A fluorescence analysis method for rapid determination of copper and zinc content and adhesion in brass-plated steel cord

By using an energy dispersive X-ray fluorescence spectrometer (EDX) in steel cord detection combined with calibration curve method and shape correction function, the composition and adhesion of steel cord coating is directly analyzed, and the problem of cumbersome and time-consuming measurement process in the prior art is solved, achieving a fast and accurate detection effect.

CN119619204BActive Publication Date: 2025-05-02SHIMADZU (CHINA) CO LTD
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Patent Information

Application Number
CN202510163579.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-02-14
Publication Date
2025-05-02
Estimated Expiration
2045-02-14

AI Technical Summary

Technical Problem

The prior art requires the destruction of the coating when determining the components and adhesion amount of steel cord coating, which is cumbersome and time-consuming, and cannot achieve fast and accurate detection.

Method used

The energy dispersion X-ray fluorescence spectrometer (EDX) is used for direct analysis, combined with the calibration curve method and shape correction function, to determine the adhesion amount of copper-zinc plating, avoiding the damage and deplating process of the plating.

Benefits of technology

It realizes rapid and accurate detection of the composition and adhesion of steel cord coating, fast test speed and good stability, and is suitable for the analysis of steel cord samples.

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Abstract

The present application relates to a fluorescence analysis method for rapidly determining the copper and zinc content and adhesion amount in brass-plated steel cords, and the fluorescence analysis method comprises the following steps: sample preparation, standard sample selection, instrument measurement conditions, working curve drawing, and accuracy and precision determination. The present invention arranges the samples of brass-plated steel cords or strands in an orderly manner and places them in an X-ray fluorescence analyzer to directly test the copper and zinc content, and the standard curve method to test the adhesion amount of the copper and zinc coating. The fluorescence analysis method of the present invention does not require stripping treatment, is simple to operate, and has a fast test speed; a shape correction function is introduced into the calibration curve, and the analysis results are accurate and reliable, providing a fast and accurate determination method for testing the element content and adhesion amount in the steel cord coating, solving the problem of testing the adhesion amount of steel cord samples, and meeting the fast and accurate testing needs of enterprises.
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Description

Technical Field

[0001] The present application belongs to the technical field of steel cord detection and analysis, and specifically relates to a fluorescence analysis method for rapidly determining the copper and zinc content and adhesion amount in brass-plated steel cords. Background Art

[0002] Steel cord is a fine steel strand or rope made of high-quality high-carbon steel with a brass-plated surface and has special uses. It is mainly used for the skeleton materials of passenger car tires, light truck tires, heavy truck tires, construction machinery tires, aircraft tires and other rubber products. The radial tires using steel cord as the skeleton material have become the mainstream of automobile tires due to a series of advantages such as long service life, good safety performance and comfortable use, which has promoted the rapid development of the automobile industry. As the skeleton material of the tire, the quality of the steel cord and its adhesion to rubber plays a vital role in the product quality of the radial tire, and the components of the steel cord and the amount of coating adhesion are one of the main factors affecting its adhesion to rubber. In order to make the steel cord have good bonding performance with rubber, the surface of the steel wire needs to be electroplated. The coating components and adhesion amount affect the bonding performance, thereby affecting the quality of the radial tire. It is very important to quickly and accurately determine the coating components and adhesion amount of the steel cord.

[0003] At present, the methods for determining the coating composition and adhesion amount of steel cord in the industry include weight method, titration method, spectrophotometry, atomic absorption spectroscopy, inductively coupled plasma emission spectroscopy, etc. These methods for analyzing the coating composition and adhesion amount require accurate weighing of samples, chemical reagent stripping, dilution, and volume determination. The operation process is cumbersome and time-consuming.

[0004] X-ray fluorescence spectrometry is an analytical method with simple sample preparation, fast analysis speed, wide analysis content range, high accuracy and non-destructive analysis of solid samples. At present, some companies also use X-ray fluorescence spectrometry to test steel cords, but they still use the method of testing deplating liquid, which is cumbersome and time-consuming compared to direct testing of steel cord solid samples.

