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

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...

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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" No. 3, September 2006) using hydrochloric acid, nitric acid, perchloric acid and hydrofluoric acid mixed acid to dissolve and emit perchloric acid fumes, tartaric acid to dissolve salts, Since a certain amount of hydrofluoric acid needs to be added in the process of sample processing, and about 2 grams of tartaric acid dissolved salts need to be added to each sample after acid dissolution, the total dissolved solids (TDS) in the analysis test solution is high, which is easy to cause fog Blockage of chemical system and ICP torch

The above methods are all due to the defects of the sample dissolution method, so it is difficult to popularize in scientific research and production inspection

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