Preparation method of high-temperature alloy direct-reading spectrum quality control sample

Abstract

The invention discloses a preparation method of a high-temperature alloy direct-reading spectrum quality control sample. The preparation method comprises the following steps: S1, sample pretreatment; s2, preparing a sample; s3, grouping the samples; dividing the sample solutions into two groups, and respectively detecting the sample solutions by adopting a direct-reading spectrometry and an ICP (Inductively Coupled Plasma) test method; s4, detection and spectral analysis; and S5, setting quality control sample data. Existence and concentration of elements in a sample are obtained under the cooperation of a direct-reading spectrometry and an ICP test method, and standard deviation and uncertainty data of the quality control sample can be set more accurately, so that the high-precision quality control sample is obtained, the property and concentration of an actual sample can be reflected more accurately, the accuracy and reliability of an analysis result are ensured, and the accuracy and reliability of the analysis result are improved. And the performance and stability of the analysis system are effectively evaluated, a laboratory and a factory are helped to monitor the analysis process in real time, and potential problems are found and corrected in time.

Description

Technical Field

[0001] The invention belongs to the technical field of alloy quality control sample preparation, and in particular relates to a method for preparing a high-temperature alloy direct-reading spectrum quality control sample. Background Art

[0002] Quality control samples, also known as reference samples or standard samples, are samples used to test and verify the accuracy and reliability of the analytical process. In analytical laboratories and industrial production, the use of quality control samples is one of the key steps to ensure product quality and the credibility of analytical results. It can ensure the stability and reliability of the analytical process in analytical laboratories and industrial production, improve product quality and ensure compliance with various standards and regulatory requirements.

[0003] In the direct reading analysis method, the closer the alloying element content of the standard sample is to the alloying element content of the sample to be tested, the more accurate the test result will be. In order to use the direct reading analysis method to determine the ideal result, it is necessary to prepare the same brand of quality control samples to verify the linearity of the standardized working curve drawn by multiple standard samples. However, the prepared quality control samples will have low accuracy due to the quality and accuracy of the raw materials, which will affect the misleading analysis results and lead to the failure of quality control. Summary of the invention

[0004] The present invention aims at the problem that the quality control samples prepared in the prior art due to the quality and accuracy of raw materials may affect the misleading analysis results and lead to quality control failure, and proposes the following technical solutions: A method for preparing a high-temperature alloy direct-reading spectrum quality control sample comprises the following steps: S1. Sample pretreatment; After grinding the selected alloy material to remove the surface oxide layer thereof, a block alloy material is obtained at multiple points on the grinding surface of the alloy material, and then the block alloy material is ground into powder; S2, sample preparation; The alloy material is added into an acid solution to prepare an acid-dissolved sample, and the sample is diluted and stirred and divided into a plurality of sample solutions in equal proportions; S3, sample grouping; The sample solutions were divided into two groups, and the sample solutions were tested by direct reading spectroscopy and ICP testing respectively; S4, detection and spectral analysis; The sample solution is placed in a detection instrument, and the detection instrument is used to obtain the presence and concentration of different elements in the sample; S5. Set quality control sample data; After recording and summarizing the data from multiple sample dissolution tests, the standard deviation is set based on a measure of the average distance of the measured values ​​from their mean for the two measurement methods, and the uncertainty is set based on a measure of the estimated error range of the measurement results.

[0005] As a preferred embodiment of the above technical solution, the step S1 further includes cleaning the powdered alloy material; S1a, placing the alloy powder in an ultrasonic cleaner, adding a cleaning agent, and removing tiny contaminants from the surface of the alloy powder by ultrasonic oscillation; S1b, properly drying the cleaned alloy powder to remove the residual solvent or moisture on the surface of the alloy powder; S1c, use a sieve of appropriate size to screen the alloy powder, screen out larger or unevenly ground particles and re-grind them, and after grinding, re-enter the powdered alloy material cleaning work; S1d: After screening out larger or unevenly ground particles, they enter S2.