[0005] Therefore, there is an urgent need for a fluorescence analysis method that can directly measure the copper-zinc content and the amount of copper-zinc coating adhesion without stripping or destroying the steel cord coating, with fast analysis speed and high accuracy. Summary of the invention

[0006] In view of the problem that the current measurement of the coating component content and the adhesion amount of steel cords requires the destruction of the coating, the purpose of this application is to provide a fluorescence analysis method for quickly determining the copper and zinc content and adhesion amount in brass-plated steel cords.

[0007] The present application provides a fluorescence analysis method for rapidly determining the copper and zinc content and adhesion amount in brass-plated steel cords. The energy dispersive X-ray fluorescence spectrometer (EDX) is used to directly analyze the coating composition of the steel cords. The copper and zinc coating adhesion amount can be determined by combining the calibration curve method. The difficult problem of X-ray fluorescence in the analysis of the adhesion amount of steel cords is solved by introducing the shape correction function. The test results are basically consistent with the chemical results. The method has high accuracy, good stability, and fast test speed, and is very suitable for the analysis of the coating composition and adhesion amount of steel cord samples.

[0008] A fluorescence analysis method for rapidly determining the copper and zinc content and adhesion amount in brass-plated steel cords comprises the following steps:

[0009] S1: Sample preparation;

[0010] S2: Standard sample selection:

[0011] Select a series of standard samples with a certain gradient of copper-zinc coating adhesion and copper and zinc content;

[0012] S3: Instrument measurement conditions

[0013] S31: The test instrument for copper and zinc content and copper-zinc coating adhesion is an energy dispersive X-ray fluorescence spectrometer;

[0014] S32: Optimizing and selecting the detection conditions for copper and zinc;

[0015] S33: Copper and zinc contents were tested using the thin film FP method;

[0016] S4: Draw working curve

[0017] Under the optimized instrument measurement conditions, the standard samples were used to test the fluorescence intensity of copper and zinc respectively using an energy dispersive X-ray fluorescence spectrometer, and the shape correction function was evaluated using the standard samples. The Cu and Zn contents and the copper-zinc coating adhesion of single-root, multi-root, single-strand and multi-strand samples were tested, and the working curve was drawn with the ratio of the fluorescence intensity of copper and zinc in the standard samples to the internal standard as the ordinate and the copper-zinc coating adhesion in the standard samples as the abscissa.

[0018] S5: Detection

[0019] The fluorescence intensity of copper and zinc in the sample to be tested is also tested using an energy dispersive X-ray fluorescence spectrometer, and then the amount of copper-zinc coating adhesion in the sample to be tested is calculated using the obtained fluorescence intensity and the working curve.

[0020] Steel cord is a high-strength metal wire made of multiple strands of fine steel wire. In order to improve the corrosion resistance of steel cord and improve the bonding performance of steel cord with other materials, the surface of steel cord is plated. In order to further understand the relationship between bonding performance and coating, it is necessary to conduct detailed measurement of the adhesion amount and metal content of the coating on the surface of steel cord. The test of coating adhesion and metal content in steel cord is generally carried out according to two standards, namely GB / T33159-2016 and YB / T 135-2017. Part 7 of GB / T 33159-2016 provides several methods for measuring the chemical properties of coatings, including X-ray fluorescence spectrometry (XRFS wet method), chemical titration, atomic absorption spectrometry and inductively coupled plasma emission spectrometry (ICP method). However, no matter which of the above methods is used, when processing the sample, it is necessary to dissolve the coating on the surface of the steel cord through ammonia, ammonium persulfate, nitric acid and other deplating solutions, and then conduct subsequent testing. This not only increases the steps of sample processing, but also damages the steel cord itself, making the test more cumbersome. YB / T135-2017 also provides several methods for measuring the coating adhesion and analyzing the composition, including weight method, spectrophotometry, chemical volumetric method, atomic absorption spectrometry and inductively coupled plasma atomic emission spectrometry. However, without exception, the above methods also require ammonia water, hydrogen peroxide and other solutions to dissolve the copper cord coating first.

[0021] X-ray fluorescence spectrometry is also mentioned in YB / T 135-2017. The primary ray generated by the ray source is used to irradiate the steel wire with tin bronze coating. Under certain conditions, characteristic X-rays of the coating metal copper and tin, namely fluorescent X-rays, are excited in the steel wire coating. The intensity of the fluorescent X-rays is detected, and the tin content in the steel wire coating and the coating weight and thickness are calculated based on the calibration curve and the intensity of the X-ray fluorescence of the measured sample. Although the coating is not dissolved in this process, it has a specific sample preparation process. The preparation process of the test sample is as follows:

[0022] Accurately measure the diameter of the tire bead wire to an accuracy of 0.01mm, cut the tire bead wire into about 33mm lengths according to the size of the sample piece, and neatly stick it on the side of the sample piece with double-sided tape, and mark the sample information on the other side of the sample piece.

[0023] The sample should meet the following requirements:

[0024] a) The sample is flat and smooth, without any bumps;

[0025] b) The steel wires are arranged neatly, compactly and without gaps;

[0026] c) The steel wire should be firmly glued to prevent it from falling off.

[0027] Therefore, even though there is a method in the prior art that uses X-ray fluorescence spectroscopy to directly test the coating and metal content of steel cords, it is seriously affected by the shape of the sample to be tested. During the sample preparation process, the steel cord must be completely split into steel wires to ensure that the diameter and length can be spliced ​​into smooth, compact and neat sample pieces to meet the test standards. It is impossible to test stranded and single-filament steel wires.

[0028] In view of the above problems, the present invention first uses EDX (energy dispersive X-ray fluorescence spectrometer) to conduct qualitative analysis on steel cord samples, mainly detecting Fe, Cu, and Zn elements, and determining that the main component of the substrate is Fe, and the main components of the coating are Cu and Zn. The thin film FP method is used to quantitatively test the Cu and Zn contents in the coating, and the standard curve method is used to test the coating adhesion (g / kg). The calibration curve uses steel cord samples calibrated by chemical method as calibration samples. Considering that the steel cord is a single filament or twisted into strands, a shape correction function is introduced into the calibration curve, and the shape correction effect of the method is evaluated in different test states. The present invention combines shape correction with the standard curve method. For the same steel cord sample, the test consistency of the coating adhesion is very good under various test states such as single, multiple or multiple strands, and is not affected by the sample morphology. The analysis of the coating adhesion is generally carried out by the thin film FP method, but this method has high requirements on the surface flatness of the sample. Therefore, the adhesion of steel cord samples has always been a difficulty in X-ray fluorescence analysis. The present invention solves the above difficulties by combining the standard curve and shape correction, breaking through the application bottleneck of X-ray fluorescence analysis in this field.

[0029] The fluorescence analysis method of the present invention does not need to strip the steel cord or destroy the coating of the steel cord, directly tests the copper and zinc content, and uses the standard curve method to test the copper and zinc coating adhesion. It can also correct the test deviation caused by inconsistent steel cord shapes, and has fast analysis speed and high accuracy.

[0030] In some embodiments of the present application, in step S1, the specific steps are:

[0031] S11: Split and cut the steel cord into small segments;

[0032] S12: cleaning the cut small segments;

[0033] S13: After cleaning, drying is performed to obtain a sample to be tested.

[0034] In some embodiments of the present application, in step S11, the steel cord is split into monofilaments or strands, and each of the monofilaments or strands is cut into small segments of 2 to 15 cm in length.

[0035] In some embodiments of the present application, in step S12, an organic solvent is used to clean the oil stains on the surface of the cut small segments.

[0036] In some embodiments of the present application, in step S2, the copper-zinc coating adhesion amount in the standard sample is obtained by chemical method evaluation.

