Method for testing content of multiple elements in corrosion-resistant boron carbide reinforced aluminum-based composite material

Abstract

The invention provides a method for testing the content of multiple elements in a corrosion-resistant boron carbide reinforced aluminum-based composite material. The method comprises the following steps: S1, preparing a to-be-tested sample; s2, setting working parameters of the inductively coupled plasma emission spectrometer; s3, system blank test: preparing a blank standard solution, and testing under the instrument parameters in S2; s4, instrument calibration: preparing a multi-element calibration solution, testing under the parameters of the instrument in S2, and obtaining a calibration curve of each element in combination with a test result in S3; and S5, determining the content of multiple elements in a to-be-detected sample: preparing a to-be-detected solution, testing under the parameters of the instrument in S2, and calculating the mass fraction of each to-be-detected element in the sample by combining the calibration curve of each element in S4. According to the method, test results of multiple elements are obtained through one-time analysis, and the problems that a detection method in the prior art is long in detection time, high in reagent consumption and large in error interference are solved.

Description

Technical Field

[0001] The present invention relates to the technical field of chemical analysis of metal materials, in particular to a method for testing the content of multiple elements in a corrosion-resistant boron carbide reinforced aluminum-based composite material. Background Art

[0002] Boron carbide-reinforced aluminum-matrix composites (BCMs) have broad application prospects in aerospace, automotive, and defense due to their excellent mechanical properties, wear resistance, and high-temperature resistance. However, since the material's properties are closely related to its composition, testing for multiple elements is crucial. Due to the complex nature of BCMs, testing methods for their performance are still underdeveloped.

[0003] JB / T7993-2012, "Chemical Analysis Methods for Boron Carbide," uses spectrophotometry, which yields relatively reliable results. However, the color development conditions and the accuracy and precision of the test results are easily affected by ambient temperature and solution pH. YS / T423-2000, "Chemical Analysis Methods for Nuclear-Grade Boron Carbide Powder," fails to consider matrix interference with aluminum alloys and its impact on the precision and accuracy of test results, making it unsuitable for the chemical analysis of boron carbide-reinforced composite aluminum-based alloys. GB / T20975.25-2020, "Chemical Analysis Methods for Aluminum and Aluminum Alloys," uses inductively coupled plasma atomic emission spectrometry to determine multiple elements in aluminum and aluminum alloys. However, this standard is only applicable to the testing of multiple elements in aluminum and aluminum alloys.

[0004] Chinese patent CN109738419A discloses a method for determining the boron content in aluminum-based boron carbide materials. The method comprises the following steps: 1) adding an excess amount of acid to the aluminum-based boron carbide material, dissolving it completely, filtering it, collecting the filter membrane and insoluble matter, and ashing the residue; adding a basic carbonate to the residue, melting it, and then dissolving it in an excess amount of acid to obtain a test solution; preparing a series of aluminum-containing standard working solutions with increasing boron content; 2) subjecting the series of aluminum-containing standard working solutions to inductively coupled plasma optical emission spectroscopy analysis and plotting a working curve; performing inductively coupled plasma optical emission spectroscopy on the test solution, substituting the analysis results into the working curve, calculating the boron content in the test solution, and then converting it to obtain the boron content in the aluminum-based boron carbide material. This patent is complex in sample preparation and cannot provide test results for multiple elements in a single analysis.

[0005] It can be seen that a method for testing the multi-element content in corrosion-resistant boron carbide reinforced aluminum matrix composites is needed to meet the actual needs of testing boron carbide reinforced aluminum matrix composites. Summary of the Invention

[0006] The present invention aims to provide a method for testing the multi-element content of corrosion-resistant boron carbide reinforced aluminum-based composites. This method uses inductively coupled plasma optical emission spectrometry to simply, quickly, and accurately determine the multi-element content of corrosion-resistant boron carbide reinforced aluminum-based composites. This method provides test results for multiple elements in a single analysis, addressing the issues of existing detection methods, such as long detection times, high reagent consumption, and significant error and interference.

