CN112649456A - Light-burned magnesium ball high-temperature melting X-ray fluorescence analysis method - Google Patents
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 57
- 239000011777 magnesium Substances 0.000 title claims abstract description 57
- 238000002844 melting Methods 0.000 title claims abstract description 33
- 230000008018 melting Effects 0.000 title claims abstract description 33
- 238000004876 x-ray fluorescence Methods 0.000 title claims abstract description 31
- 238000004458 analytical method Methods 0.000 title claims abstract description 18
- 238000001304 sample melting Methods 0.000 claims abstract description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 19
- 239000010703 silicon Substances 0.000 claims abstract description 19
- 238000011088 calibration curve Methods 0.000 claims abstract description 17
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 17
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 17
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000005259 measurement Methods 0.000 claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 7
- 230000004907 flux Effects 0.000 claims description 18
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 6
- PSHMSSXLYVAENJ-UHFFFAOYSA-N dilithium;[oxido(oxoboranyloxy)boranyl]oxy-oxoboranyloxyborinate Chemical compound [Li+].[Li+].O=BOB([O-])OB([O-])OB=O PSHMSSXLYVAENJ-UHFFFAOYSA-N 0.000 claims description 6
- HZRMTWQRDMYLNW-UHFFFAOYSA-N lithium metaborate Chemical compound [Li+].[O-]B=O HZRMTWQRDMYLNW-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- SWLVFNYSXGMGBS-UHFFFAOYSA-N ammonium bromide Chemical compound [NH4+].[Br-] SWLVFNYSXGMGBS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- RWDBMHZWXLUGIB-UHFFFAOYSA-N [C].[Mg] Chemical compound [C].[Mg] RWDBMHZWXLUGIB-UHFFFAOYSA-N 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- JUWSSMXCCAMYGX-UHFFFAOYSA-N gold platinum Chemical compound [Pt].[Au] JUWSSMXCCAMYGX-UHFFFAOYSA-N 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000006082 mold release agent Substances 0.000 claims 1
- 238000007689 inspection Methods 0.000 abstract description 11
- 238000001228 spectrum Methods 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 238000001514 detection method Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000001095 magnesium carbonate Substances 0.000 description 4
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 4
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 4
- 235000014380 magnesium carbonate Nutrition 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 235000019738 Limestone Nutrition 0.000 description 3
- 238000009614 chemical analysis method Methods 0.000 description 3
- 239000010459 dolomite Substances 0.000 description 3
- 229910000514 dolomite Inorganic materials 0.000 description 3
- 239000006028 limestone Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910052599 brucite Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001917 fluorescence detection Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000000705 flame atomic absorption spectrometry Methods 0.000 description 1
- 238000012921 fluorescence analysis Methods 0.000 description 1
- 238000001506 fluorescence spectroscopy Methods 0.000 description 1
- 238000005194 fractionation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical compound [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 1
- 230000033764 rhythmic process Effects 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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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
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention discloses a light-burned magnesium ball high-temperature melting X-ray fluorescence analysis method, which comprises the following steps: 1) grinding the lightly-sintered magnesium balls to prepare samples; 2) preparing a calibration sample; 3) preparing a calibration sample wafer; 4) controlling the precision of the addition amount of the release agent after mixing; 5) controlling the operation time of placing a crucible in the high-temperature sample melting furnace and the temperature of the sample melting furnace; 6) establishing a calibration curve; 7) measuring elements of a sample to be measured; 8) setting magnesium oxide measurement conditions; 9) setting the measurement condition of the silicon dioxide; the method analyzes the contents of the magnesium element and the silicon element in the light-burned magnesium balls by using an X-ray fluorescence spectrum method, can be applied to the determination of the magnesium and silicon content elements in the light-burned magnesium balls, can realize the rapid and comprehensive rapid analysis of the light-burned magnesium balls, has the inspection period of about 60min, is superior to the inspection period of the similar high-temperature melting X-ray fluorescence analysis, and meets the requirements on the accurate and rapid inspection of the contents of the magnesium element and the silicon element in the light-burned magnesium balls.
Description
Technical Field
The invention relates to the technical field of light-burned magnesium ball assay, in particular to a high-temperature melting X-ray fluorescence analysis method for light-burned magnesium balls.
Background
The soft-burned magnesium balls are used as a flux commonly used in iron and steel works, and have the functions of slag discharging, slag component adjustment, alkalinity, viscosity and reaction capacity in iron-making and steel-making smelting processes in the works. The purpose is to react with the metal to produce a metal having the required composition and temperature.
