CN116718444A - Pretreatment sample decomposition method for measuring lithium oxide content in continuous casting mold flux - Google Patents
Pretreatment sample decomposition method for measuring lithium oxide content in continuous casting mold flux Download PDFInfo
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- CN116718444A CN116718444A CN202310469127.7A CN202310469127A CN116718444A CN 116718444 A CN116718444 A CN 116718444A CN 202310469127 A CN202310469127 A CN 202310469127A CN 116718444 A CN116718444 A CN 116718444A
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- 238000009749 continuous casting Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000004907 flux Effects 0.000 title claims abstract description 30
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910001947 lithium oxide Inorganic materials 0.000 title claims abstract description 29
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 30
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 30
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 23
- 239000002893 slag Substances 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 15
- 238000004458 analytical method Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000012086 standard solution Substances 0.000 claims abstract description 14
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 12
- 238000012360 testing method Methods 0.000 claims abstract description 12
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 11
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 9
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- 229910052573 porcelain Inorganic materials 0.000 claims description 23
- 238000005303 weighing Methods 0.000 claims description 19
- -1 polytetrafluoroethylene Polymers 0.000 claims description 15
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 15
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 13
- 238000005266 casting Methods 0.000 claims description 12
- 239000012085 test solution Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 7
- 239000000779 smoke Substances 0.000 claims description 7
- 238000005070 sampling Methods 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 4
- 239000012490 blank solution Substances 0.000 claims description 3
- 238000004364 calculation method Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 2
- 238000005259 measurement Methods 0.000 abstract description 8
- 239000002253 acid Substances 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 5
- 238000001514 detection method Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000003595 spectral effect Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005262 decarbonization Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002436 steel type Substances 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to the technical field of detection of raw materials and finished products, and particularly discloses a pretreatment decomposition sample method for measuring the content of lithium oxide in continuous casting mold flux, which comprises 1) a pretreatment carbon removal treatment method; 2) Dissolving a covering slag sample by nitric acid, hydrofluoric acid and perchloric acid to prepare a solution to be tested; 3) Preparing a series of standard solutions containing lithium elements with different mass fractions; 4) Respectively testing the emission light intensity of the standard solution in the step 3) by using an inductively coupled plasma emission spectrometer, and constructing a standard curve by taking the mass fraction of lithium element as an X axis and the analysis line intensity as a Y axis; 5) Testing the emission light intensity of the test liquid obtained in the step 2) by using an inductively coupled plasma emission spectrometer, and further calculating the content of lithium oxide in the protective slag by using the standard curve in the step 4); the invention overcomes the defect of the existing single treatment method, and the measurement result is accurate and reliable; the acid consumption is reduced to the minimum in the sample decomposition process, and the decomposition time period is greatly shortened.
Description
Technical Field
The invention relates to the technical field of detection of raw materials and finished products, in particular to a pretreatment decomposition sample method for measuring the content of lithium oxide in continuous casting mold flux.
Background
In the continuous casting production process, the continuous casting protection slag is used as a medium for interaction between a crystallizer and a casting blank, is an important functional material in the continuous casting production, and has great influence on smooth running of a continuous casting process and improvement of the quality of the casting blank. Different types and purposes of casting powder can be obtained under the conditions of different steel types, different casting machines and different continuous casting process combinations, and the crystallization property, the thermal resistance and the like of the slag film can be controlled by changing the components of the casting powder, so that the defects of the surface of a casting blank can be effectively controlled. The lithium oxide added in the casting powder during smelting has great influence on the viscosity, melting temperature and glass performance of the casting powder, so that accurate determination of the content of the lithium oxide in the casting powder has great significance for smelting and product quality control. However, the product brands of the prior continuous bead mold flux are more, and the mass fraction of free carbon is 0.5% -30%, so that the mold flux sample is complex and special, the prior sample pretreatment method is single and long in time, the inaccuracy of measurement analysis and the measurement period are increased, and no good solution is found in the prior art for the problems of the pretreatment samples. According to the invention, pre-decarbonization treatment is added before the sample with high carbon content is dissolved according to the different free carbon content in the protective slag, and the problems of the prior sample decomposition treatment before the determination and analysis of lithium oxide in the protective slag are solved by improving the use amount of acid and the pretreatment control. The invention provides a pretreatment decomposition sample method for measuring the lithium oxide content in continuous casting mold flux by an inductively coupled plasma emission spectrometer, which is characterized in that different samples are treated differently, the defect of the existing single treatment method is overcome, the effective treatment of the samples can be ensured, the measurement result is accurate and reliable, and the method is simple, quick and accurate to operate and is applied in production practice quickly, so as to meet the steel-making production requirement.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a pretreatment sample decomposition method for determining the content of lithium oxide in continuous casting mold flux.
