Rapid sample dissolving method and all-element detection method of vanadium-titanium-chromium-manganese-iron quinary alloy

The vanadium titanium chromium ferromanganese five-member alloy was treated through microwave digestion and specific acid ratio, combined with ICP-AES, ICP-MS and chemical wet analysis, and the problems of incomplete dissolution and poor detection accuracy of vanadium titanium chromium ferromanganese five-member alloy were solved, achieving fast and accurate full-element detection.

CN120489702APending Publication Date: 2025-08-15CHENGDU ADVANCED METAL MATERIALS IND TECH RES INST CO LTD
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Patent Information

Application Number
CN202510698902.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-28
Publication Date
2025-08-15

AI Technical Summary

Technical Problem

The existing alloy element detection methods are incompletely dissolved in vanadium titanium chromium ferromanganese five-member alloys, are inefficient and are prone to introduce sulfuric acid or sodium salt interfering substances, resulting in poor detection accuracy and impaired instrument stability.

Method used

The microwave digestion method was used to treat vanadium, titanium, chromium, ferromanganese, five-member alloy samples of vanadium, titanium, chromium, manganese, and hydrogen peroxide in a microwave digestion instrument to avoid the introduction of sulfuric acid and a large amount of hydrofluoric acid, and conduct full-element detection in combination with ICP-AES, ICP-MS and chemical wet analysis.

Benefits of technology

The rapid dissolution and full element detection of vanadium titanium chromium ferromanganese five-member alloy are realized, ensuring the accuracy of the detection results and the stability of the instrument, and meeting the needs of rapid analysis.

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Abstract

The invention discloses a rapid sample dissolving method of a vanadium-titanium-chromium-manganese-iron quinary alloy and an all-element detection method of the vanadium-titanium-chromium-manganese-iron quinary alloy, and belongs to the field of alloy chemical component analysis and pretreatment. The rapid sample dissolving method comprises the following steps: weighing a vanadium-titanium-chromium-manganese-iron quinary alloy sample, putting the sample into a microwave digestion tank, and adding ultrapure water to wet the sample; the method comprises the following steps: respectively transferring hydrochloric acid, nitric acid and hydrofluoric acid into a microwave digestion tank, adding hydrogen peroxide when the reaction is no longer violent, then sealing the microwave digestion tank, putting the microwave digestion tank into a microwave digestion instrument, performing digestion according to set conditions, taking out the microwave digestion tank after digestion is completed, and cooling the microwave digestion tank to room temperature. Then, ICP-AES and ICP-MS are used for determining medium-content and low-content elements in the alloy, vanadium is determined through chemical wet analysis, and all-element detection is achieved. The method is simple to operate and rapid in digestion; the problems that when an existing alloy element detection method is applied to the vanadium-titanium-chromium-manganese-iron quinary alloy, dissolution is incomplete, the dissolution efficiency is low, and sulfuric acid or sodium salt interference substances are likely to be introduced can be effectively solved.
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Description

Technical Field

[0001] The present invention belongs to the technical field of alloy chemical composition analysis and pretreatment, and relates to the pretreatment process and analytical detection of multi-element alloys composed of refractory metals such as vanadium, titanium, chromium, manganese, and iron. In particular, it relates to a rapid sample dissolution method for a vanadium-titanium-chromium-manganese-iron five-element alloy and a full-element detection method thereof. Background Art

[0002] Vanadium-based hydrogen storage alloys have attracted much attention due to their high hydrogen storage performance at room temperature and at medium and low temperatures. Vanadium-titanium-chromium-manganese-iron quinary alloys, as intermediate alloys of vanadium-based hydrogen storage alloys, are widely used in the preparation of hydrogen storage materials. This type of alloy is mainly composed of vanadium and contains various proportions of elements such as titanium, chromium, iron, and manganese. For example, the quinary alloy of vanadium-titanium-chromium-manganese-iron generally contains 20% to 30% titanium, 20% to 30% chromium, 30% to 60% vanadium, 1% to 10% iron, and 3% to 7% manganese. In addition, to improve the oxidation resistance and mechanical properties of the alloy, some quinary alloys of vanadium-titanium-chromium-manganese-iron are doped with elements such as cerium, silicon, and aluminum to meet specific performance requirements. However, the complex composition system of the quinary alloy of vanadium-titanium-chromium-manganese-iron poses challenges to the accuracy and efficiency of chemical composition analysis. In particular, during sample pretreatment, conventional methods have difficulty in quickly dissolving these multi-element alloys and are prone to introducing interference factors, affecting subsequent element detection.

