A method for multi-standard steel inverse distance weighted correction of photoelectric direct-reading spectral measurements

Abstract

This invention relates to the field of metal or alloy element content measurement technology, specifically to a method for correcting photoelectric direct-reading spectroscopic measurements using multi-standard steel inverse distance weighting. This method is applied to a photoelectric direct-reading spectrometer to obtain corrected photoelectric direct-reading spectroscopic measurements of a test sample, and includes the following steps: selecting multiple sets of test standard steels for measurement to obtain the sample measurement value and the multiple sets of standard steel measurement values; obtaining multiple sets of standard steel correction values ​​based on the multiple sets of standard steel measurement values ​​and the standard values ​​of the test standard steels; calculating the absolute difference between the multiple sets of standard steels; obtaining the inverse distance weight based on the absolute difference between the multiple sets of standard steels; obtaining the sample correction value based on the multiple sets of standard steel correction values ​​and the inverse distance weight λ; and summing the sample measurement value and the sample correction value to obtain the corrected photoelectric direct-reading spectroscopic measurement value. This invention can quickly and accurately correct the measured values ​​of a sample, reduce the method error caused by the calibration of a single standard steel, and improve the accuracy of measurements obtained using a photoelectric direct-reading spectrometer.

Description

Technical Field

[0001] This invention relates to the field of metal or alloy element content measurement technology, specifically to a method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values. Background Technology

[0002] Photoelectric direct-reading spectrometers utilize controlled electric arcs and sparks to excite metal samples and generate characteristic spectra. Based on the wavelength and intensity of the characteristic spectra of each element received by photoelectric conversion, multi-element qualitative and quantitative analysis is performed. It features fast analysis speed and high precision, and can quickly analyze the content of major and trace elements in metal and alloy samples. It is widely used for rapid analysis before furnaces. The accuracy of test results can be improved by calibration with standard steel.

[0003] Currently, the correction of measurements by direct-reading photoelectric spectrometers mainly adopts the linear correction method using a single standard steel with elemental content similar to that of the sample. This method has a large measurement error, which is manifested in the difficulty of ensuring that the selected standard steel is the same grade as the sample. On the other hand, the linear correction method using a single standard steel is prone to amplifying the one-way error of the measurement value.

[0004] In existing technologies, Lu Guibo et al. disclosed "Analysis of OCrBNi5Mo using a Direct-Reading Photoelectric Spectrometer" (Chemical Engineer, 1 / 2000), which specifically disclosed the use of direct-reading photoelectric spectrometer analysis results to find the regularity of deviation from chemical analysis results, correct the instrument's working curve according to the found regularity, and use the corrected curve to analyze the sample. The correction method disclosed therein is translation correction, and the measured values ​​still have a large error.

[0005] Luo Xiaoyan published "A Discussion on the Standardized Sample Replacement Principle of Photoelectric Direct-Reading Spectrometer" (Nonferrous Metals Processing, December 2008), which specifically disclosed the use of a linear equation for correction. This method, also based on the instrument's linear correction, amplifies the one-way error of the measured values.

[0006] Therefore, it is of great significance to provide a new method for correcting photoelectric direct-reading spectral measurements using multi-standard steel inverse distance weighting. Summary of the Invention

[0007] To overcome the above-mentioned technical deficiencies, this invention provides a method for correcting photoelectric direct-reading spectroscopic measurement values ​​using multiple sets of standard steels with inverse distance weighting. This method uses multiple sets of standard steels and corrects the sample measurement values ​​based on inverse distance weighting. It can quickly and accurately correct the measured values ​​of the sample, reduce the method error caused by the calibration of a single standard steel, and improve the accuracy of the measurement values ​​obtained using a photoelectric direct-reading spectrometer.

[0008] A method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​is applied to a photoelectric direct-reading spectrometer to obtain photoelectric direct-reading spectral correction measurement values ​​of the content of multiple target elements in a test sample. The method includes the following steps:

[0009] a. Select multiple sets of test standard steels, and use a photoelectric direct-reading spectrometer to measure the contents of the test sample and the multiple sets of test standard steels to obtain the sample measurement values ​​and multiple sets of standard steel measurement values ​​X of the content of multiple target elements. 测量 ;

[0010] b. Based on the multiple sets of standard steel measurement values ​​X from step a 测量 and the corresponding test standard value X 标准 Obtain multiple sets of standard steel correction values ​​Δ b ;

[0011] c. Calculate the multiple sets of standard steel measurement values ​​X in step a. 测量 Multiple sets of absolute differences L between the measured values ​​of the standard steel samples were obtained.

