CN112345570A - Method for measuring components of glass fibers - Google Patents

Method for measuring components of glass fibers Download PDF

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CN112345570A
CN112345570A CN202011166172.8A CN202011166172A CN112345570A CN 112345570 A CN112345570 A CN 112345570A CN 202011166172 A CN202011166172 A CN 202011166172A CN 112345570 A CN112345570 A CN 112345570A
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glass
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CN112345570B (en
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李勇
王小丽
师卓
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Nanjing Fiberglass Research and Design Institute Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/2202—Preparing specimens therefor
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/07—Investigating materials by wave or particle radiation secondary emission
    • G01N2223/076—X-ray fluorescence
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

The invention discloses a method for measuring components of glass fibers, which comprises the steps of preparing a sample to be measured, preparing a sample wafer of the sample to be measured, preparing a calibration sample, preparing a sample wafer of the calibration sample, preparing the sample wafer of the calibration sample, establishing a working curve, analyzing the sample wafer to be measured and the like.

Description

Method for measuring components of glass fibers
Technical Field
The invention relates to the technical field of chemical analysis, in particular to a method for measuring components of glass fibers.
Background
The glass fiber is fibrous glass composed of inorganic oxides, is used as a novel structural material and functional material, and is widely applied to the industries of electronics, electricity, architecture, national defense, biomedicine and the like. The component composition and content of the glass fiber determine the physical and chemical properties and classification characteristics of the fiber, and the rapid, accurate and efficient determination of the components of the glass fiber has important significance for glass fiber production enterprises.
The detection of the glass fiber component is mainly SiO2、Al2O3、CaO、MgO、K2O、Na2In the prior art, the glass is generally analyzed by a wet chemical analysis method in the detection of major elements such as O and the like and the detection of heavy metals such as barium, zinc and zirconiumThe wet chemical analysis method has complex operation process, long analysis time, non-uniform test method and the test result is influenced by human errors and reagents.
An X-ray fluorescence spectrum (XRF) analysis method is an important chemical analysis means, has the advantages of simple sample preparation, high analysis speed, capability of simultaneously carrying out multi-element determination, long retention time of a sample molten glass sheet, high analysis precision, high accuracy and the like, and is widely applied to conventional detection of samples such as geology, materials, environment and the like; however, this method has not been applied to the composition analysis of glass fibers.
Disclosure of Invention
The invention aims to provide a method for measuring glass fiber components, which adopts X-ray fluorescence spectrometry to measure the glass fiber components and has the advantages of simple operation, short time consumption, high accuracy and good reproducibility.
The technical scheme adopted by the invention is as follows:
a method of determining the composition of glass fibers comprising the steps of:
A. preparing a sample to be tested: taking a proper amount of glass fiber, cleaning, firing, crushing, dividing, grinding into powder of not less than 200 meshes, storing the powder in a weighing bottle, drying in a drying oven, and cooling to room temperature for later use;
B. preparing a sample wafer to be tested: quantitatively weighing the sample to be detected prepared in the step A, adding a fusing agent, uniformly mixing, adding an oxidant, pre-oxidizing in a muffle furnace at 550-600 ℃ for 10-15 min, taking out, cooling, adding a release agent, melting in a sample melting furnace, pouring the melt into a platinum-yellow alloy casting mold, and demolding to obtain a sample wafer to be detected;
C. preparation of calibration samples: selecting a glass standard sample to be mixed with a rock standard substance, adding a pure substance into the mixture to adjust the proportion, and preparing the standard sample; the content of the substances in the standard sample is as follows: SiO2 2 30～70％、Al2O3 2～18.5％、CaO 2～22.5％、BaO 1～25％、ZnO 1～12％、ZrO 2 1～12％、MgO 0.1～5％、K2O 0.1～9.5％、Na2O0.1～13.5％；
D. Preparing a calibration sample wafer: preparing a calibration sample wafer by adopting the method in the step B;
E. establishing a working curve: performing spectral line scanning on the calibration sample wafer by using an X-ray fluorescence spectrometer, selecting optimal analysis conditions according to different elements, respectively determining spectral line intensities of barium, zinc, zirconium, silicon, aluminum, calcium, magnesium, potassium and sodium in the calibration sample wafer, taking the spectral line intensities as vertical coordinates, taking mass percentages of oxides of the elements in the calibration sample as horizontal coordinates, and establishing a working curve according to a measurement result; selecting a proper mathematical correction equation to correct the working curve;
F. analyzing the sample wafer to be tested: and E, respectively measuring the spectral line intensity of barium, zinc, zirconium, silicon, aluminum, calcium, magnesium, potassium and sodium in the sample wafer to be analyzed obtained in the step B under the same measurement condition as that in the step E, and measuring the fluorescence intensity of the sample wafer to be analyzed according to the working curve corrected in the step E to obtain the content of barium, zinc, zirconium, silicon, aluminum, calcium, magnesium, potassium and sodium in the sample wafer to be analyzed.
