阅读说明：本技术 X荧光熔片法测定铬铁合金中主量元素的方法 (Method for measuring major elements in ferrochrome alloy by X fluorescence fuse link method ) 是由 顾强 左丽峰 张秀宏 张建中 冀丽英 王敏 徐静 于 2019-08-29 设计创作，主要内容包括：X荧光熔片法测定铬铁合金中主量元素的方法,包括：1)选取多个粒度达到200目的标准样品；2)称取标准样品加入复合氧化剂和降粘剂搅拌均匀；3)在铂金坩埚中称入熔剂,将混匀后的标准样品倒入铂金坩埚中并覆盖熔剂,将铂金坩埚于马弗炉内完成合金样品预氧化；4)将预氧化完成的铂金坩埚置于熔样炉内熔样,在脱模前加入脱模剂旋转摇动后冷却脱模,制成分析用玻璃片；5)采用X射线荧光光谱仪测试标样中主元素强度值,将所测强度值与标准值建成一次工作曲线；6)将块状铬铁合金待检测样品研磨至与标样同等粒度,按步骤2)～5)熔融成玻璃片,用X射线荧光光谱仪分析其成分值,本发明延长了铂金坩埚寿命,保证了结果准确度和精密度。(The method for measuring the main elements in the ferrochrome alloy by the X fluorescence fuse link method comprises the following steps: 1) selecting a plurality of standard samples with the granularity of 200 meshes; 2) weighing a standard sample, adding a composite oxidant and a viscosity reducer, and uniformly stirring; 3) weighing a flux in a platinum crucible, pouring the uniformly mixed standard sample into the platinum crucible and covering the flux, and putting the platinum crucible in a muffle furnace to complete the pre-oxidation of the alloy sample; 4) placing the platinum crucible after pre-oxidation in a sample melting furnace for melting a sample, adding a release agent before demolding, rotating and shaking the crucible, and then cooling and demolding to prepare a glass sheet for analysis; 5) testing the intensity value of the main element in the standard sample by using an X-ray fluorescence spectrometer, and establishing a primary working curve by using the tested intensity value and the standard value; 6) grinding the block ferrochrome alloy sample to be detected to the same granularity as the standard sample, melting into a glass sheet according to the steps 2) -5), and analyzing the component value by using an X-ray fluorescence spectrometer.)

The method for measuring the main elements in the ferrochrome alloy by the X fluorescence fuse link method is characterized by comprising the following steps: the method comprises the following steps:

1) selecting a plurality of standard samples and grinding the standard samples until the granularity reaches more than 200 meshes;

2) weighing a certain amount of standard sample, adding a composite oxidant in an amount which is 10-20 times the mass of the standard sample, adding 0.2-0.5g of viscosity reducer, and uniformly stirring; the composite oxidant is prepared from solid reagents of lithium hydroxide monohydrate, boric acid and potassium nitrate;

3) weighing a flux which is 30-80 times the mass of the standard sample in a platinum crucible, pouring the uniformly mixed standard sample obtained in the step 2) into the platinum crucible, covering the platinum crucible with the flux, putting the platinum crucible into a muffle furnace, and heating the platinum crucible to 770-800 ℃ from room temperature to complete pre-oxidation of the alloy sample;

4) placing the platinum crucible subjected to preoxidation in a sample melting furnace, starting a sample melting program, adding a release agent before demolding, continuously rotating and shaking for 90-120 seconds, stopping the rotating and shaking, cooling and demolding, and finally preparing uniform and transparent glass sheets for analysis;

5) testing the intensity values of chromium, silicon, phosphorus and manganese in the standard sample by adopting an X-ray fluorescence spectrometer, establishing a primary working curve by using the tested intensity values and the standard value, and enabling the linear correlation coefficient to meet the analysis requirement;

6) grinding the massive ferrochrome alloy sample to be detected to the same granularity as the standard sample, melting into a glass sheet according to the steps 2) -5), and analyzing the component value by using an X-ray fluorescence spectrometer.

