Direct-reading spectrometer capable of simultaneously correcting and analyzing multiple control samples

Abstract

The invention relates to the field of direct-reading spectrometer element analysis. A direct-reading spectrometer suitable for simultaneous correction and analysis of multiple control samples comprises an input device, an analyzer body, a central processing unit, a storage device and a display device, and correction coefficients corresponding to different contents of multiple elements are stored in the storage device. An element needing to be analyzed is input through the input device, the analyzer body starts to analyze the initial content of the element in a sample to be detected and outputs the initial content to the central processing unit, the central processing unit compares the initial content with a corresponding element content interval in the storage device, and a correction coefficient corresponding to the element content interval corresponding to the initial content is obtained; and correcting the initial content according to the correction coefficient of the element content interval to obtain the corrected content.

Description

Technical Field

[0001] The invention relates to the field of element analysis using a direct-reading spectrometer. Background Art

[0002] Direct reading spectrometers are widely used in casting, steel, metal recycling, smelting, military industry, aerospace, electricity, chemical industry, colleges and universities, quality inspection and other fields due to their fast analysis speed, good precision and high accuracy. Direct reading spectrometers play an important role in the composition analysis of real-time samples of steel smelting. In the application of direct reading spectrometers, due to the limitations of the essential characteristics of spectral analysis, quality control samples with the same structure and similar composition must be selected for spectral analysis curve calibration according to different elements and different contents in the sample when performing sample analysis, so as to meet the accuracy requirements of element analysis of direct reading spectrometry. In actual production, since there are no quality control samples with full components that meet the requirements of sample analysis, it is often necessary to determine a main quality control sample, and then use one or more quality control samples to calibrate the main quality control sample, which brings multiple corrections and multiple analysis errors to the analysis results, affecting the stability of the analysis results. Especially under the current rapid development of artificial intelligence technology, the operation mode of manually selecting multiple quality control samples for calibration analysis can no longer meet the requirements of intelligent analysis, but seriously affects and restricts the analysis efficiency of the automated analysis system.

[0003] At present, through searching and documenting the spectrum analysis correction method, no literature has reported a better solution in the direct reading spectrum analysis of steel. Summary of the invention

[0004] The technical problem to be solved by the present invention is: how to use a direct-reading spectrometer to perform element analysis on a sample requiring multi-control sample calibration and obtain accurate results.

[0005] The technical solution adopted by the present invention is: a direct reading spectrometer suitable for simultaneous calibration and analysis of multiple control samples, including an input device, an analyzer body, a central processing unit, a storage device, and a display device. The storage device stores correction coefficients corresponding to different contents of multiple elements. During use, after the sample to be tested is placed in the analyzer body, the element to be analyzed is input through the input device, the analyzer body starts to analyze the initial content of the element in the sample to be tested and outputs it to the central processing unit, the central processing unit compares the initial content with the corresponding element content interval in the storage device, obtains the correction coefficient corresponding to the element content interval corresponding to the initial content, and then corrects the initial content according to the correction coefficient of the element content interval to obtain the corrected content, saves the analyzed element, the initial content, the correction coefficient, and the corrected content in the storage device and displays them through the display device, inputs the next element to be analyzed through the input device, and processes in the same way until all elements to be analyzed are analyzed.

[0006] The correction coefficient corresponding to each element content interval of each element is obtained according to the following steps

[0007] Step 1, prepare multiple verification samples containing XX element, the content of XX element in each verification sample is different, and the content of XX element ranges from 0 to 100% (excluding 0 and 100%), and the difference in the content of XX element in two verification samples is less than the difference set value;

[0008] Step 2: Place the verification sample in step 1 into the analyzer body in batches, analyze the measured content of each element with known element content in the verification sample through the analyzer body, and record the actual content and measured content of XX element in the verification sample during each analysis;