[0007] To achieve the above objectives, the present invention provides a method for testing the multi-element content in corrosion-resistant boron carbide reinforced aluminum-based composite materials. The technical solution of the present invention is implemented as follows:

[0008] A method for testing the content of multiple elements in a corrosion-resistant boron carbide reinforced aluminum-based composite material, the testing method comprising the following steps:

[0009] S1, prepare the sample to be tested;

[0010] S2, setting the working parameters of the inductively coupled plasma optical emission spectrometer;

[0011] S3, system blank test: prepare blank standard solution and test under the instrument parameter settings of S2;

[0012] S4, instrument calibration: prepare multi-element calibration solutions, perform tests under the instrument parameter settings of S2, and combine the test results of S3 to obtain the calibration curves of each element;

[0013] S5, determination of multi-element content in the sample to be tested: prepare the test solution, perform the test under the instrument parameter settings of S2, and calculate the mass fraction of each element to be tested in the sample in combination with the calibration curve of each element in S4.

[0014] The above steps can be used to test the content of multiple elements in the corrosion-resistant boron carbide reinforced aluminum-based composite material in one operation.

[0015] Furthermore, the sample preparation method of the test method is as follows: the sample and sodium peroxide are melted at high temperature, taken out and soaked in water, and acid is added to dissolve to obtain the test solution. The sample preparation method is simple, fast and accurate.

[0016] Furthermore, in the sample preparation method, the acids added during dissolution are nitric acid and hydrochloric acid. This operation enables the sample to be completely dissolved without the need for other steps such as filtering the residue.

[0017] Furthermore, in the sample preparation method, the high-temperature melting furnace temperature is 600-1000° C., and the burning time is 0.5-2 hours, to ensure sufficient oxidation reaction.

[0018] Furthermore, the S2 inductively coupled plasma optical emission spectrometer's analytical spectral line settings include at least one of: Fe (259.940 nm), Mn (257.610 nm), Zn (206.200 nm), Cr (267.716 nm), Cu (327.395 nm), Si (288.158 nm), Ti (337.280 nm), Mg (280.270 nm), and B (249.772 nm). Using these spectral lines ensures the absence of spectral interference from coexisting components, high signal intensity, and no signal peak saturation, resulting in more accurate testing.

[0019] Furthermore, the radio frequency power of the S2 inductively coupled plasma optical emission spectrometer is set to 1.1-1.2 kW to maintain a high signal-to-noise ratio for the test, thereby improving the precision and accuracy of the test.

[0020] Furthermore, the nebulizing gas flow rate of the S2 inductively coupled plasma optical emission spectrometer is set to 0.65-0.75 L / min to improve the precision and accuracy of the test.

[0021] Furthermore, the radial observation height of the S2 inductively coupled plasma optical emission spectrometer is set to 6-8 mm to improve the precision and accuracy of the test.

[0022] Furthermore, the plasma gas flow rate of the S2 inductively coupled plasma optical emission spectrometer is set to 10.0-12.0 L / min to improve the precision and accuracy of the test.

[0023] Furthermore, in S4, corresponding multiple standard substances are set when preparing the multi-element calibration solution to ensure the accuracy, repeatability and comparability of the test results.

[0024] Compared with the prior art, the method for testing the multi-element content in a corrosion-resistant boron carbide reinforced aluminum-based composite material described in the present invention has the following advantages:

[0025] 1. The present invention has few sample preparation steps and is simple to operate; the determination method is fast, and the single analysis time is less than 1 minute.

[0026] 2. The present invention can obtain the test results of nine elements, including Fe, Mn, Zn, Cr, Cu, Si, Ti, Mg, and B, through one analysis, which greatly improves the test efficiency and is more conducive to the quality control of corrosion-resistant boron carbide reinforced aluminum-based composite materials.

[0027] 3. The detection limit of the present invention is low and the precision is high, and the carbon content of the boron carbide reinforced aluminum-based composite material, especially the Fe, Mn, Zn, Cr, Cu, Si, Ti, Mg, and B contents, can be accurately detected.

