JPH07113607B2 - Method of changing the setting of defective discharge surface of metal sample in emission spectroscopy - Google Patents

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for changing the setting of a defective discharge surface of a metal sample when the amount of an additive element or an intervening element in a metal material is analyzed by emission spectroscopy.

[0002]

2. Description of the Related Art Various metal materials are used in the industry, and various metal elements are added to improve and strengthen the characteristics of the metal. Alternatively, when the scrap metal is reused, the intervening metal elements are inevitably grasped. An emission spectroscopic analysis method is known as a method for analyzing the amount of an additive element or an intervening element in these metal materials.

For example, in the steelmaking process of the ironmaking industry, in the refining process, a sample mold is used during the refining operation in order to adjust the components such as 5 elements (carbon, silicon, manganese, sulfur, phosphorus) in the steel. A block-shaped sample having a cross section of 25 to 30 mmφ is taken, and the solidified sample is cut and polished using a predetermined sample preparation device to prepare a measurement surface for elemental analysis, and then an electric emission spectroscopic analysis device is used to produce an electric field within a range of 5 mmφ. Discharge is performed, elemental analysis is performed, the quality of refining is judged based on the analysis result, and the additional refining or the end of refining is determined. Therefore, a quick and accurate analysis result is required.

However, pinholes and inclusions such as oxides, which are generated during solidification of the sample, may be present on the analysis and preparation surface of the solidified metal sample. When this coagulated sample is attached to an emission spectrometer and analyzed by emission spectroscopy,
If pinholes or oxide exposed areas match the discharge area, or if pinholes or oxides hidden by the initial discharge appear, fatal defects that prevent analysis of the constituent elements for measurement Becomes

When the pinholes or oxidized inclusions exposed on the analysis and preparation surface of the solidified metal sample are large, the discharge position can be determined by avoiding the area, and the discharge position can be determined. If it is too small or hidden, proper wearing is not possible. In such a case, the discharge trace after discharge can be visually observed, and there may be a sensitive judgment as to whether the discharge trace is white or black. If it is lost, the analysis will be performed again, and the waiting time during the refining process will be extended by the amount of time required for the determination, the loss, and the decision.

In place of the above-mentioned direct visual judgment, a method may be considered in which the adjusted discharge surface or discharge trace is optically photographed by a camera or the like and is monitored, or these optical data are subjected to image processing using an electronic computer. However, it requires expensive equipment to improve the judgment accuracy and process in a short time,
Since the process of scanning the discharge traces after the discharge process is required, this scanning required time and calculation processing time are required, so it is not possible to follow the rapid measurement required in the refining process, and the emission spectroscopy analysis time can be extended. It is inevitable that it will be forced to be automated, or that human intervention will be required.

[0007]

SUMMARY OF THE INVENTION As described above, according to the present invention, it is inevitable that pinholes or oxide inclusions are exposed on the analytical preparation surface of a solidified metal sample.
In addition, it is assumed that it is unavoidable that the area where pinholes or oxide inclusions are exposed and the discharge area are stochastically unavoidable. In order to complete the appropriate emission spectroscopic analysis, the quality of the sample is promptly judged quantitatively, and in the case of a defective discharge surface, the discharge is stopped at the earliest possible time and the setting of the discharge surface of the metal sample is changed. Especially.

[0008]

The present invention provides (1) an emission spectroscopic analysis method in which a solidified metal sample collected from a molten metal is electrically discharged, and the intensity of emitted light is photoelectrically converted to quantify elements in the metal. In, the light intensity measurement value of the base metal element of the solidified metal sample in the discharge process is compared with the set light intensity value, and if the light intensity measurement values at multiple points do not reach the set light intensity value continuously, the discharge is stopped. A method for changing the setting of a defective discharge surface of a metal sample in emission spectroscopy, which comprises changing the discharge position of the solidified metal sample. (2) In an emission spectroscopic analysis method in which a solidified metal sample collected from a molten metal is electrically discharged, and the emitted light intensity is photoelectrically converted to quantify the elements in the metal, the base metal element of the solidified metal sample in the discharging process is analyzed. Counting the number of discharge pulses per set time corresponding to the light intensity measurement value of a predetermined threshold value or more, and stopping the discharge if the set number of discharge pulses is not reached, and changing the discharge position of the solidified metal sample Is a method of changing the setting of the defective discharge surface of the metal sample in the emission spectroscopic analysis.

[0009]

According to the present invention, when a solidified metal sample is discharged in an emission spectroscopic analysis method, if pinholes or oxide inclusions appear in the sample discharge area, the discharge tends to take precedence in that part. In addition, the light intensity value is weaker than the light intensity value in the normal discharge part, and when the pinholes or oxide inclusions that were not exposed are exposed by the preliminary discharge or the analytical discharge, the normal discharge part also shows. Focusing on showing a light intensity value that is weaker than the light intensity value of, the light intensity measurement value of the base metal element of the solidified metal sample in the discharge process is compared with the set light intensity value, and continuously measured at a plurality of points. When the measured light intensity value does not reach the set light intensity value, the discharge is stopped and the discharge position of the solidified metal sample is changed. Alternatively, the number of discharge pulses per set time corresponding to the light intensity measurement value of the base metal element of the solidified metal sample in the discharge process corresponding to a predetermined threshold value or more is counted, and if the set discharge pulse number is not reached, the discharge is stopped. However, since the discharge position of the solidified metal sample is changed, about 50 to 90% of the discharge required time in one emission spectroscopic analysis is not wasted, and a discharge for performing an appropriate emission spectroscopic analysis is immediately performed. Can be executed.
Also, if either of the above two means is adopted,
It is possible to set the metal sample in the emission spectroscopic analyzer and reset the metal sample at the time of defective discharge by an automatic machine operation without requiring manpower.

