CN111855722A - MgO and SiO in light-burned magnesium and magnesium stone2X-ray fluorescence spectrum analysis method of content - Google Patents
MgO and SiO in light-burned magnesium and magnesium stone2X-ray fluorescence spectrum analysis method of content Download PDFInfo
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- CN111855722A CN111855722A CN202010660772.3A CN202010660772A CN111855722A CN 111855722 A CN111855722 A CN 111855722A CN 202010660772 A CN202010660772 A CN 202010660772A CN 111855722 A CN111855722 A CN 111855722A
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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
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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
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
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- 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
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
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Abstract
The invention discloses MgO and SiO in light-burned magnesium and magnesium stone2The X-ray fluorescence spectrum analysis method of the content specifically comprises the following steps: 1. establishing a standard curve and preparing a standard sample; 2. determining the granularity of an analysis sample; 3. drying the analysis sample in an oven; 4. weighing 1g of an analysis sample, and burning the analysis sample in a muffle furnace; 5. transferring the burned analysis sample into a platinum crucible filled with a mixed flux, uniformly stirring, covering the surface with the mixed flux, and dropwise adding a release agent; 6. then putting the analysis sample into a claise M4 type sample melting furnace for melting; the invention saves the analysis time; the analysis result of the sample meets the precision requirement in the chemical analysis standard of relevant countries.
Description
Technical Field
The invention relates to MgO and SiO in light-burned magnesium and magnesium stone2X-ray fluorescence spectrum analysis of the content.
Background
At present, the quality acceptance of light burned magnesium, magnesite and brucite in most steel plants adopts the chemical analysis method of GB/T5069-2015 magnesium-aluminum series refractory materials. Wherein, if the MgO acceptance test adopts an EDTA complexation titration method, the MgO is analyzed The result is the total amount of CaO and MgO, therefore, the method must analyze the CaO content and then carry out deduction to obtain the analysis value of MgO, which increases the analysis steps; if the CyTA complexation titration method is adopted, although the CaO content does not need to be analyzed, the reagent hexamethylenetetramine which belongs to easy explosion control is used. Wherein SiO is2Molybdenum blue photometry is often used, and a large number of chemical reagents are also used in the analysis process. Although the chemical analysis method is a national recommended standard method, the analysis period is long, the steps are multiple, and a large amount of chemical reagents are needed, so that with the acceleration of the production rhythm of modern enterprises and the research and development of high-quality products, the instrument analysis is adopted to replace the chemical analysis, so that the problem that the rapid, accurate and environment-friendly determination of the components of the chemical analysis method is urgently needed to be solved by the current industry is solved.
Through literature search, there are examples of analyzing magnesium materials by using X-ray fluorescence spectrometry in the prior art, such as the methods for rapidly determining the content of magnesium oxide in lightly-burned magnesium balls by using an X-ray fluorescence melting method (patents) of the limited liability company of cast tubes emerging from the u.u.s.a., the methods for determining the content of magnesium oxide in magnesite by using the X-ray fluorescence spectrometry of Tianjin steel, and the methods for determining the major and minor components in magnesite, magnesite and magnesite by using the X-ray fluorescence spectrometry of saddle steel, which are different from the methods for melting samples, specifically expressed as different standard samples for establishing wires, fluxes, dilution ratios, mixing modes, and the like. For example, the samples commonly used for establishing the standard curve are all standard substances, the analysis range of the samples is limited by the fixed value of the standard substances, the relative content of the standard substances in the standard curve needs to be calculated by ignition reduction, the standard curve is established by using a reference reagent, and the flux is supplemented and corrected, so that the problem is solved; in the selection of the flux, lithium tetraborate is often used as the flux, which has good solubility for MgO and high SiO content 2The solubility of the compound is low, and the pure lithium tetraborate is used as a fusing agent, so that the problems of insufficient mechanical strength and easy cracking are solved2Meanwhile, the analysis is carried out, and the flaking rate of the molten pieces is improved; in the selection of the mixing mode, the mixing mode which is usually used and is not covered with the flux can cause the volatilization of the sample through experiments, so that the analysis result is not stableThe analysis result of the covering mode is more stable; the method for correcting the sample comprises the steps of supplementing the ignition decrement by the weight of the flux, wherein the measured value is the analysis value, and the supplemented flux is the analysis error introduced by the ignition decrement and is far smaller than the analysis error introduced by the ignition decrement correction measured value because the weight of the flux is far larger than the weight of the sample.
Disclosure of Invention
The technical problem to be solved by the invention is to provide MgO and SiO in light-burned magnesium and magnesium stone aiming at the defects in the prior art2The X-ray fluorescence spectrum analysis method of the content is accurate and reliable, and is beneficial to the improvement of the analysis automation of instruments in the field of metallurgical analysis.
The technical scheme for solving the technical problems is as follows: MgO and SiO in light-burned magnesium and magnesium stone2The X-ray fluorescence spectrum analysis method of the content specifically comprises the following steps:
(1) establishing a standard curve and preparing a standard sample, wherein the specific preparation steps of the standard sample are as follows: weighing a certain amount of reference magnesium oxide and reference silicon dioxide, mixing the two with a certain amount of mixed flux, completely covering 4g of mixed flux on the surface of the mixed flux, adding 1mL of release agent, melting in a sample melting furnace, melting into a standard sample wafer, and analyzing by an X fluorescence spectrometer;
(2) determining the particle size of the analysis sample: the particle size is less than 0.090 mm;
(3) drying the analysis sample in an oven at 105 ℃ for 1 h;
(4) weighing 1g of the analysis sample in a porcelain ark fired to constant weight at 1025 +/-25 ℃, wherein the total weight of the analysis sample and the porcelain ark is m1(g), placing the analysis sample and the porcelain ark in a muffle furnace at 1025 +/-25 ℃ for firing for 1 hour, taking out and cooling, recording the total weight of the analysis sample and the porcelain ark as m after firing2(g) calculating the loss on ignition Δ m, in particular Δ m = m2-m1;
(5) Transferring the burned analysis sample into a platinum crucible filled with (4 + delta m) g of mixed flux, uniformly stirring, covering 4g of mixed flux on the surface, and dropwise adding 1mL of release agent;
(6) Then putting the analysis sample into a claise M4 type melting furnace for melting to prepare an analysis sample glass melting piece, putting the analysis sample glass melting piece into a Siemens fly 9900 type fluorescence spectrometer for analysis, and selecting an established standard curve for comparative analysis.
The invention further defines the scheme:
the mixed flux is lithium metaborate: lithium tetraborate =2: 1.
The melting comprises a pre-melting stage and a melting stage, wherein the temperature of the pre-melting stage is 800 ℃, the time is 7 minutes, and the rotation is carried out; the temperature of the melting stage is controlled at 1050 ℃ for 10 minutes, the rotation is carried out, and then the natural cooling is carried out for 5 minutes; and (5) performing air cooling for 3 minutes.
The mold release agent was 400g/L lithium bromide.
And (3) firing the reference magnesium oxide and the reference silicon dioxide in a muffle furnace at 1000 ℃ for 4 hours, and cooling in a dryer.
The invention has the beneficial effects that: the invention mixes the light burned magnesium, magnesite and brucite sample with the mixed flux, covers them and puts them into the platinum crucible, and adopts the melting furnace to directly melt them into glass sheets for the analysis of X-ray fluorescence spectrometer, which has the following advantages compared with the existing chemical analysis: the operation steps are few, simple and clear, and easy to master; the variety of the used reagent is small, the use amount is reduced, and the analysis cost is saved; the multiple elements can be measured simultaneously, so that the analysis time is saved; the analysis result of the sample meets the precision requirement in the related national chemical analysis standard, and is suitable for acceptance of light-burned magnesium, magnesite and brucite in steel enterprises, internal quality control of suppliers and factory inspection.
Drawings
FIG. 1 is a graph showing the analysis of MgO in example 1;
FIG. 2 is SiO in example 12The graph is analyzed.
Detailed Description
Example 1
This example provides a method for producing MgO and SiO in light-burned magnesium and magnesium stone2The X-ray fluorescence spectrum analysis method of the content specifically comprises the following steps:
(1) establishing a standard curve and preparing a standard sample, wherein the specific preparation steps of the standard sample are as follows: weighing reference magnesia and reference silica which are subjected to muffle furnace ignition at 1000 ℃ for 4 hours and are cooled in a dryer according to the weight of table 1, mixing the two with a certain amount of mixed flux, wherein the mixed flux is specifically shown in table 1, 4g of mixed flux is completely covered on the surface of the mixed flux, 1mL of 400g/L lithium bromide is added, melting is carried out in a melting furnace, a standard sample piece is made by melting, analysis is carried out by an X fluorescence spectrometer, a light intensity-content curve is drawn according to the element content in table 1, an MgO analysis curve is shown in table 1, and a SiO analysis curve is shown in table 12The analytical curve is shown in FIG. 2;
(2) determining the granularity of the light analysis sample, wherein the granularity is 0.080 mm;
(3) drying the analysis sample in an oven at 105 ℃ for 1 h;
(4) weighing 1g of the analysis sample in a porcelain ark fired to constant weight at 1025 ℃, wherein the total weight of the analysis sample and the porcelain ark is m1(g), placing the analysis sample and the porcelain ark in a muffle furnace at 1025 ℃ for firing for 1 hour, taking out and cooling, and recording the total weight m of the analysis sample and the porcelain ark after firing 2(g) calculating the loss on ignition Δ m, in particular Δ m = m2-m1;
(5) Transferring the burned analysis sample into a platinum crucible filled with (4 + delta m) g of mixed flux, uniformly stirring, covering 4 g of mixed flux on the surface, and dropwise adding 1mL of 400g/L lithium bromide;
(6) then putting the analysis sample into a claise M4 type melting furnace for melting to prepare an analysis sample glass melting piece, putting the analysis sample glass melting piece into a Siemens fly 9900 type fluorescence spectrometer for analysis, and selecting an established standard curve for comparative analysis.
