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CN-122016770-A - Method for measuring aluminum in aluminum iron by ICP-AES

CN122016770ACN 122016770 ACN122016770 ACN 122016770ACN-122016770-A

Abstract

The invention discloses a method for measuring aluminum in aluminum iron by ICP-AES, which is characterized in that a double internal standard correction system is constructed by introducing scandium (Sc) which is a main internal standard element and yttrium (Y) which is an alternative internal standard element, so that the problem of matrix effect under high aluminum content is solved, the accurate detection of the content range of 10.00% -60.00% is realized, the requirements of rapid quality control in steelmaking production and high precision in high-end steel production are met, and the application scene and flexibility of the method are widened. The invention aims to provide the method for measuring aluminum in aluminum iron by ICP-AES, which has the advantages of simple operation, rapid detection, high accuracy, strong anti-interference capability and no special requirement on instruments.

Inventors

  • YANG HANXIAO
  • WANG JIA
  • SHI LIN
  • LIU GANGYAO
  • WANG YANQIU

Assignees

  • 内蒙古包钢钢联股份有限公司

Dates

Publication Date
20260512
Application Date
20260320

Claims (7)

  1. 1. A method for measuring aluminum in aluminum iron by ICP-AES is characterized by comprising the following steps: And weighing 0.1000g of aluminum iron sample, wherein the sampling quantity can balance the detection sensitivity and the matrix concentration, so that the interference caused by the over-high matrix concentration due to over-sampling is avoided. Placing a sample in a 300 mL beaker, adding 20mL mixed acid, heating at low temperature until the sample is completely dissolved, cooling to room temperature, transferring into a 250 mL plastic volumetric flask, adding water to a constant volume, and shaking uniformly; the method comprises the steps of separating and diluting, namely, separating and extracting 10 mL to 100 mL after 250 mL is fixed in volume, namely, 10% -60% of high-content aluminum can be diluted to a linear range of 1.0% -6.0% which is matched with a conventional ICP-AES (inductively coupled plasma-atomic emission spectrometry) instrument, and meanwhile, the characteristics of a matrix are reserved, so that the detection accuracy is ensured; Preparing internal standard solution, namely respectively diluting 1000 mug/mL scandium standard solution and 1000 mug/mL yttrium standard solution to 10 mug/mL, taking the standard solution and the yttrium standard solution as main selection and alternative internal standard stock solution, sealing the stock solution and keeping the stock solution in a dark place for 6 months; according to the sequence of the standard series solution concentration from low to high, the solution is atomized and introduced into an ICP-AES instrument, the spectral line intensity ratio of the aluminum element and the main internal standard element or the alternative internal standard element is measured, and a calibration curve is drawn by taking the concentration of the element to be measured as an abscissa and the intensity ratio as an ordinate.
  2. 2. The method for measuring aluminum in aluminum iron by ICP-AES according to claim 1, wherein the sample is accurate to 0.0002g.
  3. 3. The method for determining aluminum in aluminum iron by ICP-AES according to claim 1, wherein the volume ratio of the mixed acid is hydrochloric acid, nitric acid and water=1+1+3.
  4. 4. The method for measuring aluminum in aluminum iron by ICP-AES according to claim 1, wherein scandium is the main internal standard element, the atomization energy of scandium is close to that of aluminum, the chemical property of scandium is stable, no interference exists in the aluminum iron matrix, matrix effect and instrument drift can be effectively corrected, no special instrument function is needed, and the method is preferential.
  5. 5. The method for measuring aluminum in aluminum iron by ICP-AES (inductively coupled plasma-atomic emission spectrometry) according to claim 1, wherein the alternative internal standard element is yttrium, has stable chemical property and small spectral line interference with aluminum element, can be used instead when scandium internal standard reagent is not easy to obtain or special interference exists on a matrix, and ensures the flexibility and applicability of the method.
  6. 6. The method for determining aluminum in aluminum iron by ICP-AES according to claim 4, wherein the linear correlation coefficient R2 is not less than 0.999.
  7. 7. The method for determining aluminum in aluminum iron by ICP-AES according to claim 4, wherein the scandium as the main component is subjected to ultra-high precision detection, and the relative error is within + -0.07%.