[0012] d. Obtain the inverse distance weight λ based on the absolute differences L of multiple sets of standard steel samples from step c;

[0013] e. Based on the multiple sets of standard steel correction values ​​Δ from step b b The sample correction value Δ is obtained by combining the inverse distance weight λ from step d. x ;

[0014] f. Based on the sample measurement value from step a and the sample correction value Δ from step e. x Summing these values ​​yields the photoelectric direct-reading spectral correction measurements of the content of multiple target elements.

[0015] Based on the standard value X of the element in the test steel 标准 Measurement value X of standard steel 测量 Obtain the standard steel correction value Δ for the elements in the test standard steel. b ;

[0016] Calculate the measured value X of the standard steel. 测量 The absolute difference L between the measured values ​​of the sample and the absolute difference L is used to obtain the inverse distance weight λ of the elements in the test steel.

[0017] According to the standard steel correction value Δ b The sample correction value Δ for the element content in the test sample is obtained by combining the inverse distance weight λ. x ;

[0018] Based on the sample measurement value and the sample correction value Δ x Obtain photoelectric direct-reading spectral correction measurement values.

[0019] In one specific embodiment of the present invention, step a, the selection of the test standard steel is determined based on the predicted content of the main elements in the sample to be tested.

[0020] In one specific embodiment of the present invention, the content of major elements in the test standard steel is 0.5 to 1.5 times the predicted content of each major element in the test sample.

[0021] In this invention, the content of each major element in the test standard steel is 0.5 to 1.5 times the predicted content of each major element in the test sample. Multiple sets of standard steels that meet the aforementioned requirements are selected as test standard steels. Of course, the target elements include all major elements.

[0022] In one specific embodiment of the present invention, more preferably, there are at least two sets of test standard steels, wherein the main element content of at least one set of test standard steels is 0.5 to 1 times the predicted result of the main element content of the sample to be tested, and the main element content of at least one set of test standard steels is 1 to 1.5 times the predicted result of the main element content of the sample to be tested.

[0023] In one specific embodiment of the present invention, the standard steel measurement value X 测量 The method involves using a photoelectric direct-reading spectrometer to perform parallel measurements on the standard steel multiple times and then calculating the average value.

[0024] In one specific embodiment of the present invention, the test standard steel is measured in parallel 3 to 10 times.

[0025] In one specific embodiment of the present invention, the test standard steel is measured in parallel six times.

[0026] In one specific embodiment of the present invention, the sample measurement value is obtained by measuring the test sample multiple times in parallel using a photoelectric direct-reading spectrometer and calculating the average value.

[0027] In one specific embodiment of the present invention, the number of parallel measurements of the test sample is 3 to 10.

[0028] In one specific embodiment of the present invention, the test sample is measured in parallel 6 times.

[0029] In one specific embodiment of the present invention, the standard steel correction value Δ b To test the standard value X of the steel. 标准 Compared with the standard steel measurement value X 测量 The difference is calculated using the following formula 1:

[0030] Formula 1: Δ b =X 标准 -X 测量 .

[0031] In one specific embodiment of the present invention, the inverse distance weight λ is calculated based on the following formula 2:

[0032] Formula 2:

[0033] Where L represents the absolute difference of the standard steel, i represents the target element, k represents the ordinal number of the test standard steel, and n represents the total number of test standard steel groups.

[0034] In one specific embodiment of the present invention, the sample correction value Δ x Calculated based on the following formula 3:

[0035] Formula 3:

[0036] Where i represents an element, r represents the number of test standard steels, and n represents the number of test standard steel groups.