Preferably, the glass standard samples are E glass with the standard number of GSB08-3556-2019, medium-alkali glass with the standard number of GSB08-3557-2019, alkali-free glass with the standard number of JBW04-1-1, borosilicate glass with the standard number of GBW03132 and soda-lime-silica glass with the standard number of GBW 03117.
Preferably, the rock standard substance is albite with standard number GBW03134, potassium feldspar with standard number GBW03116, and siliceous sandstone with standard number GBW 03112.
Preferably, the pure substances are BaO, ZnO and ZrO2。
Preferably, the flux in the step B is lithium tetraborate and/or lithium metaborate, and the mass ratio of the flux to the standard sample is 8-12: 1.
Preferably, in the step B, the oxidant is one of lithium nitrate, ammonium nitrate or sodium nitrate water solutions with the mass concentration of 100-250 g/L, and the dosage of the oxidant is 0.7-1.5 mL/g of standard sample.
Preferably, in step B, the release agent is one of ammonium iodide, lithium bromide, potassium iodide or potassium bromide solution.
Preferably, in the step B, the melting temperature is 1000-1100 ℃, shaking up is carried out at the frequency of 5 times per second in the melting process, the melting is carried out for 10-20 min, and the mixture is poured into a platinum yellow alloy casting mold after shaking for 5-10 min.
Preferably the optimal assay conditions in step E are as follows:
Figure BDA0002745850310000021
Figure BDA0002745850310000031
the invention has the beneficial effects that: the invention provides a method for determining components of glass fibers by using an X-ray fluorescence spectrometry, which can solve the problems that the existing glass fibers are detected by using a wet chemical analysis method, the operation process is complicated, the analysis time is long, the test methods of different elements are different, the test results are greatly influenced by human errors and reagents, and the like.
Drawings
Fig. 1 is a graph of the line L α operation of Ba of example 1.
Fig. 2 is a K α line graph of Zn in example 1.
Fig. 3 is a K α line graph of Zr in example 1.
Fig. 4 is a K α line graph of Si in example 1.
FIG. 5 is a K.alpha.curve of Al in example 1.
Fig. 6 is a K α curve operation chart of Ca in example 1.
FIG. 7 is a K.alpha.line graph of Mg of example 1.
Fig. 8 is a K α -line operation curve diagram of K in example 1.
Fig. 9 is a Na K α curve operation chart of example 1.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
The raw materials used in the following examples are all purchased from the market, wherein:
the standard number of albite is GBW 03134;
the standard number of the potassium feldspar is GBW 03116;
standard number of siliceous sandstone is GBW03112
The standard number of the medium alkali glass is GSB 08-3557-2019;
the standard number of the alkali-free glass is JBW 04-1-1;
the standard number of the E glass is GSB 08-3556-2019;
standard number of borosilicate glass is GBW 03132;
the standard number of soda-lime-silica glass is GBW 03117.
Example 1
1.1 preparation of samples to be tested: taking a proper amount of glass fiber containing barium, zinc and zirconium, cleaning, then burning for 30min at 625 ℃, removing organic matters such as wetting agents and the like, then carrying out condensation grinding to obtain a powder sample with the granularity of 200 meshes and the mass of not less than 10g, storing the ground sample in a weighing bottle, drying in an oven at 105-110 ℃ for not less than 1h, and cooling to room temperature in a dryer for later use.
1.2 preparing a sample wafer to be tested: weighing 0.7000g of the sample to be tested prepared in the step 1.1, accurately placing the sample to be tested into a platinum yellow alloy crucible, adding 7.000 +/-0.001 g of mixed flux prepared from lithium tetraborate and lithium metaborate according to the mass ratio of 66:34, uniformly mixing by using a plastic rod, adding 1mL of 220g/L lithium nitrate solution, pre-oxidizing for 10min at 600 ℃ in a muffle furnace, taking out, cooling, adding 0.5mL of 200g/L ammonium iodide solution, placing into a sample melting furnace at 1050 ℃ for melting, and shaking uniformly at the frequency of 5 times per second in the melting process; melting for 20min, swinging for 8min, pouring into platinum yellow alloy casting mold, taking out, air cooling for 5min, automatically peeling sample and mold, cooling, taking out sample, labeling, and storing in a drier for use to prevent moisture absorption and pollution. The prepared sample is a uniform glass body, the surface is flat and smooth, and no bubbles, unmelted small particles and the like are mixed.
1.3 preparation of calibration samples: selecting E glass, medium-alkali glass, alkali-free glass, borosilicate glass, soda-lime-silica glass, albite, potassium feldspar, siliceous sandstone, zinc oxide, barium oxide and zirconium oxide, checking the initial granularity, and processing the mixture by grinding equipment until the granularity reaches 200 meshes if the granularity is less than 200 meshes; quantitatively weighing the amounts of the standard substance and the pure substance according to the table 1, adding 7.000 +/-0.001 g of mixed flux prepared from lithium tetraborate and lithium metaborate according to the mass ratio of 66:34, mixing in a platinum-yellow alloy crucible, and preparing 15 calibration samples for later use; the ingredients and composition of the 15 calibration samples are shown in tables 1 and 2.
Table 1 ingredient table for calibration samples
Figure BDA0002745850310000041
Figure BDA0002745850310000051
TABLE 2 compositions and amounts of calibration samples
Figure BDA0002745850310000052
Figure BDA0002745850310000061
1.4 preparation of calibration sample coupons: and (3) respectively preparing the 15 calibration samples prepared in the step (1.3) into 15 calibration sample samples by adopting the method in the step (1.2), wherein the serial numbers of the samples are 1-15.
1.5, establishing a working curve: preheating an X-ray fluorescence spectrometer to stabilize the X-ray fluorescence spectrometer, scanning spectral lines of 15 calibration sample samples prepared in the step 1.4 by using the X-ray fluorescence spectrometer, selecting the optimal analysis conditions, and respectively measuring the spectral line intensities of Ba, Zn, Zr, Si, Al, Ca, Mg, K and Na in the calibration sample samples, wherein the measurement and analysis results are shown in tables 4-12;
TABLE 3 optimal analysis conditions for X-ray fluorescence spectrometer measurement
Figure BDA0002745850310000062
Table 4 table for BaO content measurement statistics of calibration sample wafer
Figure BDA0002745850310000063
Figure BDA0002745850310000071
According to table 4, the spectral line intensity of barium oxide is used as the ordinate, the mass percentage content of barium oxide in the calibration sample wafer is used as the abscissa, and the working curve of the L α line of Ba is established, and is shown in fig. 1.