[0003] At present, there are no relevant testing standards, melting methods or literature reports for multi-element alloys containing refractory metals such as vanadium, titanium, chromium, manganese and iron. In the process of chemical pretreatment of alloys or multi-element alloys, acid dissolution, alkali dissolution, acid-base separation process or microwave digestion are mostly used. For example, "Determination of molybdenum content in molybdenum-iron alloy by microwave digestion-inductively coupled plasma atomic emission spectrometry" and "Determination of 7 trace elements in manganese-iron alloy by microwave digestion-flame atomic absorption spectrometry" provide effective methods for the detection of specific alloy elements. However, the vanadium-titanium-chromium-manganese-iron five-element alloy is composed of high contents of vanadium, chromium, titanium and other refractory elements. In the currently reported literature, the microwave digestion technology cannot completely dissolve the vanadium-titanium-chromium-manganese-iron five-element alloy.

[0004] In addition, the "Determination of 11 Elements in Vanadium-Chromium-Titanium Alloy by Inductively Coupled Plasma Atomic Emission Spectrometry" uses a specific mixed acid system to dissolve the sample, and the "Detection of Arsenic in Vanadium-Ferroalloy by Plasma Atomic Emission Spectrometry" uses a mixed acid system such as nitric acid and sulfuric acid to treat the sample by microwave digestion. However, these methods have significant defects when dealing with vanadium-titanium-chromium-manganese-iron five-element alloys. For example: (1) The acid dissolution method requires the use of a mixed system of nitric acid, hydrochloric acid, hydrofluoric acid, sulfuric acid, and boric acid. The melting time exceeds 6 hours, and about 10-15 mL of hydrofluoric acid needs to be added. During the low-temperature melting process, the acid will continue to volatilize, and the acid needs to be continuously replenished to maintain the reaction, which is inefficient. In addition, hydrofluoric acid easily reacts with silicon and cerium to generate volatile SiF4 gas or cerium fluoride precipitation, resulting in deviations in the determination of silicon and cerium content. The introduction of sulfuric acid will reduce the atomization efficiency, increase the detection blank value, and even clog the atomizer and the matrix tube.

[0005] (2) Although the alkali fusion method can dissolve the sample, the operation is cumbersome and it will also introduce high concentrations of sodium salts, which will increase the viscosity of the solution and cause the atomization system to be blocked. The spectral lines of sodium may overlap with the spectral lines of other elements (such as Al and Si), interfering with spectral detection. In mass spectrometry analysis, sodium will also form polyatomic ions with the background gas, causing interference with the mass-to-charge ratio detection of low-content elements (such as Ce).

[0006] (3) Although the mixed dissolution process (such as acid dissolution combined with alkaline dissolution) can improve the dissolution effect, the steps are cumbersome and time-consuming, and it is difficult to avoid the introduction of sodium salts or sulfuric acid, which does not meet the requirements of modern industry for high efficiency and environmental protection.

[0007] Therefore, it is urgent to develop a pretreatment method that can quickly dissolve vanadium-titanium-chromium-manganese-iron five-element alloy samples without the introduction of sulfuric acid or sodium salts and is suitable for the detection of all elements (including V, Cr, Ti, Fe, Mn, Al, Si, and Ce) to improve the efficiency and accuracy of hydrogen storage alloy composition analysis. Summary of the Invention

[0008] The technical problem to be solved by the present invention is that when the existing alloy element detection method is applied to the vanadium-titanium-chromium-manganese-iron five-element alloy, there are problems such as incomplete dissolution, low dissolution efficiency, and easy introduction of sulfuric acid, a large amount of hydrofluoric acid or sodium salt interfering substances during the sample pretreatment process, resulting in poor accuracy of full element detection and impaired instrument stability.

