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CN-122017122-A - Method for detecting alumina content of high-alumina material

CN122017122ACN 122017122 ACN122017122 ACN 122017122ACN-122017122-A

Abstract

The invention discloses a method for detecting the content of alumina in a high aluminum material, which is based on an EDTA complexation titration principle, and comprises the steps of forming a stable complex (lgK =16.1) by EDTA and aluminum ions in a buffer system with pH=6.0, judging an end point through color change (brilliant yellow to purplish red) of an indicator, wherein the method has the advantages that refractory matters such as aluminum nitride and the like can be completely decomposed by adopting alkali fusion pretreatment of YST 575.1, the full release of aluminum element is ensured, and the method is suitable for detecting aluminum ash recycling products with complex components by optimizing the buffer conditions and masking agents to effectively overcome the interferences such as iron (III), calcium, magnesium and the like in combination with a titration system with GB/T6900.

Inventors

  • HUANG ZHEN
  • Peng Diehui
  • WEN JIAXIN
  • CHEN HUINAN

Assignees

  • 东莞市新东欣环保投资有限公司
  • 广东东实环境股份有限公司

Dates

Publication Date
20260512
Application Date
20260203

Claims (10)

  1. 1. The method for detecting the alumina content of the high alumina material is characterized by comprising the following steps of: S100, sample pretreatment, namely crushing, ball milling and screening a high-alumina sample to form high-alumina powder, drying the high-alumina powder, and then placing the dried high-alumina powder in a dryer to be cooled to room temperature; S200, weighing m 1 g of the high-alumina material sample obtained in the step S100, putting the high-alumina material sample into a 30ml platinum crucible, adding anhydrous sodium carbonate and boric acid, uniformly stirring with a platinum wire, covering a crucible cover, putting the crucible cover into a high-temperature furnace at 100 ℃, heating to 1000 ℃ for melting 20 min, and then taking out and cooling; S300, decomposing a sample, adding boiling water into a crucible, heating to dissolve a dissolved block completely, transferring the solution into a 250mL beaker, washing the crucible with hot water twice, then fully cleaning with 3 mL hydrochloric acid and hot water, merging the washing liquid into the beaker, adding hydrochloric acid into the beaker, covering a watch glass, cooling to room temperature in a cold water tank, transferring the solution into a 250mL volumetric flask, cleaning the beaker with water, merging the washing liquid into the volumetric flask, diluting with water to a scale, and shaking to obtain a test solution; S400, titrating, namely transferring 50mL of the test solution obtained in the step S300 by using a pipette into a 200mL volumetric flask, diluting to about 150mL, adding 1-2 drops of phenolphthalein solution, neutralizing by using sodium hydroxide solution until the test solution is just red, then excessively adding 8mL, carrying out heat preservation for 30min in a 70 ℃ water bath, taking down, cooling to room temperature, diluting to a scale by using water, uniformly mixing, standing for 10min, carrying out dry filtration by using medium-speed filter paper, carrying out dry filtration on the obtained filtrate by using a dry beaker, and discarding the initial 15-20 mL mL of filtrate; S500, removing the filtrate obtained in the step S400 of 100mL by using a pipette, adding V 2 mL of EDTA standard solution, neutralizing the solution with hydrochloric acid until the red color disappears, adding 1 drop of bromophenol blue indicator solution, adjusting the solution to yellow to blue by using ammonia water, heating and boiling for 5 to 10min, taking down, cooling to room temperature, adding 15mLpH of hexamethylenetetramine buffer solution with a value of 5.5, 3-4 drops of xylenol orange indicator solution, adding V 3 mL of zinc acetate standard titration solution until the test solution changes from yellow to purple as an end point, and calculating according to the consumption volume of the zinc acetate standard titration solution to obtain the alumina content of the high alumina material; And S600, repeating the steps S200-S500 for three times for the same high aluminum material sample, and independently measuring three times, wherein the alumina content of the high aluminum material is averaged.