[0009] Step 3, establish a rectangular coordinate system with the point where the measured content and the actual content of the XX element are both 0 as the origin, the measured content of the XX element as the abscissa, and the actual content of the XX element as the ordinate;

[0010] Step 4, the actual content and the measured content of the XX element each time analyzed in step 2 are plotted in the rectangular coordinate system in step 3, and when the connecting line of multiple adjacent plotted points conforms to the same fitting formula, i.e., the correction formula, the measured content corresponding to the multiple adjacent plotted points is taken as an element content interval of the XX element, and all element content intervals of the XX element content from 0 to 100% are divided, and the correction formula constant corresponding to each element content interval is taken as the correction coefficient corresponding to the element content interval;

[0011] Step 5: Obtain the correction coefficient corresponding to each element content range of each element according to the method of steps 1 to 4.

[0012] The correction formula includes the following formula

[0013] Translation correction mode formula: C s =C s0 +K 1

[0014] Rotation correction mode formula: C s =C s0 *K 2

[0015] Among them, C s is the actual content, C s0 is the measured content, K 1 is the correction coefficient corresponding to the element content interval corresponding to the translation correction mode formula, K 2 It is the correction coefficient corresponding to the element content range corresponding to the rotation correction mode formula.

[0016] The beneficial effect of the present invention is that the present invention automatically matches the correction coefficient of the quality control sample with similar composition according to the different element types and contents in the actual sample for automatic analysis and calibration, so that the function of using different quality control sample element analysis and correction at the same time during the sample analysis can be realized, which greatly improves the efficiency of intelligent analysis, improves the intelligence level of the automatic analysis system, and realizes the intelligent and accurate analysis of each element in the sample. This can not only greatly improve work efficiency and shorten the sample analysis cycle, but also reduce smelting costs, shorten the smelting cycle, and promote the increase of output and cost reduction and efficiency improvement of steel smelting.

[0017] The present invention can complete the spectral analysis of multiple elements in the quality control sample through a direct-reading spectrometer, avoiding multiple errors and cumbersome operations caused by using multiple quality control sample corrections, realizing intelligent and accurate analysis of a wide range and multiple elements of real-time samples in steel smelting, shortening the analysis cycle and improving work efficiency.

[0018] Taking steel smelting analysis as an example, in production, one quality control sample often fails to meet the analysis requirements of the full range of components of the sample being analyzed, and more than two quality control samples are required for calibration analysis. This requires the use of multiple other quality control samples (the type and number of quality control samples to be used are determined according to the components of the sample being analyzed) in the calibration analysis of one quality control sample to perform manual calculations for translation or rotation correction, and manual addition and subtraction calculations in sample analysis. It is easy to make mistakes during use, especially when using multiple spectrometers to analyze samples, there will be different correction coefficients, which will bring hidden dangers to the accurate reporting of the results of the analyzed samples and affect the analysis efficiency.

[0019] The present invention utilizes a spectrum analyzer computer program, and realizes the function of correcting different elements of different content ranges by using different element contents of different quality control samples according to cross selection of different quality control samples, different analysis elements, and different correction modes. In actual analysis, after the quality control samples are calibrated, the correction coefficients of elements of different contents are stored in the analysis program. When analyzing samples, the use of quality control samples can be manually specified, or the program can automatically match the element correction coefficients of quality control samples with similar components according to the element content range of the analyzed samples, and report the analysis results. The present invention realizes the function of automatically using different quality control sample correction coefficients according to the different element contents of the samples.