[0028] 4. The present invention combines specific embodiments to provide the effects of working parameters such as RF power, atomizing gas flow, observation height, and plasma gas on multi-element determination results, and performs a comprehensive analysis for each element to be measured to obtain the optimal spectrum line. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 This is a diagram showing the influence of the instrument parameters on the spectral intensity described in Example 1 of the present invention;

[0030] Figure 2 This is a diagram showing the influence of the instrument parameters on the signal-to-noise ratio described in Example 1 of the present invention. DETAILED DESCRIPTION

[0031] A method for testing the content of multiple elements in a corrosion-resistant boron carbide reinforced aluminum-based composite material comprises the following steps:

[0032] S1, prepare the sample to be tested.

[0033] The sample can be made by drilling, milling, planing, sawing, turning or shearing. The sample chips should be in the form of thin strips (length ≤ 5mm, thickness ≤ 1mm), as small and uniform as possible, free of grease, oxidation, paper scraps and other foreign matter. The mass of each sample should be no less than 10g, and the sample to be tested is obtained;

[0034] S2, set the operating parameters of the inductively coupled plasma optical emission spectrometer.

[0035] The operating parameters of the inductively coupled plasma optical emission spectrometer were set as follows: RF power of 1.15 kW; nebulizer gas flow rate of 0.7 L / min; observation height of 7 mm; plasma gas flow rate of 11.0 L / min; carrier gas of argon; pump speed of 12 rpm; stabilization time of 10 s; read time of 6 s; lift delay of 20 s; radial observation mode; repetition number of 3 times; and calibration method of fitting. This improves the precision and accuracy of the test.

[0036] The analytical spectral lines include at least one of: Fe (259.940 nm), Mn (257.610 nm), Zn (206.200 nm), Cr (267.716 nm), Cu (327.395 nm), Si (288.158 nm), Ti (337.280 nm), Mg (280.270 nm), and B (249.772 nm). Using these spectral lines ensures the absence of spectral interference from coexisting components, high signal intensity, and no signal peak saturation, resulting in more accurate testing.

[0037] S3, system blank test: prepare blank standard solution and perform the test under the instrument parameter settings of S2.

[0038] Take a nickel crucible, weigh sodium peroxide and place it on the bottom of the nickel crucible, then weigh high-purity aluminum (accurate to 0.0001g) and place it on the sodium peroxide, and then cover the high-purity aluminum with a certain amount of sodium peroxide.

[0039] Place the nickel crucible in a high-temperature furnace at 600-1000°C and heat until melted for 0.5-2 hours. Preferably, the furnace temperature is 800°C and the heating time is 1 hour to ensure a sufficient oxidation reaction.

[0040] Remove the nickel crucible and allow it to cool to room temperature. Transfer the nickel crucible to a polytetrafluoroethylene beaker, add water, and heat and soak it on a hot plate. Preferably, the heating temperature is 200°C and the soaking time is 0.5 hours.

[0041] Wash out the nickel crucible, add nitric acid and hydrochloric acid, and slowly heat on a hot plate until the solution is clear. Preferably, the ratio of nitric acid to hydrochloric acid is 4:1. This procedure allows the sample to be completely dissolved, eliminating the need for additional steps such as filtering the residue.

[0042] Remove the polytetrafluoroethylene beaker, cool to room temperature, transfer to a 250 mL plastic volumetric flask, make up to volume, and shake well to serve as the blank standard solution.

[0043] The test was performed under the S2 instrument parameter settings.

[0044] S4, instrument calibration: prepare multi-element calibration solution, perform the test under the instrument parameter settings of S2, and combine the test results of S3 to obtain the calibration curve of each element.

[0045] Take 7 nickel crucibles, weigh sodium peroxide and place it on the bottom of the nickel crucible, then weigh 22#, 30#, 31#, 33#, 34#, 52#, and 62# standard substances (accurate to 0.0001g) and place them on the sodium peroxide, and then cover the standard substances with a certain amount of sodium peroxide.

[0046] Take three nickel crucibles, weigh sodium peroxide and place it on the bottom of the nickel crucible, then weigh high-purity aluminum (accurate to 0.0001g) and place it on the sodium peroxide, and then cover the high-purity aluminum with a certain amount of sodium peroxide.