[0037] In one specific embodiment of the present invention, the method further includes performing type normalization calibration on the photoelectric direct-reading spectrometer before step a, the type normalization calibration including the following steps:

[0038] 1) Select standardized calibration steel based on the predicted content of major elements in the sample to be tested;

[0039] 2) Preset the measurement deviation threshold, and obtain multiple calibration measurement values ​​by repeatedly measuring the standardized calibration standard with the photoelectric direct-reading spectrometer. If the deviation of the multiple calibration measurement values ​​is less than the measurement deviation threshold, the type standardization calibration of the photoelectric direct-reading spectrometer is qualified.

[0040] If the deviation of multiple calibration measurements exceeds the measurement deviation threshold, adjust the operating parameters of the photoelectric direct-reading spectrometer and / or treat the surface of the standardized calibration steel, and then perform multiple parallel measurements using the photoelectric direct-reading spectrometer until the deviation of multiple calibration measurements is less than the measurement deviation threshold.

[0041] In one specific embodiment of the present invention, the content of the main elements in the standardized calibration steel is 0.8 to 1.3 times that in the main element content of the test sample.

[0042] In one specific embodiment of the present invention, the measurement deviation threshold is 0.005%.

[0043] In one specific embodiment of the present invention, the number of parallel measurements of the standardized calibration steel is 3 to 10.

[0044] In one specific embodiment of the present invention, the standardized calibration steel is measured in parallel six times.

[0045] The beneficial effects of this invention are as follows: This invention calculates the correction value of the standard steel by using the difference between the standard value and the measured value of multiple sets of test standard steels, then obtains the inverse distance weight by using the absolute difference between the measured value of the standard steel and the measured value of the sample, and obtains the correction value of the sample by using the inverse distance weight and the correction value of the standard steel, thereby obtaining the photoelectric direct-reading spectral measurement value, reducing method error and improving the accuracy of photoelectric direct-reading spectral measurement value. Attached Figure Description

[0046] Figure 1 This is a schematic diagram illustrating the principle of a method for correcting photoelectric direct-reading spectral measurements using two sets of test steel with inverse distance weighting, as described in an embodiment of the present invention.

[0047] Figure 2 This is a line graph showing the relative deviation results of the linear correction for single-standard steel and the inverse distance weight correction for multi-standard steel according to the present invention. Detailed Implementation

[0048] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be described in detail below. Obviously, the described embodiments are merely some embodiments of this invention, and not all embodiments. Based on the embodiments of this invention, all other implementation methods obtained by those skilled in the art without creative effort are within the scope of protection of this invention.

[0049] A method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​is applied to a photoelectric direct-reading spectrometer to obtain photoelectric direct-reading spectral correction measurement values ​​of the content of multiple target elements in a test sample. The method includes the following steps:

[0050] a. Select multiple sets of test standard steels, and use a photoelectric direct-reading spectrometer to measure the contents of the test sample and the multiple sets of test standard steels to obtain the sample measurement values ​​and multiple sets of standard steel measurement values ​​X of the content of multiple target elements. 测量 ;

[0051] b. Based on the multiple sets of standard steel measurement values ​​X from step a 测量 and the corresponding test standard value X 标准 Obtain multiple sets of standard steel correction values ​​Δ b Test standard value X of steel 标准 The results show the content of the target elements obtained based on chemical composition analysis methods.

[0052] c. Calculate the multiple sets of standard steel measurement values ​​X in step a. 测量 Multiple sets of absolute differences L between the measured values ​​of the standard steel samples were obtained.

[0053] d. Obtain the inverse distance weight λ based on the absolute differences L of multiple sets of standard steel samples from step c;

[0054] e. Based on the multiple sets of standard steel correction values ​​Δ from step b bThe sample correction value Δ is obtained by combining the inverse distance weight λ from step d. x ;

[0055] f. Based on the sample measurement value from step a and the sample correction value Δ from step e. x Summing these values ​​yields the photoelectric direct-reading spectral correction measurements of the content of multiple target elements.

