CN114252440A - Contrast detection method for determining content of diboron trioxide in metallurgical slag system - Google Patents
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- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000002893 slag Substances 0.000 title claims abstract description 53
- 238000001514 detection method Methods 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000004448 titration Methods 0.000 claims abstract description 30
- 239000000243 solution Substances 0.000 claims description 125
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 102
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 24
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims description 21
- 229930195725 Mannitol Natural products 0.000 claims description 21
- 235000010355 mannitol Nutrition 0.000 claims description 21
- 239000000594 mannitol Substances 0.000 claims description 21
- 239000012086 standard solution Substances 0.000 claims description 21
- 239000003513 alkali Substances 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 14
- MKNQNPYGAQGARI-UHFFFAOYSA-N 4-(bromomethyl)phenol Chemical compound OC1=CC=C(CBr)C=C1 MKNQNPYGAQGARI-UHFFFAOYSA-N 0.000 claims description 12
- 230000003472 neutralizing effect Effects 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000012670 alkaline solution Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 3
- 230000000052 comparative effect Effects 0.000 claims 6
- 238000004458 analytical method Methods 0.000 abstract description 13
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 17
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 9
- 239000004327 boric acid Substances 0.000 description 9
- 239000011521 glass Substances 0.000 description 8
- 238000002479 acid--base titration Methods 0.000 description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- 238000005868 electrolysis reaction Methods 0.000 description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 4
- 229910052796 boron Inorganic materials 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 239000012085 test solution Substances 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 229910052810 boron oxide Inorganic materials 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004453 electron probe microanalysis Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method 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
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/79—Photometric titration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
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Abstract
The invention belongs to the technical field of metallurgical analysis, and provides a contrast detection method for determining the content of diboron trioxide in a metallurgical slag system. Aiming at the special component characteristics of the metallurgical slag system, the invention provides a contrast detection analysis method, and accordingly, the interference of amphoteric elements and other factors in the titration process on the titration result is eliminated, so that the accurate detection of the content of the diboron trioxide in the metallurgical slag system is realized. The method does not need to introduce other reagents, has lower cost, simple and convenient and quick operation and accurate and reliable measurement result, and provides a way for measuring the content of the diboron trioxide in the metallurgical slag system.
Description
Technical Field
The invention relates to the technical field of metallurgical analysis, in particular to a contrast detection method for determining the content of diboron trioxide in a metallurgical slag system.
Background
B2O3Is an acidic oxide, exists in the form of a grid in the slag, and B is added to the slag2O3The method can obviously improve the vitrifiability of the slag, and loosen the material structure, thereby reducing the viscosity of the slag and inhibiting the crystal precipitation. In addition, B2O3The melting point is low (450 ℃), the fluidity of the slag can be obviously increased, and the dynamic condition for dissolving and absorbing molten steel inclusions is improved. As the boron-containing slag system has extremely important function in the metallurgical production process, B in the slag2O3The content of the B-containing iron oxide directly influences the metallurgical performance of the B-containing iron oxide, so that the B-containing iron oxide is added into a metallurgical slag system2O3The content detection and analysis means is particularly important.
At present, many methods for analyzing and detecting boron trioxide have been developed at home and abroad, but mainly aiming at a glass system, an acid-base titration method is researched by more and more scholars as a simple, convenient and quick detection and analysis method with good result repeatability. A frugal et al discloses a method for testing the content of boron trioxide in lead-containing glass (CN 102042982A). Yi Yuan et al disclose a method for detecting boron oxide in glass (CN 102608111A).
In the method for measuring the content of diboron trioxide in the glass containing zinc and lead, carbonate needs to be added to separate other impurity elements, Ca-EDTA needs to be added to complex amphoteric elements of zinc and lead, the process is complicated, and a shielding agent or carbonate is introduced, so that the subsequent steps can interfere with the titration result if the subsequent steps are not properly treated.