[0047] Place 10 nickel crucibles in a high-temperature furnace and burn them at 600-1000°C until they are melted for 0.5-2 hours. Preferably, the furnace temperature is 800°C and the burning time is 1 hour.

[0048] Remove the nickel crucible and allow it to cool to room temperature. Transfer each nickel crucible to a polytetrafluoroethylene beaker, add water, and heat on a hot plate to soak. Preferably, the heating temperature is 200°C and the soaking time is 0.5 hours.

[0049] Wash out the nickel crucible, add nitric acid and hydrochloric acid, and place it on a hot plate to slowly heat until the solution is clear. Preferably, the ratio of nitric acid to hydrochloric acid is 4:1.

[0050] Remove the Teflon beakers and cool to room temperature. Transfer the seven standard substance Teflon beakers to a 250mL plastic volumetric flask, bring to volume, and shake well. Add the single-standard solutions of zinc, copper, and boron from the three high-purity aluminum Teflon beakers, transfer them to a 250mL plastic volumetric flask, bring to volume, and shake well. Ten calibration solutions are prepared, as shown in Table 1. When preparing multi-element calibration solutions, specify the appropriate number of standard substances to ensure the accuracy, repeatability, and comparability of test results.

[0051]

[0052] The test was performed under the S2 instrument parameter settings, and the calibration curves of each element were obtained by combining the S3 test results.

[0053] S5, determination of multi-element content in the sample to be tested: prepare the test solution, perform the test under the instrument parameter settings of S2, and calculate the mass fraction of each element to be tested in the sample in combination with the calibration curve of each element in S4.

[0054] Take two nickel crucibles, weigh sodium peroxide and place it on the bottom of the nickel crucible, then weigh the sample (accurate to 0.0001g) and place it on the sodium peroxide, and then cover the sample with a certain amount of sodium peroxide.

[0055] Place the nickel crucible in a high-temperature furnace at 600-1000°C and burn until it melts for 0.5-2 hours. Preferably, the furnace temperature is 800°C and the burning time is 1 hour.

[0056] Remove the nickel crucible and allow it to cool to room temperature. Transfer the nickel crucible to a polytetrafluoroethylene beaker, add water, and heat and soak it on a hot plate. Preferably, the heating temperature is 200°C and the soaking time is 0.5 hours.

[0057] Wash out the nickel crucible, add nitric acid and hydrochloric acid, and place it on a hot plate and slowly heat until the solution is clear. Preferably, the ratio of nitric acid to hydrochloric acid is 4:1.

[0058] Remove the polytetrafluoroethylene beaker, cool to room temperature, transfer to a 250 mL plastic volumetric flask, make up to volume, and shake well to prepare the test solution.

[0059] Two dissolved samples were tested under the instrument parameters set in S2. The mass fraction of each element in the sample was calculated using the calibration curves of each element in S4. The final result was obtained by averaging the two test results.

[0060] The above steps can be used to test the content of multiple elements in the corrosion-resistant boron carbide reinforced aluminum-based composite material in one operation.

[0061] The sample preparation method of the test method is as follows: the sample is melted with sodium peroxide at high temperature, taken out and soaked in water, and then dissolved with acid to obtain the test solution. The sample preparation method is simple, fast and accurate.

[0062] To make the purpose, technical solutions and advantages of the present invention more clear, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the embodiments described are part of the embodiments of the present invention, rather than all of the embodiments. The specific embodiments described herein are merely for explaining the present invention and are not intended to limit the present invention. It should be noted that, unless there is a conflict, the features in the embodiments and embodiments of the present invention may be combined with each other.

[0063] Example 1

[0064] The instruments used in the determination method of the present invention include: an inductively coupled plasma emission spectrometer and an analytical balance.

[0065] Reagents and consumables used include: pure argon (φ(Ar) ≥ 99.99%), hydrochloric acid (ρ = 1.18 g / mL, premium grade), nitric acid (ρ = 1.42 g / mL, premium grade), sodium peroxide (content ≥ 92.5%, analytical grade), zinc stock solution, copper stock solution, and boron stock solution. Water used in the experiments was grade-A water.