[0056] In this invention, the results obtained in step af are all measured or calculated based on a single target element. Taking the target element Cr (chromium) in the test sample as an example, multiple sets of test standard steels containing Cr are selected. The test sample and multiple sets of test standard steels are measured using a photoelectric direct-reading spectrometer to obtain the sample measurement value of Cr and the multiple sets of standard steel measurement values ​​of Cr. Based on the multiple sets of standard steel measurement values ​​and the standard value of Cr in the test standard steels, the standard steel correction value of Cr for each set of test standard steels is calculated. The number of standard steel correction values ​​is the same as the number of test standard steels. Based on the multiple sets of standard steel measurement values ​​and the sample measurement value, the multiple sets of standard steel absolute differences of Cr are calculated. Based on the multiple sets of standard steel absolute values, multiple sets of inverse distance weights are calculated. Based on the multiple sets of inverse distance weights and the standard steel correction value, the product is multiplied and summed to obtain the unique sample correction value corresponding to Cr. The sum of the sample correction value and the sample measurement value is calculated to obtain the photoelectric direct-reading spectroscopic correction measurement value of Cr.

[0057] When the target elements are Cr (chromium) and Mn (manganese), the photoelectric direct-reading spectral correction measurement values ​​of Cr and Mn are obtained respectively according to the aforementioned method.

[0058] In some instances, step a, the selection of the test standard steel, is determined based on the predicted content of the main elements in the sample to be tested.

[0059] In some instances, the content of major elements in the test standard steel is 0.5 to 1.3 times the predicted content of each major element in the test standard steel.

[0060] In some instances, there are at least two sets of test standard steels, wherein the content of the main element in at least one set of test standard steels is 0.5 to 1 times the predicted result of the main element content of the sample to be tested, and the content of the main element in at least one set of test standard steels is 1 to 1.2 times the predicted result of the main element content of the sample to be tested.

[0061] In some instances, step a, the standard steel measurement value X 测量 To obtain the results of multiple parallel measurements of the standard steel using a photoelectric direct-reading spectrometer and the calculation of the average value.

[0062] In some instances, the test standard steel is measured in parallel 3 to 10 times.

[0063] In some instances, the test standard steel was measured in parallel six times.

[0064] In some instances, the sample measurement values ​​are obtained by taking multiple parallel measurements of the test sample using a photoelectric direct-reading spectrometer and calculating the average value.

[0065] In some instances, the test sample is measured in parallel 3 to 10 times.

[0066] In some instances, the test sample was measured in parallel six times.

[0067] In some instances, step b, the standard steel correction value Δ b To test the standard value X of the steel. 标准 Compared with the standard steel measurement value X 测量 The difference is calculated using the following formula 1:

[0068] Formula 1: Δ b =X 标准 -X 测量 .

[0069] In some instances, in step d, the inverse distance weight λ is calculated based on the following formula 2.

[0070] In some instances, the inverse distance weight λ is calculated based on the following formula 2:

[0071] Formula 2:

[0072] Where L represents the absolute difference of the standard steel, i represents the target element, k represents the ordinal number of the test standard steel, and n represents the total number of test standard steel groups.

[0073] In some instances, step e, the sample correction value Δ x Calculated based on the following formula 3:

[0074] Formula 3:

[0075] Where i represents the target element, r represents the ordinal number of the test standard steel, and n represents the total number of test standard steel groups.

[0076] In some instances, the method further includes performing a type normalization calibration on the photoelectric direct-reading spectrometer prior to step a, the type normalization calibration comprising the following steps:

[0077] 1) Select standardized calibration steel based on the predicted content of major elements in the sample to be tested;

[0078] 2) Preset the measurement deviation threshold, and obtain multiple calibration measurement values ​​by repeatedly measuring the standardized calibration standard with the photoelectric direct-reading spectrometer. If the deviation of the multiple calibration measurement values ​​is less than the measurement deviation threshold, the type standardization calibration of the photoelectric direct-reading spectrometer is qualified.

[0079] If the deviation of multiple calibration measurements exceeds the measurement deviation threshold, adjust the operating parameters of the photoelectric direct-reading spectrometer and / or treat the surface of the standardized calibration steel, and then perform multiple parallel measurements using the photoelectric direct-reading spectrometer until the deviation of multiple calibration measurements is less than the measurement deviation threshold.