2. The method for measuring the major elements in the ferrochrome alloy by the X fluorescence fusion method according to claim 1, wherein the method comprises the following steps: the standard sample and the sample to be detected are of the same matrix type.

3. The method for measuring the major elements in the ferrochrome alloy by the X fluorescence fusion method according to claim 1, wherein the method comprises the following steps: in the step 1), the number of the standard samples is more than 8; in the step 2), 0.1-0.2 g of standard sample is weighed and placed in a ceramic crucible, and a composite oxidant and 0.2-0.5g of viscosity reducer which are 10-20 times of the standard sample in mass are added and stirred uniformly; the composite oxidant is prepared from (4-10) by mass of lithium hydroxide monohydrate, boric acid and potassium nitrate: (1-2): 1.

4. the method for measuring the major elements in the ferrochrome alloy by the X fluorescence fusion method according to claim 1, wherein the method comprises the following steps: in the step 3), weighing a flux which is 30-80 times of the mass of the standard sample in a platinum crucible, and making the central area of the flux in a sunken state; and (3) pouring all the uniformly mixed standard samples obtained in the step 2) into the central area of the platinum crucible, not directly contacting the platinum crucible, covering 1-2 g of fusing agent on the platinum crucible, putting the platinum crucible into a muffle furnace, and heating to 770-800 ℃ from room temperature at a speed of 15-20 ℃/min to complete the pre-oxidation of the alloy sample.

5. The method for measuring the major elements in the ferrochrome alloy by the X fluorescence fusion method according to claim 1, wherein the method comprises the following steps: the sample melting process is divided into four stages: the first stage is the pre-oxidation in the step 3), the temperature is increased from room temperature to 770-800 ℃, and the temperature-increasing speed is 15-20 ℃/min; the second stage is the sample melting process control of the step 4), the melting swing temperature is 1050-1150 ℃, the heat preservation time is 700s, and the swing and rotation functions of the sample melting furnace are started; the third stage is that the demoulding agent is added in the step 4) and then the sample is swung, the temperature is 1050-1150 ℃, the heat preservation time is 120s, and the swinging and rotating functions of the sample melting furnace are started; standing at the fourth stage, cooling to room temperature, and demolding; the amount of the release agent added before demolding in the step 4) is 0.05-0.2 g.

6. The method for measuring the major elements in the ferrochrome alloy by the X fluorescence fusion method according to claim 1, wherein the method comprises the following steps: the viscosity reducer can be potassium bromide, potassium iodide and lithium bromide; the flux can be lithium tetraborate, or lithium tetraborate and lithium metaborate according to the mass ratio of 67: 33 or a mixed solvent prepared from lithium tetraborate, lithium metaborate and lithium fluoride according to the mass ratio of 65:25: 10; the release agent can be ammonium bromide and ammonium iodide.

Technical Field

The invention relates to a method for determining major elements in ferrochrome alloy by an X fluorescence fuse link method, belonging to the technical field of physicochemical detection.

Background

In order to meet the requirements of the industry on the performance of steel, alloying elements such as ferrochrome and the like are required to be added in the steelmaking process for microalloying treatment so as to improve the crystal structure of the steel and improve the mechanical and physical properties of the material, so that the iron and steel production enterprises need to carry out chemical analysis on the chemical components of the ferrochrome alloy in the aspects of alloy procurement quality control and steel-making process operation guidance. The traditional wet chemical analysis and the current national standard method are adopted to determine the contents of relevant elements such as chromium, silicon, phosphorus, manganese and the like in the ferrochrome, the operation is complex, the steps are tedious, time and labor consuming and low in efficiency, the accuracy and stability of the analysis result are often influenced by the experience and level of operators, in addition, a plurality of strong acids and other chemical reagents are required to be jointly used in the analysis process, and the personal injury or the environmental pollution is easily caused. Large modern analytical instruments such as X-ray fluorescence spectrometers have been widely used in metallurgical chemical analysis, and in recent years, have also begun to be used in the field of ferroalloy analysis.