[0066] S1, prepare the sample to be tested

[0067] The sample can be made by drilling, milling, planing, sawing, turning or shearing. The sample chips should be in the form of thin strips (length ≤ 5mm, thickness ≤ 1mm), as small and uniform as possible, free of grease, oxidation, paper scraps and other foreign matter. The mass of each sample should be no less than 10g, and the sample to be tested is obtained;

[0068] S2, set the working parameters of the inductively coupled plasma optical emission spectrometer

[0069] The operating parameter settings of the inductively coupled plasma optical emission spectrometer include: RF power of 1.15 kW; nebulizer gas flow rate of 0.7 L / min; observation height of 7 mm; plasma gas flow rate of 11.0 L / min; carrier gas of argon; pump speed of 12 r / min; stabilization time of 10 s; reading time of 6 s; lifting delay of 20 s; observation mode of radial observation; number of repetitions of 3 times; and calibration method of fitting.

[0070] The analysis lines include: Fe at 259.940 nm, Mn at 257.610 nm, Zn at 206.200 nm, Cr at 267.716 nm, Cu at 327.395 nm, Si at 288.158 nm, Ti at 337.280 nm, Mg at 280.270 nm, and B at 249.772 nm.

[0071] S3, system blank test:

[0072] Take a nickel crucible, weigh 1g of sodium peroxide and place it at the bottom of the nickel crucible, then weigh 0.1g of high-purity aluminum (accurate to 0.0001g) and place it on the sodium peroxide, and then cover the high-purity aluminum with 1g of sodium peroxide. Place the nickel crucible in a high-temperature furnace and burn it at 800℃ until it melts for 1 hour. Take out the nickel crucible and let it cool to room temperature. Transfer the nickel crucible to a polytetrafluoroethylene beaker, add water, and heat it on a hot plate to soak. The heating temperature is 200℃ and the soaking time is 0.5h. Wash out the nickel crucible, add 20mL of nitric acid and 5mL of hydrochloric acid, place it on a hot plate and heat slowly until the solution is clear. Remove the polytetrafluoroethylene beaker, cool to room temperature, transfer it to a 250mL plastic volumetric flask, make up the volume, and shake well to serve as a blank standard solution.

[0073] S4, Instrument Calibration:

[0074] Take seven nickel crucibles and weigh 1g of sodium peroxide onto the bottom of each crucible. Then, weigh 0.1g of standard materials #22, #30, #31, #33, #34, #52, and #62 (accurate to 0.0001g) and place them on top of the sodium peroxide. Cover the standard materials with 1g of sodium peroxide. Take three nickel crucibles and weigh 1g of sodium peroxide onto the bottom of each crucible. Then, weigh 0.1g of high-purity aluminum (accurate to 0.0001g) and place it on top of the sodium peroxide. Cover the high-purity aluminum with 1g of sodium peroxide. Heat each nickel crucible in a high-temperature furnace at 800°C for 1 hour until melted. Remove the crucibles and allow them to cool to room temperature. Transfer each crucible to a Teflon beaker, add water, and heat on a hot plate to soak. The heating temperature is 200°C and the soaking time is 0.5 hours. Wash out the nickel crucible, add 20mL of nitric acid and 5mL of hydrochloric acid, place it on a hot plate and heat slowly until the solution is clear. Remove the polytetrafluoroethylene beaker and cool it to room temperature. Transfer the 7 standard substance polytetrafluoroethylene beakers to a 250mL plastic volumetric flask, make up the volume and shake well; add single standard solutions of zinc, copper and boron elements to the 3 high-purity aluminum polytetrafluoroethylene beakers, transfer them to a 250mL plastic volumetric flask, make up the volume and shake well. 10 calibration solutions are prepared. Test under the S2 instrument parameter settings, and combine the S3 test results to obtain the calibration curve of each element.