[0080] It should be noted that adjusting the operating parameters of the photoelectric direct-reading spectrometer includes adjusting the pressure or input of the working gas, adjusting the pressure or temperature of the optical chamber, etc.; treating the surface of the standardized calibration steel includes grinding or cleaning the surface of the standardized calibration steel to remove surface oxides, etc. Adjusting the operating parameters of the photoelectric direct-reading spectrometer is beneficial to the stability of the operating parameters when testing the sample. By treating the surface of the standardized calibration steel, it is possible to avoid the problem of unclean standardized calibration steel surface affecting the stability of the operating parameters of the photoelectric direct-reading spectrometer.

[0081] In some instances, the elemental content of the standardized calibration steel is 0.8 to 1.5 times that of the elemental content in the test sample.

[0082] In some instances, the measurement deviation threshold is 0.005%.

[0083] In some instances, the standardized calibration steel is measured in parallel 3 to 10 times.

[0084] In some instances, the standardized calibration steel is measured in parallel six times.

[0085] The present invention also provides a system for multi-calibrated steel inverse distance weighted correction photoelectric direct-reading spectral measurements, and a method for implementing multi-calibrated steel inverse distance weighted correction photoelectric direct-reading spectral measurements, the system comprising:

[0086] The standardized calibration unit for the photoelectric direct-reading spectrometer is used to determine whether the standardized calibration of the photoelectric direct-reading spectrometer is complete based on multiple calibration measurement values ​​obtained from multiple parallel measurements of the photoelectric direct-reading spectrometer according to a preset measurement deviation threshold and the standardized calibration standard obtained from multiple parallel measurements of the photoelectric direct-reading spectrometer.

[0087] The measurement calculation unit is used to calculate the average value based on the test results obtained from the photoelectric direct-reading spectrometer measuring the test standard steel and the test sample, and output the measured value X of the standard steel. 测量 and sample measurement values;

[0088] The standard steel correction value calculation unit is used to calculate the standard steel measurement value X output by the measurement value calculation unit. 测量 and the standard value X of the element in the test steel 标准 Obtain the standard steel correction value Δ for the elements in the test standard steel. bi and output;

[0089] The inverse distance weighting calculation unit is used to calculate the standard steel measurement value X output by the measurement unit based on the measurement value. 测量 The absolute difference L between the measured values ​​of the sample and the sample is calculated to obtain the inverse distance weight λ of the elements in the test steel and output it.

[0090] The sample correction value calculation unit is used to obtain the sample correction value Δ of the element content in the test sample based on the inverse distance weight λ output by the inverse distance weight calculation unit and the sample measurement value output by the measurement value calculation unit. x ;

[0091] The photoelectric direct-reading spectral measurement value calculation unit is used to calculate the sample correction value Δ output by the sample measurement value calculation unit and the sample correction value calculation unit based on the sample measurement value output by the measurement value calculation unit. x Sum the results and output the obtained photoelectric direct-reading spectral measurement values.

[0092] In some instances, the system further includes a memory for storing numerical media input and / or output from the photoelectric direct-reading spectrometer standardization calibration unit, measurement value calculation unit, standard steel correction value calculation unit, inverse distance weight calculation unit, sample correction value calculation unit, and photoelectric direct-reading spectrometer measurement value calculation unit.

[0093] In some instances, the system also includes a content prediction unit for predicting the content of major elements in the test sample. This content prediction unit collects parameters from the production process of the test sample and its target chemical composition content to obtain the prediction results of the major elements, retrieves standard steel containing the major elements from the standard steel library, determines the multiple relationship between the content of the major elements in the standard steel and the prediction results, and finds multiple sets of standard steel as test standard steel.

[0094] This invention calculates the correction value of the standard steel by using the difference between the standard value and the measured value of multiple sets of test standard steels. Then, it obtains the inverse distance weight by using the absolute difference between the measured value of the standard steel and the measured value of the sample. Using the inverse distance weight and the correction value of the standard steel, it obtains the correction value of the sample, thereby obtaining the photoelectric direct-reading spectral measurement value. This reduces method error and improves the accuracy of the photoelectric direct-reading spectral measurement value. Compared with conventional correction methods in the prior art, it overcomes the influence of excessive relative deviation of certain elements based on the linear correction method of a single standard steel on the photoelectric direct-reading spectral test results. By using a photoelectric direct-reading spectrometer for type standardization verification, it can effectively reduce random or environmental errors in the target element content determination process, which is beneficial to ensuring the accuracy of the target element content measurement of the test sample and the test standard steel. It also reduces method error, further improving the accuracy of the target element content in the tested alloy sample. Furthermore, it promotes the application of photoelectric direct-reading spectrometers in alloy chemical composition measurement. The measurement process is simple, convenient, and more efficient.

