Method for analyzing contents of aluminum oxide, ferric oxide, manganese oxide, silicon dioxide, strontium oxide and titanium dioxide in lime

Abstract

The invention discloses a method for analyzing the content of aluminum oxide, ferric oxide, manganese oxide, silicon dioxide, strontium oxide and titanium dioxide in lime, and belongs to the technical field of metallurgical analysis. According to the method, a sodium carbonate and boric acid mixed solvent is adopted to melt a sample, hydrochloric acid is utilized to extract melt, and inductively coupled plasma emission spectrometry is adopted to simultaneously determine the content of aluminum oxide, ferric oxide, manganese oxide, silicon dioxide, strontium oxide and titanium dioxide in lime. The method specifically comprises the following steps: weighing a sample, melting, extracting with hydrochloric acid, diluting to a constant volume, and determining with an inductively coupled plasma emission spectrometer. Compared with a traditional chemical analysis method which is tedious in operation, the method has the advantages that the working efficiency is improved, the environmental pollution is reduced, and the method is simple, rapid and accurate to operate.

Description

Technical Field

[0001] The invention belongs to the technical field of metallurgical analysis, and in particular relates to a method for analyzing the contents of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide and titanium dioxide in white ash. Background Art

[0002] In the iron and steel industry, quicklime plays a vital role as a raw material in the smelting process. The addition of quicklime (primarily composed of CaO) during the ironmaking process primarily serves to form slag, desulfurize, and adjust the slag pH. During the steelmaking process, quicklime neutralizes acidic impurities in the molten steel and binds them in the slag, helping to reduce the oxide content in the molten steel, thereby reducing its adverse effects and improving its quality. Due to its fine grains, high porosity, large reaction area, and unstable lattice, quicklime quickly reacts with ferrous oxide, manganese oxide, calcium fluoride, and other substances that have infiltrated the lime pores to form a low-melting-point melt, which melts into slag. This significantly shortens the melting time. The resulting slag forms a protective layer on the furnace lining, reducing wear and erosion, extending its service life, and meeting the demands of rapid steelmaking. These benefits make quicklime an indispensable auxiliary raw material in the ironmaking process.

[0003] Traditionally, chemical analysis of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide, and titanium dioxide in lime relies on gravimetric, colorimetric, and titration methods. This process is cumbersome and lengthy, requiring multiple steps and multiple processes, and is no longer suitable for modern steel and metallurgical production.

[0004] This method allows for the simultaneous determination of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide, and titanium dioxide using inductively coupled plasma optical emission spectrometry (ICP-OES) after a single sample processing. This significantly improves work efficiency and meets the high-quality development requirements of the company's testing sector, which previously required six independent individuals. Summary of the Invention

[0005] The present invention provides a method for analyzing the contents of aluminum oxide, ferric oxide, manganese oxide, silicon dioxide, strontium oxide, and titanium dioxide in lime. By using inductively coupled plasma optical emission spectrometry (ICP-AES) to simultaneously determine the contents of aluminum oxide, ferric oxide, manganese oxide, silicon dioxide, strontium oxide, and titanium dioxide in lime, a working curve is drawn using standard samples of dolomite and limestone. This method improves efficiency and reduces environmental pollution compared to traditional chemical analysis methods, which are often tedious. The method is simple, rapid, and accurate.

[0006] In order to solve the above technical problems, the present invention adopts the following technical solutions:

[0007] The invention discloses a method for analyzing the contents of aluminum oxide, ferric oxide, manganese oxide, silicon dioxide, strontium oxide and titanium dioxide in white ash. The method comprises the following steps: sample weighing, melting, extraction with hydrochloric acid, dilution and volume adjustment, and determination by inductively coupled plasma optical emission spectrometry.

[0008] Furthermore, the white ash is mixed with a mixed flux of sodium carbonate and boric acid and then melted in a muffle furnace. The melt is extracted with hydrochloric acid, transferred to a 250 ml volumetric flask, shaken and then introduced into an inductively coupled plasma optical emission spectrometer to determine the content.

[0009] Furthermore, the lime is mixed with a mixed flux of sodium carbonate and boric acid and then melted in a muffle furnace at 950°C.