Description

Method for measuring aluminum in aluminum iron by ICP-AES Technical Field The invention belongs to the technical field of metallurgical analysis, is particularly suitable for accurately and rapidly detecting 10.00% -60.00% aluminum iron, and can be widely applied to quality control of steelmaking raw materials, research and development of metallurgical products and conventional analysis of third-party detection mechanisms. Background The aluminum iron is used as an indispensable key deoxidizer and alloy additive in the steelmaking process, and the aluminum content directly determines the deoxidizing efficiency and molten steel cleanliness in the steelmaking process, so that the mechanical properties (such as strength and toughness), the processing properties (such as weldability and plasticity) and the corrosion resistance of the final steel are affected. In the production of high-end steel (such as high-strength structural steel, steel for precision machinery and steel for ocean engineering), the aluminum content needs to be strictly controlled in a specific interval, namely, the aluminum content is too low, so that incomplete deoxidization is caused, the oxygen content in molten steel is over-standard, oxide inclusion is formed, and the steel has the defects of increased brittleness, hot working cracking and the like if the oxygen content is too high, so that accurate and rapid aluminum content detection is a core link for guaranteeing the steel production stability and the steel quality. The current industry mainly adopts an EDTA titration method specified by YB/T4393-2014 standard to measure the aluminum content in aluminum iron, the method realizes quantitative analysis through chemical titration reaction, but has obvious technical limitations that the operation flow is complicated, the sample is required to be dissolved, interference ions are masked, pH value is regulated and the like, the single analysis period is as long as 2-4 hours, the quick response requirement of a steelmaking process on raw material detection is difficult to meet, the titration process depends on a manual judgment terminal point and is easily influenced by experience of operators, matrix elements such as iron, manganese and the like can interfere, the detection relative error is often more than 5%, and the high-precision requirement of high-end steel production cannot be adapted. However, the existing ICP-AES technology still has application blank in aluminum content detection of aluminum iron for steelmaking, no ICP-AES detection standard aiming at aluminum content in aluminum iron exists in the current industry standard, only an ICP detection method of aluminum iron reported by an article cannot be reproduced, and only instrument analysis standards focus on secondary elements such as calcium, magnesium and the like, so that the detection requirement of main parameters of aluminum content cannot be met. Therefore, the ICP-AES detection method which is adaptive to the characteristics of the aluminum-iron matrix for steelmaking and has the advantages of accuracy and high efficiency is developed, the problems of complicated operation, insufficient precision and limited application of the traditional chemical method and the existing instrument method are solved, and the urgent need for guaranteeing the quality control of steelmaking raw materials is met. Based on the current situation, the invention provides a method for measuring aluminum in aluminum iron by ICP-AES. Disclosure of Invention Aiming at the defects of the existing detection method, the invention aims to provide the method for determining aluminum in aluminum iron by ICP-AES, which has the advantages of simple operation, rapid detection, high accuracy, strong anti-interference capability and no special requirement on instruments, and the method is characterized in that a double internal standard correction system is constructed by introducing scandium (Sc) which is a main internal standard element and yttrium (Y) which is an alternative internal standard element, so that the problem of matrix effect under high aluminum content is solved, the accurate detection within the content range of 10.00% -60.00% is realized, the requirements of rapid quality control in steelmaking production and high precision in high-end steel production are met, and the application scene and flexibility of the method are widened. In order to solve the technical problems, the invention adopts the following technical scheme: The invention discloses a method for measuring aluminum in aluminum iron by ICP-AES, which comprises the following steps: And weighing 0.1000g of aluminum iron sample, wherein the sampling quantity can balance the detection sensitivity and the matrix concentration, so that the interference caused by the over-high matrix concentration due to over-sampling is avoided. Placing a sample in a 300 mL beaker, adding 20mL mixed acid, heating at low temperature until the sample is