[0095] To further demonstrate the effectiveness of the multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement method of the present invention in improving the measurement values ​​of photoelectric direct-reading spectrometers, the following embodiments and comparative examples are provided:

[0096] Example

[0097] The experimental instrument used in this embodiment is a LAB LAWM10 photoelectric direct-reading spectrometer; the working gas is argon (purity 99.999%, pressure 0.7MPa); the plasma generator conditions are: WDD power supply voltage 11.3V, Vcc power supply voltage 5.1V, heating bath temperature 29.94℃; the optical chamber conditions are: pressure 944hPa, temperature 17.1℃; the LAB LAWM10 photoelectric direct-reading spectrometer was used to measure the content of 14 target elements in the test sample. The 14 target elements are: C (carbon), Si (silicon), Mn (manganese), P (phosphorus), S (sulfur), Cr (chromium), Ni (nickel), Mo (molybdenum), V (vanadium), Cu (copper), Al (aluminum), Ti (titanium), Co (cobalt), and Nb (niobium).

[0098] This embodiment includes the following steps:

[0099] 1. Estimate the elemental content of the sample to be tested. Select standard steel 2453-4 for the type standardization calibration of the photoelectric direct-reading spectrometer. The experimental method is Fe-10 Low alloy steel. Six parallel measurements of the type standard steel were performed. The measured deviation was 0.001% < 0.005%. The type standardization calibration of the photoelectric direct-reading spectrometer is qualified.

[0100] In this embodiment, the standard chemical analysis value X of standard steel 2453-4 标准 The measurement results of the six parallel measurements of the standardized steel are shown in Table 1.

[0101] Table 1

[0102]

[0103] 2. Estimate the elemental content of the sample to be tested. Select 2453-1 and 2453-5 as test standard steels. Use a photoelectric direct-reading spectrometer that has passed the standardization calibration in step 1 to measure the elements in the test standard steel three times in parallel to obtain three measurement values. Calculate the average of the three measurement values, which is the measured value X of the test standard steel. 测量 ,2453-1 Test standard steel test standard steel measurement value X 测量 and standard value X 标准 The statistical results are shown in Table 2.

[0104] Table 2

[0105]

[0106] In this embodiment, the measured value X of the 2453-5 test standard steel is... 测量 and standard value X 标准 The statistical results are shown in Table 3.

[0107] Table 3

[0108]

[0109] Using a photoelectric direct-reading spectrometer that has passed the standardization calibration in step 1, three parallel measurements were taken of the elements in the test sample to obtain three measurement values. The average of the three measurement values ​​was taken as the sample measurement value. The results are shown in Table 4.

[0110] Table 4

[0111]

[0112] 3. Based on the standard value X of the test steel. 标准 The standard steel measurement values ​​X obtained in step 2 and the two sets of test standard steels. 测量 Calculate the standard value X using Formula 1. 标准 Compared with the standard steel measurement value X 测量 The difference is represented by the standard steel correction value Δ for each element in the test standard steel. b ;

[0113] Formula 1: Δ b =X 标准 -X 测量 ;

[0114] In this embodiment, the standard steel correction value Δ of the target element in the 2453-1 test standard steel is used. b The calculation results are shown in Table 5.

[0115] Table 5

[0116]

[0117] Correction value Δ for target element in test standard steel 2453-5 b The calculation results are shown in Table 6.

[0118] Table 6

[0119]

[0120] 4. Based on the measured value X of the test standard steel obtained in step 2 测量 Calculate the measured value X of the test standard steel from the measured values ​​of the sample and the test specimen. 测量 The absolute difference between the measured value and the sample value is used to calculate the inverse distance weight λ of each group of test standard steels using Formula 2.

[0121] Formula 2:

[0122] Where n represents the total number of test standard steel groups; i represents the target element.

[0123] In this embodiment, the statistical results of the inverse distance weight λ of the target element in the 2453-1 test standard steel are shown in Table 7.