[0020] Compared with the traditional analysis method, the present invention solves the problem that the composition of a quality control sample cannot fully meet the analysis requirements, and avoids the overlapping errors caused by multiple calibrations; compared with the traditional correction method, the present invention greatly reduces the hidden dangers of errors in the analysis and correction calculations, the analysis and correction method has a higher degree of freedom, a better sample analysis method, and a faster analysis speed. The use of the present invention can improve the automation and intelligent reporting level of the spectrometer, improve the online analysis efficiency of real-time samples in the steel smelting process, and improve the analysis accuracy. The use of the present invention has a strong practical value for promoting the increase in output and reducing costs and increasing efficiency in steel smelting. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is a schematic diagram of the process of the present invention. DETAILED DESCRIPTION

[0022] like Figure 1 As shown, first, according to the element type and composition range of the analyzed sample, select several quality control samples that meet the element type of the analyzed sample (determine whether there are interfering elements, and if necessary, analyze twice to get the results) and the composition analysis range, add the quality control samples and element contents to be used in the spectrometer, set the element calibration mode as needed, analyze the quality control samples, calibrate the instrument, and save the correction coefficients of each element of the quality control samples. According to the element type and composition range of the analyzed sample, manually set or intelligently match the quality control samples and corresponding elements to be used in the program, and different quality control samples can be selected for different elements. Analyze the tested sample on the spectrometer, and the tested sample automatically uses the quality control sample correction coefficient to perform correction analysis of different elements, display the analysis results, and automatically save the analyzed sample results and related information in the spectrometer, and complete the analysis for the reported analysis results.

[0023] The present invention is further illustrated by examples below. For the sake of simplicity and understanding, it is taken as an example that eight elements, namely carbon, silicon, manganese, phosphorus, sulfur, chromium, nickel and nitrogen, need to be reported for a steel smelting sample X (in actual analysis, more types of elements need to be reported, usually more than 20), but it is not limited to the following examples.

[0024] Example:

[0025] Table 1 lists the component range requirements of the analyzed samples and the types and components of the existing quality control samples that can be used. In this example, three quality control samples are selected for use: quality control sample a for calibration analysis of C, S, and Cr, quality control sample b for calibration analysis of Si and Ni, and quality control sample C for calibration analysis of Mn, P, and N.

[0026] Table 1 Requirements for the composition of the samples to be analyzed and the composition of the quality control samples to be used

[0027]

[0028] First, quality control samples a, quality control samples b, and quality control samples c are analyzed on the spectrum analyzer. The spectrum analysis results, correction modes, and correction coefficients of the quality control samples are listed in Table 2. In this example, except for the Cr element which uses the rotation correction mode, other elements use the translation correction mode. After the quality control sample analysis, the correction coefficients of each element are automatically saved in the analysis program of the spectrum analyzer. In this example, only the correction coefficients of the quality control sample elements that need to be used are listed in Table 2.

[0029] Table 2 Spectral analysis results of quality control samples, calibration modes and calibration factors to be used

[0030]

[0031] In this example, the quality control samples use two calibration modes: translation calibration and rotation calibration. The formulas for the two calibration modes are listed below:

[0032] Translation correction mode formula: C S1 =C S0 +(C K0 -C k1 )........................(1)

[0033] Rotation correction mode formula:

[0034] in:

[0035] C S1 : The corrected element content of the analyzed sample; C S0 : The element content of the analyzed sample before correction;

[0036] C K1 : Element content analysis value of quality control sample; C K0 : Certified value of element content in quality control samples;

[0037] (C K0 -C k1 ): QC sample translation correction factor; Correction factor for rotation of quality control samples.

[0038] The analyzed samples were analyzed on the spectrum analyzer. After the analysis, the content of each element in the sample was automatically corrected and the analysis results were reported. The analysis correction results of the analyzed samples are listed in Table 3.

[0039] Table 3 Analysis correction coefficients of analyzed samples and reported results after correction

[0040]

[0041]

[0042] In daily sample analysis, you can freely choose to use different elements of different quality control samples. After automatic calibration, the calibration coefficient is automatically saved in the analysis program. The analysis results are automatically corrected and reported to complete the analysis. There is no human intervention in the entire sample analysis process, ensuring the authenticity, reliability, accuracy and speed of the analysis results.

[0043] In the case of interference, a two-measurement method is used, and the measurement process is similar to the above.