In the method for detecting boron oxide in glass, an alkaline fluxing agent is required to be added for heating and melting, and then an acid is used for neutralizing the alkaline fluxing agent, so that the cost is high, and in the subsequent steps, carbonate and a proper amount of complexing agent are also required to be added, and if the adding amount is not properly treated, the carbonate and the complexing agent can interfere with the titration result.
Disclosure of Invention
The invention aims to eliminate the interference of amphoteric elements and other factors on titration results by using an acid-base titration method as a basis according to the special component characteristics of a metallurgical slag system and by contrasting a detection and analysis method, thereby realizing the accurate detection of the content of boron trioxide in the metallurgical slag system.
The invention provides a contrast detection method for determining the content of diboron trioxide in a metallurgical slag system based on an acid-base titration method, and aims to eliminate the influence of the titration process on the detection result of the content of diboron trioxide. Heating and acid-dissolving a boron-containing slag sample, diluting the boron-containing slag sample to a certain multiple, taking a proper amount of diluted solution, adding a contrast reagent mannitol to strengthen boric acid electrolysis, adding a bromocresol green-methyl red mixed indicator to detect the boric acid electrolysis degree, adding a phenolphthalein indicator as an end point indicator, and titrating the boron-containing slag sample to an end point by using an alkali solution. And simultaneously taking the diluted solution with the same amount as the diluted solution, only adding a bromocresol green-methyl red mixed indicator and a phenolphthalein indicator, not adding a contrast reagent mannitol, and titrating the solution to the end point by using an alkali solution. And calculating the content of the diboron trioxide in the slag sample according to the difference of the volumes of the alkali solutions consumed in the two titration processes. The method provides a way for measuring the content of the diboron trioxide in the metallurgical slag system, and has the characteristics of simple and convenient operation, rapidness and accurate and reliable measurement result.
In order to achieve the purpose, the invention adopts the technical scheme that: a contrast detection method for determining the content of diboron trioxide in a metallurgical slag system comprises the following specific steps:
first, taking CaO-Al2O3-Ce2O3-B2O3Adding an acid solution into the slag sample, heating and stirring until the slag sample is completely dissolved, and cooling to room temperature; diluting the cooled solution with distilled water to obtain a solution to be detected; equally measuring two parts of solution to be detected, namely a solution A to be detected and a solution B to be detected;
secondly, adding 2-3 drops of bromocresol green-methyl red mixed indicator into the solution A to be detected, and neutralizing the solution A to be detected by using an alkali solution until the solution A to be detected is just changed from dark red to green; adding mannitol to change the solution A to be detected which is changed into green into dark red again; dropwise adding a 2-3 phenolphthalein indicator, and titrating the solution A to be detected which is changed into dark red again to be just gray pink by using an alkali solution, wherein the color is not faded within 30 s;
thirdly, adding mannitol into the solution obtained in the second step, changing the gray pink color into green again, and continuously titrating the solution with alkali solution until the gray pink color is fadeless within 30 s; repeating the step until the solution is not discolored after adding mannitol, and recording the volume of the alkaline solution consumed in the titration process as V1;
Fourthly, adding 2-3 drops of bromocresol green-methyl red mixed indicator into the solution B to be detected, and neutralizing the solution B to be detected by using an alkali solution until the solution B to be detected is just changed from dark red to green; continuously adding 2-3 drops of phenolphthalein indicator, and titrating the indicator with an alkali solution until the color is just grey pink and does not fade within 30 s; record the volume of alkaline solution consumed during titration as V2。
The V is1And V2For calculating B2O3The content is as follows:
c-concentration of sodium hydroxide solution, mol/L;
69.62——B2O3molar mass of (a), g/mol;
m is the mass of the slag sample, g;
f is dilution multiple.
CaO-Al per 1g2O3-Ce2O3-B2O3120ml to 150ml of acid solution is correspondingly taken from the slag sample.
The heating temperature is controlled at 95-100 ℃.
The acid solution is 0.3mol/L hydrochloric acid solution.