[0124] Table 7

[0125]

[0126] The statistical results of the inverse distance weight λ of elements in the 2453-5 test standard steel are shown in Table 8.

[0127] Table 8

[0128]

[0129] 5. Based on the inverse distance weight λ obtained in step 4 and the standard steel correction value Δ obtained in step 3... b Formula 3 is used to calculate the inverse distance weight λ and the standard steel correction value Δ. b The product of these products and summation yields the sample correction value Δ. x ;

[0130] Formula 3:

[0131] Where i represents the target element and n represents the total number of test standard steel groups;

[0132] Sample correction value Δ of elements in the test sample x The calculation results are shown in Table 9.

[0133] Table 9

[0134]

[0135] 6. Based on the sample correction value Δ obtained in step 5 x The measured values ​​of the test sample obtained in step 2 are summed to obtain the corrected measured values ​​output by the photoelectric direct-reading spectrometer.

[0136] The statistical results of the corrected measurements are shown in Table 10.

[0137] Table 10

[0138] target element C Si Mn P S Corrected measurement value of the test sample 0.2529 0.0702 1.0910 0.0280 0.0125 target element Cr Ni Mo V Cu Corrected measurement value of the test sample 0.3240 0.0880 0.0929 0.0227 0.2291 target element Al Ti Co Nb - Corrected measurement value of the test sample 0.0446 0.1067 0.1019 0.0619 -

[0139] 7. The relative deviations of the corrected measurement values ​​of the test samples provided in Table 9 relative to the standard values ​​of the test samples provided in Table 3 are statistically shown in Table 11.

[0140] Table 11

[0141]

[0142] Comparative Example

[0143] The difference between this comparative example and the embodiment is that: after obtaining the standard steel correction value Δb of the test standard steel in step 3, it is summed with the sample measurement value of the test sample to obtain the single standard steel correction result; the relative deviation of the single standard steel correction result relative to the standard value of the test sample is calculated.

[0144] Table 12 shows the single standard steel correction results and relative deviation results of the test standard steel of Comparative Example 2453-1.

[0145] Table 12

[0146]

[0147] Table 13 shows the single standard steel correction results and relative deviation results of the test standard steel of Comparative Example 2453-5.

[0148] Table 13

[0149]

[0150] Table 11 shows the statistical results of the relative deviation of the multi-standard steel reverse distance weight correction and Tables 12 and 13 show the relative deviation of the linear correction for single-standard steel. Figure 2 As shown.

[0151] From Table 11-13 and Figure 2 As can be seen, by using two sets of test steels, the photoelectric direct-reading spectral correction measurement values ​​obtained based on the inverse distance weighting method reduce the method error caused by the calibration of a single test steel. Among the 14 elements in the test sample, the relative deviations of C, Mn, Cr, Mo, and V are all lower than the relative deviations when using a single test steel. The relative deviations of the remaining 10 elements, including Si, P, S, Ni, Cu, Al, Ti, Co, and Nb, are all between the relative deviations of the two single test steels. This overcomes the influence of excessive relative deviations of certain elements on the photoelectric direct-reading spectral test results caused by a single test steel based on the single-steel linear correction method.

