Method for detecting rare earth elements in steel

A technology of rare earth elements and constant volume, which is applied in the preparation of test samples, thermal excitation analysis, material excitation analysis, etc. It can solve the problems of cumbersome operation, unheard of successful reports, expensive equipment, etc., and the method has fewer steps , Satisfy operability requirements, and the effect of not demanding operation requirements

Inactive Publication Date: 2011-02-16
COMPREHENSIVE TECH SERVICE CENT OF CHANGSHU ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, ICP-MS equipment is expensive and requires high experimental conditions, making it difficult to popularize and apply
[0005] In addition to the shortcomings mentioned above, the methods listed above also have problems such as cumbersome operation, difficulty in ensuring the

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  • Method for detecting rare earth elements in steel
  • Method for detecting rare earth elements in steel
  • Method for detecting rare earth elements in steel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A) Sampling and sample dissolution, by weight, weigh 1.00g of steel sample cut into crumbs below 1mm, and place the weighed 1.00g steel sample in the first container served by a beaker. Add 30mL of concentrated nitric acid into the first container, and heat it to boiling, then add dropwise 20mL of concentrated hydrochloric acid to completely dissolve the steel sample, and obtain the undetermined content after evaporation to nearly dryness;

[0025] B) constant volume, with a concentration of 50mL of hydrochloric acid of 6mol / L to the volume to be determined obtained by step A), to obtain a constant volume solution;

[0026] C) ion exchange, pipette 10mL (one-fifth of the weight of the constant volume solution) constant volume solution from the constant volume solution obtained by step B) as a dissolved sample, and introduce the dissolved sample into the container with a flow rate of 0.8mL / min An anion exchange resin column with a particle size of 100-200 mesh and prefer...

Embodiment 2

[0031] A) Sampling and sample dissolution, by weight, take 2.50g of steel samples cut into crumbs below 1mm, and place the weighed 2.50g steel samples in the first container served by a beaker. Add 50mL of concentrated nitric acid into the first container, and heat it to boiling, then add dropwise 25mL of concentrated hydrochloric acid to completely dissolve the steel sample, and obtain the undetermined content after evaporation to nearly dryness;

[0032] B) constant volume, with the hydrochloric acid 100mL that is 7mol / L with concentration to the content to be determined volume that obtains by step A) constant volume, obtain constant volume solution;

[0033]C) ion exchange, pipette 10mL (one tenth of the weight of the constant volume solution) constant volume solution from the constant volume solution obtained by step B) as a dissolved sample, and introduce the dissolved sample into the container with a flow rate of 1.2mL / min. An anion exchange resin column with a particle ...

Embodiment 3

[0038] A) Sampling and dissolving, by weight, weigh 4.00g of the steel sample cut into crumbs below 1mm, and place the weighed 4.00g steel sample in the first container served by a beaker, Add 60mL of concentrated nitric acid into the first container, and heat it to boiling, then add 20mL of concentrated hydrochloric acid dropwise to completely dissolve the steel sample, and obtain the undetermined content after evaporation to nearly dryness;

[0039] B) constant volume, with the hydrochloric acid 250mL that is 8mol / L with concentration to the content to be determined that is obtained by step A) constant volume, obtain constant volume solution;

[0040] C) ion exchange, pipette 30mL (one-eighth of the weight of the constant volume solution) constant volume solution from the constant volume solution obtained by step B) as a dissolved sample, and introduce the dissolved sample into the container with a flow rate of 1.0mL / min. An anion exchange resin column with a particle size o...

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Abstract

The invention discloses a method for detecting rare earth elements in steel, comprising the steps of: sampling and sample dissolving: weighing a crushed steel sample, placing the crushed steel sample in a first container, adding nitric acid into the first container, heating till boiling, dropwise adding hydrochloric acid to completely dissolve the steel sample, and steaming to be almost dry to obtain a substance to be set with constant volume; setting volume: setting the volume of the substance to be set with the constant volume with the hydrochloric acid, and controlling the proportion of the steel sample to the hydrochloric acid to obtain a constant volume solution; ion exchanging: taking partial constant volume solution from the constant volume solution, to be used as a solution sample, leading the solution sample into an anion exchange resin column under a state with controlled flow velocity, collecting an outflow solution in a second container, washing unabsorbed rare earth elements with the hydrochloric acid, collecting the rare earth elements obtained through washing into the second container, controlling the volume of the collected solution, uniformly mixing to obtain a solution to be detected; and detecting: detecting the content of all rare earth elements in the solution to be detected by using an inductive coupling plasma emission spectrometer. The invention can be used for separating and detecting fourteen rare earth elements in a lanthanum series, has fewer steps and is convenient to operate.

Description

technical field [0001] The invention belongs to the technical field of metallurgical analysis, in particular to a method for measuring rare earth elements in steel. Background technique [0002] Trace rare earth elements are known as the vitamins of steel. The addition of rare earths to steel can improve the performance of the steel and make it have a satisfactory microstructure, thereby improving the physical properties such as strength and chemical properties such as oxidation resistance of the steel. [0003] The analysis of trace rare earths in steel is difficult, and the core problem is the overlapping interference of the ferrographic lines of the matrix. Many scholars believe that in order to avoid the spectral overlapping interference of ferrographic lines, it is necessary to separate the matrix iron. Regarding the method for the separation of trace rare earths in steel, the article published in Volume 130 of "Mikrochimica Acta" magazine in 1998 (Extraction Chromato...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N21/73
Inventor 许玉宇王慧吴骋顾伟王国新周锦帆俞璐朱玉燕卢书媛王卫忠
Owner COMPREHENSIVE TECH SERVICE CENT OF CHANGSHU ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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