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Method for Determining Content of Impurity Elements in Alloy and Preparation Method of Sample Solution

A technology of impurity elements and sample solutions, applied in the preparation of test samples, etc., can solve problems such as inappropriateness, complicated and cumbersome operation, long inspection cycle, etc., and achieve the effect of ensuring reliability

Active Publication Date: 2018-09-11
PANGANG GROUP RESEARCH INSTITUTE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of chemical analysis method has technical shortcomings such as complicated and cumbersome operation, many interference factors, long inspection cycle, and low efficiency of single element determination, and cannot meet the requirements of fast and accurate determination of boron and other impurity elements in alloy materials such as silicon manganese, ferromanganese, and ferrosilicon. Content requirements, its technical principles and operating steps are not related to this program
Moreover, the sample preparation method of high-temperature melting of alkaline reagents used in chemical methods is not suitable for ICP-OES determination of the content of impurity elements such as boron, cobalt, chromium, copper, molybdenum, nickel, lead, titanium and other impurity elements in the sample digestion preparation solution, because the The method introduces a large amount of alkali metal ions such as sodium, which greatly increases the interference factors such as matrix effect and background effect, resulting in a decrease in the accuracy and precision of the test results.

Method used

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  • Method for Determining Content of Impurity Elements in Alloy and Preparation Method of Sample Solution
  • Method for Determining Content of Impurity Elements in Alloy and Preparation Method of Sample Solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Digestion of silicon-manganese alloy samples

[0053] Weigh 0.2g of the silicon-manganese alloy sample (hereinafter referred to as sample No. 1), add 4mL of undiluted concentrated nitric acid and 2mL of hydrogen peroxide to the cup wall by washing the cup wall, heat the reaction at high temperature and keep it in a boiling state for 4min ;Add 2mL of hydrogen peroxide to carry out strong oxidation reaction when the solution is boiling, and keep the solution boiling for 3 minutes; Add 4mL of concentrated hydrochloric acid and continue to react under high temperature heating and boiling until there is no brown smoke in the solution. The color gradually changes Shallow; wash the container wall with about 3mL water, and continue to react for 5min under the boiling state of the solution; wash the container wall with about 3mL water and cool the solution to 55°C, and keep the solution at a temperature range of 55°C on a low-temperature electric heating plate Add a total of 1m...

Embodiment 2

[0057] The sample to be digested is 0.5000g silico-manganese sample (hereinafter referred to as No. 2 sample), add 10mL concentrated nitric acid and 5mL hydrogen peroxide, react at high temperature and keep it in boiling state for 8min; add 5mL hydrogen peroxide again for strong oxidation and keep Boil for 5 minutes; add 10 mL of concentrated hydrochloric acid and boil at high temperature until no nitrogen dioxide brown smoke is generated; rinse the container with about 5 mL of water and evaporate the concentrated solution volume to about 5 mL; rinse the container with 5 mL of water and cool the solution to 57 ° C, and dissolve the solution Place it in a 57°C water bath to keep warm, and add a total of 2.5mL of hydrofluoric acid twice for reaction.

[0058] In addition, the silicon-manganese alloy sample was digested in the same manner as in Example 1, and the content of impurity elements was determined by ICP-OES.

Embodiment 3

[0060] The sample to be digested is 0.3000g ferromanganese alloy sample (hereinafter referred to as No. 3 sample), add 6mL concentrated nitric acid and 3mL hydrogen peroxide, react at high temperature and keep boiling for 5min; add 3mL hydrogen peroxide again for strong oxidation and keep boiling for 4min ;Add 6mL of concentrated hydrochloric acid and boil at high temperature until no brown smoke of nitrogen dioxide is produced; Rinse the container with about 4mL of water and evaporate the concentrated solution volume to about 5mL; Rinse the container with 5mL of water and cool the solution to 58°C, place the solution in Keep it warm in a water bath at 58°C, and add a total of 1.5mL of hydrofluoric acid twice for reaction.

[0061] Besides, the ferromanganese sample was digested according to the same method as in Example 1 and the content of impurity elements was determined by ICP-OES.

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Abstract

The invention relates to a method for determining the contents of impurity elements in alloy and a preparation method for a sample solution, belonging to the technical field of element detection. According to the invention, the sample solution is prepared by digesting a sample with nitric acid, hydrogen peroxide, hydrochloric acid and hydrofluoric acid according to specific steps; then ICP-OES is used for direct and simultaneous determination of the contents of impurity elements including boron, cobalt, chromium, copper, molybdenum, nickel, lead, titanium, phosphorus, etc. in the sample solution. The preparation method for the sample solution has the characteristics that sample digestion is complete and lossless; operation is rapid; an examination period is short; the prepared sample solution is simple in composition; the usage amount of reagents is small; blank is low; the number of interference factors is small; etc. The determination method has the advantages of few interference factors, high efficiency, rapidness and high precision, and meets demands for both product quality examination and control on the impurity elements in an alloy material.

Description

technical field [0001] The invention relates to a method for measuring the content of impurity elements in an alloy and a method for preparing a sample solution, belonging to the technical field of element detection. Background technique [0002] Silicon-manganese alloys, ferromanganese alloys and ferrosilicon alloys are necessary auxiliary materials in the iron and steel smelting process. They are most commonly used as alloy additives, composite deoxidizers or desulfurizers. In the past, the quality of such alloy products mainly focused on silicon and manganese. , phosphorus, aluminum, carbon, sulfur and other alloys or impurity components, with the continuous improvement of smelting control and steel quality requirements, gradually increasing the boron, cobalt, chromium, The product inspection requirements for the content of copper, molybdenum, nickel, lead, titanium and other impurity elements are becoming more and more stringent. The reason is that it has been found in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28
CPCG01N1/28
Inventor 成勇
Owner PANGANG GROUP RESEARCH INSTITUTE CO LTD
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