Claims

1. A method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values, applied to a photoelectric direct-reading spectrometer to obtain photoelectric direct-reading spectral correction measurement values ​​of the content of multiple target elements in a test sample, characterized in that, The method includes the following steps: a. Select multiple sets of test standard steels, and use a photoelectric direct-reading spectrometer to measure the contents of the test sample and the multiple sets of test standard steels to obtain the sample measurement values ​​and multiple sets of standard steel measurement values ​​X of the content of multiple target elements. 测量 ; b. Based on the multiple sets of standard steel measurement values ​​X from step a 测量 and the corresponding test standard value X 标准 Obtain multiple sets of standard steel correction values ​​Δ b ; c. Calculate the multiple sets of standard steel measurement values ​​X in step a. 测量 Multiple sets of absolute differences L between the measured values ​​of the standard steel samples were obtained. d. Obtain the inverse distance weight λ based on the absolute differences L of multiple sets of standard steel samples from step c; the inverse distance weight λ is calculated based on the following formula 2: Formula 2: ; in, It is represented as the inverse distance weight of target element i in the test standard steel with ordinal number k; It is expressed as the absolute difference between the measured value of target element i in the test standard steel and the measured value of target element i in the test sample, expressed as ordinal number k. It represents the sum of absolute differences for target element i in n groups of test standard steels, k represents the ordinal number of the test standard steel (k=1,2,...,n), n represents the total number of test standard steels, and n≥2; e. Based on the multiple sets of standard steel correction values ​​Δ from step b b The sample correction value Δ is obtained by combining the inverse distance weight λ from step d. x The sample correction value Δ x Calculated based on the following formula 3: Formula 3: ; in, This is expressed as the sample correction value for target element i. This represents the correction value of target element i in the test standard steel for ordinal number r. The inverse distance weight of target element i in the test standard steel with ordinal r The product, r represents the ordinal number of the test standard steel (r=1,2,...,n), n represents the total number of test standard steel groups, n≥2; f. Based on the sample measurement value from step a and the sample correction value Δ from step e. x Summing these values ​​yields the photoelectric direct-reading spectral correction measurements of the content of multiple target elements.

2. The method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​according to claim 1, characterized in that: Step a, the selection of the test standard steel is determined based on the predicted content of the main elements in the sample to be tested.

3. The method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​according to claim 2, characterized in that: The content of major elements in the test standard steel is 0.5 to 1.5 times the predicted content of each major element in the test standard steel.

4. The method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​according to claim 3, characterized in that: The test standard steel shall be in at least two sets, wherein the content of the main element in at least one set of test standard steel is 0.5 to 1 times the predicted result of the content of the main element in the sample to be tested, and the content of the main element in at least one set of test standard steel is 1 to 1.5 times the predicted result of the content of the main element in the sample to be tested.

5. The method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​according to claim 1, characterized in that: Step a, the measured value X of the standard steel 测量 The sample measurement values ​​are obtained by taking multiple parallel measurements of the test standard steel using a photoelectric direct-reading spectrometer and calculating the average value.

6. The method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​according to claim 5, characterized in that: The test standard steel is measured in parallel 3 to 10 times.

7. The method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​according to claim 6, characterized in that: The test standard steel was measured in parallel 6 times.

8. The method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​according to claim 5, characterized in that: The number of parallel measurements of the test sample is 3 to 10.

9. The method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​according to claim 8, characterized in that: The test sample was measured in parallel 6 times.

10. The method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​according to claim 1, characterized in that: Step b, the standard steel correction value Δ b To test the standard value X of the steel. 标准 Compared with the standard steel measurement value X 测量 The difference is calculated using Formula 1 below: Formula 1: .

11. The method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​according to any one of claims 1-6, characterized in that: The method further includes performing a type normalization calibration on the photoelectric direct-reading spectrometer before step a, the type normalization calibration including the following steps: 1) Select standardized calibration steel based on the predicted content of major elements in the sample to be tested; 2) Preset the measurement deviation threshold, and obtain multiple calibration measurement values ​​by repeatedly measuring the standardized calibration standard with the photoelectric direct-reading spectrometer. If the deviation of the multiple calibration measurement values ​​is less than the measurement deviation threshold, the type standardization calibration of the photoelectric direct-reading spectrometer is qualified. If the deviation of multiple calibration measurements exceeds the measurement deviation threshold, adjust the operating parameters of the photoelectric direct-reading spectrometer and / or treat the surface of the standardized calibration steel, and then perform multiple parallel measurements using the photoelectric direct-reading spectrometer until the deviation of multiple calibration measurements is less than the measurement deviation threshold.

12. The method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​according to claim 11, characterized in that: The content of the main elements in the standardized calibration steel is 0.8 to 1.3 times that in the sample to be tested.

13. The method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​according to claim 11, characterized in that: The measurement deviation threshold is 0.005%.

14. The method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​according to claim 11, characterized in that: The number of parallel measurements of the standardized calibration steel is 3 to 10.

15. The method for multi-standard steel inverse distance weighted correction photoelectric direct-reading spectral measurement values ​​according to claim 14, characterized in that: The standardized calibration steel was measured in parallel six times.

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