Method for determining valence state of transition metal in slag by using high-temperature mass spectrum method

A transition metal, high-temperature technology, applied in the field of analysis of the valence state of melt ions, can solve the problems of acid oxidation, hidden dangers, and inability to be widely used, which are difficult to eliminate oxidation, and achieve good application prospects, easy to implement, and reliable Transplantation effect

Inactive Publication Date: 2012-12-26
UNIV OF SCI & TECH BEIJING
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0009] We know Cr 2+ It is easily oxidized, and it is difficult to rule out the possibility of being oxidized by oxidizing acids. The acid solutions mentioned in the literature have H 2 SO 4 , HCl and HNO 3 etc., some even dissolve the sample under the heating condition of 50oC, these experimental conditions are Cr 2+ The hidden danger of oxidation
With the development of science and technology, the emergence of X-ray near-angle absorption spectroscopy is an important way to accurately determine Cr 2+ The content provides reliable technical support [3,4] , but due to the limitations of experimental conditions, the XANES method cannot be widely used

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  • Method for determining valence state of transition metal in slag by using high-temperature mass spectrum method
  • Method for determining valence state of transition metal in slag by using high-temperature mass spectrum method
  • Method for determining valence state of transition metal in slag by using high-temperature mass spectrum method

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Embodiment 1

[0032] Experiments were carried out using double tungsten Knudsen cells, one of which was filled with pure Cr 2 o 3 The sample serves as a standard, and a slag sample is placed in another cell. The system is calibrated with liquid gold. In CaO-MgO-Al 2 o 3 -Cr 2 o 3 -FeO-SiO 2 During the volatilization process, CrO in the gas phase + and CrO 2 + The ionic current intensity was recorded by the mass spectrometer and compared with the reference sample Cr 2 o 3 The volatilization process was compared.

[0033] 2: Analysis method

[0034] In the temperature range of 1850-2000K, there are three kinds of Cr-containing gas phase substances, namely Cr, CrO and CrO 2 . From the standard sample Cr 2 o 3 It can be seen that the possible reactions between the three substances are as follows:

[0035] Cr 2 o 3 (solid)=2Cr(gas)+3O(gas) (1)

[0036] Cr 2 o 3 (solid)=2CrO(gas)+O(gas) (2)

[0037] Cr 2 o 3 (solid)=CrO 2 (gas)+CrO(gas) (3)

[0038] And according to li...

Embodiment 2

[0042] Taking the analysis of the valence state of V in slag as an example, starting from the literature, we can make a judgment that there may be a valence state, and then study the 3+ / V 4+ price ratio.

[0043] 1. At alkalinity (CaO / SiO 2 ) is less than 1 and the partial pressure of oxygen is less than 10 -1 Pa, only V 3+ and V 4+ coexist. Considering the reality of low oxygen partial pressure in the steelmaking process and the low oxygen partial pressure conditions in the process of high-temperature mass spectrometry, the influence of alkalinity is ignored here, and it is considered that V 3+ and V 4+ is the main valence state present in the studied slag samples. This assumption is consistent with V 5+ The fact that it cannot exist under conditions of low oxygen partial pressure.

[0044] 2. The slag sample chamber is volatilized from two parallel Knudsen pools, and the ratio of the volatilization gap to the volatilization area of ​​the Knudsen pool is 1:100. Thi...

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Abstract

The invention belongs to a method for analyzing the ionic valence state of a melt, and in particular relates to a method for determining the valence state of a transition metal in slag by using a high-temperature mass spectrum method. By the method, an intrinsic standoff ratio of substances of the same element in a gas phase can be obtained through Knudsen-high-temperature-mass-spectrum test and is compared with corresponding partial pressure of a reference substance, so that a valence state proportional relation of transition metal elements in a condensed phase can be obtained. By the method, the possibility that the transition metal is oxidized when slag samples are melted by a wet chemical method is reduced, and the original state of the sample can be kept; furthermore, the volatilization experiment is easier than an X-ray nearly angle refraction absorption spectrum method; and moreover, the method is high in transportability and has a good application prospect.

Description

technical field [0001] The invention relates to a method for analyzing the valence states of melt ions, in particular to an analysis method for the distribution of various valence states of transition metal ions in metallurgical slag. Background technique [0002] There are many methods for analyzing the valence state of compounds, such as elemental chemical analysis, density measurement, thermogravimetric analysis, electrochemical coulometric titration, redox balance, thermodynamic measurement, X-ray diffraction, neutron scattering, etc. [1] . Specific to metallurgical melts, wet chemical methods are widely used [2] . It is often used to analyze the valence state of chromium. The principle is to dissolve the slag sample in an acidic solution and oxidize it by titration to obtain the content and ratio of divalent and trivalent chromium ions. After the slag is dissolved, dilute the solution with deionized water, and add an excess of 0.5mol / L ferric chloride solution (disso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/62
Inventor 王丽君瑟萨迪·西塔拉曼周国治
Owner UNIV OF SCI & TECH BEIJING
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