The technical scheme adopted for solving the technical problems is as follows: a pretreatment decomposition sample method for determining the content of lithium oxide in continuous casting mold flux comprises the following steps:
1) The pre-decarbonizing treatment method comprises the following steps: for continuous casting mold flux with free carbon content less than 5%, directly weighing a sample and dissolving the sample in a polytetrafluoroethylene beaker; for the continuous casting protection slag with the free carbon content of 5-20%, the sampling article is weighed in a porcelain boat;
2) Dissolving a covering slag sample by nitric acid, hydrofluoric acid and perchloric acid to prepare a solution to be tested;
3) Preparing a series of standard solutions containing lithium elements with different mass fractions;
4) Respectively testing the emission light intensity of the standard solution in the step 3) by using an inductively coupled plasma emission spectrometer, and constructing a standard curve by taking the mass fraction of lithium element as an X axis and the analysis line intensity as a Y axis;
5) And (3) testing the emission light intensity of the test liquid obtained in the step (2) by using an inductively coupled plasma emission spectrometer, and further calculating the content of lithium oxide in the protective slag by using the standard curve in the step (4).
Specifically, the pre-decarbonizing treatment method in the step 1) comprises the following steps: for continuous casting mold flux with free carbon content less than 5%, directly weighing 0.2g sample and dissolving in a polytetrafluoroethylene beaker; for the continuous casting protection slag with the free carbon content of 5-20%, 0.2g of sample is weighed in a porcelain boat, burned in a muffle furnace at 700-750 ℃ for 2 hours, taken out, cooled and transferred into a polytetrafluoroethylene beaker for dissolution.
Specifically, the specific steps of preparing the liquid to be tested in the step 2) are as follows: weighing 0.2000g of the sampling sample, putting the covering slag into a 150mL polytetrafluoroethylene beaker, sequentially adding 1mL of nitric acid, 5mL of hydrofluoric acid and 6mL of perchloric acid, heating at low temperature on an electric hot plate until the sample emits thick white smoke, taking down and cooling the liquid with the volume of 3mL, and continuously adding 1mL of nitric acid and H 2 O10mL dissolved salts until the test solution is clear, then taking down and cooling to room temperature, transferring into a 100mL volumetric flask, and fixing the volume to the scale with distilled waterShaking up and measuring.
Specifically, the adding amounts of nitric acid, hydrofluoric acid and perchloric acid in the step 2) are as follows:
nitric acid: ρ1.42g/ml;
hydrofluoric acid: ρ1.70g/ml;
perchloric acid: ρ1.67g/ml.
Specifically, the early preparation of the mold flux sample: after the sample to be detected is crushed by a crusher, the crushed sample is ground by a grinder until the granularity of the crushed sample completely passes through sieve holes with the diameter of 0.097mm, and the sample is baked for 1 to 2 hours at the temperature of between 105 and 110 ℃ before analysis and is stored in a drying dish for standby.
Specifically, the calculation formula of the content of lithium oxide in the mold flux in the step 5) is as follows:
wherein: v: the volume of the liquid to be tested is in milliliters;
c: the lithium element concentration in the solution to be tested is calculated from the standard curve, and the unit is microgram per milliliter;
C 0 : the concentration of lithium element in the blank solution is expressed in micrograms per milliliter;
m: the mass of the covering slag sample is given in grams;
2.1524: conversion coefficient between lithium oxide and lithium.
Specifically, the analysis spectral line of the inductively coupled plasma emission spectrometer in the step 4) and the step 5) is 670.783nm analysis spectral line.
The invention has the following beneficial effects:
the pretreatment decomposition sample method for measuring the lithium oxide content in the continuous casting mold flux, which is designed by the invention, considers the specificity of the continuous casting mold flux sample, and different samples are treated differently, thereby overcoming the defect of the existing single treatment method, ensuring that the sample is effectively treated and the measurement result is accurate and reliable; the acid consumption is reduced to the minimum in the sample decomposition process, and the decomposition time period is greatly shortened; the sample is completely dissolved, and the accuracy of the detection result is improved.
Drawings
FIG. 1 is a schematic diagram of a standard curve construction.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described in further detail below with reference to the accompanying drawings in the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
A pretreatment decomposition sample method for measuring the content of lithium oxide in continuous casting mold flux comprises the following steps:
(1) Preparation of test analysis samples
After the sample to be detected is crushed by a crusher, the crushed sample is ground by a grinder until the granularity of the crushed sample completely passes through sieve holes with the diameter of 0.097mm (160 meshes), and the sample is baked for 1 to 2 hours at the temperature of 105 to 110 ℃ before analysis and is stored in a drying dish for standby.
(2) Reagent(s)
Nitric acid: ρ1.42g/ml;
hydrofluoric acid: ρ1.70g/ml;
perchloric acid: ρ1.67g/ml;
(3) Experimental method
(1) The pre-decarbonizing treatment method comprises the following steps: for continuous casting mold flux with free carbon content less than 5%, directly weighing 0.2g sample and dissolving in a polytetrafluoroethylene beaker; for the continuous casting covering slag with the free carbon content of 5-20%, 1g of sample is weighed in a porcelain boat, burned in a muffle furnace at 700-750 ℃ for 2 hours, and then taken out for cooling, and 0.2g of ash is weighed to be dissolved in a polytetrafluoroethylene beaker.
(2) The acid decomposition treatment method of the sample comprises the following steps: weighing 0.2000g of the sampling sample, putting the covering slag into a 150mL polytetrafluoroethylene beaker, sequentially adding 1mL of nitric acid, 5mL of hydrofluoric acid and 6mL of perchloric acid, heating at low temperature on an electric hot plate until the sample emits thick white smoke, taking down and cooling the liquid with the volume of 3mL, and continuously adding 1mL of nitric acid and H 2 O10mL of dissolved salts are removed and cooled to room temperature until the test solution is clear, and the test solution is transferred into a 100mL volumetric flask, is subjected to constant volume to scale shaking by distilled water, and is to be measured.
The invention firstly proposes that the specificity of the continuous casting mold flux sample is considered, different samples are treated differently, the defect of the existing single treatment method is overcome, the effective treatment of the sample can be ensured, and the measurement result is accurate and reliable. In addition, the method can realize complete dissolution of the sample and shorten the pretreatment period of ICP measurement of lithium oxide element in the casting powder through control of the acid amount and dissolution degree, improves the accuracy of the detection result, provides powerful technical support for development and quality control of steel products, and has indirect economic benefit.
The test samples in the following examples were obtained by pulverizing the sample of the continuous bead mold flux to be measured with a crusher, and grinding the crushed sample to a particle size of 160 mesh.
Preparation of standard solution and determination of standard curve:
(1) Preparing a standard solution: the lithium standard solution of 1000ug/ml is diluted by distilled water to obtain the lithium standard solution of 100ug/ml, the volumes of different standard solutions are removed, and 1ml of concentrated nitric acid is added to a volumetric flask of 100ml with distilled water to fix the volume, so that a series of standard solutions containing lithium elements with different mass fractions are obtained. The mass fraction of lithium element in the series of standard solutions is shown in table 1.
TABLE 1 mass fraction of elements in Standard solution series w%
| Sequence number | Li％ |
| Blank space | 0 |
| Standard 1 | 0.10 |
| Standard 2 | 0.20 |
| Standard 3 | 0.40 |
| Standard 4 | 0.60 |
(2) Determination of a standard curve:
carrying out spectrum measurement on an inductively coupled plasma emission spectrometer by using the standard series, wherein the analysis spectral line of the inductively coupled plasma emission spectrometer is 670.784nm analysis spectral line, then, the mass fraction of lithium element is taken as an X axis, the intensity of the analysis line is taken as a Y axis, a standard curve is constructed as shown in figure 1, and the linear correlation coefficient R2 is 1.000; and detecting the liquid to be tested after the sample is decomposed by using the established standard curve.
(3) The calculation formula of the content of lithium oxide in the covering slag is as follows:
wherein V: volume of the solution to be tested in milliliters (mL);
c: the concentration of lithium element in the solution to be tested calculated from the standard curve is expressed in micrograms per milliliter (ug/mL);
C 0 : the concentration of lithium element in the blank solution is expressed in micrograms per milliliter (ug/mL);
m: the mass of the casting powder sample is expressed as gram (g);
2.1524: conversion coefficient between lithium oxide and lithium.
Example 1:
weighing a continuous casting protection slag 1# sample (Fc4.06), weighing 0.2000g in a 150mL polytetrafluoroethylene beaker, sequentially adding 1mL of nitric acid, 5mL of hydrofluoric acid and 6mL of perchloric acid, heating at low temperature on an electric heating plate until the sample emits thick white smoke, wherein the liquid volume is equal to that ofTaking about 3mL, cooling, and continuously adding 1mL of nitric acid and H 2 O10mL of dissolved salts are removed and cooled to room temperature until the test solution is clear, and the test solution is transferred into a 100mL volumetric flask, is subjected to constant volume to scale shaking by distilled water, and is to be measured.
The results are shown in Table 2.
Example 2:
weighing a continuous casting mold flux 2# sample (Fc9.94), weighing 1g of the sample, putting the sample into a porcelain boat, burning the porcelain boat in a muffle furnace at 700-750 ℃ for 2 hours, taking out and cooling the porcelain boat, weighing 0.2g of ash into a polytetrafluoroethylene beaker to dissolve the porcelain boat, sequentially adding 1mL of nitric acid, 5mL of hydrofluoric acid and 6mL of perchloric acid, heating the porcelain boat at a low temperature on an electric plate until the sample emits thick white smoke, taking down and cooling the porcelain boat at a liquid volume of about 3mL, and continuously adding 1mL of nitric acid and H 2 O10mL of dissolved salts are removed and cooled to room temperature until the test solution is clear, and the test solution is transferred into a 100mL volumetric flask, is subjected to constant volume to scale shaking by distilled water, and is to be measured.
The results are shown in Table 2.
Example 3:
weighing a continuous casting mold flux 3# sample (Fc 14.49), weighing 1g of the sample, putting the sample into a porcelain boat, burning the porcelain boat in a muffle furnace at 700-750 ℃ for 2 hours, taking out and cooling the porcelain boat, weighing 0.2g of ash into a polytetrafluoroethylene beaker to dissolve the porcelain boat, sequentially adding 1mL of nitric acid, 5mL of hydrofluoric acid and 6mL of perchloric acid, heating the porcelain boat at a low temperature on an electric plate until the sample emits thick white smoke, taking down and cooling the porcelain boat at a liquid volume of about 3mL, and continuously adding 1mL of nitric acid and H 2 O10mL of dissolved salts are removed and cooled to room temperature until the test solution is clear, and the test solution is transferred into a 100mL volumetric flask, is subjected to constant volume to scale shaking by distilled water, and is to be measured.
The results are shown in Table 2.
Example 4:
weighing a continuous casting protection slag No. 4 sample (Fc18.14), weighing 1g of the sample, putting the sample into a porcelain boat, burning the porcelain boat in a muffle furnace at 700-750 ℃ for 2 hours, taking out and cooling the porcelain boat, weighing 0.2g of ash into a polytetrafluoroethylene beaker to dissolve the porcelain boat, sequentially adding 1mL of nitric acid, 5mL of hydrofluoric acid and 6mL of perchloric acid, heating the porcelain boat at a low temperature on an electric plate until the sample emits thick white smoke, taking down and cooling the porcelain boat at a liquid volume of about 3mL, and continuously adding 1mL of nitric acid and H 2 O10mL dissolved salts until the test solution is clear, then taking down and cooling to room temperature, transferring into a 100mL volumetric flask for distillationAnd (5) water is subjected to constant volume until the scale is shaken uniformly to be measured.
The results are shown in Table 2.
Table 2 test results
The present invention is not limited to the above embodiments, and any person who can learn the structural changes made under the teaching of the present invention can fall within the scope of the present invention if the present invention has the same or similar technical solutions.
The technology, shape, and construction parts of the present invention, which are not described in detail, are known in the art.
Claims (7)
1. The pretreatment decomposition sample method for determining the content of lithium oxide in the continuous casting mold flux is characterized by comprising the following steps:
1) The pre-decarbonizing treatment method comprises the following steps: for continuous casting mold flux with free carbon content less than 5%, directly weighing a sample and dissolving the sample in a polytetrafluoroethylene beaker; for the continuous casting protection slag with the free carbon content of 5-20%, the sampling article is weighed in a porcelain boat;
2) Dissolving a covering slag sample by nitric acid, hydrofluoric acid and perchloric acid to prepare a solution to be tested;
3) Preparing a series of standard solutions containing lithium elements with different mass fractions;
4) Respectively testing the emission light intensity of the standard solution in the step 3) by using an inductively coupled plasma emission spectrometer, and constructing a standard curve by taking the mass fraction of lithium element as an X axis and the analysis line intensity as a Y axis;
5) And (3) testing the emission light intensity of the test liquid obtained in the step (2) by using an inductively coupled plasma emission spectrometer, and further calculating the content of lithium oxide in the protective slag by using the standard curve in the step (4).
2. The pretreatment decomposition sample method for determining lithium oxide content in continuous casting mold flux according to claim 1, wherein the pretreatment method for carbon removal in step 1) comprises: for continuous casting mold flux with free carbon content less than 5%, directly weighing 0.2g sample and dissolving in a polytetrafluoroethylene beaker; for the continuous casting protection slag with the free carbon content of 5-20%, 0.2g of sample is weighed in a porcelain boat, burned in a muffle furnace at 700-750 ℃ for 2 hours, taken out, cooled and transferred into a polytetrafluoroethylene beaker for dissolution.
3. The method for pretreating decomposed samples for determining the content of lithium oxide in continuous casting powder according to claim 1, wherein the specific steps of preparing the solution to be tested in the step 2) are as follows: weighing 0.2000g of the sampling sample, putting the covering slag into a 150mL polytetrafluoroethylene beaker, sequentially adding 1mL of nitric acid, 5mL of hydrofluoric acid and 6mL of perchloric acid, heating at low temperature on an electric hot plate until the sample emits thick white smoke, taking down and cooling the liquid with the volume of 3mL, and continuously adding 1mL of nitric acid and H 2 O10mL of dissolved salts are removed and cooled to room temperature until the test solution is clear, and the test solution is transferred into a 100mL volumetric flask, is subjected to constant volume to scale shaking by distilled water, and is to be measured.
4. The method for determining the content of lithium oxide in continuous casting mold flux according to claim 1, wherein the amounts of nitric acid, hydrofluoric acid and perchloric acid added in step 2) are as follows:
nitric acid: ρ1.42g/ml;
hydrofluoric acid: ρ1.70g/ml;
perchloric acid: ρ1.67g/ml.
5. The pretreatment decomposition sample method for measuring lithium oxide content in continuous casting mold flux according to claim 1, 2 or 3, wherein the mold flux sample is prepared in a preliminary stage: after the sample to be detected is crushed by a crusher, the crushed sample is ground by a grinder until the granularity of the crushed sample completely passes through sieve holes with the diameter of 0.097mm, and the sample is baked for 1 to 2 hours at the temperature of between 105 and 110 ℃ before analysis and is stored in a drying dish for standby.
6. The method for determining the content of lithium oxide in the continuous casting mold flux according to claim 1, wherein the calculation formula of the content of lithium oxide in the mold flux in step 5) is:
wherein: v: the volume of the liquid to be tested is in milliliters;
c: the lithium element concentration in the solution to be tested is calculated from the standard curve, and the unit is microgram per milliliter;
C 0 : the concentration of lithium element in the blank solution is expressed in micrograms per milliliter;
m: the mass of the covering slag sample is given in grams;
2.1524: conversion coefficient between lithium oxide and lithium.
7. The method for pretreating decomposed samples for determining the content of lithium oxide in casting powder according to claim 1, wherein the analytical lines of the inductively coupled plasma emission spectrometer in the step 4) and the step 5) are 670.783nm analytical lines.
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