In order to meet the requirement of production inspection indexes, the light-burned magnesium balls are inspected in a laboratory according to GB/T3286.1-2012, the first part of a limestone and dolomite chemical analysis method: measurement of calcium oxide and magnesium oxide content Complex titration and flame atomic absorption Spectroscopy "and GB/T3286.2-2012 limestone and Dolomite chemical analysis method second part: determination of the silica content silicon molybdenum blue spectrophotometry and perchloric acid dehydration gravimetric method. When the test is carried out by referring to the national standard method, operations such as acidolysis, constant volume, fractionation, titration and the like are required to be carried out after the mixed solvent is melted. About 4 hours is needed for one sample, for large-scale inspection in steel plants, the inspection amount of the light-burned magnesium balls is about 20 batches per day at present, the defects of low efficiency, long time, multiple occupied times and high labor intensity of workers exist in actual inspection operation, and the rhythm of the existing inspection task is also seriously restricted and influenced.
It is known that the laboratory test unit uses a new technology of fluorescence analysis after melting at high temperature for the light-burned magnesium balls, but in a specific operation, the magnesium oxide test needs to obtain the calculation result of the ignition loss, and then the fluorescence data is calibrated. When the detection of the ignition decrement of the light-burned magnesium balls is carried out according to the GB/T3286.8 standard of determination of ignition decrement of limestone and dolomite chemical analysis method, about 3 hours is needed, and meanwhile, the detection is greatly influenced by the environmental humidity, so that the detection error is easily caused, the calibration coefficient in the fluorescence detection is influenced, and the accuracy of the light-burned magnesium balls is improved. Therefore, a light-burned magnesium ball high-temperature melting X-ray fluorescence analysis method needs to be designed to solve the problems of long detection time, low efficiency and detection error in the existing light-burned magnesium ball fluorescence detection.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a high-temperature melting X-ray fluorescence analysis method for light-burned magnesium balls.
The technical scheme adopted by the invention for solving the technical problems is as follows: a light-burned magnesium ball high-temperature melting X-ray fluorescence analysis method comprises the following steps:
1) grinding a sample by using a light-burned magnesium ball: the grinding granularity is more than or equal to 180 meshes, the quantitative amount of a magnesium-carbon ball sample put into a mortar for grinding is 60 +/-2 grams, and the grinding time is 100 seconds;
2) preparation of calibration samples: preparing a calibration sample for establishing a calibration curve, wherein the element contained in the calibration sample is one or two of magnesium element and silicon element;
3) preparing a calibration sample wafer: mixing the burned calibration sample with a flux, melting at a high temperature, uniformly mixing, pouring into a preheated platinum-gold mold, and cooling to prepare a calibration sample wafer;
4) precision control of addition amount of release agent after mixing: accurately dropwise adding 0.5ml +/-0.05 ml of 30% ammonium bromide solution by using a micropipette;
5) controlling the operation time of placing a crucible in the high-temperature sample melting furnace and the temperature of the sample melting furnace: opening a furnace cover, placing a crucible, keeping the temperature of the sample melting furnace to be not lower than 970 ℃, prolonging the early-stage heating time by about 1min when the temperature of the sample melting furnace is reduced to 950 ℃, and keeping the magnesium oxide to be lower than a standard value by 0.08-0.19%; after the melting is finished, taking out the crucible within 30 seconds after the prompt tone of the high-temperature sample melting furnace;
6) establishing a calibration curve: respectively measuring the fluorescence intensity values of magnesium element and silicon element in the prepared calibration sample wafer by using an X-ray fluorescence spectrometer, correcting elements by using a theoretical alpha coefficient, establishing a calibration curve of element content and the corrected fluorescence intensity value, and obtaining the slope and intercept of the calibration curve;
7) and (3) determination of elements of the sample to be detected: preparing a sample wafer of the sample to be detected according to the method for preparing the sample wafer of the calibration sample in the step 2, and analyzing the sample wafer of the sample to be detected by using an X-ray fluorescence spectrometer to obtain fluorescence intensity values after correcting magnesium and silicon elements;
8) setting of magnesium oxide measurement conditions: crystal RX35 SPC, target Rh40kV 70mA, 2 theta 21.050 degree, PHA 100-326;
9) setting of silica measurement conditions: crystal RX4 SPC, target Rh40kV 70mA, 2 theta 144.780 degree, PHA 102-319.