In the published data, it can be seen that the oxidants used in the current stage of the determination of elements in ferrochrome alloy by X-fluorescence spectroscopy are mainly barium peroxide and nitrate. Barium peroxide is used as an oxidant, ferrochrome can be completely oxidized, but barium has serious spectral line overlapping interference on elements such as vanadium, titanium, manganese and the like, and the barium peroxide is avoided being used as the oxidant when the elements such as vanadium, titanium, manganese and the like which are easy to be subjected to spectral line overlapping interference are tested.

Chinese patent with publication No. CN103149074B discloses a method for preparing a molten sample of molybdenum, manganese, vanadium or ferrochromium alloy by X-ray fluorescence spectrum analysis, which comprises the following three steps of 1, weighing lithium tetraborate, lithium carbonate and a sample, uniformly mixing, and wrapping the mixture into a sphere; 2. Putting the materials into a crucible at the bottom of a graphite powder pad, then putting the crucible into a high-temperature furnace for melting and pre-oxidizing, taking out the crucible, and cooling to obtain pre-oxidized molten balls; 3. Weighing a certain amount of flux into a platinum crucible, adding a release agent and a melting ball, melting for 12-20 minutes, taking out, shaking up, removing bubbles, melting for 12-20 minutes, taking out, shaking up, standing and cooling to obtain a sample wafer. The technical scheme aims at ferrochrome, a reagent for wrapping the ferrochrome into balls is an oxidant, and the formula of the ferrochrome comprises the following components: 2 parts by weight of lithium tetraborate +1 part by weight of lithium carbonate +0.5 part by weight of sodium nitrate, the sample amount being 0.1 part by weight, in practice usually 1 gram per part by weight, which is not without the following disadvantages: 1. in the process of firing the balls, due to the existence of lithium carbonate, the mixture of the oxidant and the ferrochrome powder seriously splashes in the graphite powder, part of the alloy splashes into the graphite powder, and the splashing amount cannot be controlled, so that the material loss of an alloy sample is caused, and the test result is lower; 2. if the used graphite powder is repeatedly used, when a sample is oxidized, the current sample has splash loss, and meanwhile, the part of the previous sample splashed into the graphite powder can pollute the current sample, so that the data obtained by final testing cannot represent the sample; and 3, the melting time is too long, the residual quantity of the release agent is not enough to ensure the release quality, and the residue on the platinum crucible is serious.

At present, the X fluorescence tabletting method has more reports on the analysis of the ferroalloy, but the tabletting method is greatly influenced by the granularity effect and the matrix effect of a sample, so that the accuracy of analysis data is poor; however, in the attempt of analyzing the iron alloy by using the X fluorescence fuse method, the iron alloy sample cannot be completely oxidized due to the failure to find a proper oxidizing agent, so that the platinum crucible is corroded, or in order to protect the platinum crucible from being corroded, the oxidizing effect of the oxidizing agent can meet the requirement, but the alloy is easily lost due to splashing, so that the final test result is unstable, and therefore, the application of the X fluorescence fuse method in the iron alloy test is not wide.

Disclosure of Invention

The invention aims to provide a method for measuring major elements in ferrochrome by an X fluorescence fuse link method, which can ensure the complete oxidation of the ferrochrome, prolong the service life of a platinum crucible, ensure that the accuracy and precision of a measurement result meet requirements and improve the analysis efficiency.

