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Method for measuring content of major elements in multi-component alloy by proportionality coefficient correction glow mass spectrometry

A multi-element alloy, proportional coefficient technology, applied in the field of analysis and testing, can solve the problems of polluting the environment, difficult to directly quantitatively analyze the content of major elements in the sample, and difficult to observe.

Pending Publication Date: 2022-03-01
JIANGSU LONGDA SUPERALLOY MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Among the above detection methods, the gravimetric method has many steps and the measurement time is too long; the titration method usually adopts the complexometric titration method, the reaction rate is slow at room temperature, the titration interference is serious, the end point will appear repeatedly, and it is difficult to observe; the inductively coupled plasma atomic emission spectrometry is mainly It is used for micro-measurement, and it needs to add a large amount of acid and alkali to dissolve the sample, which consumes a lot of reagents and pollutes the environment
As a direct analysis technique for solid samples, glow discharge mass spectrometry (GDMS) needs to use the relative sensitivity factor (RSF) data to convert the ion current intensity when measuring the sample, and establish the relationship between the content of each element and the ion current intensity, such as Tang Yichuan et al. in "Research on Relative Sensitivity Factors in Glow Discharge Mass Spectrometry Measurements", this method has been widely used in the analysis of trace and ultra-trace impurities in high-purity metals, semiconductors and other materials, but it is affected by factors such as mass spectrometry interference For example, the various interference types listed in the paper "Multi-element Glow Discharge Mass Spectrometry and Interference Correction in Superalloys" by Yu Xing et al. make it difficult to directly quantitatively analyze the content of major elements in samples.
Therefore, glow discharge mass spectrometry (GDMS) has been applied to the qualitative and semi-quantitative analysis of trace, trace, and ultra-trace elements, which limits its application in the analysis of major element content in multi-component samples.

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  • Method for measuring content of major elements in multi-component alloy by proportionality coefficient correction glow mass spectrometry
  • Method for measuring content of major elements in multi-component alloy by proportionality coefficient correction glow mass spectrometry
  • Method for measuring content of major elements in multi-component alloy by proportionality coefficient correction glow mass spectrometry

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Embodiment 1

[0022] Embodiment 1 is illustrated with Ni-Cr alloy as example:

[0023] a. Determination of Cr in Ni-Cr alloy, reference standard HB5220.15-2008: put 5 Ni-Cr chip samples -1~5 with different Ni and Cr contents in a 500mL conical flask, add hydrochloric acid, Nitric acid, heating and dissolving is complete, then add sulfuric acid-phosphoric acid mixed acid. Add nitric acid dropwise for oxidation, add approximately water, add silver nitrate and ammonium persulfate solution and heat to oxidize to purple. Add sodium chloride for reduction. With N-phenyl anthranilic acid as indicator, titrate with ferrous ammonium sulfate standard solution to obtain the mass fraction C of each sample Cri , the results are shown in Table 1.

[0024] b. Determination of Ni in Ni-Cr alloy, reference standard HB5220.23-2008: put 5 Ni-Cr chip samples -1~5 with different Ni and Cr contents in a beaker, add hydrochloric acid and nitric acid, heat After the dissolution is completed, in the ammonium me...

Embodiment 2

[0033] Embodiment 2 is illustrated by taking the Mg-Al-V ternary alloy as an example:

[0034]a. Determination of Mg in Mg-Al-V ternary alloy, reference standard GB / T 20975.16-2008: Mg-Al-V ternary alloy chips are placed in a 500mL beaker, heated and dissolved with hydrochloric acid, and nitric acid is added After the dissolution is completed, filter the residue; after ashing, add sulfuric acid, hydrofluoric acid, nitric acid to dissolve, smoke sulfuric acid, add hydrochloric acid to dissolve, add hydrogen peroxide, potassium cyanide and a small amount of iron, and separate magnesium and a large amount of aluminum with NaOH precipitation. Separate iron, manganese, aluminum, etc. again, use methyl thymol blue as indicator, titrate magnesium with CyDTA standard solution, and calculate the mass fraction of magnesium C Mgi , the results are shown in Table 3.

[0035] b. Determination of Al in Mg-Al-V ternary alloy, reference standard YS / T 1075.8-2015: Mg-Al-V ternary alloy chips ...

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Abstract

The invention relates to a method for determining the content of major elements in a multi-component alloy through proportionality coefficient correction glow mass spectrometry, and belongs to the technical field of analytical testing. The method comprises the following steps: determining a group of multi-component alloys with different major elements and different contents by adopting a glow discharge mass spectrometer to obtain mass counts of the major elements; establishing a proportion coefficient f of the major element content to mass counting; and finally, rapidly obtaining the mass count of the major elements in the to-be-detected multi-element alloy sample by using glow discharge mass spectrometry, correcting by using a proportionality coefficient f, and quantitatively obtaining the content of the major elements. According to the method, the constant-value multicomponent alloy is used, the mass counting proportionality coefficient relation with the glow discharge mass spectrometry is established, so that the content of the major elements in the multicomponent alloy is quantitatively determined, and the method has the advantages of rapidness, accuracy, reliability and the like, and is an effective content analysis method for the major elements in binary and ternary alloy materials.

Description

technical field [0001] The invention relates to a method for determining the content of major elements in multi-element alloys by proportional coefficient corrected glow mass spectrometry, and belongs to the technical field of analysis and testing. Background technique [0002] Titanium, nickel, cobalt, iron and other multi-element alloys are widely used in military, aerospace and other cutting-edge defense industries and civilian industries, such as Ni-Cr alloys, Ni-Mg alloys, Al-V alloys, Ni-B alloys, Ni- Ca alloys, Fe-Cr-Al alloys, Ni-Cr-Mo alloys, Fe-Cr-Ni-Mo alloys and other intermediate alloys are important raw materials for the production of titanium, nickel, cobalt, and iron alloys, which can mainly improve the heat resistance of the alloys With cold workability, the alloy has good weldability and fairly high mechanical strength. Multi-component alloys are generally composed of metal elements or metal elements and non-metal elements, and have metallic properties. D...

Claims

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Application Information

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IPC IPC(8): G01N27/68
CPCG01N27/68
Inventor 年季强浦益龙吕水永于闲
Owner JIANGSU LONGDA SUPERALLOY MATERIAL CO LTD
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