Detection method for determining contents of niobium and tantalum in steel by applying microwave digestion-ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry)
A technology of ICP-AES and microwave digestion, which is applied in the field of iron and steel composition detection, can solve the problems of affecting the accuracy of analysis results, large consumption of chemical reagents, and high difficulty in chemical sample preparation
Active Publication Date: 2013-03-27
PANGANG GROUP JIANGYOU CHANGCHENG SPECIAL STEEL
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Problems solved by technology
In the chemical determination method of niobium and tantalum, it has always been quite difficult to eliminate the mutual interference between niobium and tantalum. Generally, only the total amount of niobium and tantalum can be determined, and the method is very cumbersome, which cannot meet the needs of current special steel production
In recent years, with the continuous development of instrumental analysis, the separation and interference of niobium and tantalum can be solved by using spectral analysis technology. Although X-ray-fluorescence spectroscopy can determine the components of niobium and tantalum in steel, for specific samples, First of all, it is necessary to prepare a series of standard samples with the same chemical composition as the sample to be analyzed, which requires high difficulty in chemical sample preparation; there are also reports on the use of inductively coupled emission spectrometry (ICP-AES) to test niobium and tantalum, but the sample pretreatment Nitric acid-hydrochloric acid-hydrofluoric acid is generally used, but the use of hydrofluoric acid has special requirements for equipment, that is, a hydrofluoric acid-resistant atomizer and atomization system must be used, and an ordinary electric heating plate is used for heating and digestion , the consumption of chemical reagents is large, not only the operation is cumbersome, but also the sample is easily contaminated during the processing process, which affects the accuracy of the analysis results
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example 1
[0039] Weigh 0.1000g of the sample to be tested (such as GH350) into a digestion tank (accurate to 0.0001g), add 1mL of 68% nitric acid, 14mL of 37% hydrochloric acid, 5mL of 98% sulfuric acid, cover Tighten the digestion tank and start the microwave digester according to the set program, that is, first raise the temperature to 150°C with 1000W power for 5 minutes, keep at 150°C for 5 minutes, then raise the temperature to 220°C with 1000W power for 5 minutes Minutes, keep at 220°C for 15-30 minutes. After the digestion is completed, cool to room temperature, transfer to a 100mL volumetric flask, dilute to the mark with water, and mix well. Measurements are performed in conventional nebulizers and nebulization systems.
[0040] Weigh 6 parts of the alloy base sample with the same mass as the sample to be tested, which contains the same matrix composition but does not contain the measured elements or the content of the measured elements is known, and put them in six 150mL beak...
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The invention discloses a detection method for determining the contents of niobium and tantalum in steel by applying a microwave digestion-ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry). The detection method comprises the following steps of: digesting a sample to be detected by hydrochloric acid, nitric acid and sulfuric acid through a microwave digestion apparatus, and then diluting the sample to be up to a certain volume to obtain liquid to be detected; measuring the intensity of an emission spectrum of the liquid at the wavelength part of an optimum analytical line of an ICP-AES apparatus, and detecting the concentration of the niobium and the tantalum according to a working curve; and calculating the contents of the niobium and the tantalum of the sample to be detected. The detection method can be used for processing the sample simply and obtaining an accurate analysis result, can well meet the requirements on analysis of the contents of the niobium and the tantalum in the steel with various types such as GH350, and can provide the guarantee of the improvement of the quality of the steel and the control on the contents of niobium and tantalum elements.
Description
technical field [0001] The invention belongs to the technical field of iron and steel composition detection, and more specifically relates to a detection method for determining the content of niobium and tantalum in iron and steel by applying microwave digestion-ICP-AES. Background technique [0002] Due to its chemical composition and the addition of various elements, special steel has excellent properties such as light specific gravity, high strength, oxidation resistance, and high temperature resistance, and is widely used in the aviation industry. In the metallurgical process of military industry and newly tested products, niobium and tantalum are alloying elements, which are strengthening elements in steel. Therefore, the role of niobium and tantalum in improving the material of metal functional materials has attracted more and more attention. [0003] Because niobium and tantalum are easily hydrolyzed elements, and niobium and tantalum belong to the same group in the p...
Claims
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Inventor 吴世凯
Owner PANGANG GROUP JIANGYOU CHANGCHENG SPECIAL STEEL