Method for measuring content of aluminum in aluminum-iron alloy by using X-ray fluorescence energy disperse spectroscopy
The determination of aluminum content in aluminum-iron alloys by X-ray fluorescence spectrometry solves the problems of time-consuming and polluting chemical analysis, and realizes rapid, accurate and environmentally friendly aluminum content detection.
Patent Information
- Application Number
- CN202511490011.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-17
- Publication Date
- 2026-01-16
AI Technical Summary
Existing chemical analysis methods for aluminum-iron alloys are time-consuming, resource-intensive, and cause serious environmental pollution, making rapid and accurate detection impossible.
The method for determining the aluminum content in aluminum-iron alloys using X-ray fluorescence spectrometry includes sample preparation, powder sample pressing, plotting of working curves, and determination of the fluorescence excitation energy intensity of aluminum using X-ray fluorescence spectrometry. The aluminum content is then calculated using mathematical formulas.
It achieves rapid and accurate aluminum content detection with a short detection cycle, no human error, no material consumption, environmental friendliness and safety, and a wide range of applications.
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Figure CN121347569A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of metallurgical analysis and testing technology, specifically relating to a method for determining the aluminum content in aluminum-iron alloys using X-ray fluorescence spectrometry. Background Technology
[0002] Ferroalloys are an extremely important raw material for steelmaking, playing a role in deoxidation and adding necessary components, and directly affecting the quality of steel. However, ferroalloys present the biggest challenge in chemical analysis, as the analysis time is extremely long (generally more than 5 hours), wasting manpower, material resources and financial resources, and requiring the use of large amounts of chemicals, causing environmental pollution.
[0003] X-ray fluorescence spectrometry (XRF) is a physical analysis instrument that can analyze powder directly from ground powder tablets without the need for chemical reagents. It features one-time calibration and long-term use and is currently widely used in the analysis of steel, ferroalloy and other industries. It has the advantages of fast analysis speed (simultaneous analysis of the target element in the material in 2-5 minutes), short detection cycle, high accuracy and no human error. In addition, XRF spectrometry has no material consumption, is simple to operate, has no pollutant emissions, is environmentally friendly and safe, and can be inspected in time, which facilitates production guidance. Its technical advantages are obvious. Summary of the Invention
[0004] To address the shortcomings of existing chemical analysis methods for aluminum-iron alloys, such as excessively long analysis times (over 5 hours), wasted manpower, material resources, and financial resources, excessive use of chemicals, and environmental pollution, this invention aims to provide a method for determining the aluminum content in aluminum-iron alloys using X-ray fluorescence spectrometry. This method enables rapid, stable, and accurate detection of the aluminum content in aluminum-iron alloys, achieving the effects of short detection cycle, no human error, no material consumption, simple operation, no pollutant emissions, and environmental safety.
[0005] To achieve the above-mentioned objective, this invention provides a method for determining the aluminum content in aluminum-iron alloys using X-ray fluorescence spectrometry, the method comprising the following steps:
[0006] S1 Sample Preparation
[0007] Clean the sample bowl containing the sample with the test sample to be prepared;
[0008] The test sample with a particle size of less than 1 mm to be prepared is loaded into a ceramic crucible with a volume of 30 mL, and the loading amount is 90% to 100%.
[0009] Place the test sample from the grinding mortar into the grinder, add 7-9 drops of anhydrous ethanol, grind for 70-90 seconds, then remove and bag.
[0010] S2 powder sample tableting
[0011] Clean the sample press and all sample pressing molds. According to the specifications of the sample press, place the feeder in the sample pressing groove. The feeder is a concentric circular sleeve. Place the test sample into the inner cylinder of the feeder.
[0012] Hold the leveling device in your hand, and after the bottom plane of the leveling device contacts the surface of the test sample in the inner cylinder of the feeder, gently rotate the leveling device to make the test sample flat, and then remove the leveling device.
[0013] Place boric acid on the surface of the test sample in the inner cylinder of the feeder, then evenly sprinkle boric acid into the outer cylinder of the feeder. Gently lift the feeder vertically and remove it vertically from the pressing tank. During the removal process, confirm that the sample does not stick to the feeder. Sweep the boric acid from the edge of the feeder and around the base of the pressing machine into the pressing tank. The boric acid purity is analytical grade, and the amount of boric acid added is 6-9g.
[0014] According to the specifications of the sample press, place the top seat on top of the test sample in the sample press chamber and confirm that it is level;
[0015] When using a sample press, ensure that boric acid is evenly covered on the surface of the test sample, and remove the sample after pressing.
[0016] S3 plots the working curve and obtains the calculation formula.
[0017] A standard sample with a known aluminum content in an aluminum-iron alloy is selected, pressed, and placed in an X-ray fluorescence spectrometer. The X-ray fluorescence excitation energy conditions of the aluminum composition in the standard sample are set on the X-ray fluorescence spectrometer. The sample is then irradiated with X-rays to obtain the intensity of the fluorescence excitation energy generated by the aluminum element.
[0018] The X-ray fluorescence spectrometer was set to the following excitation conditions: X-ray tube voltage 45V, tube current 5mA, and detection time 1800s. The aluminum-iron alloy standard sample used to plot the working curve had an aluminum content of 39.55%–46.09%.
[0019] Based on a series of standard samples with determined aluminum content and their corresponding fluorescence excitation energies, a mathematical relationship curve between the fluorescence excitation energy intensity of aluminum in aluminum-iron alloys and the aluminum content was plotted using an X-ray fluorescence spectrometer. Based on the mathematical relationship curve, a mathematical formula for the relationship between the intensity and percentage content of aluminum in aluminum-iron alloys was obtained.
[0020] Based on the fluorescence energy intensity of aluminum in the standard sample detected by X-ray fluorescence spectrometry, the mathematical formula for the percentage content of aluminum in the aluminum-iron alloy sample is obtained:
[0021] y = b + a*x
[0022] Where y is the mass percentage of aluminum in the sample, x is the intensity of aluminum in the sample obtained in X-ray fluorescence spectrometry, a is the slope of the working curve, and b is the intercept of the working curve.
[0023] S4 uses an X-ray fluorescence spectrometer to determine the intensity of the fluorescence excitation energy generated by aluminum in the aluminum-iron alloy sample, and calculates the mass percentage of aluminum in the aluminum-iron alloy using the mathematical formula.
[0024] The X-ray fluorescence intensity of aluminum is related to its content. The content of an unknown sample is determined by comparing the measured intensity with the X-ray fluorescence intensity of the same element and spectral line in a standard substance. The experimental conditions for the X-ray fluorescence spectrometer are identical for both the test sample and the standard sample. The pressed sample is placed in the X-ray fluorescence spectrometer, and the sample is irradiated with X-rays under the X-ray fluorescence excitation and detection conditions set on the spectrometer. The intensity of aluminum in the aluminum-iron alloy is obtained by measuring the fluorescence excitation energy generated by aluminum in the sample irradiated by X-rays within the spectrometer. The detected aluminum excitation energy intensity value is then substituted into the mathematical formula for the aluminum intensity and percentage content of the aluminum-iron alloy standard sample to obtain the mass percentage content of aluminum in the aluminum-iron alloy.
[0025] S5 Result Verification: Take more than 20 batches of aluminum-iron alloy samples and use the X-ray fluorescence spectrometer method of this invention to determine the aluminum content in the aluminum-iron alloy, and the traditional chemical analysis method (EDTA titration method) to detect the Al content respectively. Then, analyze and verify the detection data obtained by the two detection methods.
[0026] S6 Data Analysis: By statistically analyzing the "difference" and "allowable error" of the detection data obtained by the two different methods, it is determined whether the accuracy of the method of the present invention meets the requirements; the t-test method is used to determine whether there is a significant difference between the method of the present invention and the chemical analysis method.
[0027] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0028] This invention overcomes the technical defects of traditional wet chemical analysis methods, such as complex analysis process, cumbersome steps, time-consuming process, and high labor intensity. It greatly reduces analysis time and labor intensity, and has the advantages of short detection cycle, high accuracy, no human error, no material consumption, simple operation, no pollutant emission, environmental safety, and wide applicability. Attached Figure Description
[0029] Figure 1 This is a schematic diagram of the inspection process for a method of determining the aluminum content in aluminum-iron alloys using X-ray fluorescence spectrometry according to the present invention.
[0030] Figure 2This is a comparative analysis trend chart of the aluminum content detection results in the aluminum-iron alloy of Example 1. Detailed Implementation
[0031] The present invention will be further described below with reference to specific embodiments, but this does not limit the invention in any way. To avoid redundancy, unless otherwise specified, the raw materials used in the following embodiments are all commercially available products, and the methods used are all conventional methods unless otherwise specified.
[0032] A method for determining the aluminum content in aluminum-iron alloys using X-ray fluorescence spectrometry includes the following steps:
[0033] S1 Sample preparation: The test sample with a particle size of less than 1 mm to be prepared is loaded into a ceramic crucible with a volume of 30 mL, and the loading amount is 90% to 100%.
[0034] Place the test sample from the grinding mortar into the grinder, add 7-9 drops of anhydrous ethanol, grind for 70-90 seconds, then remove and bag.