[0006] As a preferred embodiment of the above technical solution, in the step S1d, after screening out larger or unevenly ground particles, the sieved alloy powder is not re-aggregated and weighed to ensure that the total weight of the alloy powder is the same as the total weight of the bulk alloy material.

[0007] As a preferred embodiment of the above technical solution, the step S1 also includes alloy material uniformity detection, using chemical composition analysis and electron probe analysis to analyze the alloy material sample to ensure the uniformity of the composition at different positions of the alloy material sample.

[0008] As a preferred embodiment of the above technical solution, in the S4 step, when the sample solution is detected by direct reading spectroscopy, light of a specific wavelength emitted by the light source passes through the sample and is absorbed or partially absorbed by the sample, and the presence and concentration of different elements in the sample are determined by measuring the intensity change of the light of the sample at the specific wavelength.

[0009] As a preferred embodiment of the above technical solution, in the S4 step, when the ICP test method is used to detect the sample solution, the sample solution is sprayed into a plasma generator and excited by the electric energy provided by a high-frequency power supply to form a high-temperature plasma. The sample atoms in the plasma are excited to a high energy level and then emit specific photons when returning to the ground state. The presence and concentration of different elements in the sample are determined by detecting and analyzing the photons emitted by the atoms.

[0010] As a preferred embodiment of the above technical solution, in the step S1, when grinding the alloy material, the surface of the alloy material is smoothed with fine sandpaper, and the surface is cleaned with anhydrous alcohol and then dried with hot air at 90°C to 95°C. As a preferred embodiment of the above technical solution, the alloy material is ground by abrasive dry grinding and mechanical processing, and abrasive dry grinding is: dry grinding with a rotary disc type spectral grinding machine or a sanding machine or a grinding wheel machine; The mechanical processing method is: use a lathe, milling machine or grinder to perform surface treatment, control the processing speed to achieve the required surface finish and prevent the sample from overheating and oxidation.

[0011] As a preferred embodiment of the above technical solution, in the step S3, the number of portions of the two groups of sample solutions is 6 to 8.

[0012] As a preferred embodiment of the above technical solution, in the step S2, the acid solution is a nitric acid solution or a hydrochloric acid solution, and the nitric acid solution or the hydrochloric acid solution is analytically pure.

[0013] As a preferred embodiment of the above technical solution, the alloy materials include the following nine alloy materials: GH536, GH4169G, GH706, GH2132, GH901, GH738, GH698, GH907, and GH625.

[0014] The beneficial effects of the present invention are: 1. The direct reading spectrometry and ICP test methods are used to obtain the presence and concentration of elements in the sample, which can more accurately set the standard deviation and uncertainty data of the quality control sample, thereby obtaining high-precision quality control samples, which can more accurately reflect the properties and concentration of the actual sample, ensure the accuracy and reliability of the analysis results, and effectively evaluate the performance and stability of the analysis system, helping laboratories and factories to monitor the analysis process in real time and promptly discover and correct potential problems; 2. Cleaning the powdered alloy material can prevent the contaminants generated by the lubricant itself from mixing with the alloy powder during grinding and affecting the purity of the alloy powder, thereby ensuring that the prepared sample solution does not contain other influencing factors and avoiding affecting the presence and concentration of elements in the sample. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 Shown is a flow chart of an embodiment. DETAILED DESCRIPTION

[0016] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments and the accompanying drawings of the specification.

