CN-117706021-B - Method for detecting content of aluminum oxide in aluminum-manganese-calcium alloy

Abstract

The invention discloses a method for detecting the content of aluminum oxide in an aluminum-manganese-calcium alloy, which mainly solves the technical problem that the content of aluminum oxide in the existing aluminum-manganese-calcium alloy cannot be accurately and rapidly detected. The technical scheme is that the method for detecting the content of alumina in the aluminum-manganese-calcium alloy comprises the steps of 1) preparing a sample, removing an oxide layer on the surface of the sample, placing the sample in a reagent bottle containing an organic solvent for storage, 2) extracting alumina in the sample by an electrolysis method, firstly extracting alumina in the sample by an electrolysis method, placing the sample in an electrolysis tank for electrolysis, wherein the sample is an anode, a platinum electrode is a cathode, and a saturated calomel electrode is a reference electrode, 3) detecting alumina in the sample, placing a filter membrane and a filter material in the step 2) in a platinum crucible, removing the filter membrane by high-temperature ashing, and 4) calculating the mass percentage of the alumina in the aluminum-manganese-calcium alloy. The method for measuring the aluminum oxide content in the aluminum-manganese-calcium alloy has the advantages that the Relative Standard Deviation (RSD) is less than 3%, and the detection data precision is good, accurate and reliable.

Inventors

• ZHOU GUIHAI

Assignees

• 上海梅山钢铁股份有限公司

Dates

Publication Date

20260505

Application Date

20220907

Claims (8)

1. 1. The method for detecting the content of aluminum oxide in the aluminum-manganese-calcium alloy is characterized by comprising the following steps of: 1) Preparing a sample, intercepting the sample, controlling the size of the sample to be 20-50 mm long, the width of the sample to be 20-40 mm, and the thickness of the sample to be 0.5-2.0 mm, removing an oxide layer on the surface of the sample, and placing the sample into a reagent bottle containing an organic solvent for preservation; 2) The method comprises the steps of extracting alumina from a sample by an electrolytic method, placing the sample in an electrolytic tank for electrolysis, wherein the sample is an anode, a platinum electrode is a cathode, a saturated calomel electrode is a reference electrode, the electrolytic current is 70-120 mA, the electrolytic quantity is 500-10000C, the temperature of the electrolyte is 50-60 ℃, and the electrolyte comprises 5-10% hydrochloric acid, 1-1.5% triethanolamine, 2-3% tartaric acid and 1-2% disodium ethylenediamine tetraacetate solution; Then soaking the electrolyzed sample with a cleaning solution, and ultrasonically cleaning the sample in the cleaning solution by using ultrasonic waves; then, carrying out reduced pressure filtration on the electrolyte after the electrolysis of the sample and the cleaning solution for cleaning the sample after the electrolysis, and collecting a filtrate and a filter membrane; 3) Detecting alumina in the sample, placing the filter membrane and the filter material in the step 2) in a platinum crucible, and removing the filter membrane by high-temperature ashing; Then adding 1.0-2.0 g of potassium pyrosulfate into the crucible, placing the crucible in a 300-400 ℃ high-temperature furnace, melting at a high temperature for 15-25 min, and taking out and cooling; Heating and dissolving the melt in the crucible by using 10-20 mL of hydrochloric acid solution, wherein the volume concentration of the hydrochloric acid solution is 20-30%; After the dissolution is completed, adding 5-10 mL of sodium hydroxide solution with the mass concentration of 50% and 10-25 mL of disodium ethylenediamine tetraacetate standard solution with the concentration of 0.0100mol/L into the solution; Adjusting the pH value of the solution to 4-5; adding 15-20 mL of acetic acid-ammonium acetate buffer solution into the solution, heating and boiling for 2-3 min, taking out and cooling to 25-35 ℃; Adding 3-5 mL of nitroso-R salt solution with the mass concentration of 0.1% into the solution, wherein the nitroso-R salt solution is used as an indicator; Titrating the solution, titrating the solution to be yellow green by using a copper sulfate standard solution with the concentration of 0.0100mol/L, stopping titrating, and reading the titration volume of the copper sulfate; 4) Calculating the mass percent of aluminum oxide in the aluminum-manganese-calcium alloy, calculating the mass percent of aluminum oxide in the aluminum-manganese-calcium alloy according to a formula I, In the formula I, W is the mass percentage of aluminum oxide in the aluminum-manganese-calcium alloy, v 1 is the volume of an EDTA standard solution, c 1 is the concentration of the EDTA standard solution, v 2 is the volume of a titrated copper sulfate standard solution, c 2 is the concentration of the titrated copper sulfate standard solution, M is the molar mass of aluminum oxide, M 1 is the mass of a sample before electrolysis, M 2 is the mass of the sample after electrolysis, and g.
2. 2. The method for detecting the content of alumina in the aluminum-manganese-calcium alloy according to claim 1, wherein the sample surface oxide layer in the step 1) is polished by zirconia sand paper, and the organic solvent is any one of acetone, diethyl ether and methanol.
3. 3. The method for detecting the content of alumina in the aluminum-manganese-calcium alloy according to claim 1, wherein hydrochloric acid, tartaric acid, disodium ethylenediamine tetraacetate and triethanolamine in the electrolyte are all of an analytical grade or more, and water in the electrolyte is of a grade of two or more than that of laboratory analysis water.
4. 4. The method for detecting the content of alumina in the aluminum-manganese-calcium alloy according to claim 1, wherein in the electrolysis process, the electrolytic tank is placed in a constant-temperature water tank, and the water temperature in the constant-temperature water tank is 50-60 ℃.
5. 5. The method for detecting the content of alumina in the aluminum-manganese-calcium alloy according to claim 1, wherein the cleaning solution is a hydrochloric acid solution with a volume concentration of 5-10%.
6. 6. The method for detecting the content of alumina in the aluminum-manganese-calcium alloy according to claim 1, wherein the filter membrane is made of polytetrafluoroethylene, and the diameter of a membrane hole of the filter membrane is 0.05-0.10 μm.
7. 7. The method for detecting the alumina content in the aluminum-manganese-calcium alloy according to claim 1, wherein the ashing temperature of the filter membrane is 300-500 ℃, and the ashing time of the filter membrane is 20-30 min.
8. 8. The method for detecting the content of alumina in the aluminum-manganese-calcium alloy according to claim 1, wherein the method for preparing the acetic acid-ammonium acetate buffer solution comprises the steps of weighing 77g of ammonium acetate, dissolving in water, adding 59mL of glacial acetic acid, diluting to 1000mL with water, and shaking uniformly.

