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Method for detecting total iron content in iron material by X fluorescent cobalt internal standard-ICP cobalt compensation

A technology of iron content and fluorescence method, which is applied in the directions of measuring devices, analytical materials, material excitation analysis, etc., can solve the problems of complex process, poor accuracy of total iron content results, and not being widely used, and achieve low detection cost and high efficiency The effect of improving and better fluidity

Active Publication Date: 2019-10-29
新余钢铁股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The three sample dissolution methods belong to manual analysis methods, and the process is relatively complicated. After the sample is dissolved, Fe 3+ Reduced Fe 2+ After reducing all the iron ions to a low price, add sulfur and phosphorus mixed acid, use sodium diphenylamine sulfonate as indicator, and titrate with potassium dichromate standard solution to determine the total iron content
The internal standard method uses cobalt trioxide for matrix correction, so when the detected iron material itself contains cobalt, the results of total iron are quite different
Although the direct determination method is fast and simple, since the iron materials of various enterprises come from all over the world, the changeable matrix effect will eventually affect the accuracy of the total iron results.
The calculation method is used to indirectly measure the total iron content. Due to the burning increase of low-valence impurity elements during the burning process, the accuracy of the calculated total iron content is relatively poor.
Due to the inherent shortcomings of the adaptability of the three detection methods, X-ray fluorescence spectroscopy has not been widely used to detect the total iron content in iron materials

Method used

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  • Method for detecting total iron content in iron material by X fluorescent cobalt internal standard-ICP cobalt compensation
  • Method for detecting total iron content in iron material by X fluorescent cobalt internal standard-ICP cobalt compensation
  • Method for detecting total iron content in iron material by X fluorescent cobalt internal standard-ICP cobalt compensation

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Embodiment 1

[0063] X fluorescence cobalt internal standard-ICP cobalt compensation detects the method for total iron content in iron material, comprises the following steps:

[0064] (1) Cobalt internal standard X-ray fluorescence method detects the total iron content in iron material, comprises the following steps:

[0065] (1-1) The preparation of the cobalt-containing standard iron sample standard substance of known total iron and cobalt element content is as follows:

[0066] (1-1-1) Preparation of standard cobalt material: Weigh 90.0000g of lithium tetraborate, 15.0000g of lithium carbonate, and 10.000g of cobalt trioxide, mix them in a beaker and distribute them in 6 platinum crucibles. Add 10 drops of ammonium iodide solution to a crucible, put it into an electric heating melting furnace, shake and melt it at 1120°C for 20 minutes, take it out, and after cooling, crush it until the particle size is less than 0.150mm to obtain the standard cobalt material;

[0067] (1-1-2) Preparat...

Embodiment 2

[0089] X fluorescence cobalt internal standard-ICP cobalt compensation detects the method for total iron content in iron material, comprises the following steps:

[0090] (1), the cobalt internal standard X-ray fluorescence method detects the total iron in the iron material, and the specific operation steps are as follows:

[0091] Weigh 90.0000g of lithium tetraborate, 15.0000g of lithium carbonate, and 10.000g of cobalt trioxide, mix them in a beaker and distribute them in 6 platinum crucibles, add 10 drops of ammonium iodide solution to each crucible, put them into the Heating and melting the furnace at 1120°C for 20 minutes to shake and melt, take out, cool and crush until the particle size is less than 0.150mm, then the standard cobalt material can be obtained;

[0092] Weigh 5.000g of lithium tetraborate, 1.000g of lithium carbonate, 0.6000g of standard cobalt material, and 0.6000g of dry iron material sample, stir well and transfer to a platinum crucible, add about 5 dr...

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Abstract

The invention discloses a method for detecting the total iron content in an iron material by X fluorescent cobalt internal standard-ICP cobalt compensation. The method comprises the steps of: by usinga cobalt internal standard method, establishing an iron element working curve by an X-ray fluorescence method to detect the total iron content in an iron material, and calculating the compensation coefficient of cobalt for the total iron content based on a ratio of the iron element content to the element strength and the cobalt element strength; establishing a cobalt element working curve by using ICP spectroscopy to detect the content of cobalt elements in iron material; multiplying the cobalt element content by the compensation coefficient, and adding the product to the total iron content measured by the X-ray fluorescence method to obtain the total iron content in an iron sample to be detected. The method detect multiple elements simultaneously, detect a single sample within 18 minutes, has a detection speed nearly 10 times faster than a national standard method, a half detection cost of a national standard manual method, and a detection result error superior to a national standard.

Description

technical field [0001] The invention belongs to the technical field of iron and steel element detection, and in particular relates to a method for detecting total iron content in iron materials with X fluorescent cobalt internal standard-ICP cobalt compensation. Background technique [0002] Iron material is an important raw material for sintering, pelletizing and ironmaking in the process of iron and steel smelting. powder, iron-containing dust and other types. The main components in the iron material are TFe, SiO 2 、Al 2 o 3 、TiO 2 , S, P, Pb, Zn, K 2 0. Na 2 O, Mn and other elements add up to more than 99%. However, since the iron material belongs to the original mineral material, according to the different territories, such as Guangdong mine, Fujian mine, Jiangxi mine, Brazil mine, South Africa mine, Australia mine, India mine, secondary iron material, etc., the internal element content has certain difference. [0003] To detect the total iron content in iron ma...

Claims

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Application Information

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IPC IPC(8): G01N23/223G01N21/73
CPCG01N21/73G01N23/223G01N2201/129G01N2223/076G01N2223/652
Inventor 付志军曾波王涛张强李敏
Owner 新余钢铁股份有限公司
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