[0017] Example Figure 1 A method for preparing a high-temperature alloy direct-reading spectroscopy quality control sample comprises the following steps: S1. Sample pretreatment; After grinding the selected alloy material to remove the surface oxide layer thereof, a block alloy material is obtained at multiple points on the grinding surface of the alloy material, and then the block alloy material is ground into powder; S2, sample preparation; The alloy material is added into an acid solution to prepare an acid-dissolved sample, and the sample is diluted and stirred and divided into a plurality of sample solutions in equal proportions; S3, sample grouping; The sample solutions were divided into two groups, and the sample solutions were tested by direct reading spectroscopy and ICP testing respectively; S4, detection and spectral analysis; The sample solution is placed in a detection instrument, and the detection instrument is used to obtain the presence and concentration of different elements in the sample; S5. Set quality control sample data; After recording and summarizing the data from multiple sample dissolution tests, the standard deviation is set based on a measure of the average distance of the measured values ​​from their mean for the two measurement methods, and the uncertainty is set based on a measure of the estimated error range of the measurement results.

[0018] The step S1 also includes cleaning the powdered alloy material; S1a, placing the alloy powder in an ultrasonic cleaner, adding a cleaning agent, and removing tiny contaminants from the surface of the alloy powder by ultrasonic oscillation; S1b, properly drying the cleaned alloy powder to remove the residual solvent or moisture on the surface of the alloy powder; S1c, use a sieve of appropriate size to screen the alloy powder, screen out larger or unevenly ground particles and re-grind them, and after grinding, re-enter the powdered alloy material cleaning work; S1d: After screening out larger or unevenly ground particles, they enter S2.

[0019] In the step S1d, after screening out larger or unevenly ground particles, the sieved alloy powder is re-collected and weighed to ensure that the total weight of the alloy powder is the same as the total weight of the bulk alloy material.

[0020] The step S1 also includes alloy material uniformity detection, which uses chemical composition analysis and electron probe analysis to analyze the alloy material sample to ensure the uniformity of the composition at different positions of the alloy material sample.

[0021] In step S4, when the sample solution is detected by direct reading spectroscopy, light of a specific wavelength emitted by a light source passes through the sample and is absorbed or partially absorbed by the sample. The presence and concentration of different elements in the sample are determined by measuring the intensity change of the light at the specific wavelength of the sample.

[0022] Direct reading spectroscopy is a spectral technique used to analyze and measure the concentration of specific elements in a sample. Its basic principle is to determine the presence and concentration of target elements in a sample by measuring the specific wavelength of light absorbed or emitted by the sample. Direct reading spectroscopy generally includes the following steps:

[0023] (1) Light source selection: Different types of light sources can be used for direct emission spectroscopy, such as xenon lamps, sodium lamps or LEDs, depending on the elements and wavelength range to be measured.

[0024] (2) Sample injection: Samples usually enter the analytical instrument in solid or liquid form.

[0025] For liquid samples, the sample can be directly introduced into the measurement chamber using the injection system.

[0026] For solid samples, it may be necessary to process them by dissolving or grinding them, and then the sample in solution or powder form enters the measurement chamber.

[0027] (3) Spectral measurement: Light of a specific wavelength emitted by the light source passes through the sample and is absorbed or partially absorbed by the sample.

[0028] By measuring the change in the intensity of light at a specific wavelength from the sample, the concentration of the target element in the sample can be inferred.

[0029] (4) Data processing and result output: The measured spectral data can be directly output as the concentration value of the target element after being processed by the instrument's internal processing and analysis software.

[0030] The accuracy and precision of measurements can usually be improved by calibration with a standard curve or by using an internal standard.

[0031] In the step S4, when the ICP test method is used to detect the sample solution, the sample solution is sprayed into a plasma generator and excited by the electric energy provided by a high-frequency power supply to form a high-temperature plasma. The sample atoms in the plasma are excited to a high energy level and then emit specific photons when returning to the ground state. The presence and concentration of different elements in the sample are determined by detecting and analyzing the photons emitted by the atoms.

[0032] ICP is a commonly used analytical technique for determining the element content in a sample. The ICP test method generally includes the following steps: (1) Sample preparation: The sample first needs to be properly pretreated to ensure accurate results when analyzed. Pretreatment may include steps such as dissolving the sample, diluting it, filtering it, etc.

[0033] (2) Loading samples: The processed sample solution is loaded into the sample injection system of the ICP instrument. An automatic injection system is usually used to ensure stability and accuracy.