  2. 2. The method for detecting alumina content of high alumina according to claim 1, wherein in the step S500, the alumina content of the high alumina is calculated by mass fraction, and the value is expressed as % Is calculated as: wherein: -the value of EDTA standard solution concentration in mol/L; -adding the value of the EDTA standard solution volume in mL; -back-dropping the value of the volume of the zinc acetate standard titration solution used for the excess EDTA standard solution in mL; -the zinc acetate standard titration solution is converted into the coefficient of the EDTA standard solution; -the number of molar masses of alumina, in g/mol, m= 101.961; The mass value of the high-alumina sample is expressed in g.
  3. 3. The method for detecting alumina content in high alumina according to claim 1, wherein in the step S100, a screen with a pore size of 74 μm is used for screening.
  4. 4. The method according to claim 1, wherein in the step S100, the drying temperature of the high alumina powder is 105 to 110 ℃ and the drying time is 2 hours.
  5. 5. The method for detecting alumina content in high alumina according to claim 1, wherein in the step S200, the anhydrous sodium carbonate is added in an amount of 1.7g, and the boric acid is added in an amount of 0.8g.
  6. 6. The method according to claim 1, wherein in the step S400, the concentration of the sodium hydroxide solution is 500g/L.
  7. 7. The method for detecting the alumina content of the high alumina material according to claim 2, wherein the specific steps of measuring the coefficient K of the standard titration solution of zinc acetate converted into the standard solution of EDTA are as follows: 3 parts of 10mL EDTA standard solution are removed and respectively placed in a 400mL beaker, water is added to about 200mL, 15mL of hexamethylenetetramine buffer solution is added, 1 drop of bromophenol blue indicator solution, 3 drops to 4 drops of xylenol orange indicator solution are added, the titration of zinc acetate standard titration solution is carried out until the test solution changes from yellow to purple, the standard deviation of milliliters of the zinc acetate standard titration solution consumed by 3 parts of EDTA standard solution is not more than 0.10mL, the average value is taken, and the calculation formula of the coefficient K of the zinc acetate standard titration solution converted into the EDTA standard solution is as follows: wherein: 10-transferring the numerical value of the EDTA standard solution volume, wherein the unit is mL; v-the value of the average value of the volumes of the standard titration solutions of zinc acetate used at the time of dripping, in mL.
  8. 8. The method for detecting the alumina content of the high alumina material according to claim 2, wherein the specific steps of determining the concentration of the EDTA standard solution are as follows: Transferring 3 parts of 40mL of alumina standard solution with the concentration of 0.02 mol/L into a 400mL beaker, adding 45mL of EDTA standard solution, adding water to 200mL, adding 1 drop of bromophenol blue indicator solution, adjusting the pH value to be the yellow-blue value of the test solution by using ammonia water, heating and boiling for 5 min-10 min, taking down, cooling to room temperature, adding 15 mL hexamethylenetetramine buffer solution, 2 drops-3 drops of xylenol orange indicator solution, taking titration of zinc acetate standard titration solution until the test solution changes from yellow to purple as an end point, taking the standard deviation of milliliters of zinc acetate standard titration solution consumed by 3 parts of alumina standard solution as the average value, and taking the average value, wherein the concentration of the EDTA standard solution is equal to the mass concentration of a substance The unit is mol/L, The calculation formula of (2) is as follows: wherein: -transferring the value of the volume of the alumina standard solution in mL; -adding the value of the EDTA standard solution volume in mL; -dripping back the value of the average value of the volumes of the zinc acetate standard titration solutions used for the excess EDTA standard solution, in mL; -the value of the concentration of the alumina standard solution, in mol/L; -the zinc acetate standard titration solution is converted into the coefficient of EDTA standard solution.
  9. 9. The method for detecting alumina content in high alumina according to claim 1, wherein in the step S400, the concentration of the phenolphthalein solution is 10 g/L, and the high alumina is prepared from 60% by mass of ethanol solution.
  10. 10. The method according to claim 1, wherein in the step S500, the concentration of the xylenol orange indicator solution is 5g/L, and the concentration of the bromophenol blue indicator solution is 18g/L.