[0035] S2 Powder Sample Compression: A sample press is used to compress the sample. Boric acid is placed in the inner cylinder of the feeder to cover the surface of the test sample. After the sample is compressed, the sample tablet is removed.
[0036] Plot the working curve using S3 to obtain the calculation formula:
[0037] Based on the fluorescence energy intensity of aluminum in the standard sample detected by X-ray fluorescence spectrometry, the mathematical formula for the percentage content of aluminum in the sample is obtained:
[0038] y = b + a*x
[0039] Where y is the mass percentage of aluminum in the sample, x is the intensity of aluminum in the sample obtained in X-ray fluorescence spectrometry, a is the slope of the working curve, and b is the intercept of the working curve.
[0040] S4 uses an X-ray fluorescence spectrometer to determine the intensity of the fluorescence excitation energy generated by aluminum in the aluminum-iron alloy sample, and calculates the mass percentage content of aluminum using the mathematical formula.
[0041] S5 Result Verification;
[0042] S6 data analysis.
[0043] A schematic diagram of the testing procedure for determining the aluminum content in aluminum-iron alloys using X-ray fluorescence spectrometry, as shown below. Figure 1As shown: First, a powder sample pellet preparation experiment is conducted to ensure the pellet is flat, crack-free, and has sufficient strength to prevent breakage. The sample preparation process should meet the requirement of stable excitation intensity of aluminum in the aluminum-iron alloy. If unstable, the sample preparation method needs to be re-explored. Stable excitation intensity of aluminum indicates the feasibility of the sample preparation method. Then, a working curve is plotted using aluminum-iron alloy samples with varying gradients to obtain the calculation formula. The aluminum detection results in the samples with established working curves should not exceed the standard value. If they do, the working curve should be re-plotted. Finally, more than 20 groups of aluminum-iron alloy samples are tested to verify the results and perform data analysis. If the method meets the accuracy requirements and shows no significant difference from the chemical analysis method, it can be applied to routine aluminum-iron detection; otherwise, the cause needs to be investigated in the sample preparation process.
[0044] The X-ray fluorescence spectrometer used in the examples is a CIT-3000SMD(D) X-ray fluorescence spectrometer manufactured by Sichuan Xinxianda Measurement and Control Technology Co., Ltd., with a measurement range of 0.001% to 99.99% and an energy resolution of better than 127 eV.
[0045] Any aspects not described in the following embodiments are the same as those described in the specific embodiments above.
[0046] Example 1
[0047] A method for determining the aluminum content in aluminum-iron alloys using X-ray fluorescence spectrometry includes the following steps:
[0048] S1 Sample preparation: The test sample with a particle size of less than 1 mm to be prepared is loaded into a ceramic crucible with a volume of 30 mL, and the loading amount is 95%.
[0049] Place the test sample from the grinding mortar into the grinder, add 8 drops of anhydrous ethanol, grind for 80 seconds, and then remove and bag it.
[0050] S2 Powder Sample Compression: The sample is compressed using a sample press. 8g of analytical grade boric acid is placed in the inner cylinder of the feeder to cover the surface of the test sample with boric acid. After the sample is compressed, the sample tablet is removed.
[0051] Plot the working curve using S3 to obtain the calculation formula:
[0052] Based on the fluorescence energy intensity of aluminum in the standard sample detected by X-ray fluorescence spectrometry, the mathematical formula for the percentage content of aluminum in the sample is obtained:
[0053] y = b + a*x
[0054] Where y is the mass percentage of aluminum in the sample, x is the intensity of aluminum in the sample obtained in X-ray fluorescence spectrometry; b is the intercept of the working curve, which is calculated to be 3.295352; a is the slope of the working curve, which is calculated to be 15.0595053; the calculation formula is: y = 3.295352 + 15.0595053 * x.
[0055] S4 uses an X-ray fluorescence spectrometer to determine the intensity of the fluorescence excitation energy generated by aluminum in the aluminum-iron alloy sample, and calculates the mass percentage of aluminum in the aluminum-iron alloy using the mathematical formula.
[0056] S5 Result Verification: 22 batches of aluminum-iron alloy samples were taken, and the aluminum content in the aluminum-iron alloy was determined by an X-ray fluorescence spectrometer according to the present invention. The Al content was detected by the traditional chemical analysis method (EDTA titration method). The comparison and analysis results of the Al content detection results of the aluminum-iron alloy obtained by the two detection methods are shown in Table 1.