[0034] (3) Plasma formation: The solution in the sample is sprayed into the plasma generator and excited by the electric energy provided by the high-frequency power supply to form a high-temperature plasma.

[0035] Plasma is generally formed by exciting an inert gas such as argon.

[0036] (4) Atomic emission: The sample atoms in the plasma are excited to high energy levels and then emit specific photons when they return to the ground state.

[0037] The wavelength and intensity of the photons are proportional to the type and concentration of elements in the sample.

[0038] (5) Spectral analysis: By detecting and analyzing the photons emitted by atoms through spectroscopic instruments, the presence and concentration of different elements in a sample can be determined.

[0039] Spectroscopic instruments typically include components such as gratings or interferometers to analyze different wavelengths of light.

[0040] (6) Data processing and result output: By comparing with standard samples, the concentration of each element in the sample can be calculated.

[0041] The results can be directly exported or interpreted and used after further data processing.

[0042] In the step S1, when grinding the alloy material, the surface of the alloy material is smoothed with fine sandpaper, and the surface is cleaned with anhydrous alcohol and then dried with hot air at 90°C to 95°C. The alloy material grinding method is abrasive dry grinding and mechanical processing method, and abrasive dry grinding is: dry grinding with a turntable spectrum grinder or a sand belt machine or a grinding wheel machine; The mechanical processing method is: use a lathe, milling machine or grinder to perform surface treatment, control the processing speed to achieve the required surface finish and prevent the sample from overheating and oxidation.

[0043] In the step S3, the two groups of sample solutions have 6 to 8 portions.

[0044] In the step S2, the acid solution is a nitric acid solution or a hydrochloric acid solution, and the nitric acid solution or the hydrochloric acid solution is analytically pure.

[0045] The alloy materials include the following nine alloy materials: GH536, GH4169G, GH706, GH2132, GH901, GH738, GH698, GH907, and GH625.

[0046] Table 1 GH536 test results (%) Table 2 GH4169G test results (%) Table 3 GH706 test results (%) Table 4 GH2132 test results (%) Table 5 GH901 test results (%) Table 6 GH738 test results (%) Table 7 GH4698 test results (%) Table 8 GH907 test results (%) Table 9 GH625 test results (%) ICP test methods can be divided into different categories according to their application, sample status and test purpose: 1. Atomic absorption spectroscopy. It realizes new instrumental analysis and is an important method for quantitative elemental analysis of inorganic compounds. This test method has high accuracy, good sensitivity, and rapid analysis results. After the sample is made into a solution, a large number of correction solutions are made to correctly analyze the elements. We record the values ​​of the standard sample and the blank sample in turn, draw a calibration curve, and then determine the corresponding value of the sample to obtain the accurate concentration value of the sample.

[0047] 2. Atomic fluorescence method. Atomic vapor produces fluorescence of a certain emission intensity at a certain frequency, which can be used to determine the element to be measured. It includes atomic absorption and atomic emission analysis. It is not only simple in principle, but also highly accurate. It eliminates the disturbance of spectral line cleaning and has high accuracy.

[0048] 3. Visible spectrophotometry. Usually, the color developer and heavy metals produce complex reactions to produce colored molecular clusters, and the sample solution concentration and color depth undergo various changes. At the set wavelength, we perform colorimetric tests. The color developer achieves advance extraction processing and colorimetric testing, etc.

[0049] In the present technical solution, visible spectrophotometry is not the preferred method for directly measuring the content of metal elements in metal alloys. Visible spectrophotometry is suitable for compounds or solutions with strong colors or obvious absorption characteristics. Metal alloys usually do not have obvious visible light absorption characteristics, and their wavelength range is generally between 400 and 800 nanometers. For metal elements, their absorption usually occurs in the shorter wavelength range of ultraviolet or visible light, which exceeds the wavelength range of visible spectrophotometry. Therefore, atomic absorption spectroscopy and atomic fluorescence spectrometry can be used to detect the alloy to be tested.

[0050] When the ICP test method adopts atomic absorption spectroscopy, the principle of atomic absorption spectroscopy is: Atomization: The metallic elements in the sample are first converted into a gaseous atomic state, usually by a flame or electrothermal atomizer.

[0051] Spectroscopic analysis: A light source with a specific wavelength (such as a holmium lamp or a lanthanum lamp) is used to emit light, and the metal atoms in the sample absorb the light of a specific wavelength. The concentration of the metal element in the sample is determined by measuring the intensity of the absorbed light.

[0052] The basic steps of atomic absorption spectroscopy include: (1) Sample preparation: Samples often need to be dissolved into liquid form for easy injection and analysis. Pretreatment steps may include dissolution, dilution and filtration.

[0053] (2) Set the light source: A light source of a specific wavelength is used, usually generated by a hollow cathode lamp (HCL) in a spectrometer.

[0054] Each metal element has its own specific absorption wavelength, so the corresponding HCL needs to be selected to match the metal element to be measured.

[0055] (3) Sample injection: The treated sample solution enters the spectrometer through the injection system. An automatic injection system can be used to ensure stable and accurate injection volume.

[0056] (4) Spectral measurement: After light from the HCL is absorbed by the sample, the spectrometer measures the light intensity of the sample at the absorbed wavelength.

[0057] The metal atoms in the sample absorb light of a specific wavelength, and the amount absorbed is proportional to the concentration of the metal element.

[0058] (5) Data processing and result output: By comparing with a standard curve or a standard solution of known concentration, the concentration of the metal element in the sample can be calculated.

[0059] Results are usually output in concentration units (such as ppm or mg / L).

[0060] When the ICP test method adopts the atomic fluorescence method, the principle of the atomic fluorescence method is: Atomization: The metallic elements in the sample are first converted into a gaseous atomic state, usually by a flame or electrothermal atomizer.

[0061] Excitation and emission: Use an excitation light source to excite the metal atoms in the sample. After absorbing photons, the metal atoms will emit a specific fluorescence spectrum. The concentration of the metal element in the sample is determined by measuring the intensity of the fluorescence spectrum.

[0062] The basic steps of atomic fluorescence spectroscopy include: (1) Sample preparation and injection Sample preparation: Depending on the analysis requirements, the sample is prepared into a form suitable for analysis, which can be solution, gas or solid.

[0063] Injection system: The sample is introduced into the instrument through an automatic sampler or a manual injection system.

[0064] (2) Atomization Atomization method: The sample enters the atomization device. Commonly used atomization methods include electrothermal atomization, flame atomization, chemical evaporation, etc.

[0065] Purpose: To convert the target elements in the sample into free atomic states for subsequent fluorescence measurement.

[0066] (3) Fluorescence measurement Light source: A light source with a specific wavelength (such as a xenon or mercury lamp) is used to excite the free atoms in the sample.

[0067] Fluorescence detector: detects and records the fluorescence signals emitted by free atoms during electron transitions.

[0068] Fluorescence signal acquisition: collect the intensity and characteristic wavelength of the fluorescence signal.

[0069] (4) Data processing and analysis Standard curve or internal standard method: calibrate and calculate the concentration of the target element in the sample by comparing with a standard solution of known concentration or using an internal standard substance.

[0070] Result output: Calculate the concentration of target elements in the sample and generate an analysis report or record data.

[0071] The above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit them.

