KR19980051244A - Ingot Analysis Method Using Luminescence Spectroscopy - 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 with excellent conductivity from the upper surface of the secondary electrode to the sample mounting table, and changes the circuit so that the sample mounting table acts 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 1-3 times and argon gas pressure 30 ~ Determining the element by measuring the luminous intensity of the element under a measurement condition of 50 psi, while measuring the segregation 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 under 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 sample contained in the sample. As an analytical method for quantifying the type and concentration of components, in this method, arcs and sparks are generated under a high voltage of 30 kV at a light emitting stand, but the result of the analysis of the sparks generated at this time has a decisive influence on the analysis result.

Conventionally, when ingots (ingots), steel structures, and slurries are analyzed with large samples with a non-uniform sample size, all samples must be cut and then the upper and lower surfaces should be polished. In addition to cutting at least 2 sides and 4 sides during the analysis, the upper part of the sample was rounded and the upper electrode was sharp when the sample was mounted on the analysis stand. In the presence of oxide slag or other foreign substances on the ground surface of the back of the sample, damage to the equipment may occur due to 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 this severe.

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, etc., and the elements are quantified by using an atomic absorption analyzer or a plasma emission analyzer. It was. 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 invention

2 is a schematic cross-sectional view of the device 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 the main parts of the drawings

1 ... high voltage cable 2 ... sample stand

3 ... ruler 4 ... secondary electrode

5 ... Ingots

According to the present invention, in the method for analyzing an ingot or steel structure sample using a luminescence spectrometer,

From the top of the secondary electrode, connect the metal cable with excellent conductivity to the sample holder and change the circuit so that the sample holder acts as the secondary electrode. Voltage 300V ~ 500V without using the secondary electrode, preheating time 1 Determination of the element by measuring the luminous intensity of the element under measurement conditions of ˜7 seconds, preburn time 1-5 seconds, stone 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 the segregation of the partial or a predetermined interval is measured using the ruler.

Hereinafter, the present invention will be described according to the needle drawing.

FIG. 1 is a schematic perspective view of an emission spectrometer for carrying out the method of the present invention. FIG. 2 is a schematic cross-sectional view of FIG. 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 shown. ) Is connected to the sample holder (2) to make the sample holder (2) to serve as a secondary electrode by changing 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 of less than 2000 is calculated under 300V, 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 that the intensity ratio is the highest from 1 second to 5 seconds, and after 5 seconds, the intensity ratio changes. 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, and when it is less than 8 seconds, the intensity ratio is about 3000, and when more 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 the highest intensity ratio when the number of detections is one to three times, and there is no change in the intensity ratio more than three times.

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 intensity ratio is the highest as 4000, and when the psi is below 40 psi, the strength ratio is very poor between 2000 -3000 and the intensity 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 measurement 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 has the highest strength in the range of 30 to 50 psi.

Example 2

The seven major elements of C, Si, Mn, P, S, So1-Al and Ti were analyzed 10 times on the steel sheets (pure iron) of the standards FN4A and N101, and the results are shown in Table 2 below. 5 is shown.

As shown in Tables 2 to 5, in the case of the standard FN4A, the standard deviation is C (0.0020), Si (0.0021), Mn (0.0044), P (0.0002), and S (0.0003), which is extremely excellent in accuracy and reproducibility. 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 is measurable by analytical methods.

Claims (2)

A method of analyzing an ingot or a steel structure sample using a luminescence spectrometer, wherein a secondary cable is changed by connecting a metal cable having excellent conductivity from the upper end surface of the secondary electrode to the sample holder to change the circuit to serve as the secondary electrode. Spark is induced without using an electrode, and a ruler is fixed on the mounting table, and the voltage is 300V to 500V, the preheat time is 1-7 seconds, the preburn time is 1-5 seconds, the analysis time is 8-20. The element is quantified by measuring the luminescence intensity of the element under the measurement conditions of 1 to 3 times of analysis detection times and 30 to 50 psi of argon gas pressure, and the segregation degree of the partial or constant interval is measured using the ruler. Ingot analysis method using luminescence spectrometer The method of claim 1, wherein the metal cable is made of copper.