TABLE 5 statistical table for measuring ZnO content of calibration sample wafer
Figure BDA0002745850310000072
According to the table 5, the work curve of the K α line of Zn is established by taking the spectral line intensity of zinc oxide as the ordinate and the mass percentage content of zinc oxide in the calibration sample wafer as the abscissa, and is shown in fig. 2.
TABLE 6 statistical table for ZrO2 content measurement of calibration sample specimens
Figure BDA0002745850310000081
According to the table 6, the work curve of the K α line of Zr was established by using the spectral line intensity of zirconia as the ordinate and the mass percentage of zirconia in the calibration sample piece as the abscissa, and is shown in fig. 3.
Table 7 SiO2 content measurement statistics table for calibration sample coupons
Figure BDA0002745850310000082
Figure BDA0002745850310000091
According to the table 7, the K α line intensity of the silica is taken as the ordinate, the mass percentage content of the silica in the calibration sample wafer is taken as the abscissa, and the K α line work curve of Si is established, and the work curve is shown in fig. 4.
Table 8 Al2O3 content measurement statistics table for calibration sample coupons
Figure BDA0002745850310000092
Figure BDA0002745850310000101
According to the table 8, the spectral line intensity of the aluminum oxide is taken as the ordinate, the mass percentage content of the aluminum oxide in the calibration sample wafer is taken as the abscissa, and the K α line working curve of Al is established, and the working curve is shown in fig. 5.
TABLE 9 CAO content measurement statistical table of calibration sample wafer
Figure BDA0002745850310000102
According to table 9, the mass percentage of calcium oxide in the calibration sample piece is plotted as abscissa and the spectral line intensity of calcium oxide is plotted as ordinate, and the working curve of the ka line of Ca is established as shown in fig. 6.
TABLE 10 MgO content measurement statistical table for calibration sample specimens
Figure BDA0002745850310000103
Figure BDA0002745850310000111
According to the table 10, the work curve of the K α line of Mg was established by using the spectral line intensity of magnesium oxide as the ordinate and the mass percentage content of magnesium oxide in the calibration sample piece as the abscissa, and is shown in fig. 7.
Table 11 statistical table for K2O content measurements of calibration sample coupons
Figure BDA0002745850310000112
Figure BDA0002745850310000121
According to table 11, the K α line working curve of K was established using the spectral line intensity of potassium oxide as the ordinate and the mass percentage of potassium oxide in the calibration sample piece as the abscissa, and is shown in fig. 8.
Table 12 statistical table for Na2O content measurement of calibration sample coupons
Figure BDA0002745850310000122
According to table 12, the mass percentage of sodium oxide in the calibration sample piece is plotted as abscissa and the spectral line intensity of sodium oxide is plotted as ordinate, and a working curve of Na K α line is established as shown in fig. 9.
1.6 correcting the working curve: and drawing a calibration curve of each element according to a calibration equation through background correction, spectral line overlapping correction and alpha coefficient correction.
1.7 analysis of the sample to be tested: and (3) respectively measuring the spectral line intensities of Ba, Zn, Zr, Si, Al, Ca, Mg, K and Na in the sample to be analyzed obtained in the step (1.2) under the same measurement condition as that in the step (1.5), and measuring the fluorescence intensity of the sample to be analyzed according to the working curve corrected in the step (1.6) to obtain the contents of Ba, Zn, Zr, Si, Al, Ca, Mg, K and Na in the sample to be analyzed.
As can be seen from tables 4 to 12, the measurement method of the present invention has high accuracy and precision.
The sample 1 is selected and repeatedly measured for 10 times according to the method, the statistical result of the measurement result is shown in the table 13, and the reproducibility of the measurement method is better as can be seen from the table 13.