In order to solve the technical problems, the technical scheme adopted by the invention is as follows:

the method for measuring the main elements in the ferrochrome alloy by the X fluorescence fuse link method comprises the following steps:

1) selecting a plurality of standard samples and grinding the standard samples until the granularity reaches more than 200 meshes;

2) weighing a certain amount of standard sample, adding a composite oxidant in an amount which is 10-20 times the mass of the standard sample, adding 0.2-0.5g of viscosity reducer, and uniformly stirring; the composite oxidant is prepared from solid reagents of lithium hydroxide monohydrate, boric acid and potassium nitrate;

3) weighing a flux which is 30-80 times the mass of the standard sample in a platinum crucible, pouring the uniformly mixed standard sample obtained in the step 2) into the platinum crucible, covering the platinum crucible with the flux, putting the platinum crucible into a muffle furnace, and heating the platinum crucible to 770-800 ℃ from room temperature to complete pre-oxidation of the alloy sample;

4) placing the platinum crucible subjected to preoxidation in a sample melting furnace, starting a sample melting program, adding a release agent before demolding, continuously rotating and shaking for 90-120 seconds, stopping the rotating and shaking, cooling and demolding, and finally preparing uniform and transparent glass sheets for analysis;

5) testing the intensity values of chromium, silicon, phosphorus and manganese in the standard sample by adopting an X-ray fluorescence spectrometer, establishing a primary working curve by using the tested intensity values and the standard value, and enabling the linear correlation coefficient to meet the analysis requirement;

6) grinding the massive ferrochromium alloy sample to be detected to the same granularity as the standard sample, melting into a glass sheet according to the steps 2) -5), and analyzing the component value by using an X-ray fluorescence spectrometer.

In the method for measuring the main elements in the ferrochrome alloy by the X fluorescence fuse link method, the standard sample and the sample to be detected have the same matrix type.

In the method for measuring the main elements in the ferrochrome alloy by the X fluorescence fuse link method, in the step 1), the number of the standard samples is more than 8; in the step 2), 0.1-0.2 g of standard sample is weighed and placed in a ceramic crucible, and a composite oxidant and 0.2-0.5g of viscosity reducer which are 10-20 times of the standard sample in mass are added and stirred uniformly; the composite oxidant is prepared from (4-10) by mass of lithium hydroxide monohydrate, boric acid and potassium nitrate: (1-2): 1.

in the step 3), a flux with the mass 30-80 times of that of a standard sample is weighed into a platinum crucible, and the central area of the flux is in a concave state; and (3) pouring all the uniformly mixed standard samples obtained in the step 2) into the central area of the platinum crucible, not directly contacting the platinum crucible, covering 1-2 g of fusing agent on the platinum crucible, putting the platinum crucible into a muffle furnace, heating to 770-800 ℃ from room temperature at the speed of 15-20 ℃/min, and completing the pre-oxidation of the alloy sample.

According to the method for measuring the main elements in the ferrochrome alloy by the X fluorescence fuse link method, the sample melting process is divided into four stages: the first stage is the pre-oxidation in the step 3), the temperature is increased from room temperature to 770-800 ℃, and the temperature-increasing speed is 15-20 ℃/min; the second stage is the sample melting process control of the step 4), the melting swing temperature is 1050-1150 ℃, the heat preservation time is 700s, and the swing and rotation functions of the sample melting furnace are started; the heat preservation time at this stage is set to 700 seconds, which aims to have enough time to enable the sample to be uniformly mixed with the flux in a molten state; the third stage is that the demoulding agent is added in the step 4) and then the sample melting furnace is swung, the temperature is 1050-1150 ℃, the heat preservation time is 120s, and the swinging and rotating functions of the sample melting furnace are started, the heat preservation time is set to be 120s, the reason is that ammonium iodide is rapidly decomposed and volatilized at high temperature, the heat preservation time is too short, the decomposed and volatilized is incomplete, the residual quantity is large, the time is too long, the residual quantity of the demoulding agent is insufficient, the demoulding quality cannot be ensured, and the heat preservation time is 120s, so that the effect is optimal through a; standing at the fourth stage, cooling to room temperature, and demolding; the amount of the release agent added before demolding in the step 4) is 0.05-0.2 g.

In the method for measuring the major elements in the ferrochrome alloy by the X fluorescence fuse link method, the viscosity reducer can be potassium bromide, potassium iodide and lithium bromide; the flux can be lithium tetraborate, or lithium tetraborate and lithium metaborate according to the mass ratio of 67: 33 or a mixed solvent prepared from lithium tetraborate, lithium metaborate and lithium fluoride according to the mass ratio of 65:25: 10; the release agent can be ammonium bromide and ammonium iodide.

