deionized water, dropwise adding hydrofluoric acid into the plastic centrifugal test tube to completely dissolve the ashing residues, adding a hydrochloric acid solution into the quartz beaker to dissolve the ashing residues remained on the inner wall and the bottom of the quartz beaker, transferring the ashing residues into the plastic centrifugal test tube by using a polytetrafluoroethylene rod, cleaning the beaker by using the deionized water, and fixing the volume of the beaker in the plastic centrifugal test tube to a scale.
5. The method for determining impurity elements in a polyacrylonitrile-based carbon fiber sample according to claim 1, wherein: the standard use solution for mixing potassium, sodium, calcium, magnesium and iron prepared in the step (3) is specifically as follows: preparing standard use solutions containing 0.00, 0.50, 1.00, 2.00, 4.00, 6.00, 8.00 and 10.0mg/L of potassium, sodium, calcium, magnesium and iron respectively; the preparation of the silicon standard use solution specifically comprises the following steps: preparing standard silicon use solutions with silicon contents of 0.00, 5.00, 10.0, 20.0, 30.0, 40.0, 50.0, 80.0 and 100.0mg/L respectively.
6. The method for determining impurity elements in a polyacrylonitrile-based carbon fiber sample according to claim 1, wherein: the impurity elements in the step (4) are potassium, sodium, calcium, magnesium, iron and silicon elements.
7. The method for determining impurity elements in polyacrylonitrile-based carbon fiber samples according to claim 6, wherein: the sample solution in the step (4) is used for measuring impurity elements in the sample solution by an inductively coupled plasma atomic emission spectrometer provided with a hydrofluoric acid resistant sampling system; when potassium, sodium, calcium, magnesium, iron and silicon elements are measured, the wavelengths of the inductively coupled plasma atomic emission spectrometer are 766.490nm, 589.592nm, 317.933nm, 279.553nm, 259.940nm and 212.412nm respectively.
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|---|---|---|---|---|
| CN113804525A (en) * | 2021-09-01 | 2021-12-17 | 山西钢科碳材料有限公司 | Pretreatment method of fiber sample |
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| CN114216873A (en) * | 2021-12-15 | 2022-03-22 | 中复神鹰碳纤维股份有限公司 | Method for measuring impurity content of polyacrylonitrile polymer liquid |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002020927A (en) * | 2000-07-03 | 2002-01-23 | Mitsubishi Rayon Co Ltd | Carbon fiber precursor fiber bundle |
| US6489027B1 (en) * | 1999-02-24 | 2002-12-03 | Toyo Tanso Co., Ltd. | High purity carbon fiber reinforced carbon composites and manufacturing apparatus for use thereof |
| CN101968436A (en) * | 2010-09-03 | 2011-02-09 | 沈阳工业大学 | Quantitative analysis method for measuring trace nickel in water by microwave digestion-flame atomic absorption spectrometry (FAAS) |
| CN104406956A (en) * | 2014-11-11 | 2015-03-11 | 中国纺织科学研究院 | Method for determining content of trace metal element in PAN-based carbon fiber |
| CN111351779A (en) * | 2018-12-20 | 2020-06-30 | 上海宝钢工业技术服务有限公司 | Method for measuring content of heavy metal cobalt, manganese, nickel, strontium and vanadium in waste oil |
-
2020
- 2020-11-09 CN CN202011251416.2A patent/CN112414998A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6489027B1 (en) * | 1999-02-24 | 2002-12-03 | Toyo Tanso Co., Ltd. | High purity carbon fiber reinforced carbon composites and manufacturing apparatus for use thereof |
| JP2002020927A (en) * | 2000-07-03 | 2002-01-23 | Mitsubishi Rayon Co Ltd | Carbon fiber precursor fiber bundle |
| CN101968436A (en) * | 2010-09-03 | 2011-02-09 | 沈阳工业大学 | Quantitative analysis method for measuring trace nickel in water by microwave digestion-flame atomic absorption spectrometry (FAAS) |
| CN104406956A (en) * | 2014-11-11 | 2015-03-11 | 中国纺织科学研究院 | Method for determining content of trace metal element in PAN-based carbon fiber |
| CN111351779A (en) * | 2018-12-20 | 2020-06-30 | 上海宝钢工业技术服务有限公司 | Method for measuring content of heavy metal cobalt, manganese, nickel, strontium and vanadium in waste oil |
Non-Patent Citations (2)
| Title |
|---|
| 刘孟刚: "《ICP-AES测定碳纤维材料的碱金属 、碱土金属元素》", 《现代仪器》 * |
| 姚亮: "《电感耦合等离子体发射光谱法测定聚丙烯腈基碳纤维中钾、钙、钠、镁、铁》", 《世界有色金属》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113804525A (en) * | 2021-09-01 | 2021-12-17 | 山西钢科碳材料有限公司 | Pretreatment method of fiber sample |
| CN113804525B (en) * | 2021-09-01 | 2024-04-19 | 山西钢科碳材料有限公司 | Pretreatment method of fiber sample |
| CN114199667A (en) * | 2021-12-13 | 2022-03-18 | 山西钢科碳材料有限公司 | Pretreatment method of azobisisobutyronitrile and determination method of trace element content |
| CN114216873A (en) * | 2021-12-15 | 2022-03-22 | 中复神鹰碳纤维股份有限公司 | Method for measuring impurity content of polyacrylonitrile polymer liquid |
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