Table 13 calibration sample replicate measurement statistics
Figure BDA0002745850310000131
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (9)

1. A method of determining the composition of glass fibers comprising the steps of:
A. preparing a sample to be tested: taking a proper amount of glass fiber, cleaning, firing, crushing, dividing, grinding into powder of not less than 200 meshes, storing the powder in a weighing bottle, drying in a drying oven, and cooling to room temperature for later use;
B. preparing a sample wafer to be tested: quantitatively weighing the sample to be detected prepared in the step A, adding a fusing agent, uniformly mixing, adding an oxidant, pre-oxidizing in a muffle furnace at 550-600 ℃ for 10-15 min, taking out, cooling, adding a release agent, melting in a sample melting furnace, pouring the melt into a platinum-yellow alloy casting mold, and demolding to obtain a sample wafer to be detected;
C. preparation of calibration samples: selecting a glass standard sample to be mixed with a rock standard substance, adding a pure substance into the mixture to adjust the mixture ratio, and preparing the standard sample(ii) a The content of the substances in the standard sample is as follows: SiO22 30～70％、Al2O3 2～18.5％、CaO 2～22.5％、BaO 1～25％、ZnO 1～12％、ZrO2 1～12％、MgO 0.1～5％、K2O 0.1～9.5％、Na2O 0.1～13.5％；
D. Preparing a calibration sample wafer: preparing a calibration sample wafer by adopting the method in the step B;
E. establishing a working curve: performing spectral line scanning on the calibration sample wafer by using an X-ray fluorescence spectrometer, selecting optimal analysis conditions according to different elements, respectively determining spectral line intensities of barium, zinc, zirconium, silicon, aluminum, calcium, magnesium, potassium and sodium in the calibration sample wafer, taking the spectral line intensities as vertical coordinates, taking mass percentages of oxides of the elements in the calibration sample as horizontal coordinates, and establishing a working curve according to a measurement result; selecting a proper mathematical correction equation to correct the working curve;
F. analyzing the sample wafer to be tested: and E, respectively measuring the spectral line intensity of barium, zinc, zirconium, silicon, aluminum, calcium, magnesium, potassium and sodium in the sample wafer to be analyzed obtained in the step B under the same measurement condition as that in the step E, and measuring the fluorescence intensity of the sample wafer to be analyzed according to the working curve corrected in the step E to obtain the content of barium, zinc, zirconium, silicon, aluminum, calcium, magnesium, potassium and sodium in the sample wafer to be analyzed.
2. The method as claimed in claim 1, wherein the glass standard samples are E glass with standard number GSB08-3556-2019, medium alkali glass with standard number GSB08-3557-2019, alkali-free glass with standard number JBW04-1-1, borosilicate glass with standard number GBW03132 and soda-lime-silica glass with standard number GBW 03117.
3. The method according to claim 1, wherein the rock standard substance is albite with standard number GBW03134, potassium feldspar with standard number GBW03116, and siliceous sandstone with standard number GBW 03112.
4. According to claimThe method according to claim 1, wherein the pure substances are BaO, ZnO and ZrO2。
5. The method according to claim 1, wherein the fusing agent in the step B is lithium tetraborate and/or lithium metaborate, and the mass ratio of the fusing agent to the standard sample is 8-12: 1.
6. The method according to claim 1, wherein the oxidant in step B is one of lithium nitrate, ammonium nitrate or sodium nitrate aqueous solutions with a mass concentration of 100-250 g/L, and the amount of the oxidant is 0.7-1.5 mL/g of standard sample.
7. The method of claim 1, wherein the release agent in step B is one of ammonium iodide, lithium bromide, potassium iodide, or potassium bromide solution.
8. The method according to claim 1, wherein in the step B, the melting temperature is 1000-1100 ℃, shaking up is carried out at a frequency of 5 times per second during the melting process, the melting is carried out for 10-20 min, and the mixture is poured into a platinum yellow alloy casting mold after shaking for 5-10 min.
9. The method of claim 1, wherein the optimal analysis conditions in step E are as follows:
Figure FDA0002745850300000021
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