Through a large number of long-time tests, the invention provides a method for measuring the main elements in the ferrochrome alloy by an X fluorescence fusion method, and a series of measures such as sample granularity control, compound oxidant preparation, melting condition optimization, X fluorescence analysis and the like are adopted, so that the aims of good sample analysis repeatability and high accuracy are fulfilled, the platinum crucible is effectively protected, and the analysis result of the sample meets the precision requirement in the related national chemical analysis standard. The invention innovates a ferrochrome melting sample preparation method, utilizes a composite oxidant to aim at stronger oxidizability of ferrochrome, realizes preoxidation of ferrochrome samples in the temperature rise process, melts samples at higher temperature to promote the melting of oxides and borates, adds a release agent ammonium bromide in the later period, ensures the demolding quality of sample wafers, prepares glass wafers with uniform substrates, and finally adopts an X-ray fluorescence spectrometer for analysis.

Potassium hydroxide monohydrate in the composite oxidant is alkali, potassium hydroxide anhydrous or sodium hydroxide or lithium hydroxide has extremely strong water absorption and carbon dioxide absorption capacity, rapidly deteriorates in air and cannot be accurately weighed, and lithium hydroxide monohydrate has stable properties at normal temperature, almost has no water absorption and carbon dioxide absorption capacity, and can be accurately and quantitatively weighed; other strongly basic carbonates such as lithium carbonate, sodium carbonate and potassium carbonate can ensure the oxidation effect, but the sample loss is easily caused by strong splashing caused by releasing a large amount of carbon dioxide gas in the oxidation stage, so that the potassium hydroxide, the sodium hydroxide and the carbonate can not replace the lithium hydroxide monohydrate; potassium nitrate in the composite oxidant is an oxidant, and the potassium nitrate has the same oxidation effect with strontium nitrate or sodium nitrate aiming at the ferrochrome alloy and can be mutually substituted; boric acid in the composite oxidant is a stabilizer, the boric acid has a lower melting point, and can be dissolved in liquid boric acid after the potassium nitrate and the lithium hydroxide are liquefied, so that the concentration of the oxidant around alloy powder particles is ensured, the oxidation effect of the alloy powder is further ensured, the boric acid is dehydrated and converted into diboron trioxide at high temperature, the boric acid reagent and the diboron trioxide reagent can be mutually replaced, and the effect are consistent. The invention prepares the glass fuse sheet which can be used for X fluorescence spectrum analysis by borate high temperature melting, ensures the quality of the glass sample sheet by adjusting the adding time of the release agent, and can rapidly and accurately complete the determination of the main element in the ferrochrome alloy by the X fluorescence fuse sheet method; the glass sample wafer is prepared by two steps of pre-oxidation and melting, equipment can be selected according to the existing conditions, a muffle furnace and a sample melting furnace can be respectively used, a sample melting furnace which can control the temperature rise speed and has the rapid temperature rise capacity can also be used, for example, a silicon carbide rod heating sample melting furnace produced by Luoyang Tetolerance company is used, pre-oxidation and sample melting are respectively needed, for example, a full-automatic electric heating sample melting furnace produced by Canada Katanax company or a high-frequency heating full-automatic sample melting furnace produced by Beijing Jingyuan company is used, and pre-oxidation and sample melting of a sample can be finished in one step. The method can replace the currently and commonly used chemical analysis method, X-ray fluorescence tabletting method and the like, has the advantages of short analysis period, few operation steps, high oxidation efficiency, accurate and reliable analysis result and the like, and can be popularized and applied to the acceptance of ferrochrome in the steel industry, the quality control of ferrochrome production enterprises and the like.

Compared with the prior art, the invention solves the technical bottlenecks of granularity effect and mineral effect brought by tabletting analysis and incapability of directly melting the alloy by adopting a platinum crucible; the preparation of the composite oxidant improves the oxidizing ability, can completely oxidize the ferrochrome alloy, realizes the preparation of the analysis glass fuse piece by one-time operation after sample weighing, has short whole analysis period, few operation steps and high oxidation efficiency, achieves the requirements of rapidness, accuracy and measurement, eliminates the risk of corrosion of a platinum crucible, and ensures that the analysis result of the sample achieves the precision requirement in the related national chemical analysis standard.

The invention has the beneficial effects that:

the novel composite oxidant prepared by the invention is capable of pre-oxidizing the ferrochromium alloy, has strong oxidizing capability, can completely oxidize the ferrochromium alloy, has no splashing phenomenon in the whole pre-oxidizing and sample melting process, can not cause sample and flux loss, eliminates the corrosion risk of the platinum crucible, prolongs the service life of the platinum crucible, and ensures that the accuracy and precision of the measurement result meet the requirements.

Detailed Description

The method mainly provides a stable and good-reproducibility quick analysis method for major elements in the ferrochrome alloy, and the basic principle is that composite oxidant with better oxidation effect is used for pre-oxidizing ferrochrome alloy particles with proper granularity in a temperature rise stage, the ferrochrome alloy particles and borate are melted into uniform glass sheets in a high-temperature stage, a release agent is added at a proper time to ensure the final release quality, and finally an X-ray fluorescence spectrometer is adopted to analyze chemical components. The method has the advantages of simple, rapid, safe and reliable process, no corrosion to the platinum crucible in the pre-oxidation stage, no sample residue on the platinum crucible after demolding, no interference to the manufacture of the next sample wafer, accurate analysis result and better precision.

The invention relates to a method for measuring contents of main elements chromium, silicon, phosphorus and manganese in ferrochrome by an X fluorescence fuse link method, which comprises the following steps:

1) and selecting a standard sample: selecting more than 8 standard samples with the same matrix type as the sample to be detected, wherein the content range of the alloy elements of the standard samples must cover the content of the alloy elements of the sample to be detected, checking the initial granularity of the standard samples, and processing the standard samples to the granularity of 200 meshes by adopting grinding equipment if the granularity is less than 200 meshes;

2) and preparing and storing the composite oxidant: the method comprises the following steps of (1) preparing a required reagent, namely a lithium hydroxide monohydrate solid reagent, boric acid and potassium nitrate solid reagent by mass (4-10): (1-2): 1, mixing and preparing;

3) and preparing a working curve standard sample: weighing 0.1-0.2 g of standard sample into a ceramic crucible, adding a composite oxidant and 0.2-0.5g of viscosity reducer which are 10-20 times of the standard sample in mass, uniformly stirring, weighing a flux lithium tetraborate which is 30-80 times of the standard sample in mass in a platinum crucible, uniformly stirring, slightly sinking the central area, completely pouring the standard sample in the ceramic crucible into the sunk part, putting the ceramic crucible into a muffle furnace, raising the room temperature to 770-800 ℃ at the speed of 15-20 ℃/min, completing pre-oxidation, transferring the platinum crucible into a sample melting furnace, melting according to a set program, rotationally shaking, adding a release agent ammonium bromide, continuously rotationally shaking, and finally preparing an even and transparent glass sheet for analysis;

selecting melting conditions, optimizing parameters such as melting temperature, time, swing and the like of pre-oxidation in the first stage, melting in the second stage, melting in the third stage and cooling in the fourth stage, and determining the final melting conditions by aiming at the glass fuse piece forming rate of 100%, smooth surface without pits, perfect platinum crucible and smooth demolding without sample contamination; the specific melting process is divided into four stages: the first stage of pre-oxidation, wherein the temperature is increased to 770 ℃ and 800 ℃ at a temperature increase speed of 15-20 ℃/min; melting and swinging at 1050-1150 ℃ in the second stage, keeping the temperature for 700s, and starting the swinging and rotating functions of the sample melting furnace; in the third stage, adding a release agent, swinging at 1050-1150 ℃ for 120s, and starting the swinging and rotating functions of the sample melting furnace; standing at the fourth stage, cooling to room temperature, and demolding;