Description

Method for detecting alumina content of high-alumina material Technical Field The invention relates to the technical field of high aluminum material alumina content detection, in particular to a high aluminum material alumina content detection method. Background The stable operation and product quality control of the aluminum ash recycling project are highly dependent on accurate alumina content detection. The main components of the aluminum ash comprise aluminum simple substance, aluminum oxide and aluminum nitride, most of metal aluminum is recovered through pretreatment means such as crushing, ball milling, screening and the like, and the rest materials enter a wet reaction system. In the system, aluminum simple substance reacts with water to generate aluminum hydroxide and hydrogen, aluminum nitride is hydrolyzed to generate ammonia gas and aluminum hydroxide, aluminum oxide is reserved as a stable component and is enriched in a final product, and a high aluminum material product taking the aluminum oxide content as a core index is formed. However, the detection of the component content of the high aluminum ash produced in the current aluminum ash recycling treatment process faces the dilemma of standard deficiency, and enterprises can only apply the detection standards of various industries according to different purposes of the high aluminum ash due to the lack of uniform detection standards, so that the detection methods are disordered and the data comparability is poor. The three outstanding problems exist in the current situation, namely, firstly, different detection methods have different requirements on sample pretreatment and influence the comparability of detection results, secondly, the difference of detection equipment causes data deviation, thirdly, the lack of uniform quality control standards makes the detection data difficult to effectively compare and causes the fluctuation and incomparability of the detection data, and the existence of the problems not only influences the stable control of the production process, but also is unfavorable for the accurate assessment of the product quality. Therefore, it is important to establish a scientific, stable and practical method for detecting the content of alumina in high-alumina products. The method not only can ensure the accuracy of production data and optimize process parameters, but also can provide reliable quality basis for high-aluminum material sales, enhance customer trust and promote market competitiveness. Disclosure of Invention The invention mainly aims to provide a method for detecting the alumina content of a high alumina material, and aims to solve the problems that the method for detecting the alumina content in a high alumina material product in the background art is disordered, the detection standard is not uniform, the data comparability is poor, the detection data is not coherent, the alumina content of the high alumina material cannot be truly reflected, and the production and sales of an aluminum ash project cannot be correctly guided. In order to achieve the above purpose, the method for detecting the alumina content of the high alumina material provided by the invention comprises the following steps: S100, sample pretreatment, namely crushing, ball milling and screening a high-alumina sample to form high-alumina powder, drying the high-alumina powder, and then placing the dried high-alumina powder in a dryer to be cooled to room temperature; S200, weighing m 1 g of the high-alumina material sample obtained in the step S100, putting the high-alumina material sample into a 30ml platinum crucible, adding anhydrous sodium carbonate and boric acid, uniformly stirring with a platinum wire, covering a crucible cover, putting the crucible cover into a high-temperature furnace at 100 ℃, heating to 1000 ℃ for melting 20 min, and then taking out and cooling; S300, decomposing a sample, adding boiling water into a crucible, heating to dissolve a dissolved block completely, transferring the solution into a 250mL beaker, washing the crucible with hot water twice, then fully cleaning with 3 mL hydrochloric acid and hot water, merging the washing liquid into the beaker, adding hydrochloric acid into the beaker, covering a watch glass, cooling to room temperature in a cold water tank, transferring the solution into a 250mL volumetric flask, cleaning the beaker with water, merging the washing liquid into the volumetric flask, diluting with water to a scale, and shaking to obtain a test solution; S400, titrating, namely transferring 50mL of the test solution obtained in the step S300 by using a pipette into a 200mL volumetric flask, diluting to about 150mL, adding 1-2 drops of phenolphthalein solution, neutralizing by using sodium hydroxide solution until the test solution is just red, then excessively adding 8mL, carrying out heat preservation for 30min in a 70 ℃ water bath, taking down, cooling to room temperature, diluting to a scale by