[0075] S5, determination of multi-element content in the sample to be tested:

[0076] Take two nickel crucibles and weigh 1g of sodium peroxide into each crucible, placing it at the bottom. Then weigh (0.100±0.001)g of sample (accurate to 0.0001g) and place it on top of the sodium peroxide. Cover the sample with 1g of sodium peroxide. Heat the nickel crucible in a high-temperature furnace at 800°C for 1 hour until melted. Remove the crucible and allow it to cool to room temperature. Transfer the crucible to a polytetrafluoroethylene beaker, add water, and heat on a hot plate to soak the solution at 200°C for 0.5 hours. Rinse the crucible, add 20mL of nitric acid and 5mL of hydrochloric acid, and slowly heat on a hot plate until the solution is clear. Remove the polytetrafluoroethylene beaker, cool to room temperature, and transfer the sample to a 250mL plastic volumetric flask, bringing it to volume for analysis. Two dissolved samples were tested using the instrument's S2 settings. The mass fraction of each element in the sample was calculated using the calibration curves for each element in S4. The final result is obtained by taking the average of the two test results.

[0077] In order to further optimize the working parameter settings of the test method of the present invention, the method of controlling a single variable was adopted to investigate the effects of RF power, atomizing gas flow rate, observation height and plasma gas on the element determination results. Taking standard solution 31# as an example, the relationship between the above parameters and spectral intensity and signal-to-noise ratio was obtained. The results are as follows Figure 1 and Figure 2 shown.

[0078] The increase of RF power increases the excitation energy, which promotes the ionization of the solution to be tested, but also increases the background interference, which can easily cause the signal-to-noise ratio to decrease. Figure 1 (A) and Figure 2 (A) It can be seen that RF power has a significant impact on spectral intensity and signal-to-noise ratio. As RF power increases, the spectral intensity of each element increases approximately linearly, while the signal-to-noise ratio decreases. The RF power is set to 1.1-1.2 kW, and preferably, 1.15 kW.

[0079] The size of the atomizing gas flow rate will affect the amount of solution lifting, the level of atomization efficiency and the size of the droplet diameter. Increasing the atomizing gas flow rate will lead to excessive dilution of the sample in the channel, a reduction in the plasma residence time and a decrease in the temperature of the channel center, resulting in a decrease in spectral intensity. Figure 1 (B) and Figure 2 (B) As can be seen, increasing the nebulizer gas flow rate reduces the spectral intensity of each element, while increasing the background noise, leading to an increase in the signal-to-noise ratio. The nebulizer gas flow rate is set to 0.65-0.75 L / min, and preferably, the nebulizer gas flow rate is 0.7 L / min.

[0080] The radial observation height has a significant effect on the spectral intensity but a weaker effect on the signal-to-noise ratio. Figure 1 (C) and Figure 2(C) It can be seen that as the radial observation height increases, the spectral intensity of each element decreases. The radial observation height is set to 6-8 mm, and preferably, the radial observation height is 7 mm.

[0081] The plasma gas flow rate has a weak effect on the spectral intensity and signal-to-noise ratio. Figure 1 (D) and Figure 2 (D) It can be seen that as the radial observation height of the plasma gas flow increases, the spectral intensity and signal-to-noise ratio do not change much. The plasma gas flow rate is set to 10.0~12.0L / min, and preferably, the plasma gas flow rate is 11.0L / min.

[0082] Interference effects in inductively coupled plasma atomic emission spectrometry primarily include spectral interference and physical interference. Selecting appropriate analytical lines is an important method for reducing spectral overlap interference. For each analyte, the top three spectral lines recommended by the instrument are listed in Table 2 below.

[0083]

[0084] According to the information provided in the table, spectral lines are selected based on the principle of no spectral interference from coexisting components, high signal intensity values, and no signal peak saturation.

[0085] Comprehensive analysis of the spectral lines of each element is as follows: Fe is 259.940nm, Mn is 257.610nm, Zn is 206.200nm, Cr is 267.716nm, Cu is 327.395nm, Si is 288.158nm, Ti is 327.280nm, Mg is 280.270nm, and B is 249.772nm.

[0086] A series of calibration solutions were measured according to the experimental method, and calibration curves were plotted with spectral intensity (I / cps) as the ordinate and mass fraction (w / %) as the abscissa. The fitting equations and correlation coefficients are shown in Table 3 below. The blank solution was measured 10 times in parallel according to the experimental method, and the detection limit and quantification limit were calculated using 3 times and 10 times the blank standard deviation, respectively. The results are shown in Table 3 below.