4) drawing a working curve: testing the intensity values of chromium, silicon, phosphorus and manganese in the ferrochrome standard sample by adopting an X-ray fluorescence spectrometer, establishing a primary working curve by using the tested intensity values and the standard values, and enabling the linear correlation coefficient to meet the analysis requirement;

5) and analysis of the sample: replacing the standard sample with the sample to be detected according to the step 3), melting the sample into a glass sheet, and analyzing the component value by using an X-ray fluorescence spectrometer, so that the determination of the main quantity elements in the ferrochrome tested by the X-ray fluorescence spectrometer is completed.

Through a large number of tests, the invention has the advantages that three solid reagents, namely lithium hydroxide monohydrate, boric acid and potassium nitrate, are prepared according to the mass ratio of 4: 1: 1, the oxidation effect on the ferrochrome alloy is better in the process of increasing from room temperature to 770-800 ℃ at the speed of 15-20 ℃/min; in the melting process, the addition of the viscosity reducer enables the flux and the sample to reduce viscosity and increase fluidity in the melting state, so that the flux and the sample can be uniformly mixed, the release agent ammonium bromide is added 2 minutes before the sample melting is finished, the sample piece demoulding quality effect is the best, the finally formed sample piece is high in quality, the platinum crucible is not corroded in the melting process, and no residue is left on the inner wall of the platinum crucible.

The key innovative technology of the invention is as follows: 1) the granularity of the sample and the standard sample is controlled to be more than 200 meshes, and the forming rate of the melting piece is 100 percent; tests show that when the sample has a coarse particle size, the oxidation effect is poor, the platinum crucible is corroded, and the prepared sample is easy to crack; 2) the composite oxidant is prepared by three solid reagents of lithium hydroxide monohydrate, boric acid and potassium nitrate according to a certain mass ratio, the oxidation effect on the ferrochrome alloy is consistent with the effect of using barium peroxide, but the spectral line overlapping interference of barium on titanium element is effectively eliminated, and more elements can be analyzed and detected; 3) the alkaline substance in the composite oxidant adopts the lithium hydroxide monohydrate, so that the composite oxidant has stable property and weaker water absorption and carbon dioxide absorption capacity, overcomes the problem that the anhydrous lithium hydroxide or potassium hydroxide and sodium hydroxide are easy to absorb water and carbon dioxide can not be accurately and quantitatively weighed, and simultaneously overcomes the problem that a sample seriously splashes due to the adoption of carbonate such as lithium carbonate or sodium carbonate or potassium carbonate in an oxidation stage. 4) The smelting conditions are controlled by stages by adopting the muffle furnace and the sample smelting furnace, the low-temperature pre-oxidation of ferrochrome alloy and the high-temperature melting of the flux and the mixture after pre-oxidation are realized in the smelting process, the manufacture of glass sheets can be finished with high quality, the platinum crucible is effectively protected, the method efficiency is high, and the operation is simple and convenient. 5) The direct contact between the alloy powder and the platinum crucible is isolated by adopting a flux bottom laying mode, the condition that the glass lining formed by a wall hanging method splashes due to heating in an oxidation stage to cause flux loss is avoided, the platinum crucible can be effectively prevented from being damaged under the condition that a prepared oxidant is proper, and the covered flux is a mixed solvent prepared from lithium tetraborate, lithium metaborate and lithium fluoride according to the mass ratio of 65:25:10, so that the viscosity of a sample piece in a molten state can be reduced, the flowability is improved, the sample piece is favorably mixed uniformly, and the slight splashing phenomenon possibly generated can be effectively prevented by adding a small amount of flux for covering.

The analytical method of the present invention will be described in detail below with reference to specific examples, in which the purity of the reagent is analytical grade or higher.