TABLE 1 Standard specimen preparation Standard reagent, Prime flux weighing and standard specimen relative content
Selecting 1 light-burned magnesium as an analysis sample, preparing 6 light-burned magnesium as the analysis sample according to the preparation method of the analysis sample, and analyzing, wherein the experimental data are shown in the table 2.
Table 2 experimental data (%)
Numbering | 1 | 2 | 3 | 4 | 5 | 6 |
MgO | 69.55 | 69.54 | 69.35 | 69.30 | 69.47 | 69.33 |
SiO2 | 3.71 | 3.71 | 3.66 | 3.68 | 3.68 | 3.67 |
As can be seen from Table 2: the relative standard deviation of MgO is 0.16, and the precision is good; SiO 22The degree of (c) is 0.84% for standard deviation, and is also within the smaller range. The sample melting method is stable and reliable.
Selecting 2 magnesite, brucite standards and light-burned magnesium standard substances, respectively preparing magnesite, brucite analysis samples and light-burned magnesium analysis samples according to an analysis sample preparation method, and comparing the magnesite, brucite analysis samples and light-burned magnesium analysis samples with standard value contents; the experimental data are shown in table 3.
TABLE 3 Experimental data (%)
Note: the allowable error is determined by the chemical analysis method of the magnesium-aluminum series refractory material GB/T5069-2015
And (4) conclusion: the analysis errors are within the allowable error range specified by the national standard, and the daily analysis and sample valuing can be met.
In conclusion, the method is used for measuring MgO and SiO in light-burned magnesium, magnesite and brucite2The melting sample preparation-X-ray fluorescence spectrum analysis technology of the content simplifies the analysis process, shortens the analysis time, saves the cost of the analysis reagent and improves the analysis efficiency.
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (5)
1. MgO and SiO in light-burned magnesium and magnesium stone2The X-ray fluorescence spectrum analysis method of the content is characterized in that: the method specifically comprises the following steps:
(1) establishing a standard curve and preparing a standard sample, wherein the specific preparation steps of the standard sample are as follows: weighing a certain amount of reference magnesium oxide and reference silicon dioxide, mixing the two with a certain amount of mixed flux, completely covering 4g of mixed flux on the surface of the mixed flux, adding 1mL of release agent, melting in a sample melting furnace, melting into a standard sample wafer, and analyzing by an X fluorescence spectrometer;
(2) Determining the particle size of the analysis sample: the particle size is less than 0.090 mm;
(3) drying the analysis sample in an oven at 105 ℃ for 1 h;
(4) weighing 1g of the analysis sample in a porcelain ark fired to constant weight at 1025 +/-25 ℃, wherein the total weight of the analysis sample and the porcelain ark is m1(g), placing the analysis sample and the porcelain ark in a muffle furnace at 1025 +/-25 ℃ for firing for 1 hour, taking out and cooling, recording the total weight of the analysis sample and the porcelain ark as m after firing2(g), calculating the ignition loss Delta m,in particular Δ m = m2-m1;
(5) Transferring the burned analysis sample into a platinum crucible filled with (4 + delta m) g of mixed flux, uniformly stirring, covering 4 g of mixed flux on the surface, and dropwise adding 1mL of release agent;
(6) then putting the analysis sample into a claise M4 type melting furnace for melting to prepare an analysis sample glass melting piece, putting the analysis sample glass melting piece into a Siemens fly 9900 type fluorescence spectrometer for analysis, and selecting an established standard curve for comparative analysis.
2. The light-burned magnesite or magnesite magnesium silicate as claimed in claim 12The X-ray fluorescence spectrum analysis method of the content is characterized in that: the mixed flux is lithium metaborate: lithium tetraborate =2: 1.
3. The light-burned magnesite or magnesite magnesium silicate as claimed in claim 12The X-ray fluorescence spectrum analysis method of the content is characterized in that: the melting comprises a pre-melting stage and a melting stage, wherein the temperature of the pre-melting stage is 800 ℃, the time is 7 minutes, and the rotation is performed; the temperature of the melting stage is controlled at 1050 ℃ for 10 minutes, the rotation is carried out, and then the natural cooling is carried out for 5 minutes; and (5) performing air cooling for 3 minutes.
4. The light-burned magnesite or magnesite magnesium silicate as claimed in claim 12The X-ray fluorescence spectrum analysis method of the content is characterized in that: the release agent is 400g/L of lithium bromide.
5. The light-burned magnesite or magnesite magnesium silicate as claimed in claim 12The X-ray fluorescence spectrum analysis method of the content is characterized in that: and (3) burning the reference magnesium oxide and the reference silicon dioxide in the standard sample in a muffle furnace at 1000 ℃ for 4 hours, and cooling in a dryer.
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