And 5-20 times of dilution times interval of the cooled solution diluted by adding distilled water.
The alkali solution is 0.05 mol/L-0.1 mol/L sodium hydroxide standard solution.
The invention sets a contrast detection method on the basis of an acid-base titration method, and eliminates the interference of other influencing factors on the titration process by comparing the detection results of the mannitol with and without the mannitol to realize the accurate detection of the content of the diboron trioxide in the metallurgical slag system slag sample.
The invention has the beneficial effects that: provides a contrast detection method for measuring the content of boron trioxide in a metallurgical slag system based on an acid-base titration method. Compared with the traditional acid-base titration method, the method provided by the invention can eliminate the interference of influencing factors on the detection result without introducing other reagents, is simpler and faster to operate, and has a more accurate detection result. The boron trioxide detection and analysis method can be applied to the accurate detection of the content of the boron trioxide in all metallurgy slag systems.
Detailed Description
Example 1
In this example, 0.3g of CaO-Al, which is a metallurgical slag containing rare earth, was taken2O3-Ce2O3-10%B2O3And putting the slag sample 1 into an erlenmeyer flask, adding 40ml of acid solution into the erlenmeyer flask, placing the erlenmeyer flask on a magnetic stirrer, heating and stirring the erlenmeyer flask until the slag sample is completely dissolved, taking down the erlenmeyer flask, and cooling the erlenmeyer flask to room temperature. 5ml of the cooled solution was taken out of a beaker, diluted to 50ml with distilled water, and used as a test solution after being mixed with a glass rod. 10ml of the solution to be tested is put into a conical flask, 2 drops of a bromocresol green-methyl red mixed indicator are added, and the solution is dark red when the pH value is less than 5.0 due to the existence of free acid. The free acid in the solution was neutralized with 0.05mol/L NaOH standard solution until the solution appeared just green, at which time the pH of the solution was > 5.2 and the volume of NaOH standard solution consumed in the process was not counted. Adding 2g mannitol into the solution to enhance boric acid electrolysis, and generating H due to combination of mannitol and boric acid+So that the solution turned from green to dark red again. And adding 2 drops of phenolphthalein indicator into the solution as a titration end point, titrating by using 0.05mol/L sodium hydroxide standard solution, and fully shaking the solution from dark red, grey green, green and grey pink until the grey pink is titrated, wherein the titration end point is obtained if the solution does not fade within 30 seconds. 0.5g of mannitol is added to the solution and, if the solution changes from grey to green, titration with 0.05mol/L sodium hydroxide standard solution is continued until grey. Repeating the operation until the solution is not discolored after the mannitol is added, indicating that the boric acid in the solution is completely strengthened, and recording the total volume of the sodium hydroxide consumed in the titration process as V1。
Continuously taking 10ml of solution to be detected, adding 2 drops of bromocresol green-methyl red mixed indicator into the conical flask, enabling the solution to be dark red, neutralizing the solution with 0.05mol/L of sodium hydroxide standard solution until the solution is just green, and not counting the volume of the sodium hydroxide consumed in the process. Adding 2 drops of phenolphthalein indicator into the solution, continuously titrating with 0.05mol/L sodium hydroxide standard solution, wherein the solution is in green-grey pink color and does not fade within 30s, namely the end point of titration, and recordingThe volume of sodium hydroxide consumed by titration was recorded as V2。
Based on the difference V between the volumes of the alkaline solutions consumed by the two detection analysis methods1-V2I.e. the volume of the sodium hydroxide standard solution consumed by the boric acid fortified with mannitol (V)1-V2). The obtained result is substituted into the following formula to calculate B2O3The content is as follows:
V1-V2the volume of sodium hydroxide solution consumed by boric acid, mL;
c-concentration of sodium hydroxide solution, mol/L;
69.62——B2O3molar mass of (a), g/mol;
m-mass of sample, g;
f is dilution multiple.
