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Vanadium chromium titanium alloy material microwave digestion method and its element component detection method

A technology of microwave digestion and element composition, which is applied in the direction of material analysis, material analysis, and measuring device by electromagnetic means, which can solve the problems of easy fatigue loss, unusability, complex alloy structure, etc., and achieve the level of accuracy and precision High, prolong the service life, the effect of high safety factor

Inactive Publication Date: 2018-10-23
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Most of these methods use nitric acid, hydrofluoric acid or a combination of nitric acid, hydrofluoric acid, and phosphoric acid as digestion reagents. After adding each reagent at one time, microwave heating is performed, and the microwave heating temperature is usually set at a high level. This type of method is suitable for digestion For vanadium oxy or vanadium nitrogen compounds with simple composition and slow reaction with acid, the reagent combination, ratio, dosage, addition sequence and timing, and reaction control conditions cannot be used to prepare vanadium-chromium-titanium ternary metal alloys for digestion samples. Material sample detection solution, because compared to the chemical reaction speed of vanadium oxide or vanadium nitrogen compound and acid, vanadium chromium titanium alloy is an alloy compound of pure metal, especially the metal vanadium with a content greater than 90% in the sample can be Rapid reaction with acid produces a large amount of gas, causing the pressure in the airtight container to increase rapidly and excessively high, resulting in an explosion hazard; at the same time, the microwave heating in the current method is controlled at a high temperature reaction condition of about 200 ° C or above, and the reaction time is long and energy consumption is high. high, and prone to fatigue loss and greatly shorten the safe service life of expensive polytetrafluoroethylene and other digestion vessels; moreover, the alloy structure of the vanadium-chromium-titanium ternary metal alloy material is more complex and the matrix components include higher content that is difficult to Soluble amount of matrix alloy elements chromium, titanium and product quality requirements Inspection of tungsten, silicon, palladium, zirconium, niobium and other impurity elements to be tested that are insoluble or easy to condense or hydrolyze
In addition, the original method using inductively coupled plasma atomic emission spectrometry (ICP-OES) can only meet the needs of the determination of trace elements with a content of 0.01% or above 0.001%, and it is completely unable to meet the determination of 0.0001%-0.01% in vanadium-chromium-titanium alloy materials. Inspection of trace levels of impurity elements requires

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  • Vanadium chromium titanium alloy material microwave digestion method and its element component detection method
  • Vanadium chromium titanium alloy material microwave digestion method and its element component detection method
  • Vanadium chromium titanium alloy material microwave digestion method and its element component detection method

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Embodiment 1

[0043] The present embodiment provides a microwave digestion method of vanadium-chromium-titanium alloy material, which comprises the following steps:

[0044] Weigh 0.1g vanadium-chromium-titanium alloy sample, directly add 3.0mL concentrated nitric acid, and pre-react in an open state until the liquid level is calm and the brown fume of nitrogen oxides completely escapes; add 2.0mL concentrated nitric acid again and let stand for 2min. Rinse the wall of the vessel with 5mL water and add 0.5mL hydrofluoric acid, and conduct microwave digestion in a closed container; the microwave reaction conditions are set to use a ramp temperature rise method, and the pressure is controlled to be less than 800psi. First, the temperature is programmed to rise to 90°C for 3 minutes and kept for 3 minutes, and then the temperature is programmed for 3 minutes. Heat at 120°C and keep it warm for 5 minutes. After the digestion reaction, cool the solution to room temperature, dilute with water to a...

Embodiment 2

[0049] The microwave digestion method of the vanadium-chromium-titanium alloy material provided in this embodiment and the element composition detection method of the vanadium-chromium-titanium alloy material comprise the following steps:

[0050] Weigh 0.15g sample, add 5.0mL concentrated nitric acid to pre-react completely; then add 3.0mL concentrated nitric acid and let it stand for 3min, rinse the wall of the vessel with 8mL water and add 1.0mL hydrofluoric acid, and carry out microwave digestion in a closed container; the microwave reaction condition is slope Heating method, pressure is less than 800psi, raised to 95°C for 5 minutes and kept for 5 minutes, raised to 130°C for 5 minutes and kept for 10 minutes, cooled the solution to room temperature after digestion, and mixed with water to a 100mL volumetric flask for testing. 10ng / mL (ppb) Rh standard solution was used as internal standard calibration solution.

[0051] Except for the above parameters, the vanadium chrom...

Embodiment 3

[0053] The microwave digestion method of the vanadium-chromium-titanium alloy material provided in this embodiment and the element composition detection method of the vanadium-chromium-titanium alloy material comprise the following steps:

[0054]Weigh 0.12g sample, add 4.0mL concentrated nitric acid to complete the pre-reaction; then add 2.0mL concentrated nitric acid and let it stand for 3min, rinse the wall of the vessel with 7mL water and add 0.5mL hydrofluoric acid, microwave digestion in a closed container; the microwave reaction condition is 4min Raise the temperature to 90°C and keep it warm for 4 minutes, raise the temperature to 125°C after 4 minutes and keep it warm for 8 minutes. After the digestion, cool the solution to room temperature, dilute it with water in a 50mL volumetric flask and mix it for testing. 5ng / mL (ppb) Rh standard solution was used as internal standard calibration solution.

[0055] Except for the above parameters, the vanadium chromium titanium...

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Abstract

The invention discloses a vanadium chromium titanium alloy material microwave digestion method and its element component detection method, which relate to the technical field of detection analysis ofimpurity elements. The microwave digestion method comprises the following steps: mixing a vanadium chromium titanium alloy material and concentrated nitric acid, and performing a pre-reaction on a mixture under an opening state until no bubbles is generated; mixing a pre-reacted solution and a concentrated nitric acid solution and performing standing for a reaction, and mixing the solution after the reaction with water and hydrofluoric acid to obtain to-be-digested mixed liquor; and performing microwave digestion on the to-be-digested mixed liquor under enclosed condition. According to the detection method, the reaction liquor after microwave digestion obtained in the above microwave digestion method is subjected to volume metering, and an ion mass spectrometry is used as a detection meansfor detection. The digestion method has the advantages that the safety coefficient is high, the equipment damage is less, the whole detection method has the high accuracy and precision level, and realizes a purpose of rapid and accurate detection.

Description

technical field [0001] The invention relates to the technical field of detection and analysis of impurity elements, and in particular to a microwave digestion method for a vanadium-chromium-titanium alloy material and a method for detecting elemental components thereof. Background technique [0002] Vanadium-chromium-titanium alloy (baseline composition V-4Cr-4Ti) is an important candidate structural material for nuclear fusion reactors. Usually, V-Cr-Ti alloys are mostly made of high-purity metal vanadium and several hundred μm-1mm metal chromium powder and metal titanium powder. As the basic raw material, according to the ratio of V-4.5Cr-4Ti, it is produced by magnetic levitation melting, powder metallurgy, vacuum consumable arc remelting and other methods. Vacuum consumable arc remelting (VAR) method is produced and prepared. The VAR method uses high-purity metal vanadium, chromium and titanium as raw materials to prepare electrodes for vacuum melting. The scarcity and h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/44G01N27/62
CPCG01N1/44G01N27/62
Inventor 成勇
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP