Hydride-atomic fluorescence optical spectrum rapid measuring method for micro-trace amount of tellurium in hull steel

Abstract

The invention introduces a quick atomic fluorescence spectroscopic measuring method of a hydride of a micro trace element tellurium in hull steels, which realizes measurement on the basis of the atomic fluorescence spectrometry generation detecting principle of hydrides and comprises the steps of experimental condition selection, sample processing, working curve plotting, interfering and eliminating, and building of the linear relation of the working curves, the detection limit condition, the relative standard deviation and the recycling rate. The quick atomic fluorescence spectroscopic measuring method implements accurate measurement and strict control on the tellurium content in the hull steels, thus ensuring the quality and the performance of the hull steels, the method has good application effect and the advantages of small substrate interference, wide linear range and good stability, etc., and the method has the recycling rate from 98 to 103 percent, the linear range from 0 to 60 nanogram per milliliter, the detection limit of 0.30 nanogram per milliliter, and the measuring range from 0.0001 to 0.05 percent.

Description

technical field [0001] The invention belongs to the technical field of metal testing and analysis, and in particular relates to a rapid determination method for hydride-atomic fluorescence spectroscopy of trace tellurium in ship hull steel. Background technique [0002] Tellurium is in the same family as sulfur, and its properties are similar to sulfur. Tellurium is usually a harmful element in hull steel. The presence of trace amounts of tellurium will seriously reduce the mechanical properties of the material, reduce the ductility and toughness of the steel, damage the corrosion resistance of the steel, and have an adverse effect on welding. Advanced alloys used as aerospace materials generally require the amount of tellurium to be less than 0.001%, but currently many data suggest that the amount of tellurium must be controlled to be less than 1-0.5ug / g. Therefore, accurate analysis of tellurium content in hull steel is required. [0003] For the determination of telluri...

AI Technical Summary

Problems solved by technology

[0004] 1. The "Photometric Determination of Trace Tellurium in Steel" published in the third issue of "Metallurgical Analysis" in 1996 is a method obtained by improving the Japanese standard JIS G1234-86 method (turbidimetric method). The equipment used in this method It is a 721 spectrophotometer with a narrow scope of application. It is only suitable for the determination of Te in ordinary steel and medium-low alloy steel that does not contain selenium and molybdenum content <1%. The lower detection limit is 0.002%, which is relatively high;

[0005] 2. "Separation of arsenic coprecipitation-determination of trace tellurium in steel by oscillographic polarography" published in the third issue of "Special Steel Technology" in 1997 is about the determination of trace amounts of tellurium in steel. This method has many test steps. After several times of smoking and filtering, the workload is heavy and many factors are affected. For example, when the titanium content in the weighing sample is greater than 8mg, titanium affects the co-precipitation and separation of tellurium and affects the determination of tellurium; It will lead to incomplete co-precipitation of tellurium and affect the determination of tellurium, which is not suitable for production control;

The ion exchange method is cumbersome, with many steps, heavy workload, and high relative standard deviation

[0007] However, the determination of tellurium in foreign countries adopts iodide extraction and flame atomic absorption method, and there are certain problems.