Example 2
In this example, 0.3g of CaO-Al, which is a metallurgical slag containing rare earth, was taken2O3-Ce2O3-15%B2O3And putting the slag sample 2 into an erlenmeyer flask, adding 40ml of acid solution into the erlenmeyer flask, placing the erlenmeyer flask on a magnetic stirrer, heating and stirring the erlenmeyer flask until the slag sample is completely dissolved, taking down the erlenmeyer flask, and cooling the erlenmeyer flask to room temperature. 10ml of the cooled solution was taken out of a beaker, diluted to 50ml with distilled water, and used as a test solution after being mixed with a glass rod. Taking 10ml of solution to be detected, putting into a conical flask, adding 2 drops of bromocresol green-methyl red mixed indicator, and neutralizing free acid in the solution by using 0.1mol/L sodium hydroxide standard solution until the solution is just green, wherein the volume of the sodium hydroxide standard solution consumed in the process is not counted. Adding 3g mannitol to the solution intensifies the boric acid electrolysis, at which time the solution changes from green to dark red again. To the direction ofAnd adding 2 drops of phenolphthalein indicator into the solution as a titration end point, titrating by using 0.05mol/L sodium hydroxide standard solution, and fully shaking the solution from dark red, grey green, green and grey pink, wherein the titration end point is obtained if the solution does not fade within 30 s. 0.75g of mannitol was added to the solution and, if the solution changed from grey to green, titration with 0.05mol/L sodium hydroxide standard solution was continued to grey. Repeating the operation until the solution is not discolored after adding the mannitol, and recording the total volume of the sodium hydroxide consumed in the titration process as V1。
Continuously taking 10ml of solution to be detected, adding 2 drops of bromocresol green-methyl red mixed indicator into the conical flask, enabling the solution to be dark red, neutralizing the solution with 0.1mol/L of sodium hydroxide standard solution until the solution is just green, and not counting the volume of the sodium hydroxide consumed in the process. Adding 2 drops of phenolphthalein indicator into the solution, continuously titrating with 0.05mol/L sodium hydroxide standard solution, wherein the solution is in green-gray pink color and does not fade within 30s, namely a titration end point, and recording the volume of sodium hydroxide consumed by titration as V2。
Example 3
In this example, 0.3g of CaO-Al, which is a metallurgical slag containing rare earth, was taken2O3-Ce2O3-5%B2O3And putting the slag sample 3 into an erlenmeyer flask, adding 40ml of acid solution into the erlenmeyer flask, placing the erlenmeyer flask on a magnetic stirrer, heating and stirring the erlenmeyer flask until the slag sample is completely dissolved, taking down the erlenmeyer flask, and cooling the erlenmeyer flask to room temperature. 5ml of the cooled solution was taken out in a beaker, diluted to 25ml with distilled water, and used as a test solution after being mixed with a glass rod. Taking 10ml of solution to be detected, putting into a conical flask, adding 2 drops of bromocresol green-methyl red mixed indicator, and neutralizing free acid in the solution by using 0.1mol/L sodium hydroxide standard solution until the solution is just green, wherein the volume of the sodium hydroxide standard solution consumed in the process is not counted. Adding 2g mannitol to the solution intensifies the boric acid electrolysis, at which time the solution changes from green to dark red again. Adding 2 drops of phenolphthalein indicator into the solution as a titration end point, titrating with 0.05mol/L sodium hydroxide standard solution to obtain a solution with dark red-grayish green-grayish pink color, and sufficiently shaking after titrating to the grayish pink color, wherein if the solution is not within 30sAnd (4) fading, namely, obtaining a titration end point. 0.5g of mannitol is added to the solution and, if the solution changes from grey to green, titration with 0.05mol/L sodium hydroxide standard solution is continued until grey. Repeating the operation until the solution is not discolored after adding the mannitol, and recording the total volume of the sodium hydroxide consumed in the titration process as V1。
Continuously taking 10ml of solution to be detected, adding 2 drops of bromocresol green-methyl red mixed indicator into the conical flask, enabling the solution to be dark red, neutralizing the solution with 0.05mol/L of sodium hydroxide standard solution until the solution is just green, and not counting the volume of the sodium hydroxide consumed in the process. Adding 2 drops of phenolphthalein indicator into the solution, continuously titrating with 0.05mol/L sodium hydroxide standard solution, wherein the solution is in green-gray pink color and does not fade within 30s, namely a titration end point, and recording the volume of sodium hydroxide consumed by titration as V2。
According to the contrast detection method, the content of boron trioxide in the metallurgical slag system is detected and analyzed, and compared with the detection and analysis results of the traditional acid-base titration method and an Electronic Probe (EPMA), the results are shown in Table 1.
TABLE 1 analysis results of samples (% by mass)
As can be seen from Table 1, the results obtained by the control detection and analysis method used in the present invention are more consistent with the results of the chemical detection and analysis, which indicates that the control detection and analysis method of the present invention is accurate and reliable.
Claims (7)
1. A contrast detection method for determining the content of diboron trioxide in a metallurgical slag system is characterized by comprising the following specific steps:
first, taking CaO-Al2O3-Ce2O3-B2O3Adding an acid solution into the slag sample, heating and stirring until the slag sample is completely dissolved, and cooling to room temperature; diluting the cooled solution with distilled water to obtain a solution to be detected; equally measuring two parts of solution to be measured, wherein the two parts are respectively to be measuredSolution A and solution B to be detected;
secondly, adding a bromocresol green-methyl red mixed indicator into the solution A to be detected, and neutralizing the solution A to be detected by using an alkali solution until the solution A to be detected is just changed from dark red to green; adding mannitol to change the solution A to be detected which is changed into green into dark red again; then, a phenolphthalein indicator is added dropwise, and the solution A to be detected which is changed into dark red again is titrated to be just gray pink by using an alkali solution and does not fade within 30 s;
thirdly, adding mannitol into the solution obtained in the second step, changing the gray pink color into green again, and continuously titrating the solution with alkali solution until the gray pink color is fadeless within 30 s; repeating the step until the solution is not discolored after adding mannitol, and recording the volume of the alkaline solution consumed in the titration process as V1;
Fourthly, adding a bromocresol green-methyl red mixed indicator into the solution B to be detected, and neutralizing the solution B to be detected by using an alkali solution until the solution B to be detected is just changed from dark red to green; continuously adding a phenolphthalein indicator, and titrating the indicator with an alkali solution until the color is just grey pink and does not fade within 30 s; record the volume of alkaline solution consumed during titration as V2。
2. The comparative detection method for determining the content of diboron trioxide in a metallurgical slag system according to claim 1, wherein V is1And V2For calculating B2O3The content is as follows:
c-concentration of sodium hydroxide solution, mol/L;
69.62——B2O3molar mass of (a), g/mol;
m is the mass of the slag sample, g;
f is dilution multiple.
3. The comparative detection method for determining the content of diboron trioxide in a metallurgical slag system according to claim 1 or 2, characterized in that each 1g of CaO-Al is used2O3-Ce2O3-B2O3120ml to 150ml of acid solution is correspondingly taken from the slag sample.
4. The comparative detection method for determining the content of diboron trioxide in a metallurgical slag system according to claim 3, characterized in that the heating temperature is controlled at 95-100 ℃.
5. The comparative detection method for determining the content of diboron trioxide in a metallurgical slag system according to claim 4, characterized in that the acid solution is 0.3mol/L hydrochloric acid solution.
6. The comparative detection method for determining the content of diboron trioxide in a metallurgical slag system according to claim 5, wherein the dilution factor of the cooled solution diluted by adding distilled water is 5-20 times of that of the original solution.
7. The comparative detection method for determining the content of diboron trioxide in a metallurgical slag system according to claim 6, wherein the alkali solution is 0.05-0.1 mol/L sodium hydroxide standard solution.
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