Specifically, the flux in the step 3 is a mixed flux of lithium tetraborate and lithium metaborate, wherein the mass ratio of the lithium tetraborate to the lithium metaborate is 67:33, and the mass ratio of the flux to the sample is 16: 1; the mixed flux is weighed to be 8.0g, the light-burned magnesium ball sample is weighed to be 0.5g, the proportion of the platinum yellow crucible is 95% + 5%, and the diameter of the bottom is more than or equal to 35 mm.
Specifically, the high-temperature melting temperature in the step 3 is 1000 ℃, and the melting time is 15 min.
Specifically, when the addition amount of the release agent in the step 4 is 0.6ml, the magnesium oxide is lower than a standard value by 0.09-0.21%; when the addition amount of the release agent is 0.4ml, the magnesium oxide is higher than the standard value by 0.12-0.29%.
Specifically, when the melting in step 5 is completed and the crucible is taken out after 90 seconds after the prompt tone of the high-temperature sample melting furnace, the bottom of the sample piece is cooled after the sample piece is formed, and the sample piece cannot be used.
Specifically, the X-ray fluorescence spectrometer in step 6 is a japanese physical Rigaku 14 type wavelength dispersion spectrometer, and both the magnesium element and the silicon element are fixed channels.
The invention has the following beneficial effects:
the high-temperature melting X-ray fluorescence analysis method for the light-burned magnesium balls, which is designed by the invention, can be used for analyzing the contents of magnesium and silicon in the light-burned magnesium balls by using an X-ray fluorescence spectrum method, can be applied to the determination of the contents of the magnesium and the silicon in the light-burned magnesium balls, can realize the rapid, comprehensive and rapid analysis of the light-burned magnesium balls, has the inspection period of about 60min, is superior to the inspection period of the similar high-temperature melting X-ray fluorescence analysis, and meets the requirements on accurate and rapid inspection of the contents of the magnesium and the silicon in the light-burned magnesium balls.
Drawings
FIG. 1 is a graph of the working curve of the magnesium oxide established in the present invention. (y-1.5962 Xx-8.2815, correlation coefficient 0.988006)
Figure 2 is a graph of the silica work curve established by the present invention. (y-3.1206 Xx-0.59038, correlation coefficient 0.995972)
FIG. 3 is a diagram of the PHA region of magnesium oxide in the present invention.
FIG. 4 is a diagram of the PHA region of silica in the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described in further detail in the following clearly and completely with reference to the accompanying drawings in the embodiments of the present 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.
As shown in fig. 1-4, a method for analyzing light-burned magnesium balls by high-temperature melting X-ray fluorescence comprises the following steps:
1) grinding a sample by using a light-burned magnesium ball: the grinding granularity is more than or equal to 180 meshes, the quantitative amount of a magnesium-carbon ball sample put into a mortar for grinding is 60 +/-2 grams, and the grinding time is 100 seconds.
2) Preparation of calibration samples: preparing a calibration sample for establishing a calibration curve, wherein the calibration sample respectively comprises different types of elements with different contents, namely one or two of magnesium element and silicon element, and the used calibration sample can be a national standard substance or a mixture of the national standard substance and a high-purity reagent.
3) Preparing a calibration sample wafer: mixing the burned calibration sample with a flux, melting at 1000 ℃ for 15min, pouring the mixture into a preheated platinum-gold mold after uniform mixing, and cooling to prepare a calibration sample wafer;
the flux is a mixed flux of lithium tetraborate and lithium metaborate, wherein the mass ratio of the lithium tetraborate to the lithium metaborate is 67:33, and the mass ratio of the flux to the sample is 16: 1; the mixed flux is weighed to be 8.0g, the light-burned magnesium ball sample is weighed to be 0.5g, the proportion of the platinum yellow crucible is 95% + 5%, and the diameter of the bottom is more than or equal to 35 mm.
4) Precision control of addition amount of release agent after mixing: accurately dropwise adding 0.5ml +/-0.05 ml of 30% ammonium bromide solution by using a micropipette; the addition amount of the release agent is in a required range, and when the addition amount of the release agent is 0.6ml, the magnesium oxide is lower than a standard value of 0.09-0.21%; when the addition amount of the release agent is 0.4ml, the magnesium oxide is higher than the standard value by 0.12-0.29%.