Description

Method for detecting content of aluminum oxide in aluminum-manganese-calcium alloy Technical Field The invention relates to a method for detecting chemical components in aluminum-manganese-calcium alloy, in particular to a method for detecting the content of aluminum oxide in aluminum-manganese-calcium alloy, specifically relates to a method for detecting the content of aluminum oxide in aluminum-manganese-calcium alloy for steelmaking, and belongs to the technical field of ferrous metallurgy chemical analysis. Background The deoxidation of molten steel is the most important link in the steelmaking production process, and the aim of removing dissolved oxygen in molten steel is achieved by adding metal elements with stronger affinity than iron into molten steel and reacting with oxygen to generate oxides which are insoluble in molten steel. Common steelmaking deoxidizers include manganese, calcium, silicon, aluminum and the like. The Al-Mn-Ca alloy is a common composite deoxidizer in steelmaking, and the metallic Al-Mn-Ca element in the Al-Mn-Ca alloy is mainly utilized to react with oxygen to achieve the steelmaking deoxidization effect. The effective deoxidizing component of the aluminum-manganese-calcium alloy is mainly a metal element, and aluminum oxide in the aluminum-manganese-calcium alloy cannot deoxidize molten steel, and can directly influence the deoxidizing effect and the quality of molten steel. The prior art can not measure and grade aluminum oxide in aluminum-manganese-calcium alloy, and the quality evaluation of the aluminum-manganese-calcium alloy is judged only by measuring the content of aluminum element in a sample, so that great risks exist for steelmaking deoxidization. The detection of the content of aluminum oxide mainly comprises a capacity method, a photometry method, an inductively coupled plasma emission spectrometry method, an X-ray fluorescence spectrometry method and the like, wherein the methods basically measure the content of aluminum element in a sample and report the content of aluminum oxide in the form of aluminum oxide, and the aluminum oxide content in the sample cannot be detected without distinguishing the metal aluminum and the aluminum oxide in the sample. The Chinese patent application No. CN104215541A discloses a method for efficiently and accurately detecting the content of high-purity alumina and the content of impurities, and the method comprises the steps of detecting impurity elements in alumina after a sample is treated by hydrochloric acid, weighing unreacted alumina, and calculating the content of the alumina and the impurity elements. The method is only suitable for detecting high-purity alumina materials, can not separate and detect metal aluminum and alumina, and can not meet the detection of the content of alumina in the aluminum-manganese-calcium alloy. The Chinese patent application with application publication number CN109001192A discloses an automatic titration analysis method for soluble alumina, which comprises the steps of controlling a peristaltic pump to titrate a measured liquid by a computer, collecting an image of color change in a titration process by a machine vision sensor, analyzing and judging the image by a digital image processing algorithm, closing the peristaltic pump when a titration end point is analyzed, and calculating the content of the soluble alumina after the titration is finished. The method is only suitable for measuring the soluble aluminum oxide, does not solve the problems of separation and detection of aluminum oxide and metal aluminum, and cannot meet the detection of the aluminum oxide content in the aluminum-manganese-calcium alloy. The Chinese patent application of application publication No. CN112986486A discloses a method for detecting the metal aluminum content of aluminum slag deoxidizer and a sample preparation method, wherein the sample preparation component is powdery, feCl3 solution is used for selectively reacting with metal aluminum to distinguish metal aluminum from aluminum oxide, and the method firstly needs the sample to be prepared into the powdery state, so that the problem of rapid oxide of the powdery metal aluminum cannot be avoided, and the detection of the aluminum oxide content in the aluminum-manganese-calcium alloy cannot be satisfied. The Chinese patent application of application publication No. CN102607934A discloses a melting sample preparation method for X-ray fluorescence spectrum analysis of aluminum-manganese-calcium-iron alloy, and the method is only suitable for detecting the content of aluminum element in the aluminum-manganese-calcium alloy, and does not distinguish the aluminum oxide content and the metal aluminum content of the aluminum-manganese-calcium alloy. In the prior art, the method disclosed in the prior art can not accurately separate and extract alumina in an aluminum-manganese-calcium sample from a sample, and the prior art can not accurately determine the content