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Method for digesting vanadium-chromium-titanium alloy and detection method for digestion solution

The technology of a vanadium-chromium-titanium alloy and a detection method is applied in the field of detection and analysis, and can solve the problems that the simultaneous determination of secondary alloy elements cannot be satisfied, the complete digestion of vanadium-chromium-titanium is difficult to ensure, and the structure of the digestion alloy is complex, so as to improve product detection efficiency, The effect of reducing the influence of the matrix effect and shortening the inspection cycle

Active Publication Date: 2019-12-03
PANGANG GROUP RESEARCH INSTITUTE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest problem with this type of method is that it is only suitable for rapid and complete digestion of material samples such as vanadium-iron alloys and vanadium-aluminum alloys, which have a relatively simple crystal structure and only soluble elements such as vanadium, iron, and aluminum, and cannot be used to digest alloy structures. The sample detection solution is more complex and the matrix components include the vanadium-chromium-titanium ternary alloy material with high content of insoluble elements chromium and titanium. Even if the reaction time is greatly prolonged, it is difficult to guarantee the complete digestion of the vanadium-chromium-titanium sample
Moreover, the existing ICP-OES detection methods for vanadium-iron and vanadium-aluminum are only suitable for the determination of trace impurity elements in samples. Usually minor alloy elements need to be determined by chemical analysis methods such as titration, which cannot meet the requirements of simultaneous determination of vanadium-chromium-titanium alloy materials. Requirements for medium amount alloying elements Cr, Ti and trace impurity elements

Method used

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  • Method for digesting vanadium-chromium-titanium alloy and detection method for digestion solution
  • Method for digesting vanadium-chromium-titanium alloy and detection method for digestion solution
  • Method for digesting vanadium-chromium-titanium alloy and detection method for digestion solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Sample detection solution digestion preparation of vanadium-chromium-titanium alloy

[0026] Weigh 0.2 vanadium-chromium-titanium alloy sample (No. 1 sample), add 30mL digestion reagent, place on a hot plate and heat to boil until the sample particles are dissolved and only a small amount of residue remains and the solution produces uniform large bubbles (the first digestion step); And keep the solution temperature at 65-75°C, add 0.5mL hydrofluoric acid to completely digest the sample residue, cool the solution to room temperature, dilute it with water and mix it evenly in a 100mL volumetric flask for testing (the second digestion step).

[0027] Determination of Minor Alloy Elements and Trace Impurity Elements in Sample Detection Solution by ICP-OES

[0028] Using Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-OES) as a detection method, the prepared vanadium chromium titanium sample detection solution is directly introduced into the ICP-OES instrument, ...

Embodiment 2

[0032] Weigh 0.3 vanadium-chromium-titanium alloy sample (No. 2 sample), add 45mL sample combination digestion reagent in proportion to carry out the digestion reaction of the first step, then add 0.8mL hydrofluoric acid to carry out the digestion reaction of the second step, in addition, The vanadium-chromium-titanium sample solution was prepared in the same manner as in Example 1, and the contents of minor alloying elements and trace impurities in the solution were determined by ICP-OES.

Embodiment 3

[0034] Weigh 0.4 vanadium-chromium-titanium alloy sample (No. 3 sample), add 60mL sample combination digestion reagent in proportion to carry out the digestion reaction of the first step, then add 1.0mL hydrofluoric acid to carry out the digestion reaction of the second step, in addition, The vanadium chromium titanium sample solution was prepared according to the same method as in Example 1, and the contents of minor alloy elements and trace impurities in the solution were determined by ICP-OES.

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Abstract

The invention relates to the technical field of detection analysis, and in particular to a method for digesting a chromium vanadium titanium alloy and a detection method. The method for digesting the chromium vanadium titanium alloy comprises the following steps: mixing hydrochloric acid, nitric acid and water so as to obtain a digestive reagent, adding the digestive reagent into the chromium vanadium titanium alloy, and heating to boil the solution to react till solids are not reduced any longer; reducing the temperature to 65-75 DEG C, adding hydrofluoric acid, keeping the temperature to react till residual solid substances are completely digested, and cooling, thereby obtaining the digestion solution. The method is capable of achieving rapid complete digestion of a chromium vanadium titanium alloy sample and meanwhile testing secondary alloy elements and trace impurity elements of the chromium vanadium titanium alloy, and has the characteristics of being simple, convenient, efficient and rapid to operate, small in interference factor, accurate and reliable, short in detection procedure, high in speed and the like.

Description

technical field [0001] The invention belongs to the technical field of detection and analysis, and in particular relates to a method for digesting a vanadium-chromium-titanium alloy and a detection method for a digestion solution. Specifically, the present invention relates to a method for determining minor alloy elements Cr and Ti with a mass fraction of 2.5 to 5.5%, and trace impurity elements Al, As, and Co, Cu, Fe, Mg, Mn, Ni, P, Pb, Si, Sn, W, Zn, Zr and the sample solution digestion preparation method with mass fraction of 0.005-0.25% K, Na and the detection method of the contained elements . 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 metal chromium powder and metal titanium powder of hundreds of μm to 1mm. As a basic raw material, it is produced and prepared by method...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/71
CPCG01N21/71
Inventor 成勇
Owner PANGANG GROUP RESEARCH INSTITUTE CO LTD
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