Claims

1. A direct reading spectrometer for simultaneous calibration and analysis of multiple control samples, characterized in that: The analyzer comprises an input device, an analyzer body, a central processing unit, a storage device, and a display device. The storage device stores correction coefficients corresponding to different contents of multiple elements. During use, after the sample to be tested is placed in the analyzer body, the element to be analyzed is input through the input device, and the analyzer body starts to analyze the initial content of the element in the sample to be tested and outputs it to the central processing unit. The central processing unit compares the initial content with the corresponding element content interval in the storage device, obtains the correction coefficient corresponding to the element content interval corresponding to the initial content, and then corrects the initial content according to the correction coefficient of the element content interval to obtain the corrected content. The analyzed element, initial content, correction coefficient, and corrected content are stored in the storage device and displayed through the display device. The next element to be analyzed is input through the input device, and the process is performed in the same way until all elements to be analyzed are analyzed.

2. A direct reading spectrometer for simultaneous calibration and analysis of multiple control samples according to claim 1, characterized in that: The correction coefficient corresponding to each element content interval of each element is obtained according to the following steps Step 1: prepare multiple verification samples containing element XX, the content of element XX in each verification sample is different, and the content of element XX ranges from 0 to 100%, and the difference in the content of element XX between two verification samples is less than the difference set value; Step 2: Place the verification sample in step 1 into the analyzer body in batches, analyze the measured content of each element with known element content in the verification sample through the analyzer body, and record the actual content and measured content of XX element in the verification sample during each analysis; Step 3, establish a rectangular coordinate system with the point where the measured content and the actual content of the XX element are both 0 as the origin, the measured content of the XX element as the abscissa, and the actual content of the XX element as the ordinate; Step 4: Draw points on the rectangular coordinate system in step 3 for the actual content and measured content of the XX element each time analyzed in step 2. When the connecting line of multiple adjacent drawn points conforms to the same fitting formula, i.e., the correction formula, the measured content corresponding to the multiple adjacent drawn points is taken as an element content interval of the XX element, and all element content intervals of the XX element from 0 to 100% are divided, and the correction formula constant corresponding to each element content interval is taken as the correction coefficient corresponding to the element content interval; Step 5: Obtain the correction coefficient corresponding to each element content range of each element according to the method of steps 1 to 4.

3. A direct reading spectrometer for simultaneous calibration and analysis of multiple control samples according to claim 2, characterized in that: The correction formula includes the following formula Translation correction mode formula: C s1 =C s0 +K1 Rotation correction mode formula: C s1 = C s0 * K2 Among them, C s1 is the actual content, C s0 is the measured content, K1 is the correction coefficient corresponding to the element content interval corresponding to the translation correction mode formula, and K2 is the correction coefficient corresponding to the element content interval corresponding to the rotation correction mode formula.

4. A direct reading spectrometer for simultaneous calibration and analysis of multiple control samples according to claim 2, characterized in that: When the element to be measured in the sample to be tested has other interfering elements in the sample to be tested, the multiple verification samples containing XX element prepared in step one are all verification samples containing interfering elements, and the content of the interfering element in the verification sample is in the same interfering element content interval as the interfering element in the sample to be tested. The interfering element content interval is a content range of the interfering element. When the interfering element content is in its content range, the same influence will be produced during the measurement of the element to be tested, that is, compared with the presence of no interfering elements, when the element to be tested is in the interfering element content range, the actual measured content difference is a constant. When measuring the sample to be tested, firstly adopt conventional measurement, i.e., non-interference mode, and then adopt interference mode to measure again. When measuring again, the correction coefficient corresponding to the element content interval corresponding to the initial content is the interference correction coefficient corresponding to the element content interval corresponding to the initial content in the interfering element content interval, and the correction coefficient obtained when the element to be measured in the sample to be tested has other interfering elements in the sample to be tested is the interference correction coefficient.

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