[0037] In some embodiments of the present application, in step S32, the detection conditions include analytical lines of copper and zinc, internal standards, collimators, filters, integration time and voltage; specifically, the analytical line selects the K series, the internal standard uses the matrix element Fe or the scattered line of the target material; the collimator can be 1mm~10mm; there is no filter; the integration time is 30s~300s; the voltage is 15~50kV.

[0038] In some embodiments of the present application, step S5 is further provided with a step of measuring accuracy and precision, and the specific process is as follows:

[0039] The steps of determining the accuracy are: testing the sample to be tested by energy dispersive X-ray fluorescence spectrometer and inductively coupled plasma emission spectrometry respectively, comparing whether the content of copper and zinc and the amount of copper-zinc coating adhesion are consistent;

[0040] The steps for measuring precision are as follows: after cutting the sample to be tested into appropriate lengths, repeat the measurement on single-strand, two-strand and three-strand steel cords, and compare whether the coating composition and the copper-zinc coating adhesion are consistent under different test conditions of the number of strands.

[0041] Compared with the prior art, the present application at least achieves the following technical effects:

[0042] The present application relates to a fluorescence analysis method for rapidly determining the copper and zinc content and adhesion amount in brass-plated steel cords. An energy dispersive X-ray fluorescence spectrometer (EDX) is used to directly analyze the coating composition of the steel cord. The difficult problem of X-ray fluorescence in analyzing the adhesion amount of the steel cord is solved by introducing a shape correction function. The coating adhesion amount can be determined by combining with a calibration curve method, which is basically consistent with the chemical result, and at least the following technical effects are obtained: (1) This method has high accuracy, good stability, and fast testing speed, and is very suitable for analyzing the coating composition and adhesion amount of steel cord samples; (2) Traditional chemical analysis methods require the sample to be dissolved, which is not only time-consuming but also may cause irreversible damage to the sample. The X-ray fluorescence spectrometry of the present invention can directly test the steel cord, retaining the integrity and original state of the sample, which is convenient for subsequent further analysis and use; (3) The fluorescence analysis method of the present invention does not require deplating treatment, is simple to operate, and has a fast testing speed; (4) The X-ray fluorescence spectrometer in the present invention has a fast testing speed, and can usually complete the testing of a sample within a few minutes, which is very convenient for those who need It is very important for production process and quality control to obtain results quickly, which can greatly improve work efficiency and reduce waiting time; (5) The shape and structure of steel cord are complex. Traditional X-ray fluorescence spectrometry may be affected by the shape of the sample when analyzing the adhesion amount. The present invention introduces a shape correction function in the calibration curve, and the analysis result is accurate and reliable. It provides a fast and accurate determination method for the element content and adhesion test in the steel cord coating, solves the problem of adhesion test of steel cord samples, and meets the fast and accurate testing needs of enterprises; (6) The X-ray fluorescence spectrometer of the present invention can simultaneously determine the content of multiple elements, such as copper and zinc, without the need for multiple separate tests, which not only saves time and resources, but also reduces the errors caused by multiple tests, and improves the efficiency and accuracy of the test; (7) The fluorescence analysis method of the present invention is not only suitable for the analysis of brass-plated steel cord, but can also be extended to the analysis of other types of metal coatings and thin film materials. For example, it can be used to determine the composition and adhesion of different coatings such as zinc plating, nickel plating, and silver plating, and has wide applicability and flexibility. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] Figure 1 It is the appearance picture of the sample to be tested before and after it is cut;

[0044] Figure 2 is the working curve of copper;

[0045] Figure 3 is the working curve of zinc;

[0046] Figure 4 This is a schematic diagram of the sample test status of standard sample 1#;

[0047] Figure 5 It is the spectrum of copper, zinc and iron;

[0048] Figure 6 This is a schematic diagram of the sample test status of samples 4# and 5# to be tested. DETAILED DESCRIPTION

[0049] In order to make the purpose, technical solution and advantages of the present invention more clear, the present invention is further described in detail below. However, it should be understood that the description herein is only used to explain the present invention and is not intended to limit the scope of the present invention.

[0050] Unless otherwise defined, all technical terms and scientific terms used herein have the same meaning as those generally understood by those skilled in the art of the present invention, and the terms used in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The reagents and instruments used herein are all commercially available, and the characterization means involved can refer to the relevant descriptions in the prior art, which will not be repeated herein.

[0051] Example

[0052] A fluorescence analysis method for rapidly determining the copper and zinc content and adhesion amount in brass-plated steel cords comprises the following steps:

[0053] S1: Sample preparation

[0054] S11: Split the steel cord into single filaments or strands, and cut them into small pieces about 12 cm long. The appearance before and after cutting is shown in the figure. Figure 1 ;

[0055] S12: Use organic solvent (acetone) to clean the oil stains on the surface of the cut small section;

[0056] S13: After cleaning, drying is performed to obtain a sample to be tested.

[0057] S2: Standard sample selection

[0058] Select standard samples 1#, 2#, and 3#, whose copper-zinc coating adhesion amount and copper and zinc contents present a certain gradient; the copper-zinc coating adhesion amount and copper and zinc contents in standard samples 1#, 2#, and 3# are obtained by chemical method;

[0059] The chemical method mainly tests the coating adhesion and copper and zinc content according to the inductively coupled plasma emission spectrometry in GB / T 33159-2016. The specific process is as follows:

[0060] S21: Take 2 g of steel cord sample, cut it into small pieces, wash it with ethanol and then dry it;

[0061] S22: Weigh 0.5 g (accurate to 0.0001 g) of the dried steel cord sample, place two parallel portions in a clean beaker, add 5 mL of concentrated nitric acid, and gently shake until the coating is completely dissolved;

[0062] S23: Transfer the solution to a 100 mL glass volumetric flask and dilute to volume with deionized water and shake well;

[0063] S24: Prepare a series of standard solutions using single element standard solutions of copper and zinc, select wavelengths of Cu 324.754nm and Zn 206.200nm, and use an inductively coupled plasma emission spectrometer to test the concentrations of copper and zinc in the stripping solution;

[0064] S25: Calculate the copper and zinc content in the coating (in %) and the coating adhesion (in g / kg) based on the concentration of copper and zinc in the solution, the constant volume and the 0.5g sample weight.

[0065] S3: Instrument measurement conditions

[0066] S31: The test instrument for copper and zinc content and copper-zinc coating adhesion is an X-ray fluorescence spectrometer (Shimadzu EDX-LE Plus energy dispersive X-ray fluorescence spectrometer);

[0067] S32: Optimize the analysis lines, internal standards, collimators, filters, integration time and voltage of copper and zinc; specifically, the K series is selected for the analysis line, and the scattered line of the target material Rh is used as the internal standard; the collimator is 10mm; there is no filter; the integration time is 40s; the voltage is 50kV, and the test atmosphere is air.

[0068] S33: The copper and zinc contents in the coating were tested using the thin film FP method;

[0069] S34: establishing thin film FP method measurement conditions, setting sample information to thin film and metal;

[0070] S35: Set the layer structure, register the analysis elements copper and zinc, and select the quantitative method as quantitative FP;

[0071] S36: The sample is placed in EDX to test the copper and zinc content in the coating.

[0072] S4: Draw working curve

[0073] Under the optimized instrument measurement conditions, standard samples 1#, 2#, and 3# were tested for the fluorescence intensity of copper and zinc respectively by X-ray fluorescence spectrometer. The ratio of the fluorescence intensity of copper and zinc in the standard samples to the internal standard was used as the ordinate, and the adhesion amount of copper-zinc coating in the standard samples was used as the abscissa to draw the working curve. The adhesion amount of standard samples 1#, 2#, and 3# is shown in Table 1; the working curve is shown in Appendix Figure 2 and attached Figure 3 .

[0074] Table 1 Copper and zinc adhesion in standard samples

[0075]

[0076] S5: Procedure for determining accuracy and precision

[0077] S51: In order to verify the effectiveness of the method of the present invention, the shape correction function is evaluated using standard sample 1#, and the Cu, Zn content and coating adhesion of single-root, multi-root, single-strand and multi-strand samples are tested.

[0078] The shape correction function uses the signal of the Fe element of the substrate to correct the adhesion of copper and zinc in the coating. The coating test is mainly aimed at samples that are flat and can completely cover the collimator. Due to the irregular shape of the steel cord, the fluorescence intensity of the Fe element of the substrate is used to correct the fluorescence intensity of copper and zinc when setting the method during the test.

[0079] First, the steel cord samples were qualitatively analyzed using EDX, and the main elements Fe, Cu, and Zn were detected. It was determined that the main component of the substrate was Fe, and the main components of the coating were Cu and Zn. The thin film FP method was used to quantitatively test the Cu and Zn contents in the coating, and the standard curve method was used to test the coating adhesion (g / kg). The calibration curve uses steel cord samples calibrated by chemical method as calibration samples. Considering that the steel cord is a single filament or twisted into strands, a shape correction function is introduced into the calibration curve. The shape correction effect of the method was evaluated using standard sample 1# in different test states. The results and test state diagrams are shown in Tables 2 and Figure 4 .

[0080] Table 2 Shape correction effect evaluation test

[0081]

[0082] Note: Cu and Zn in the table refer to the ratio of the two components in the coating, and the coating adhesion is the ratio of the coating mass to the total mass of the steel cord.

[0083] The results in Table 2 show that, by combining shape correction and standard curve method, the same steel cord sample has very good test consistency for coating adhesion under various test conditions such as single, multiple or multiple strands, and is not affected by the sample morphology. The analysis of coating adhesion is generally carried out by the thin film FP method, but this method has high requirements for sample surface flatness, so the adhesion of steel cord samples has always been a difficulty in X-ray fluorescence analysis. The data in Table 2 show that the method of the present invention solves this difficult problem well and breaks through the application bottleneck of X-ray fluorescence analysis in this field.

[0084] S52: In order to verify the accuracy of the method of the present invention, the samples 4# and 5# to be tested are tested using X-ray fluorescence spectrometry and inductively coupled plasma emission spectrometry (GB / T 33159-2016) to compare whether the contents of copper and zinc and the amount of coating adhesion are consistent;

[0085] The composition and adhesion of the steel cord coating were tested simultaneously using EDX and inductively coupled plasma emission spectroscopy (ICP). The results are shown in Table 3.

[0086] Table 3 Corrected steel cord analysis results

[0087]

[0088] S53: In order to conduct repeatability inspection, the samples 4# and 5# to be tested were cut into appropriate lengths, and the single-strand, two-strand and three-strand steel cords were tested repeatedly. The coating composition and coating adhesion were compared under different test conditions.

[0089] After cutting the steel cord into appropriate lengths, the single-strand, two-strand and three-strand steel cords were tested six times. The results are shown in Tables 4 and 5. Figure 6 The results show that the coating composition and coating adhesion have good consistency and repeatability under different strand test conditions, and the RSD values ​​are all less than 0.6%.

[0090] Table 4 Analysis results of sample 4#

[0091]

[0092] Table 5 Analysis results of sample 5#

[0093]

[0094] The applicant declares that the present application uses the above-mentioned embodiments to illustrate a fluorescence analysis method for rapidly determining the copper and zinc content and adhesion amount in brass-plated steel cords of the present application, but the present application is not limited to the above-mentioned embodiments, that is, it does not mean that the present application must rely on the above-mentioned embodiments to be implemented. The technicians in the relevant technical field should understand that any improvement to the present application, the equivalent replacement of the raw materials of the present application product, the addition of auxiliary components, the selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present application.