Claims

1. A method for preparing a high-temperature alloy direct-reading spectrum quality control sample, characterized in that: The following steps are involved: S1. Sample pretreatment; After grinding the selected alloy material to remove the surface oxide layer thereof, a block alloy material is obtained at multiple points on the grinding surface of the alloy material, and then the block alloy material is ground into powder; S2, sample preparation; The alloy material is added into an acid solution to prepare an acid-dissolved sample, and the sample is diluted and stirred and divided into a plurality of sample solutions in equal proportions; S3, sample grouping; The sample solutions were divided into two groups, and the sample solutions were tested by direct reading spectroscopy and ICP testing respectively; S4, detection and spectral analysis; The sample solution is placed in a detection instrument, and the detection instrument is used to obtain the presence and concentration of different elements in the sample; S5. Set quality control sample data; After recording and summarizing the data from multiple sample dissolution tests, the standard deviation is set based on a measure of the average distance of the measured values ​​from their mean for the two measurement methods, and the uncertainty is set based on a measure of the estimated error range of the measurement results.

2. The method for preparing a high-temperature alloy direct-reading spectrum quality control sample according to claim 1, characterized in that: The step S1 also includes cleaning the powdered alloy material; S1a, placing the alloy powder in an ultrasonic cleaner, adding a cleaning agent, and removing tiny contaminants from the surface of the alloy powder by ultrasonic oscillation; S1b, properly drying the cleaned alloy powder to remove the residual solvent or moisture on the surface of the alloy powder; S1c, use a sieve of appropriate size to screen the alloy powder, screen out larger or unevenly ground particles and re-grind them, and after grinding, re-enter the powdered alloy material cleaning work; S1d: After screening out larger or unevenly ground particles, they enter S2.

3. The method for preparing a high-temperature alloy direct-reading spectrum quality control sample according to claim 1, characterized in that: In the step S1d, after screening out larger or unevenly ground particles, the sieved alloy powder is re-collected and weighed to ensure that the total weight of the alloy powder is the same as the total weight of the bulk alloy material.

4. The method for preparing a high-temperature alloy direct-reading spectrum quality control sample according to claim 1, characterized in that: The step S1 also includes alloy material uniformity detection, which uses chemical composition analysis and electron probe analysis to analyze the alloy material sample to ensure the uniformity of the composition at different positions of the alloy material sample.

5. The method for preparing a high-temperature alloy direct-reading spectrum quality control sample according to claim 1, characterized in that: In step S4, when the sample solution is detected by direct reading spectroscopy, light of a specific wavelength emitted by a light source passes through the sample and is absorbed or partially absorbed by the sample. The presence and concentration of different elements in the sample are determined by measuring the intensity change of the light at the specific wavelength of the sample.

6. The method for preparing a high-temperature alloy direct-reading spectrum quality control sample according to claim 1, characterized in that: In the step S4, when the ICP test method is used to detect the sample solution, the sample solution is sprayed into a plasma generator and excited by the electric energy provided by a high-frequency power supply to form a high-temperature plasma. The sample atoms in the plasma are excited to a high energy level and then emit specific photons when returning to the ground state. The presence and concentration of different elements in the sample are determined by detecting and analyzing the photons emitted by the atoms.

7. The method for preparing a high-temperature alloy direct-reading spectrum quality control sample according to claim 1, characterized in that: In the step S1, when grinding the alloy material, the surface of the alloy material is ground with fine sandpaper to make it smooth, and the surface is cleaned with anhydrous alcohol and then dried with hot air at 90° C. to 95° C.

8. The method for preparing a high-temperature alloy direct-reading spectrum quality control sample according to claim 7, characterized in that: The alloy material grinding method is abrasive dry grinding and mechanical processing method, and abrasive dry grinding is: dry grinding with a turntable spectrum grinder or a sand belt machine or a grinding wheel machine; The mechanical processing method is: use a lathe, milling machine or grinder to perform surface treatment, control the processing speed to achieve the required surface finish and prevent the sample from overheating and oxidation.

9. The method for preparing a high-temperature alloy direct-reading spectrum quality control sample according to claim 1, characterized in that: In the step S3, the two groups of sample solutions have 6 to 8 portions.

10. The method for preparing a high-temperature alloy direct-reading spectrum quality control sample according to claim 1, characterized in that: In the step S2, the acid solution is a nitric acid solution or a hydrochloric acid solution, and the nitric acid solution or the hydrochloric acid solution is analytically pure.

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