The present invention will be described below in detail with reference to the drawings. FIG. 1 is a schematic diagram showing the relationship between discharge time and light intensity in emission spectroscopic analysis. When the discharge surface of a solidified metal sample is normal, the light intensity of the base metal element is as shown in line (a). From the initial stage to the latter stage of discharge, the level remained strong with almost no change. However, if pinholes or oxide inclusions are exposed on the discharge surface,
Since there is a tendency that discharge in that part has priority,
As shown in the line (b), the light intensity of the base metal element was low, and the light intensity value in the early stage was low, and the light intensity value in the latter period showed a transition close to the value of the base metal element. Also,
Although not shown, pinholes, oxide inclusions, etc. do not appear on the discharge surface of the solidified metal sample, but even if pinholes or oxide inclusions appear during the discharge process, normal discharge part This is because the light intensity value is weaker than the light intensity value of.

Therefore, by performing signal processing using the light intensity at the time of discharge, it is possible to judge whether the discharge is normal or defective in the discharge process, so that the discharge is stopped without continuing the defective discharge and the solidified metal sample The discharge position can be changed promptly, and emission spectral analysis, that is, discharge can be restarted again.

Specifically, in the discharge process, when the light intensity measurement values at a plurality of points, for example, the light intensity measurement values at at least 100 points do not reach the set light intensity value continuously, it is determined that the discharge is defective. Discharge can be stopped. Since the light intensity values at a plurality of consecutive points used for determining the quality of discharge tend to approximate the light intensity value of the base metal element, which is too large, it is preferable to set it to 500 points.

Alternatively, as shown in FIG. 2, a set time corresponding to a light intensity measurement value of a base metal element of a solidified metal sample in a discharge process above a predetermined threshold value, for example, the number of discharge pulses per second, 3 Is counted and compared with a set discharge pulse number of the base metal element, for example, 300, and if the set discharge pulse number is not reached, the discharge can be judged to be defective discharge at this point and the discharge can be stopped.

Immediately after the discharge is stopped, the discharge position of the solidified metal sample is changed. The change of the discharge position of this solidified metal sample can be performed manually,
It is possible to efficiently and quickly carry out the first attachment setting of the solidified metal sample and the setting change for changing the discharge position based on the defective discharge by the automatic machine operation.

[0015]

INDUSTRIAL APPLICABILITY According to the present invention, when the elemental analysis of a metal material is carried out by emission spectroscopic analysis, the quality of the discharge surface of the prepared metal sample is determined by the light intensity value or the specific intensity of the base metal element obtained during the emission spectroscopic analysis. Since it is quantified by the count value of the discharge pulse, it can be accurately compared with the set value in the discharge process to accurately judge normal discharge or defective discharge.In the case of defective discharge, the discharge is stopped immediately and the discharge position of the discharge surface of the metal sample is determined. Since the replacement is performed, proper emission spectroscopic analysis can be achieved in a short time.
Therefore, in the case of man-operated operation and also in the case of automatic mechanical operation, only the discharge position of the metal sample is changed, and its industrial effect is great.

[Brief description of drawings]

FIG. 1 is a diagram showing a relationship between discharge time and light intensity in emission spectroscopic analysis.

FIG. 2 is an explanatory diagram of a mode of counting the number of discharge pulses corresponding to a light intensity measurement value equal to or higher than a predetermined threshold value.

Claims (2)

[Claims] 1. A base metal of a solidified metal sample in a discharge process in an emission spectroscopic analysis method for electrically discharging a solidified metal sample taken from a molten metal and photoelectrically converting emitted light intensity to quantify elements in the metal. The light intensity measurement value of the element is compared with the set light intensity value, and if the light intensity measurement values of a plurality of points do not reach the set light intensity value continuously, the discharge is stopped and the discharge position of the solidified metal sample is changed. A method of changing the setting of a defective discharge surface of a metal sample in an emission spectroscopic analysis, which is characterized in that: 2. A base metal of a solidified metal sample during a discharge process in an emission spectroscopic analysis method for electrically discharging a solidified metal sample taken from a molten metal and photoelectrically converting the emitted light intensity to quantify elements in the metal. Count the number of discharge pulses per set time corresponding to the light intensity measurement value above a predetermined threshold value of the element, stop the discharge if the set number of discharge pulses is not reached, and change the discharge position of the solidified metal sample A method of changing the setting of a defective discharge surface of a metal sample in an emission spectroscopic analysis, which comprises: