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Method for determining content of manganese, phosphorus, arsenic, potassium, sodium and copper in direct reduced iron

A technology for reducing iron and copper content, which is applied in the field of analysis and testing, can solve the problems of difficult measurement and achieve the effect of reliable method, good stability and high accuracy

Inactive Publication Date: 2011-11-23
WUKUN STEEL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Inductively coupled plasma atomic emission spectrometry is used for determination. Although multiple elements can be determined once a sample is dissolved, it saves time and effort, and does not need to consume a large amount of chemical reagents, which can reduce environmental pollution and protect the health of operators. Due to the difficulty of determination, there is currently no effective method for the determination of manganese, phosphorus, arsenic, potassium, sodium and copper in direct reduced iron

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment １

[0017] Prepare each of the following standard solutions:

[0018] 1. Preparation of manganese standard solution:

[0019] 1A. Wash commercially available electrolytic manganese (content above 99.9%) with sulfuric acid solution with a mass concentration of 4.9% until the surface is free of manganese oxide, then repeatedly wash with water, soak in absolute ethanol for 4 to 5 times, and dry ;

[0020] 1B, by the amount of 40mL / g electrolytic manganese, the above-mentioned dry electrolytic manganese is put into dilute nitric acid, wherein the volume ratio of dilute nitric acid is: HNO 3 : H 2 O=1: 3; heat and dissolve to boiling to drive off nitrogen oxides, cool, add water and dilute to 500 μg / mL to obtain manganese standard solution;

[0021] 1C. Pipette 10.00 mL of the manganese standard solution prepared in step 1B into a 100 mL volumetric flask, dilute to the mark with water, and shake well. This solution contains 25 μg / mL manganese;

[0022] 2. Preparation of phosphorus...

Embodiment 2

[0049] Determination of manganese, phosphorus, arsenic, potassium, sodium and copper in the direct reduced iron sample to be tested:

[0050] 1. Preparation of the DRI sample solution to be tested:

[0051] 1A. In 0.1000 g of the DRI sample to be tested, add 20 mL of a commercially available mixed acid of analytically pure hydrochloric acid and hydrofluoric acid in an amount of 200 mL / g of the sample, and heat at 100 °C until the sample dissolves. Obtain 10 mL of dissolving solution, wherein the mixed acid is the following volume ratio: HNO 3 :HF=19:1;

[0052]1B. Add 10 mL of commercially available analytically pure nitric acid to the 10 mL dissolving solution in step A at a volume of 1 mL / mL dissolving solution, and heat and dissolve at 100°C for 10 min to obtain 5 mL dissolving solution;

[0053] 1C. In the 5 mL solution of step B, add 5 mL of commercially available analytically pure perchloric acid in the amount of 1 mL / mL solution, and at 300 ℃, heat the perchloric aci...

Embodiment ２

[0058] Determination of manganese, phosphorus, arsenic, potassium, sodium and copper in the direct reduced iron sample to be tested:

[0059] 1. Preparation of the DRI sample solution to be tested:

[0060] 1A. To the 0.1000 g sample of direct reduced iron to be tested, add 50 mL of a commercially available mixed acid of analytically pure hydrochloric acid and hydrofluoric acid in an amount of 500 mL / g of the sample, and heat at 150°C until the sample dissolves. Obtain 20 mL of dissolving solution, wherein the mixed acid is the following volume ratio: HNO 3 :HF=19:1;

[0061] 1B. In the 20 mL solution of step A, add 30 mL of commercially available analytically pure nitric acid in an amount of 1.5 mL / mL solution, and heat and dissolve at 150°C for 15 minutes to obtain 10 mL of solution;

[0062] 1C. In the 10 mL solution of step B, add 15 mL of commercially available analytically pure perchloric acid in an amount of 1.5 mL / mL of the solution, and at 350 ℃, heat the perchlori...

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Abstract

The invention provides a method for determining the content of manganese, phosphorus, arsenic, potassium, sodium and copper in direct reduced iron. The method comprises the following steps: using the conventional inductive coupling plasma atomic emission spectrometry to determine spectral line strength of test sample liquid and getting the corresponding content values of the manganese, the phosphorus, the arsenic, the potassium, the sodium and the copper from standard working curves of the manganese, the phosphorus, the arsenic, the potassium, the sodium and the copper according to the spectral line strength, and the method is characterized by sequentially adding mixed acid of hydrochloric acid and hydrofluoric acid, nitric acid and perchloric acid into a test sample for dissolving, adding dilute hydrochloric acid for dissolving salts and filtering the dissolved liquid so as to prepare the test sample liquid. Not only is the operation convenient, but also the determined content of the manganese, the phosphorus, the arsenic, the potassium, the sodium and the copper is high in accuracy and the determination result further has good stability, reproducibility and accuracy. Tests prove that the method in the invention is reliable and practical and can meet the daily need of determining the content of the manganese, the phosphorus, the arsenic, the potassium, the sodium and the copper in the direct reduced iron.

Description

[0001] technical field [0002] The invention relates to a method for determining the content of manganese, phosphorus, arsenic, potassium, sodium and copper in directly reduced iron, and belongs to the technical field of analysis and testing. Background technique [0003] There is no quantitative analysis and determination method for the determination of manganese, phosphorus, arsenic, potassium, sodium and copper content in direct reduced iron. The content of other materials such as manganese, phosphorus, arsenic, potassium, sodium and copper in steel is mostly measured by spectrophotometry. Since different elements need different methods to complete the measurement, the operation is cumbersome and the analysis and measurement process is long. The inductively coupled plasma atomic emission spectrometry is used for the determination. Although the multi-element can be measured in one sample dissolution, it saves time and effort, and does not need to consume a lot of chemical...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N1/44G01N21/73
Inventor 陶俊曾海梅李玉清陈涛李文生许涯平郑玲王磊高玲高丽萍李宏萍
Owner WUKUN STEEL
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