[0087]

[0088] The spike recovery test was carried out according to the experimental method. The results are shown in Table 4 below. The recovery rates ranged from 92.3% to 120%.

[0089]

[0090] Actual samples were measured according to the experimental method, and the results are shown in Table 5. The relative standard deviations (RSD, n=6) of the actual sample measurement results were no more than 5%, indicating that the method has good accuracy and precision.

[0091]

[0092] The present invention provides a method for determining the contents of iron, manganese, zinc, chromium, copper, silicon, titanium, magnesium and boron in a corrosion-resistant boron carbide reinforced aluminum-based composite material by inductively coupled plasma optical emission spectrometry. By examining the effects of radio frequency power, atomizing gas flow rate, plasma gas flow rate and observation height on spectral intensity and signal-to-noise ratio, the preferred operating parameters of the inductively coupled plasma optical emission spectrometer are determined.

[0093] It has been verified that the linear correlation coefficients of the calibration curves of all elements are greater than 0.999, the element quantification limit is low, the relative standard deviation (n=6) of the actual sample measurement results is no more than 5%, and the spiked recovery rate is 92.3~120%. It is accurate, reliable, precise and practical.

[0094] The determination method is fast, with a single analysis time of less than 1 minute. It is easy to operate and can realize simultaneous testing of multiple elements, providing a fast and accurate inspection method for quality control of the multi-element content of boron carbide reinforced aluminum-based composites.

[0095] Although the present invention is disclosed as above, the present invention is not limited thereto. Any person skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention should be based on the scope defined by the claims.

Claims

1. A method for testing the content of multiple elements in corrosion-resistant boron carbide reinforced aluminum-based composite materials, characterized in that: The test method comprises the following steps: S1, prepare the sample to be tested; S2, setting the working parameters of the inductively coupled plasma optical emission spectrometer; S3, system blank test: prepare blank standard solution and test under the instrument parameter settings of S2; S4, instrument calibration: prepare multi-element calibration solutions, perform tests under the instrument parameter settings of S2, and combine the test results of S3 to obtain the calibration curves of each element; S5, determination of multi-element content in the sample to be tested: prepare the test solution, perform the test under the instrument parameter settings of S2, and calculate the mass fraction of each element to be tested in the sample in combination with the calibration curve of each element in S4.

2. The testing method according to claim 1, wherein: The sample preparation method of the test method is: melting the sample and sodium peroxide at high temperature, taking out and soaking the sample in water, and adding acid to dissolve the sample to obtain a solution to be tested.

3. The testing method according to claim 2, wherein: In the sample dissolution preparation method, the acids added during dissolution are nitric acid and hydrochloric acid.

4. The testing method according to claim 2, wherein: In the sample preparation method, the high-temperature melting furnace temperature is 600-1000° C., and the burning time is 0.5-2 h.

5. The testing method according to claim 1, wherein: The analysis line setting of the S2 inductively coupled plasma optical emission spectrometer includes at least one of: Fe is 259.940 nm, Mn is 257.610 nm, Zn is 206.200 nm, Cr is 267.716 nm, Cu is 327.395 nm, Si is 288.158 nm, Ti is 337.280 nm, Mg is 280.270 nm and B is 249.772 nm.

6. The testing method according to claim 1, wherein: The radio frequency power of the S2 inductively coupled plasma emission spectrometer is set to 1.1-1.2 kW.

7. The testing method according to claim 1, wherein: The nebulizing gas flow rate of the S2 inductively coupled plasma optical emission spectrometer was set to 0.65-0.75 L / min.

8. The testing method according to claim 1, wherein: The radial observation height of the S2 inductively coupled plasma optical emission spectrometer is set to 6-8 mm.

9. The testing method according to claim 1, wherein: The plasma gas flow rate of the S2 inductively coupled plasma emission spectrometer was set to 10.0-12.0 L / min.

10. The testing method according to claim 1, wherein: In S4, corresponding multiple standard substances are set when preparing the multi-element calibration solution.

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