Method for Determination of Niobium Content in Iron and Steel by Separation of Chlorosulfophenol S by Beryllium Hydroxide

Abstract

The invention discloses a method for measuring niobium content in iron steel through a beryllium hydroxide separating sulfochlorophenol S spectrophotometric method. The method comprises the following steps: (1) weighing a sample, and dissolving into a first container with acid; (2) adding perchloric acid; (3) adding an ethylenediamine tetraacetic acid tetramine solution and / or an ethylenediamine tetraacetic acid disodium diamine solution; (4), adding ammonia water, a beryllium sulfate solution and oxalic acid; (5) filtering; (6) dissolving precipitation into a second container through acid; (7) after the precipitation is dissolved, adding tartaric acid so as to obtain a to-be-measured solution; (8) moving quantitative to-be-measured solution into a second container, and adding a sulfochlorophenol S solution, an ethylenediamine tetraacetic acid disodium diamine solution and hydrochloric acid so as to obtain a color developing liquid; (9) adding the color developing liquid into an absorption vessel, preparing a reference liquid, adding the reference liquid into the absorption vessel, and measuring the absorbency of the color developing liquid by comparison with the reference liquid at the position with the wavelength of 652 or 654; (10) calculating the niobium content in the sample according to a niobium working curve. According to the method, the measuring precision of the niobium content in the measured iron steel can be obviously improved.

Description

technical field [0001] The invention relates to a photometric method for determining niobium content in iron and steel by separating chlorosulfonol S from beryllium hydroxide. Background technique [0002] The methods for determining the content of niobium in iron and steel in the prior art mainly include the gravimetric method and the chlorosulfonol S photometric method, wherein the gravimetric method mainly includes the paper chromatography gravimetric method and the tannic acid decomposition gravimetric method, and the chlorosulfonol S Photometric methods mainly include ion exchange separation method and EDTA-ascorbic acid reduction method for masking molybdenum. The separation steps of the gravimetric method are long, generally needing 10h to 12h; the operation of the ion exchange separation method is complicated; the method of EDTA-ascorbic acid reduction masking molybdenum has poor masking effect and method stability. Contents of the invention [0003] The object of...

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Problems solved by technology

The separation steps of the gravimetric method are long, generally needing 10h to 12h; the operation of the ion exchange separation method is complicated; the method of EDTA-ascorbic acid reduction masking molybdenum has poor masking effect and method stability

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