5) Controlling the operation time of placing a crucible in the high-temperature sample melting furnace and the temperature of the sample melting furnace: after the furnace cover is opened and the crucible is placed, the temperature of the sample melting furnace cannot be lower than 970 ℃, so that the phenomenon that the temperature is too much reduced to cause the lengthening of the temperature rise time and the inconsistent melting time is avoided, when the temperature of the sample melting furnace is reduced to 950 ℃, the early temperature rise time is lengthened by about 1min, and the magnesium oxide is lower than the standard value by 0.08-0.19%;
after the melting is finished, taking out the crucible within 30 seconds after the prompt tone of the high-temperature sample melting furnace; when the crucible is taken out after 90 seconds after the sample melting furnace is finished, bubbles exist at the bottom of the sample wafer after the sample wafer is formed and cooled, and the crucible cannot be used.
6) Establishing a calibration curve: respectively measuring the fluorescence intensity values of magnesium and silicon elements in the prepared calibration sample wafer by using an X-ray fluorescence spectrometer, correcting the elements by using a theoretical alpha coefficient, establishing a calibration curve of the element content and the corrected fluorescence intensity value, and obtaining the slope and intercept of the calibration curve;
the X-ray fluorescence spectrometer is a Nippon Rigaku 14 type wavelength dispersion spectrometer, and both magnesium element and silicon element are fixed channels.
7) And (3) determination of elements of the sample to be detected: and (3) preparing a sample wafer of the sample to be detected according to the method for preparing the sample wafer of the calibration sample in the step (2), and analyzing the sample wafer of the sample to be detected by using an X-ray fluorescence spectrometer to obtain the fluorescence intensity values of the corrected magnesium and silicon elements.
8) Setting of magnesium oxide measurement conditions: crystal RX35 SPC, target Rh40kV 70mA, 2 theta 21.050 degree, PHA 100-326.
9) Setting of silica measurement conditions: crystal RX4 SPC, target Rh40kV 70mA, 2 theta 144.780 degree, PHA 102-319.
The invention discloses an embodiment:
1) preparation of calibration samples
Firstly, preparing calibration samples for establishing a calibration curve, wherein the calibration samples respectively comprise elements with different types and different contents. Wherein the number of the calibration samples should meet the requirement of the precision of the calibration curve, and the larger the number, the better the calibration curve.
The invention adopts the national standard substance and the way of matching the national standard substance with the high-purity reagent to prepare the calibration sample. The adopted national standard substances comprise GBW03128 (brucite), GBW03129 (brucite), YSBC28726-2014 (magnesite), YSBC28726a-2014 (magnesite), YSBC28727-2014 (magnesite) and YSBC28728-2014 (magnesite).
2) Preparation of a series of calibration sample coupons
About 5.0g of calibration sample is weighed, dried in a muffle furnace at 175 ℃ to constant weight, cooled to room temperature, and placed in a desiccator for use. And firing the mixed flux in a muffle furnace at 500 ℃ for 4 hours, taking out, cooling to room temperature, and placing in a dryer for later use. Weighing 8.0g of mixed flux into a platinum yellow crucible, weighing 0.5g of sample into the crucible, stirring uniformly, dropwise adding 0.5ml of 30% ammonium bromide solution by using a micropipette, and placing the mixture into a sample melting furnace which is preheated to 1000 ℃ for melting for 15 min. When the crucible is placed, the rapid operation is required, and the temperature of the sample melting furnace is ensured not to be lower than 970 ℃. And (4) taking out the crucible within 30 seconds after the sample melting is finished and the prompt tone, placing the crucible on a horizontal table, and cooling to room temperature. Taking out the sample, and pasting the serial number for later use.
3) Establishment of calibration Curve
Respectively measuring the fluorescence intensity values of magnesium and silicon elements of the prepared analysis sample by using an X-ray fluorescence spectrometer, correcting the elements by using a theoretical alpha coefficient, and establishing a working curve between the element content and the corrected fluorescence intensity as shown in a figure 1-2; wherein the measured parameters of the respective elements are shown in fig. 3-4.
4) Determination of elements in a sample to be tested
Obtaining a sample wafer for X-ray fluorescence spectrum analysis of the sample to be detected according to the method in the step 2), and analyzing the sample wafer by using an X-ray fluorescence spectrometer.
