KR100205093B1 - Ingot analyzing method using emission spectrochemical analysis - Google Patents

Abstract

Provided are methods for analyzing ingots or steel structures by luminescence spectroscopy without further cutting samples.

This method connects a metal cable having excellent conductivity from the upper surface of the secondary electrode onto the sample mounting table, and changes the circuit so that the sample mounting table functions as a secondary electrode, thereby inducing spark without using the secondary electrode, and Fix the ruler to adjust voltage 300V ~ 500V, preheat time 1-7 seconds, preburn time 1-5 seconds, analysis time 8-20 seconds, analysis detection frequency, 1-3 times and argon gas pressure 30 Determining the element by measuring the luminous intensity of the element under the measurement conditions of ˜50 psi, while measuring the segregation degree of the partial or constant interval using the ruler.

According to the method of the present invention, the segregation degree between the quantitative analysis and the partial or constant interval of the sample can be measured quickly and accurately.

Description

Ingot Analysis Method Using Luminescence Spectroscopy

The present invention relates to an ingot analysis method using luminescence spectroscopy, and more particularly, it is possible to quickly and accurately measure the quantitative analysis of the sample and the segregation degree between partial or total intervals without cutting a large sample such as an ingot (ingot) or steel structure. An ingot analysis method using luminescence spectroscopy.

In the emission spectrochemical analysis, a high voltage of about 30 kV is applied to the surface of a metal sample in an inert gas atmosphere such as argon to generate an inherent spectrum for each element, and convert the light energy at that time into electrical energy to contain each component contained in the sample. In this method, an arc and spark are generated under a high voltage of 30 kV in a light emitting stand, but the result of the analysis is decisively affected by the presence or absence of the spark generated at this time.

Conventionally, in the case of analyzing large samples with inconsistent sample sizes such as ingots or steel structures, after cutting all samples, the upper and lower surfaces should be polished. In addition, at least two or more four sides should be cut at the time of mounting, and when the sample was mounted on the analysis stand, the upper part of the sample was rounded and the upper electrode was sharp, so that a source error occurred frequently. In the presence of oxide slag or other foreign substances on the ground surface of the back of the sample, equipment damage is caused by arc discharge, resulting in a long recovery time. Especially when cutting high carbon steel, pinholes and unevenness are severe, and irregularities in the center of the sample There was a problem of light leakage.

Due to these problems, when analyzing ingots or steel structures in the related art, the parts to be analyzed are cut in detail, processed into chips, liquefied with an acid solution, and the elements are quantified by using an atomic absorption analyzer or a plasma emission analyzer. . However, there are many problems due to the delay of analysis for samples of melting work or samples of field products that require rapid analysis.

Accordingly, an object of the present invention is to provide a method of solving the above-mentioned conventional problems by luminescence spectroscopy quickly and accurately without cutting the ingot or steel structure sample in detail.

This object of the present invention can be achieved by changing the secondary power source circuit of the luminescence analyzer and deriving the measurement conditions most suitable for the analysis of ingots or steel structures.

1 is a schematic perspective view of an apparatus used in the method of the present invention.

2 is a schematic cross-sectional view of the apparatus of FIG.

3A to 3F are graphs showing changes in luminescence intensity according to measured voltage, preheating time, analysis time, analysis detection frequency and argon gas pressure difference in the implementation of the method of the present invention.

* Explanation of symbols for main parts of the drawings

1: high voltage cable 2: sample stand

3: ruler 4: secondary electrode

5: ingot (ingot)

According to the invention,

In the method of analyzing ingot or steel structure sample using a luminescence spectrometer,

Change the circuit to connect the sample holder as a secondary electrode by connecting a metal cable with excellent conductivity from the upper surface of the secondary electrode to the sample holder, so that the voltage is 300V to 500V without using the secondary electrode. Determination of the element by measuring the luminous intensity of the element under measurement conditions of ˜7 seconds, preburn time 1-5 seconds, analysis time 8-20 seconds, analysis detection frequency 1-3 times and argon gas pressure of 30-50 psi On the other hand, there is provided an analysis method using a luminescence spectrometer, characterized in that for measuring the segregation degree of a partial or a predetermined interval using the ruler.

Hereinafter, the present invention will be described with reference to the accompanying drawings.