[0009] To achieve the above application objectives, the technical solutions adopted in this application are as follows: In a first aspect, the present invention provides a method for rapid sample dissolution of a vanadium-titanium-chromium-manganese-iron five-element alloy, comprising the following steps: S1. Weigh a vanadium-titanium-chromium-manganese-iron five-element alloy sample in a microwave digestion tank and add ultrapure water to wet the sample; S2. Separately transfer hydrochloric acid, nitric acid, and hydrofluoric acid into a microwave digestion vessel. When the reaction is no longer intense, add hydrogen peroxide. Seal the microwave digestion vessel and place it in a microwave digester. Perform digestion according to the set conditions. After digestion is complete, remove the microwave digestion vessel and cool it to room temperature.

[0010] The chemical elements contained in the above-mentioned vanadium-titanium-chromium-manganese-iron quinary alloy include V, Cr, Ti, Fe, Mn, Al, Si, and Ce.

[0011] In the above-mentioned rapid sample dissolution method, in step S1, the amount of the vanadium-titanium-chromium-manganese-iron quinary alloy added is 0.1-0.2 g, and the amount of ultrapure water added is 2-4 mL.

[0012] In the above-mentioned rapid sample dissolution method, in step S1, the microwave digestion tank needs to be cleaned before use. The specific method is: soak in dilute hydrochloric acid for 12h~24h, rinse with ultrapure water and dry, then add dilute aqua regia for pre-digestion for half an hour, and then rinse with ultrapure water and dry.

[0013] In the above-mentioned rapid sample dissolution method, in step S2, the amount of hydrochloric acid added is 2-4 mL, the amount of nitric acid added is 1-2 mL, the amount of hydrofluoric acid added is 0.1-0.5 mL, and the amount of hydrogen peroxide added is 1-3 mL.

[0014] In the above-mentioned rapid sample dissolution method, in step S2, the hydrochloric acid and nitric acid are of high purity, with mass concentrations of 36%-38% and 68%-70%, respectively; the mass concentration of hydrofluoric acid is 65%-68%; and the mass concentration of hydrogen peroxide is ≥30%.

[0015] In the above-mentioned rapid sample dissolution method, in step S2, after adding hydrogen peroxide, wait for 1 to 5 minutes before sealing the digestion tank.

[0016] In the above-mentioned rapid sample dissolution method, in step S2, the setting conditions are: heating to 60°C within 5 minutes and keeping warm for 5 minutes, then heating to 180°C within 10 minutes and keeping warm for 10 minutes, and finally heating to 220°C within 5 minutes and keeping warm for 30 minutes.

[0017] In the above-mentioned rapid sample dissolution method, in step S2, after digestion is completed, the microwave digestion vessel is taken out, cooled in cold water for more than 2 hours, rinsed with ultrapure water, and opened in a fume hood.

[0018] In a second aspect, the present invention provides a method for full-element detection of a vanadium-titanium-chromium-manganese-iron five-element alloy: according to the above-mentioned rapid sample dissolution method of the vanadium-titanium-chromium-manganese-iron five-element alloy, the vanadium-titanium-chromium-manganese-iron five-element alloy to be tested is dissolved and then transferred to a container to be fixed to obtain a solution to be tested; then ICP-AES, ICP-MS and chemical wet analysis are used to detect the element content in the solution to be tested.

[0019] In the above-mentioned full-element detection method, the vanadium-titanium-chromium-manganese-iron quinary alloy to be tested is dissolved and completely transferred into a 250 mL polytetrafluoroethylene beaker, and the volume is fixed in a 100 mL quartz beaker.