The present invention is not limited to the above embodiments, and any structural changes made under the teaching of the present invention shall fall within the scope of the present invention, which is similar or similar to the technical solutions of the present invention.
The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.
Claims (6)
1. A light-burned magnesium ball high-temperature melting X-ray fluorescence analysis method is characterized by comprising the following steps:
1) grinding a sample by using a light-burned magnesium ball: the grinding granularity is more than or equal to 180 meshes, the quantitative amount of a magnesium-carbon ball sample put into a mortar for grinding is 60 +/-2 grams, and the grinding time is 100 seconds;
2) preparation of calibration samples: preparing a calibration sample for establishing a calibration curve, wherein the element contained in the calibration sample is one or two of magnesium element and silicon element;
3) preparing a calibration sample wafer: mixing the burned calibration sample with a flux, melting at a high temperature, uniformly mixing, pouring into a preheated platinum-gold mold, and cooling to prepare a calibration sample wafer;
4) precision control of addition amount of release agent after mixing: accurately dropwise adding 0.5ml +/-0.05 ml of 30% ammonium bromide solution by using a micropipette;
5) controlling the operation time of placing a crucible in the high-temperature sample melting furnace and the temperature of the sample melting furnace: opening a furnace cover, placing a crucible, keeping the temperature of the sample melting furnace to be not lower than 970 ℃, prolonging the early-stage heating time by about 1min when the temperature of the sample melting furnace is reduced to 950 ℃, and keeping the magnesium oxide to be lower than a standard value by 0.08-0.19%; after the melting is finished, taking out the crucible within 30 seconds after the prompt tone of the high-temperature sample melting furnace;
6) establishing a calibration curve: respectively measuring the fluorescence intensity values of magnesium element and silicon element in the prepared calibration sample wafer by using an X-ray fluorescence spectrometer, correcting elements by using a theoretical alpha coefficient, establishing a calibration curve of element content and the corrected fluorescence intensity value, and obtaining the slope and intercept of the calibration curve;
7) and (3) determination of elements of the sample to be detected: preparing a sample wafer of the sample to be detected according to the method for preparing the sample wafer of the calibration sample in the step 2, and analyzing the sample wafer of the sample to be detected by using an X-ray fluorescence spectrometer to obtain fluorescence intensity values after correcting magnesium and silicon elements;
8) setting of magnesium oxide measurement conditions: crystal RX35 SPC, target Rh40kV 70mA, 2 theta 21.050 degree, PHA 100-326;
9) setting of silica measurement conditions: crystal RX4 SPC, target Rh40kV 70mA, 2 theta 144.780 degree, PHA 102-319.
2. The method for analyzing the high-temperature melting X-ray fluorescence of the light-burned magnesium spheres as claimed in claim 1, wherein the flux in the step 3 is a mixed flux of lithium tetraborate and lithium metaborate, the mass ratio of the lithium tetraborate to the lithium metaborate is 67:33, and the mass ratio of the flux to the sample is 16: 1; the mixed flux is weighed to be 8.0g, the light-burned magnesium ball sample is weighed to be 0.5g, the proportion of the platinum yellow crucible is 95% + 5%, and the diameter of the bottom is more than or equal to 35 mm.
3. The method for high-temperature melting X-ray fluorescence analysis of the light-burned magnesium spheres as claimed in claim 1, wherein the high-temperature melting temperature in the step 3 is 1000 ℃ and the melting time is 15 min.
4. The method for carrying out high-temperature melting X-ray fluorescence analysis on the light-burned magnesium spheres according to claim 1, wherein when the addition amount of the mold release agent in the step 4 is 0.6ml, the magnesium oxide is lower than a standard value by 0.09-0.21%; when the addition amount of the release agent is 0.4ml, the magnesium oxide is higher than the standard value by 0.12-0.29%.
5. The method for high-temperature melting X-ray fluorescence analysis of a light-burned magnesium ball according to claim 1, wherein the melting in the step 5 is completed, and when the crucible is taken out 90 seconds after the prompt sound of the high-temperature melting furnace, the bottom of the sample piece is cooled after the sample piece is molded, and bubbles are formed at the bottom, so that the sample piece cannot be used.
6. The method for high-temperature melting X-ray fluorescence analysis of the light-burned magnesium spheres as claimed in claim 1, wherein the X-ray fluorescence spectrometer in the step 6 is a Nippon Rigaku 14 type wavelength dispersion spectrometer, and both magnesium and silicon are fixed channels.
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