JPS5999336A - Sensitivity adjusting device for emission spectrochemical analysis apparatus - Google Patents

Abstract

PURPOSE:To alleviate the load of sensitivity adjusting work and to improve reliability in analysis, by storing the objective measured output of each element in a standard sample in a computer in advance, and increasing and decreasing the measuring sensitivity for each element step by step until the measured output of each element reaches the objective value. CONSTITUTION:The output of light measurement is inputted into a CPU, and whether the output is located in a specified range holding an objective value or not is judged in accordance with the attached Table. When the result is YES, whether those events have occurred three consecutive times or not is checked. When the result is YES, adjustment is finished. The set value of a sensitivity adjusting device 3 at this time is filed in a memory. When the result is NO, whether the sensitivity can be simply increased or decreased by one step or not is checked. When the result is YES, whether the sensitivity is lower than the objective range or not is checked. When the result is YES, the sensitivity is increased by +alpha. When the result is NO, the sensitivity is increased by -alpha. When the judgment is NO, a fraction of a sensitivity adjusting value, which is used for bringing the measured value within the objective range, is computed. Based on the result, the sensitivity adjusting device is controlled, the set sensitivity value is filed in the memory, and the adjusting operation for one element is finished.

Description

[Detailed description of the invention] The present invention relates to a sensitivity adjustment device for emission spectrometry.

When performing quantitative analysis of various elements in a sample by causing the sample to emit light by spark discharge, the emission intensity of each element is different, so it is necessary to appropriately set the measurement sensitivity for each element. The present invention relates to an apparatus for automatically setting measurement sensitivity for each element in luminescence analysis.

Quality control of materials manufactured by one device B, C, etc. The contents of these impurity elements are within their respective ranges; for example, element A varies in the range of 0.01 to 0.1%, and element B varies in the range of 0.5 to 2%. shall be. On the other hand, assuming that the luminescence intensity for the same content of both elements A and B is twice that of the element B, in this case, the ratio of the luminescence intensity is 0.02 to 0.2 for the element B and 0 for the element B. This means that the luminescence intensity of the two is approximately 10 times as large. In such a case, if the sensitivity of the analyzer is set so that the measured value does not exceed the scale of the B element, the A element will be said to be insufficiently sensitive. In order to use the analyzer efficiently, the maximum content of each element (normal maximum content, not abnormally large content) should be close to the maximum scale on the display of Analysis 81, and the displayed value should be Simple integer 5, 10 or 0
．． It is preferable to set the measurement sensitivity for each element such that multiplying by 1 or the like yields the actual value of the CH content. On the other hand, in emission spectroscopy, the sensitivity changes over time due to wear of the electrode facing the sample and the decrease in transmittance of the light entrance window of the spectrometer over time. Need to readjust.

To adjust the sensitivity described above, prepare a standard sample with a known and appropriate amount of element content, Conventionally, this adjustment has been done by the operator, but as mentioned above, sensitivity adjustment has to be done over and over again, which is a heavy burden on the analyst and can lead to incorrect sensitivity settings. There was something to be said.

The present invention aims to reduce the burden on the operator of sensitivity adjustment in emission spectrometry and to eliminate erroneous settings of sensitivity.

In the present invention, the use of a standard sample is the same as in the prior art. In the present invention, the computer stores the eye pillow measurement output of each element in the standard sample in advance, and runs the sensitivity adjustment program while making the standard sample emit light.
The computer increases or decreases the measurement sensitivity of each element one step at a time until the measurement output of each element reaches the target value. The present invention will be explained below with reference to Examples.

The following table shows the contents of the computer's memory as a table. It has 4 columns. The 3 columns on the left are data related to the standard sample, and the 1 column on the right is the sensitivity that changes each time the sensitivity is adjusted. This is the setting value of the regulator.

This example is for testing pig iron, and the elements to be analyzed are as shown in the first column on the left. Standard samples are A, B,
Three types are available: C. This is because for each element below carbon, it is preferable to use the highest content near the intermediate value of the variation in content as a standard sample, but it is not possible to obtain a sample that contains all the elements in appropriate amounts. , for example c,
Sample A is used for p and s, and sample B is used for Si and Mn. The third column is the displayed measured value that should be shown for each element when the standard sample is analyzed, and the computer operates the sensitivity adjuster corresponding to each element so that the displayed measured value becomes this value.

(blank below) FIG. 1 shows an entire apparatus according to an embodiment of the present invention.

1 causes the sample to emit light using a light source. Reference numeral 2 denotes a spectrometer, and photodetectors PI, P2, .

In the figure, the circuit configuration is shown with the photodetector P as a representative. The photometric output is sent to the computer CPU via an amplifier AMP and an A/D converter AD.

3 is a sensitivity adjuster for the photodetector. Sensitivity adjustment is done using amplifier A.
This can also be done by changing the amplification degree of MP.

The sensitivity adjuster is operated by the computer CP'U. T
is a computer console, and CRT is a display cathode ray tube used to interactively operate a computer.

When adjusting sensitivity, light source 1. Set the standard sample described above to emit light, and code the standard sample (A, B in the previous table).

C) is notified to the computer via the console T, the sensitivity adjustment mode is specified, and the program is started. When using A as a standard sample, the computer CPU
Perform the sensitivity adjustment operation on e, C, P, and S. FIG. 2 is a flowchart of a program for sensitivity adjustment operation for one element. When sensitivity adjustment is started, the photometric output is input to the CPU via the A/D converter AD (B), and it is checked whether or not the range has been obtained three times in a row (C).
, if it does not reach 3 times, return to X. 40 Judgment operation (B): If the judgment of ``Confucian'' is YES, go to the adjustment path ``S'' and file the setting value of the sensitivity adjuster at that time (4M on the right side of the previous table) in the memory.
If the answer is No, it is checked in (d) whether the sensitivity adjustment can be simply raised or lowered by -steps. The meaning of this operation is as follows. Sensitivity adjustment is not continuous, but is done step by step. Therefore, if you increase the sensitivity by one step, the measured value may exceed the target value range, and if you lower the sensitivity, the measured value may exceed the target range below. The answer is YES if you can increase or decrease the sensitivity.
become. Note that the reason for providing this determination step will be explained in detail later. Let us first describe the case where the judgment in (d) is YES. In (e), it is asked whether the sensitivity is below the 1" standard range, and if it is YES, the sensitivity is increased by +α (to).
If so, increase the sensitivity by -α (decrease by α) (1.). At N or (g), the updated sensitivity value is output to the sensitivity adjuster to execute sensitivity adjustment (ch), and the operation returns to point X. In this way, the sensitivity approaches the target value by α. Now, when the judgment in (d) is NO (this is the state reached by repeating the cycle of 2, E, H or 1, H, X), adjust the sensitivity to keep the measured value within the target range. The fraction of the value is calculated (
Based on this, the sensitivity adjuster is controlled (step), and the sensitivity setting value is filed in the memory through the Y point, and the adjustment operation for the - element is completed.

In the above-mentioned program, there are two routes by which the key Drk operation ends. One is a route that repeats the route (A) (Ol (C), X three times in a row) and the other is (21 (S1)
(nu) route. (d) In the (ul) route, after trimming is started so that the measurement output falls within the 11 standard range, the adjustment operation is immediately finished without checking three times. This is due to the following reason.If we consider the case where the determination in (d) is NO, there are two cases.

One is when the judgment in (b) becomes NO after going through the routes (a), (b), and (c) once or twice, and this is done by changing the sensitivity step by step by α. If the measured output falls within the target range at the final stage, but the sensitivity is set close to the upper or lower limit, repeating the check may cause it to fall outside the target range. Another case is when the sensitivity is changed by α and the measured output is near the upper and lower limits of the target range and the sensitivity is seven steps outside the target range.For example, if the sensitivity is too high and you lower it by α, it will fall within the target range. It falls below the lower limit of . In either of these two cases, when the sensitivity is changed by α, the measured output reaches a point close to the upper and lower limits of the target range. Therefore, in such a case, if you do not trim the path of (d) (libanun), you will not be able to escape from the state where (d) is No no matter how long it takes.On the other hand (narrow mouth) (c) three times (this is (as many times as you like)
If confirmation is omitted, it will not be possible to distinguish between a case where the sensitivity is set near the center of the target overheating range and a case where it is set near the upper and lower limits in the stepwise adjustment of the sensitivity.

With the above operations, the measurement sensitivity for each element is set to the target value, and the setting amount of the sensitivity adjuster at that time is stored in the memory as shown in the rightmost column of the previous table, until the sensitivity adjustment is performed again. - The set amount is maintained. The reason for storing this in memory is that test 71'='l is not just one type, and when analyzing samples of different types of total heat, the measurement sensitivity of each element is set to a different value, so It is not possible to restore the sensitivity.

The present invention has the above-described configuration, and the analyst can automatically set the sensitivity for each element simply by making the standard sample emit light and commanding the sensitivity adjustment, which reduces the burden of sensitivity adjustment work. 01 is reduced, errors in sensitivity setting are eliminated, and the reliability of analysis is improved.

[Brief explanation of drawings]

FIG. 1 is a block diagram of an apparatus according to an embodiment of the present invention, and FIG. 2 is a flow chart of the operation of the embodiment.

Claims (1)

[Claims] Memorize the target value of measurement output of each element in the standard sample1
Emission spectroscopy has a control circuit programmed to adjust the sensitivity of the analyzer so that the measured output of each element reaches the target value based on the data in the memory according to the sensitivity adjustment command. Sensitivity adjustment device for analyzers.