[0010] Furthermore, the weighed sample was placed in a 25 mL platinum crucible, 2.5 g of a mixed flux of sodium carbonate and boric acid was added, stirred with a glass rod, and then placed in a 950°C muffle furnace to melt for 30 minutes. The crucible was taken out and cooled, and the surface of the platinum crucible was wiped clean with filter paper and placed in a 300 mL beaker. 40 mL of hydrochloric acid was added and heated on a low-temperature hot plate until the melt was completely decomposed and the solution was transparent. After the solution was cooled, it was transferred to a 250 mL volumetric flask, diluted to the scale and shaken. The intensity was measured using an inductively coupled plasma emission spectrometer, and the content of the measured component was obtained from the working curve.

[0011] Furthermore, the mass ratio of sodium carbonate to boric acid in the mixed flux is 2:1.

[0012] Furthermore, the main operating parameters of the inductively coupled plasma optical emission spectrometer used are: high frequency: 40.68 MHZ; power: 1300 W; carrier gas flow rate: 0.8 L / min.

[0013] Furthermore, this method can accurately determine the contents of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide, and titanium dioxide in white ash. The operation is simple and fast, with good accuracy and precision, greatly improving work efficiency.

[0014] Compared with the prior art, the present invention has the following beneficial technical effects:

[0015] The present invention realizes the rapid detection of the contents of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide and titanium dioxide in white ash, conforms to the development direction of modern instrumental analysis and detection, has advancedness and scientificity and good accuracy, and meets the requirements for high-quality development in the detection field of the steel and metallurgical industry. DETAILED DESCRIPTION

[0016] An analytical method for the content of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide, and titanium dioxide in lime:

[0017] 1 Scope of application

[0018] This method is applicable to the determination of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide and titanium dioxide in lime.

[0019] 2 Principles

[0020] Mix white ash with a mixed flux of sodium carbonate and boric acid and melt it in a muffle furnace at 950°C. Extract the melt with hydrochloric acid, transfer it to a 250 ml volumetric flask, shake it well, and then introduce the solution into an inductively coupled plasma optical emission spectrometer to determine the content.

[0021] 3 Main instruments and reagents

[0022] Hydrochloric acid: (ρ1.19)

[0023] Mixed flux: sodium carbonate + boric acid = 2 + 1

[0024] Inductively Coupled Plasma Optical Emission Spectrometer

[0025] High purity iron (99.98%)

[0026] Deionized water

[0027] 4 Instrument Preparation

[0028] 4.1 Main operating parameters of the instrument

[0029] High frequency: 40.68MHZ Power: 1300W Carrier gas flow: 0.8L / min

[0030] Analytical elements and wavelengths

[0031] element Al Fe Mn Si Sr Ti Wavelength (nm) 396.153 238.204 257.610 251.611 421.552 334.941

[0032] 4.2 Working curve drawing

[0033] Using reagent blank, dolomite and limestone standard samples, the determination method in 5.3 was used for synchronous operation. After the instrument automatically measured each standard sample, a working curve was drawn with the intensity of the measured element as the ordinate and the content as the abscissa.

[0034] Drawing of standard working curve%

[0035]

[0036]

[0037] 5 Analysis Steps

[0038] 5.1 Sample size

[0039] Weigh 0.50 mg of sample to the nearest 0.1 mg.

[0040] 5.2 Blank test

[0041] Perform blank test along with the sample

[0042] 5.3 Determination

[0043] Place the weighed sample in a 25mL platinum crucible, add approximately 2.5g of a mixed flux of sodium carbonate and boric acid (mass ratio 2:1), stir thoroughly with a glass rod, and melt in a 950°C muffle furnace for 30 minutes. Remove and cool. Clean the surface of the platinum crucible with filter paper and place it in a 300mL beaker. Add 40mL of hydrochloric acid (1+1) and heat on a low-temperature hot plate until the melt is completely decomposed and the solution becomes transparent. Remove the beaker. After the solution cools, transfer it to a 250mL volumetric flask, dilute to the mark, and shake well. Measure the intensity using an inductively coupled plasma optical emission spectrometer and obtain the content of the component to be determined from the working curve.

[0044] 6 Allowable difference

[0045]

[0046]

[0047] 7. Result evaluation

[0048] 7.1 Sample precision

[0049] By measuring the white ash sample 10 times, the relative standard deviation (RSD) of each measured component was less than 5%, indicating good precision.

[0050] Precision test

[0051]

[0052] 7.2 Sample Accuracy Experiment

[0053] The white ash samples were measured and compared using this method and X-ray fluorescence spectrometer. The errors of the two methods were less than the allowable difference, so this method has good accuracy.

[0054] Method comparison experiment (%)

[0055] Analytical ingredients <![CDATA[Al2O3]]> <![CDATA[Fe2O3]]> MnO <![CDATA[SiO2]]> SrO <![CDATA[TiO2]]> This method 1.28 0.513 0.023 3.82 0.054 0.035 X-ray fluorescence 1.26 0.526 0.020 3.86 0.050 0.032 Absolute difference 0.02 0.013 0.003 0.04 0.004 0.003 Allowable difference 0.05 0.03 0.004 0.06 0.010 0.004

[0056] 8 Conclusion

[0057] This method can be used to accurately determine the contents of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide, and titanium dioxide in white ash. It is simple and rapid to operate, has good accuracy and precision, greatly improves work efficiency, is advanced and scientific, is suitable for the green and environmental protection testing requirements of the modern metallurgical industry, and has good promotion and application value.

[0058] The embodiments described above are merely descriptions of preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Without departing from the spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by persons skilled in the art should fall within the scope of protection defined by the claims of the present invention.

Claims

1. A method for analyzing the contents of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide, and titanium dioxide in lime, characterized by: The sample was melted using a mixed flux of sodium carbonate and boric acid, and the melt was extracted with hydrochloric acid. The contents of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide, and titanium dioxide in the lime were simultaneously determined by inductively coupled plasma optical emission spectrometry. The method was specifically completed in the following steps: sample weighing → melting → hydrochloric acid extraction → dilution and volume adjustment → determination by inductively coupled plasma optical emission spectrometry.

2. The method for analyzing the contents of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide and titanium dioxide in white ash according to claim 1, characterized in that: Mix the lime with a mixed flux of sodium carbonate and boric acid and melt it in a muffle furnace. Use hydrochloric acid to extract the melt, transfer it to a 250 ml volumetric flask, shake it well, and then introduce the solution into an inductively coupled plasma optical emission spectrometer to determine the content.

3. The method for analyzing the contents of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide and titanium dioxide in white ash according to claim 2, characterized in that: Mix the lime with a mixed flux of sodium carbonate and boric acid and melt it in a muffle furnace at 950°C.

4. The method for analyzing the contents of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide and titanium dioxide in white ash according to claim 1, characterized in that: The weighed sample was placed in a 25 mL platinum crucible, 2.5 g of a mixed flux of sodium carbonate and boric acid was added, and the mixture was stirred with a glass rod and melted in a 950°C muffle furnace for 30 minutes. The crucible was removed and cooled. The surface of the platinum crucible was cleaned with filter paper and placed in a 300 mL beaker. 40 mL of hydrochloric acid was added and heated on a low-temperature electric hot plate until the melt was completely decomposed and the solution was transparent. The beaker was removed. After the solution cooled, it was transferred to a 250 mL volumetric flask, diluted to the mark and shaken. The intensity was measured using an inductively coupled plasma emission spectrometer, and the content of the measured component was obtained from the working curve.

5. The method for analyzing the contents of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide and titanium dioxide in white ash according to claim 1 or 4, characterized in that: The mass ratio of sodium carbonate to boric acid in the mixed flux is 2:

1.

6. The method for analyzing the contents of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide and titanium dioxide in white ash according to claim 1, characterized in that: The main operating parameters of the inductively coupled plasma optical emission spectrometer used are: high frequency: 40.68 MHZ; power: 1300 W; carrier gas flow rate: 0.8 L / min.

7. The method for analyzing the contents of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide and titanium dioxide in white ash according to claim 1 or 4, characterized in that: This method can be used to accurately determine the contents of aluminum oxide, iron oxide, manganese oxide, silicon dioxide, strontium oxide, and titanium dioxide in white ash. The operation is simple and rapid, with good accuracy and precision, greatly improving work efficiency.

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