[0020] In the above-mentioned full-element detection method, ICP-AES is used to detect the contents of Cr, Ti, Al, Si, Fe, and Mn elements in the test solution, ICP-MS is used to detect the content of Ce element in the test solution, and chemical wet method is used to detect the content of V element in the test solution.

[0021] The beneficial effects of the present invention are as follows: after repeated tests, the present invention has determined the optimal ratio range of hydrochloric acid, nitric acid, hydrogen peroxide, and hydrofluoric acid. Under this ratio, the sample is processed by a microwave digester, and the sample can be quickly digested without the introduction of sulfuric acid and a large amount of hydrofluoric acid, thereby avoiding adverse effects on the ICP-MS and ICP-AES atomizers and rectangular tubes, and ensuring the accuracy of the silicon and cerium determination results. In practical applications, the method of the present invention is suitable for the pre-treatment of full-element detection in vanadium-titanium-chromium-manganese-iron five-element alloys, using ICP-AES and ICP-MS to determine the medium and low content elements in the alloy, and using chemical wet analysis to determine the high content of vanadium, thereby achieving full-element detection. The sample dissolution method of the present invention is simple to operate, has a fast digestion, can meet the needs of rapid analysis, and has high accuracy and good parallel linearity in the determination, and has good promotion and application value. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is the microwave digestion temperature and time curve in the rapid sample dissolution method of vanadium-titanium-chromium-manganese-iron five-element alloy; Figure 2 The comparative bar chart shows the recovery rate of Ti element in samples treated with different pretreatment methods; Figure 3 The bar chart is a comparison of the Si element recovery rates of samples treated with different pretreatment methods; Figure 4 The bar chart shows the comparison of Ce element recovery rates of samples treated with different pretreatment methods. DETAILED DESCRIPTION

[0023] In order to make the technical problems, technical solutions and beneficial effects to be solved by this application more clear, the application is further described in detail below in conjunction with the embodiments. Unless otherwise defined, all scientific and technical terms used herein have the same meanings as understood by ordinary technicians in this field.

[0024] The present invention discloses a rapid sample dissolution method for a vanadium-titanium-chromium-manganese-iron five-element alloy and a full-element detection method thereof, which specifically comprises the following steps: 1. Cleaning of microwave digestion tank: Soak in dilute hydrochloric acid for 12 hours, rinse several times with ultrapure water, dry, add dilute aqua regia to the digestion tank for pre-digestion for half an hour, open it in a fume hood after cooling, rinse several times with ultrapure water, and dry it.

[0025] 2. Sample weighing: Weigh 0.1~0.2g of vanadium-titanium-chromium-manganese-iron five-element alloy sample into a microwave digestion tank, and add 2~4mL of ultrapure water to wet the vanadium-titanium-chromium-manganese-iron five-element alloy sample.

[0026] 3. Add mixed acid: Pipette 2-4 mL of high-grade pure hydrochloric acid, 1-2 mL of high-grade pure nitric acid, and 0.1-0.5 mL of hydrofluoric acid into the microwave digestion tank. When the reaction is no longer violent, add 1-3 mL of hydrogen peroxide. Wait for 1-3 minutes, cover with a sealed lid, and place in the microwave digestion instrument.

[0027] 4. Program setting: Set the microwave digestion program as shown in Table 1. The microwave digestion temperature and time curve is as follows: Figure 1 As shown; start the instrument and perform microwave digestion. After digestion, take out the microwave digestion tank, cool it in cold water for more than 2 hours, rinse it with ultrapure water, and open it in a fume hood.

[0028] Table 1 Microwave digestion setting conditions 5. Dilute to volume: Transfer the dissolved test solution completely to a 250 mL polytetrafluoroethylene beaker and dilute to volume in a 100 mL quartz beaker to obtain the test solution.

[0029] 6. Determination: ICP-AES was used to detect the content of Cr, Ti, Al, Si, Fe, and Mn in the test solution. ICP-MS was used to detect the content of Ce in the test solution. The chemical wet method was used to detect the content of V in the test solution.

