CN111855722B - MgO and SiO in light-burned magnesium and magnesium stone 2 X-ray fluorescence spectrum analysis method of content - Google Patents
MgO and SiO in light-burned magnesium and magnesium stone 2 X-ray fluorescence spectrum analysis method of content Download PDFInfo
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- CN111855722B CN111855722B CN202010660772.3A CN202010660772A CN111855722B CN 111855722 B CN111855722 B CN 111855722B CN 202010660772 A CN202010660772 A CN 202010660772A CN 111855722 B CN111855722 B CN 111855722B
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Abstract
The invention discloses MgO and SiO in light-burned magnesium and magnesium stone 2 The X-ray fluorescence spectrum analysis method of content specifically comprisesThe method 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 Claisse 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 stone 2 X-ray fluorescence spectrum analysis of the content.
Background
At present, the quality acceptance of the light burned magnesia, magnesite and brucite in most steel mills adopts the chemical analysis method of the magnesium-aluminum series refractory material GB/T5069-2015. If the MgO acceptance test adopts an EDTA complexation titration method, the analysis result is the sum of CaO and MgO, therefore, the method needs to 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 is 2 Molybdenum 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 the prior art for analyzing magnesium materials by X-ray fluorescence spectrometry, such as WU lake emerging cast tube Limited liability company "method for rapidly determining content of magnesium oxide in lightly-burned magnesium balls by X-ray fluorescence fusion method" (patent), tianjin Steel "X-ray fluorescence spectrometry for determining main elements in magnesite", saddle Steel "X-ray fluorescence spectrometry for determining magnesite, magnesite and magnesiteThe difference between the major and minor components in the mine and the method lies in the difference between the sample melting method and the sample melting method, which is specifically represented by the difference between a standard sample for establishing a wire, a fusing agent, a dilution ratio, a mixing mode 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, and the relative content of the standard substances in the standard curve needs to be calculated by ignition reduction; in the selection of the flux, lithium tetraborate is often used as the flux, which has good solubility for MgO and high SiO content 2 The 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 solved 2 Meanwhile, the analysis is carried out, and the flaking rate of the molten pieces is improved; in the selection of the mixing mode, the frequently used mixing mode without covering flux can cause the volatilization of the sample through experiments, so that the analysis result is unstable, and the analysis result by using 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 art 2 The 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 stone 2 The 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 0.090mm;
(3) Drying the analysis sample in an oven at 105 ℃ for 1h;
(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 m 1 (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 firing 2 (g) calculating the loss on ignition Δ m, in particular Δ m = m 2 -m 1 ；
(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 sample melting furnace for melting to prepare an analysis sample glass melting sheet, putting the analysis sample glass melting sheet 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; 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 shows SiO in example 1 2 The graph is analyzed.
Detailed Description
Example 1
This example provides a method for producing MgO and SiO in light-burned magnesium and magnesium stones 2 The X-ray fluorescence spectrum analysis method for 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 1 2 The analytical curve is shown in FIG. 2;
(2) Determining the granularity of the light analysis sample, wherein the granularity is 0.080mm;
(3) Drying the analysis sample in an oven at 105 ℃ for 1h;
(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 m 1 (g) of a reaction product of,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 of the analysis sample and the porcelain ark after firing as m 2 (g), calculating the loss on ignition Δ m, specifically Δ m = m 2 -m 1 ；
(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 400g/L lithium bromide;
(6) Then putting the analysis sample into a claise M4 type sample melting furnace for melting to prepare an analysis sample glass melting sheet, putting the analysis sample glass melting sheet 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
And (3) 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 |
| SiO 2 | 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; siO2 2 The 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 reference to GB/T5069-2015 chemical analysis method for magnesium-aluminum series refractory materials
And (4) conclusion: the analysis errors are within the allowable error range specified by national standards, 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 brucite 2 The 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 (4)
1. An X-ray fluorescence spectrum analysis method for the contents of MgO and SiO2 in light-burned magnesium and magnesium stones 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 reference magnesium oxide and reference silicon dioxide, mixing the reference magnesium oxide and the reference silicon dioxide with 5g of mixed flux in total, 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, and analyzing in an X fluorescence spectrometer, wherein the mixed flux is lithium metaborate: lithium tetraborate = 2:1;
(2) Determining the particle size of the analysis sample: the particle size is less than 0.090mm;
(3) Drying the analysis sample in an oven at 105 ℃ for 1h;
(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 m 1 Placing the analysis sample and porcelain ark in a muffle furnace at 1025 +/-25 ℃ for firing for 1 hour, taking out and cooling, and recording the total weight of the analysis sample and the porcelain ark after firing as m 2 Calculating the ignition loss delta m, specifically, delta m = m 1 - m 2 ；
(5) Transferring the burned analysis sample into a platinum crucible containing 4+ Deltam grams of mixed flux, uniformly stirring, covering 4 grams of mixed flux on the surface, and dropwise adding 1mL of release agent;
(6) Then putting the analysis sample into a claise M4 type sample melting furnace for melting to prepare an analysis sample glass melting sheet, putting the analysis sample glass melting sheet into a Siemens fly 9900 type fluorescence spectrometer for analysis, and selecting an established standard curve for comparative analysis.
2. The method for analyzing the contents of MgO and SiO2 in the light-burned magnesium and magnesium stones as claimed in claim 1, wherein the method comprises the following steps: 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.
3. The method for analyzing the contents of MgO and SiO2 in the light-burned magnesium and magnesium stones as claimed in claim 1, wherein the method comprises the following steps: the release agent is 400g/L of lithium bromide.
4. The method for analyzing the content of MgO and SiO2 in the soft-burned magnesium and magnesium stones according to claim 1, wherein the method comprises the following steps: 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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