[0057] Table 1 Comparative Analysis of Al Content Detection Results in Aluminum-Iron Alloys
[0058] serial number Chemical analysis results (%) X-ray fluorescence spectrometry pellet analysis results (%) Difference (%) Permissible error (%) 240108-089 45.87 45.75 0.12 0.60 240112-127 45.39 45.24 0.15 0.60 240115-153 45.93 45.73 0.2 0.60 240125-062 45.33 45.56 -0.23 0.60 240125-138 45.66 45.71 -0.05 0.60 240203-060 45.03 45.24 -0.21 0.60 240214-065 45.08 45.42 -0.34 0.60 240311-081 45.41 45.27 0.14 0.60 240402-043 45.52 45.65 -0.13 0.60 240402-147 45.46 45.66 -0.2 0.60 240423-133 45.51 45.71 -0.2 0.60 240430-065 45.51 45.44 0.07 0.60 240513-061 45.75 45.64 0.11 0.60 240531-129 45.21 45.16 0.05 0.60 240602-065 45.89 45.66 0.23 0.60 240614-133 45.57 45.42 0.15 0.60 240629-080 45.35 45.26 0.09 0.60 240711-136 45.39 45.58 -0.19 0.60 240729-122 45.41 45.34 0.07 0.60 240808-146 45.41 45.58 -0.17 0.60 240815-080 45.54 45.43 0.11 0.60 240825-077 45.67 45.54 0.13 0.60
[0059] S6 Data Analysis: Statistical analysis is performed on the "difference" and "allowable error" of detection data obtained from two different methods, such as... Figure 2 The comparative analysis trend chart of aluminum content detection results in aluminum-iron alloys shows that the differences in the comparative analysis results are all less than the allowable tolerance of 0.6%, indicating that the accuracy of the detection method meets the requirements; the test statistic t = 0.776 < t 0.975 =2.074, and there was no significant difference between the X-ray fluorescence spectrometry pellet method and the chemical analysis method in detecting the Al content of aluminum-iron alloys.
[0060] For anyone skilled in the art, many possible variations and modifications can be made to the technical solutions of this invention, or equivalent embodiments can be modified based on the disclosed technical content, without departing from the scope of the technical solutions of this invention. Therefore, any simple modifications, equivalent changes, and modifications made to the above embodiments based on the technical essence of this invention without departing from the content of the technical solutions of this invention should still fall within the protection scope of the technical solutions of this invention.
Claims
1. A method for determining the aluminum content in an aluminum-iron alloy by X-ray fluorescence spectrometry, characterized in that, The method comprises the following steps: S1 sample preparation: the test sample with a particle size less than 1 mm to be prepared is loaded into a ceramic crucible with a volume of 30 mL, and the loading amount is 90%-100%; The test sample in the grinding bowl is placed in the grinding machine, 7-9 drops of anhydrous ethanol are added, and the sample is taken out after grinding for 70-90 s and bagged; S2 powder sample tabletting: the sample is tabletted by using a sample pressing machine, boric acid is placed in the inner cylinder of the feeder so as to cover the surface of the test sample, and the tablet is taken out after tabletting is completed; S3 drawing of a working curve to obtain a calculation formula: According to the fluorescence energy intensity of the aluminum element in the standard sample obtained by the X-ray fluorescence spectrometer, a mathematical relationship formula of the percentage content of the aluminum element in the sample is obtained: y=b+a*x Wherein, y is the mass percentage content of aluminum in the sample, x is the intensity of the aluminum element obtained by the X-ray fluorescence spectrometer, a is the slope of the working curve, and b is the intercept of the working curve; S4 using the X-ray fluorescence spectrometer to measure the fluorescence excitation energy intensity of the aluminum element in the aluminum-iron alloy sample, and calculating the mass percentage content of the aluminum element by using the mathematical relationship formula; S5 result verification; S6 data analysis.
2. The method of claim 1, wherein, In step S2, the purity of boric acid is analytical pure, and the addition amount of boric acid is 6-9 g.
3. The method of claim 1, wherein, In step S3, the standard sample with a determined aluminum content in the aluminum-iron alloy is selected, and after tabletting, it is placed in the X-ray fluorescence spectrometer to obtain the fluorescence excitation energy intensity of the aluminum element.
4. The method of claim 1, wherein, In step S3, the X-ray fluorescence excitation conditions set by the X-ray fluorescence spectrometer are: X-ray tube pressure 45 V, tube flow 5 mA, and detection time 1800 s.
5. The method of claim 1, wherein, In step S3, the aluminum content of the aluminum-iron alloy standard sample used for drawing the working curve is 39.55%-46.09%.
6. The method of claim 1, wherein, In step S4, the test conditions of the X-ray fluorescence spectrometer for the test sample and the standard sample are the same.