[0030] Specific examples will be listed below to explain the scheme of the present invention. Those skilled in the art will understand that the following examples are only used to illustrate the present invention and should not be considered as limiting the scope of the present invention. Where specific techniques or conditions are not specified in the examples, they are carried out according to the techniques or conditions described in the literature in this area or according to the product specifications. Where the manufacturer of the reagents or instruments is not specified, they are all conventional products that can be obtained commercially.

[0031] 1. Comparative test of different pretreatment methods Three samples were pretreated using traditional pretreatment methods (acid dissolution method, alkali fusion method, acid-alkali step method) and the method of the present invention, respectively.

[0032] 1. Experimental Methods (1) Alkali fusion method: Refer to the literature "Determination of chromium, iron, molybdenum and silicon in titanium-aluminum alloy by sodium peroxide alkali fusion-inductively coupled plasma optical emission spectrometry" for alkali fusion treatment.

[0033] (2) The acid dissolution method refers to the following steps: weigh 0.1 g of the sample (accurate to 0.0001 g) into a polytetrafluoroethylene beaker, add 2 to 4 mL of distilled water to rinse the sample and disperse it at the bottom of the polytetrafluoroethylene beaker, then add 10 to 15 mL of hydrofluoric acid, 10 mL of (1+1) sulfuric acid, and 10 to 15 mL of newly prepared aqua regia to dissolve the sample at low temperature. During the dissolution process, continuously add newly prepared aqua regia and distilled water until the sample is completely dissolved.

[0034] (3) Acid-base step method: weigh 0.1g of sample (accurate to 0.0001g) into a beaker, add 2~4mL of distilled water to rinse the sample and disperse it on the bottom of the beaker, add 10~15mL of freshly prepared aqua regia to dissolve the sample at low temperature, 5~8mL of (1+1) sulfuric acid, dissolve the sample until it no longer changes, rinse the bottle wall with a small amount of water, filter it with slow quantitative filter paper while it is hot, wash the residue with hot water, and collect the filtrate in a 200mL plastic volumetric flask. Place the residue together with the filter paper in a platinum crucible and perform alkali dissolution treatment according to the literature "Determination of impurity elements in vanadium-iron alloy by inductively coupled plasma atomic emission spectrometry".

[0035] 2. Result determination Ti, Si, and Ce were selected for determination and comparison, where the spike recovery rate = (measured value - true value) ÷ spike amount × 100%, as follows: (1) The Ti content in the sample was measured three times in parallel by ICP-AES. The detection line was 334.941 nm and the spike concentration was 10%. The average of the spike recovery rates of the three measurements was taken. The results are as follows: Figure 2 shown.

[0036] (2) The Si content in the sample was measured three times in parallel using ICP-AES. The detection line was 251.611 nm and the spike concentration was 50%. The average of the spike recovery rates of the three measurements was taken. The results are as follows: Figure 3 shown.

[0037] (3) When ICP-AES was used to determine the Ce content, iron (spectral line 535.337) and vanadium (535.341nm) in the sample would interfere with the 535.353nm spectral line. Therefore, ICP-MS was used to determine the Ce content in the sample. The mass number was 140, the spike concentration was 50%, and the average of the spike recovery rates of the three determinations was taken. The results are as follows: Figure 4 shown.

[0038] Experiments show that the recovery rates of Ti, Si and Ce tested by the method of the present invention are all between 97% and 104%, which meets the detection requirements.

[0039] 2. Full element detection of vanadium-titanium-chromium-manganese-iron five-element alloy Example 1: Three vanadium-titanium-chromium-manganese-iron five-element alloy samples were selected, and two portions of each were weighed for full element detection, as follows: (1) Cleaning of microwave digestion tank: Soak in dilute hydrochloric acid for 24 hours, rinse several times with ultrapure water, dry, add dilute aqua regia to the digestion tank for pre-digestion for half an hour, cool, open in a fume hood, rinse several times with ultrapure water, and dry.