[0095] The preferred embodiments of the present application are described in detail above; however, the present application is not limited to the specific details in the above embodiments. Within the technical concept of the present application, a variety of simple modifications can be made to the technical solution of the present application, and these simple modifications all fall within the protection scope of the present application.

[0096] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, this application will not further describe various possible combinations.

Claims

1. A fluorescence analysis method for rapidly determining the copper and zinc content and adhesion amount in brass-plated steel cord, characterized in that: The following steps are involved: S1: Sample preparation; S2: Standard sample selection: Select a series of standard samples with a certain gradient of copper-zinc coating adhesion and copper and zinc content; S3: Instrument measurement conditions: S31: The test instrument for copper and zinc content and copper-zinc coating adhesion is an energy dispersive X-ray fluorescence spectrometer; S32: Optimize the detection conditions of copper and zinc; S33: Copper and zinc contents were tested using the thin film FP method; S4: Draw working curve Under the optimized instrument measurement conditions, the standard samples were used to test the fluorescence intensity of copper and zinc respectively using an energy dispersive X-ray fluorescence spectrometer, and the standard samples were used to evaluate the shape correction function. The Cu, Zn content and the copper-zinc coating adhesion of single-root, multiple-root, single-strand and multiple-strand samples were tested, and the working curve was drawn with the ratio of the fluorescence intensity of copper and zinc in the standard sample to the internal standard as the ordinate and the copper-zinc coating adhesion in the standard sample as the abscissa; wherein the shape correction function is to use the fluorescence intensity of the Fe element of the substrate to correct the fluorescence intensity of copper and zinc in the coating; S5: Detection The fluorescence intensity of copper and zinc in the sample to be tested is also tested by an energy dispersive X-ray fluorescence spectrometer, and then the amount of copper-zinc coating adhesion in the sample to be tested is calculated using the obtained fluorescence intensity and the working curve; Among them, in step S1, the specific steps are: S11: Split and cut the steel cord into small segments; S12: cleaning the cut small segments; S13: After cleaning, drying is performed to obtain a sample to be tested.

2. A fluorescence analysis method for rapidly determining the copper and zinc content and adhesion amount in brass-plated steel cord according to claim 1, characterized in that: In step S11, the steel cord is split into monofilaments or strands, and each is cut into small segments of 2 to 15 cm in length.

3. A fluorescence analysis method for rapidly determining the copper and zinc content and adhesion amount in brass-plated steel cord according to claim 1, characterized in that: In step S12, an organic solvent is used to clean the oil stains on the surface of the cut small segments.

4. A fluorescence analysis method for rapidly determining the copper and zinc content and adhesion amount in brass-plated steel cord according to claim 1, characterized in that: In step S2, the coating weight of the copper-zinc coating in the standard sample is obtained by chemical method.

5. A fluorescence analysis method for rapidly determining the copper and zinc content and adhesion amount in brass-plated steel cord according to claim 1, characterized in that: In step S32, the detection conditions include the analysis lines of copper and zinc, internal standards, collimators, filters, integration time and voltage; specifically, the analysis lines are selected from the K series, the internal standards are the matrix element Fe or the scattered lines of the target material; the collimator can be 1mm~10mm; there is no filter; the integration time is 30s~300s; the voltage is 15~50kV.

6. A fluorescence analysis method for rapidly determining the copper and zinc content and adhesion amount in brass-plated steel cord according to claim 1, characterized in that: Step S5 also includes a step for measuring accuracy and precision, and the specific process is as follows: The steps of determining the accuracy are: testing the sample to be tested by energy dispersive X-ray fluorescence spectrometer and inductively coupled plasma emission spectrometry respectively, comparing whether the content of copper and zinc and the amount of copper-zinc coating adhesion are consistent; The steps for measuring precision are as follows: after cutting the sample to be tested into appropriate lengths, repeat the measurement on single-strand, two-strand and three-strand steel cords, and compare whether the coating composition and the copper-zinc coating adhesion are consistent under different test conditions of the number of strands.

Citation Information

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