Sample treatment method for measuring niobium, tungsten and zirconium in steel

A processing method and a certain amount of technology, applied in the field of measurement, can solve the problems of phosphorus pollution in the sampling system, blockage of the atomization system and ICP torch, and difficulty in popularization, and achieve the effects of avoiding phosphorus pollution, reducing matrix effect interference, and avoiding clogging.

Inactive Publication Date: 2013-02-13
ANGANG STEEL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Some people have used this technology to determine the content of niobium, tungsten and zirconium in steel, such as Zhang Guang et al. "Simultaneous Determination of Zirconium and Niobium in Low Alloy Steel by ICP-AES" ("Metallurgical Analysis", Volume 24, Issue 1, 2004) After dissolving the sample with dilute sulfuric acid, dissolve the salts with sulfuric acid and fuming tartaric acid, and decompose the sample using sulfur and phosphorus mixed acid to fume, which introduces a large amount of phosphorus into the sampling system, causing phosphorus pollution in the sampling system; Zhang Jiaxiang "ICP "Technical Analysis of Determination of Trace Nb in Steel" ("Sichuan Nonferrous Metals

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  • Sample treatment method for measuring niobium, tungsten and zirconium in steel
  • Sample treatment method for measuring niobium, tungsten and zirconium in steel

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Embodiment 1

[0018] Embodiment 1 is the determination of the content of niobium, tungsten and zirconium in the standard sample of medium and low alloy steel by using the present invention. The specific method is as follows:

[0019] 1. Prepare soluble acid

[0020] Measure 100 mL of sulfuric acid (sulfuric acid with a density of 1.84 g / mL) in a 100 mL measuring cup, pour it along the glass rod into a 1 L beaker filled with 400 mL of deionized water, and gently stir and mix with the glass rod. After the solution was cooled to room temperature, it was poured into a 1 L wide-mouth ground bottle to obtain soluble acid for use.

[0021] 2. Preparation of ammonium oxalate complexing agent

[0022] Weigh 4.0 g of ammonium oxalate on a tray balance and dissolve it in a 1 L beaker filled with 1000 mL of deionized water, stir gently with a glass rod to dissolve completely, then pour it into a 1 L wide-mouth grinding bottle to obtain the concentration It is the ammonium oxalate complexing agent of...

Embodiment 2

[0043] Embodiment 2 is the determination of the content of niobium, tungsten and zirconium in alloy steel samples by using the present invention. The specific method is as follows:

[0044] 1. Prepare dissolving acid (as in Example 1)

[0045] 2. Preparation of ammonium oxalate complexing agent (as in Example 1)

[0046] 3. Dissolve the sample

[0047] Accurately weigh 0.2000g of 1# sample and place it in a 125 ml conical flask, add 25 mL of dissolving acid (concentration: sulfuric acid: water = 1:4), heat to dissolve, add nitric acid dropwise for oxidation, continue heating until sulfuric acid smokes , the salts were precipitated, removed, cooled slightly, then added 15 mL of ammonium oxalate complexing agent (concentration: 4 g / L), heated to dissolve the salts, removed, cooled to room temperature, transferred to a 50 mL volumetric flask, and deionized Dilute to volume with water and mix well.

[0048] 4. Draw the working curve

[0049]Weigh 5 parts of 0.2000 g high-puri...

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Abstract

The invention provides a sample treatment method for measuring niobium, tungsten and zirconium in steel. The method comprises the following steps of: 1) preparing a sample acid by mixing 1 part of 1.84g/mL sulfuric acid and 4 parts of deionized water; 2) preparing a 4g/L ammonium oxalate complexing agent; 3) dissolving the sample: namely weighing 0.1000 to 0.2000g of steel scrap sample, putting the scrap sample into a conical flask, adding 20 to 25mL of sample acid, heating, dissolving, dropping nitric acid to oxidize until the solution is clarified, continuously heating until smokes of the sulfuric acid come out, precipitating salts, taking down the salts, slightly cooling, adding 10 to 15mL of ammonium oxalate complexing agent, heating, dissolving and taking the salts, cooling to room temperature, transferring the solution into a 50mL volumetric flask, diluting the solution to the scale by using deionized water, and uniformly mixing. By the method, hydrofluoric acid is not used, and the accuracy of an analysis result is not influenced; phosphoric acid is not used, and phosphorus pollution of the system is avoided; and moreover, the introduction of lots of salts is controlled, so that the matrix effect interference, spectral line interference and background interference are reduced, and blockage of an atomization system and an inductively coupled plasma (ICP) torch is avoided.

Description

technical field [0001] The invention belongs to the technical field of measurement, and relates to a sample processing method for measuring niobium, tungsten, and zirconium in steel, in particular to a sample processing method applicable to the analysis of niobium, tungsten, and zirconium in steel by inductively coupled plasma atomic emission spectrometry method. Background technique [0002] Niobium, tungsten, and zirconium are alloy elements in steel, and the content of niobium, tungsten, and zirconium has a great influence on the properties of steel. Niobium can refine the grain of steel, reduce the overheating sensitivity and temper brittleness of steel; tungsten can improve the creep strength of steel, and is also a strong accelerator of carbide in steel; zirconium can improve the strength and hardness of steel, In particular, it can improve the durable strength of steel and improve the welding performance of steel. Therefore, it is particularly important to quickly a...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N1/38G01N1/44
Inventor 杨丽荣王一凌于媛君
Owner ANGANG STEEL CO LTD
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