[0040] (2) Sample weighing: Weigh 0.1 g (accurate to 0.0001 g) of the vanadium-titanium-chromium-manganese-iron quinary alloy sample on weighing paper, carefully transfer it into a microwave digestion tank, and add 2 mL of ultrapure water to moisten the sample.

[0041] (3) Adding mixed acid: Pipette 3 mL of high-grade pure hydrochloric acid, 1 mL of high-grade pure nitric acid, and 0.4 mL of hydrofluoric acid into the microwave digestion tank. When the reaction is no longer violent, add 2 mL of hydrogen peroxide. Wait for 5 minutes, cover with a sealed lid, and place in the microwave digestion instrument.

[0042] (4) Program setting: Set the microwave digestion program as shown in Table 1, start the instrument, and perform microwave digestion. After digestion, take out the microwave digestion tank, cool it in cold water for more than 2 hours, rinse it with ultrapure water, and open it in a fume hood.

[0043] (5) Adjust the volume: Transfer the dissolved test solution to a 250 mL polytetrafluoroethylene beaker, rinse the microwave digestion tank 3 to 5 times, transfer it to a 100 mL quartz volumetric flask, and adjust the volume.

[0044] (6) Detection: ICP-AES was used to detect the contents of Cr, Ti, Al, Si, Fe, and Mn. The element detection lines were 267.716 nm, 334.941 nm, 396.152 nm, 251.611 nm, 239.562 nm, and 257.610 nm, respectively. ICP-MS was used to detect the content of Ce, with a mass number of 140. Wet chemical analysis was used to detect the content of V. Standard solutions were added to the main elements at 10%, and to the remaining elements at 50%. Each sample was measured three times in parallel and the average value was taken. The recovery results are shown in Table 2.

[0045] Table 2 Spike recovery (%) Example 2: Three vanadium-titanium-chromium-manganese-iron five-element alloy samples were selected, and two portions of each were weighed for full element testing, as follows: (1) Cleaning of microwave digestion tank: Soak in dilute hydrochloric acid for 24 hours, rinse several times with ultrapure water, dry, add dilute aqua regia to the digestion tank for pre-digestion for half an hour, cool, open in a fume hood, rinse several times with ultrapure water, and dry.

[0046] (2) Sample weighing: Weigh 0.15 g (accurate to 0.0001 g) of the vanadium-titanium-chromium-manganese-iron quinary alloy sample on weighing paper, carefully transfer it into a microwave digestion tank, and add 2 mL of ultrapure water to moisten the sample.

[0047] (3) Adding mixed acid: Pipette 3 mL of high-grade pure hydrochloric acid, 1 mL of high-grade pure nitric acid, and 0.2 mL of hydrofluoric acid into the microwave digestion tank. When the reaction is no longer violent, add 2 mL of hydrogen peroxide. Wait for 5 minutes, cover with a sealed lid, and place in the microwave digestion instrument.

[0048] (4) Program setting: Set the microwave digestion program as shown in Table 1, start the instrument, and perform microwave digestion. After digestion, take out the microwave digestion tank, cool it in cold water for more than 2 hours, rinse it with ultrapure water, and open it in a fume hood.

[0049] (5) Adjust the volume: Transfer the dissolved test solution to a 250 mL polytetrafluoroethylene beaker, rinse the microwave digestion tank 3 to 5 times, transfer it to a 100 mL quartz volumetric flask, and adjust the volume.

[0050] (6) Detection: ICP-AES was used to detect the contents of Cr, Ti, Al, Si, Fe, and Mn. The element detection lines were 267.716 nm, 334.941 nm, 396.152 nm, 251.611 nm, 239.562 nm, and 257.610 nm, respectively. ICP-MS was used to detect the content of Ce, with a mass number of 140. Wet chemical analysis was used to detect the content of V. A 10% standard solution was added to the main elements, and a 50% standard solution was added to the remaining elements. Each sample was measured three times in parallel and the average value was taken. The recovery results are shown in Table 3.

