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X fluorescence spectrum analysis method of siliceous slag conglomeration agent

A technology of fluorescence spectrum and slag gathering agent, which is applied in the field of inspection and testing, can solve the problems of inconsistency in observing the color of the indicator, difficulty in distinguishing the end point of titration, and incomplete dissolution of the sample, so as to shorten the measurement time and improve the accuracy of analysis. Effects with few types

Inactive Publication Date: 2013-09-04
ANGANG STEEL CO LTD
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Problems solved by technology

There are certain defects in this method: one is that chemical analysis adopts high-temperature melting in a nickel crucible and then acid leaching, which easily causes incomplete dissolution of the sample; when the filter paper is smashed, the test solution will splash; in the titration process, Due to the inconsistent observation of the color of the indicator, it is difficult to distinguish the titration end point, not only the procedure is cumbersome, but also the analysis error is large
It takes more than 4 hours to analyze a batch of samples, the analysis time is long, there are many interference factors, and the accuracy of the analysis is limited

Method used

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  • X fluorescence spectrum analysis method of siliceous slag conglomeration agent

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Experimental program
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Effect test

Embodiment 1

[0026] Sample preparation:

[0027] 1. Weigh 6.0000g lithium tetraborate and 0.1000g lithium fluoride reagent into a clean platinum pot, add 0.2000g sample, stir, add 5 drops of saturated potassium nitrate solution and 5 drops of 40% potassium iodide solution.

[0028] 2. Put the platinum pot containing the sample into the melting furnace and melt at 1145°C for 16 minutes.

[0029] 3. Remove the platinum pot and cool to room temperature.

[0030] Standard curve drawing:

[0031] 1. Select 10 national standard samples with a silica content in the range of 60-85wt% and a certain gradient as analysis samples.

[0032] 2. Follow the three steps of "sample preparation" to melt 10 national standard samples into glass samples.

[0033] 3. Set the analysis parameters of the X-ray fluorescence spectrometer.

[0034] a. X-ray tube voltage 40kV, current 70mA.

[0035] b. The elemental analysis time is 20s.

[0036] c. The selection range of pulse height is: PHA Low Level: 15, PHA H...

Embodiment 2

[0042] Sample preparation:

[0043] 1. Weigh 6.0000g lithium tetraborate and 0.1000g lithium fluoride reagent into a clean platinum pot, add 0.2000g sample, stir, add 5 drops of saturated potassium nitrate solution and 5 drops of 40% potassium iodide solution.

[0044] 2. Put the platinum pot containing the sample into the melting furnace, and melt it at 1150°C for 15 minutes.

[0045] 3. Remove the platinum pot and cool to room temperature.

[0046] Standard curve drawing:

[0047] 1. Select 10 national standard samples with a silica content in the range of 60-85wt% and a certain gradient as analysis samples.

[0048] 2. Follow the three steps of "sample preparation" to melt 10 national standard samples into glass samples.

[0049] 3. Set the analysis parameters of the X-ray fluorescence spectrometer.

[0050] a. X-ray tube voltage 40kV, current 70mA.

[0051] b. The elemental analysis time is 20s.

[0052] c. PHA Low Level: 15, PHA High Level: 130.

[0053] d. Spectro...

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Abstract

The invention provides an X fluorescence spectrum analysis method of a siliceous slag conglomeration agent. A lithium tetraborate reagent is taken as a fusion agent, samples are melted into glass sample sheets at a high temperature, then an X fluorescence spectrophotometer is used for drawing a national standard sample curve, and the intensity of a to-be-measured element is analyzed, so that the percentage composition of the to-be-measured element is calculated. Compared with a chemical analytical method, the process is simplified, the procedure is simple, the varieties of reagents are few, the detection cost can be reduced, the air quality is purified, and the standard curve can be drawn for one time and then can be used repeatedly; the measurement time can be shortened, the analysis time for each batch of samples can be saved by 3 hours, and the analysis efficiency is greatly improved; and analysis is performed by instruments instead of manual work, the analysis errors can be reduced, the analysis accuracy rate is improved, the interference factors are few, little influence on a machine body is caused, and the stability is good.

Description

technical field [0001] The invention belongs to the technical field of inspection and testing, and in particular relates to a method for measuring the content of elements in a siliceous slag collecting agent by using an X-ray fluorescence spectrometer. Background technique [0002] The so-called siliceous slag accumulator refers to a steelmaking auxiliary material with a silicon dioxide content of about 70%. At present, there are no detailed testing standards available in the country for the testing methods of siliceous slag accumulators. Therefore, various enterprises generally adopt chemical analysis methods for detection, that is, potassium fluorosilicate titration method is used to detect its content. There are certain defects in this method: one is that chemical analysis adopts high-temperature melting in a nickel crucible and then acid leaching, which easily causes incomplete dissolution of the sample; when the filter paper is smashed, the test solution will splash; i...

Claims

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Application Information

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IPC IPC(8): G01N23/223G01N1/28
Inventor 李奎王丽晖张道光
Owner ANGANG STEEL CO LTD
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