Figure 1 is a schematic perspective view of a luminescence spectrometer for carrying out the method of the present invention, Figure 2 is a schematic cross-sectional view of Figure 1, in the method of the present invention, a copper cable (1) having excellent conductivity on the top surface of the secondary electrode (4) ) Is connected on the sample holder (2) to make the sample holder (2) to serve as a secondary electrode to change the circuit to induce sparks without using the secondary electrode, ruler (300mm horizontal, 300mm vertical) ) To fix the luminescence intensity of the element under the measurement conditions shown in Table 1 below to quantitate the element and measure the segregation between partial or regular intervals using a ruler.

The reason for limiting the voltage to 300V-500V under the above measurement conditions is that the emission intensity ratio is the highest when the voltage is 300V-500V, while the intensity ratio is less than 2000 when 300V or less is calculated, and the analysis is impossible. This is because a lot of heat is generated without giving. The reason for limiting the flush time to 1 second to 7 seconds is because the intensity ratio is the highest at 1 second to 7 seconds and the intensity ratio does not rise after 7 seconds, but heat is generated in the sample. The reason for limiting the preburn time to 1 second to 5 seconds is because the intensity ratio from 1 second to 5 seconds is the highest and there is no change in intensity ratio after 5 seconds. The reason for limiting the analysis time to 8 seconds to 20 seconds is the highest intensity ratio when the analysis time is from 8 seconds to 20 seconds. When it is less than 8 seconds, the intensity ratio is about 3000, and when the temperature is longer than 20 seconds, a lot of heat is generated in the sample.

The reason for limiting the number of analysis detections to one to three times is that when the number of detections is one to three times, the highest intensity ratio is shown.

The reason for limiting the argon gas pressure to 30 psi-50 psi is that when the argon gas pressure is 30 psi to 50 psi, the strength ratio is highest at 4000, and when the pressure is below 40 psi, the strength ratio is very poor between 2000-3000, and the strength ratio no longer increases even when the pressure is above 50 psi. Will not.

Hereinafter, embodiments of the present invention will be described.

Example 1

According to the method of the present invention, the ingot was analyzed using the apparatus of FIG. 1 while varying the measured voltage, preheating time, preliminary emission time, analysis time, analysis detection frequency and argon gas pressure, and the emission intensity was measured. The results are shown in Figures 3a to 3f.

3A to 3F, the measured voltage is 300 to 500 V, the preheating time is 1 to 7 seconds, the preliminary emission time is 1 to 5 seconds, the analysis time is 8 to 20 seconds, the analysis detection frequency is 1 to 3 times, and argon gas. It can be seen that the pressure is the highest in the range of 30 to 50 psi.

Example 2

Analyze the seven major elements of C, Si, Mn, P, S, Sol-Al, Ti 10 times according to the method of the present invention on the steel sheet (pure iron) of the standards FN4A, N101, and the results are shown in Table 2 below. 5 is shown.

As shown in Tables 2 to 5, the standard deviation of the standard material FN4A is C (0.0020), Si (0.0021), Mn (0.0044), P (0.0002), and S (0.0003). In the case of standard material N101, the standard deviation was C (0.0010), Si (0.0082), Mn (0.0070), P (0.00052), S (0.00073), Sol-Al (0.00094), Ti (0.00073) In addition, it was confirmed that the accuracy and reproducibility are extremely excellent. In the case of the present invention, the analysis time per specimen is about 3 minutes, and in the case of atomic absorption spectroscopy or plasma emission spectrometry, which is a conventional wet method, it takes about 8 hours. Therefore, the present invention is extremely superior to the conventional method. there was.

As described above, according to the method of the present invention, by changing the circuit of the secondary power supply and using a ruler, the quantitative analysis of the sample and the segregation degree between the partial or predetermined intervals can be quickly and accurately, without further cutting the large sample such as the ingot or the steel structure. It can be measured by analytical methods.

Claims (2)

In the method of analyzing ingot or steel structure sample using a luminescence spectrometer, By connecting a metal cable with excellent conductivity from the upper surface of the secondary electrode to the sample holder and changing the circuit so that the sample holder functions as the secondary electrode, sparks are induced without using the secondary electrode, and the ruler is fixed to the substrate. A voltage of 300 V to 500 V, a preheat time of 1 to 7 seconds, a preburn time of 1 to 5 seconds, an analysis time of 8 to 20 seconds, an analysis detection frequency of 1 to 3 times, and an argon gas pressure of 30 to 50 psi Ingot analysis method using a luminescence spectrometer, characterized in that by measuring the luminous intensity of the element under the measurement conditions to quantify the element, the segregation of the partial or a predetermined interval using the ruler The method of claim 1, wherein the metal cable is made of copper.