[0051] Table 3 Spiked recovery (%) Experiments have shown that the pretreatment of the vanadium-titanium-chromium-manganese-iron quinary alloy using the present invention is simple and time-efficient, meeting the requirements of green and rapid analysis. The recovery rates of the elements tested using the present method range from 97% to 104%, meeting the requirements of analytical testing.

Claims

1. A rapid dissolution method for a vanadium-titanium-chromium-manganese-iron five-element alloy, characterized in that: The steps include: S1. Weigh a vanadium-titanium-chromium-manganese-iron five-element alloy sample in a microwave digestion tank and add ultrapure water to wet the sample; S2. Separately transfer hydrochloric acid, nitric acid, and hydrofluoric acid into a microwave digestion vessel. When the reaction is no longer intense, add hydrogen peroxide. Seal the microwave digestion vessel and place it in a microwave digester. Perform digestion according to the set conditions. After digestion is complete, remove the microwave digestion vessel and cool it to room temperature.

2. The rapid dissolution method of vanadium-titanium-chromium-manganese-iron five-element alloy according to claim 1, characterized in that: The chemical elements contained in the vanadium-titanium-chromium-manganese-iron quinary alloy include V, Cr, Ti, Fe, Mn, Al, Si, and Ce.

3. The rapid dissolution method of vanadium-titanium-chromium-manganese-iron five-element alloy according to claim 1, characterized in that: In step S1, the amount of the vanadium-titanium-chromium-manganese-iron quinary alloy added is 0.1-0.2 g, and the amount of ultrapure water added is 2-4 mL.

4. The rapid sample dissolution method of the vanadium-titanium-chromium-manganese-iron five-element alloy according to claim 1, characterized in that: In step S1, the microwave digestion tank needs to be cleaned before use. The specific method is: soak in dilute hydrochloric acid for 12 hours to 24 hours, clean with ultrapure water and dry, then add dilute aqua regia for pre-digestion for half an hour, and then clean with ultrapure water and dry.

5. The method for rapid sample dissolution of vanadium-titanium-chromium-manganese-iron quinary alloy according to claim 1, characterized in that: In step S2, the amount of hydrochloric acid added is 2-4 mL, the amount of nitric acid added is 1-2 mL, the amount of hydrofluoric acid added is 0.1-0.5 mL, and the amount of hydrogen peroxide added is 1-3 mL.

6. The method for rapid sample dissolution of a vanadium-titanium-chromium-manganese-iron five-element alloy according to claim 5, characterized in that: In step S2, the hydrochloric acid and nitric acid are of high purity with mass concentrations of 36% to 38% and 68% to 70% respectively; the mass concentration of hydrofluoric acid is 65% to 68%; and the mass concentration of hydrogen peroxide is ≥30%.

7. The method for rapid sample dissolution of a vanadium-titanium-chromium-manganese-iron quinary alloy according to claim 1, characterized in that: In step S2, after adding hydrogen peroxide, wait for 1 to 5 minutes before sealing the digestion tank.

8. The rapid sample dissolution method of vanadium-titanium-chromium-manganese-iron five-element alloy according to claim 1, characterized in that: In step S2, the setting conditions are: heating to 60°C within 5 minutes and keeping warm for 5 minutes, then heating to 180°C within 10 minutes and keeping warm for 10 minutes, and finally heating to 220°C within 5 minutes and keeping warm for 30 minutes.

9. A method for detecting all elements of a five-element vanadium-titanium-chromium-manganese-iron alloy, characterized by: According to the rapid sample dissolution method according to any one of claims 1 to 8, the vanadium-titanium-chromium-manganese-iron quinary alloy to be tested is dissolved and then transferred to a container to be fixed to volume to obtain a test solution; then, the element content in the test solution is detected by ICP-AES, ICP-MS and chemical wet analysis.

10. The method for full element detection of vanadium-titanium-chromium-manganese-iron five-element alloy according to claim 9, characterized in that: ICP-AES was used to detect the contents of Cr, Ti, Al, Si, Fe, and Mn elements in the test solution, ICP-MS was used to detect the content of Ce element in the test solution, and chemical wet method was used to detect the content of V element in the test solution.

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