CN116794078A - Method for detecting multiple elements of cold-plated zinc layer by using X-ray fluorescence without standard sample - Google Patents
Method for detecting multiple elements of cold-plated zinc layer by using X-ray fluorescence without standard sample Download PDFInfo
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- CN116794078A CN116794078A CN202310617208.7A CN202310617208A CN116794078A CN 116794078 A CN116794078 A CN 116794078A CN 202310617208 A CN202310617208 A CN 202310617208A CN 116794078 A CN116794078 A CN 116794078A
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- 238000000034 method Methods 0.000 title claims abstract description 68
- 238000004876 x-ray fluorescence Methods 0.000 title claims abstract description 30
- 239000011701 zinc Substances 0.000 title claims abstract description 26
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 18
- 238000001514 detection method Methods 0.000 claims abstract description 28
- 238000012545 processing Methods 0.000 claims abstract description 5
- 238000007747 plating Methods 0.000 claims description 28
- 238000012921 fluorescence analysis Methods 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 11
- 238000000576 coating method Methods 0.000 claims description 11
- 238000004458 analytical method Methods 0.000 claims description 9
- 238000005259 measurement Methods 0.000 claims description 9
- 230000000694 effects Effects 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 230000003595 spectral effect Effects 0.000 claims description 3
- 238000011077 uniformity evaluation Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000003814 drug Substances 0.000 abstract 1
- 229940079593 drug Drugs 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 238000012937 correction Methods 0.000 description 6
- 239000011575 calcium Substances 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 238000009675 coating thickness measurement Methods 0.000 description 2
- 238000002795 fluorescence method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000386 microscopy Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 238000010561 standard procedure Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
- G01N23/2076—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions for spectrometry, i.e. using an analysing crystal, e.g. for measuring X-ray fluorescence spectrum of a sample with wavelength-dispersion, i.e. WDXFS
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The invention belongs to the technical field of detection of elements of a cold-plated zinc layer, and particularly relates to a method for detecting multiple elements of the cold-plated zinc layer by using X-ray fluorescence without a standard sample. The method comprises the following steps: step one, selecting a sample; step two, sample processing; setting detection conditions of an X-ray fluorescence spectrometer; determining an internal standard value; and fifthly, detecting by an X-ray fluorescence spectrometer. The method is simple to operate, has short detection flow, and greatly improves the production efficiency; compared with the national standard, the method has the advantages of less chemical drugs, less environmental pollution and saving the purchase cost of instruments and standard samples.
Description
Technical Field
The invention belongs to the technical field of detection of elements of a cold-plated zinc layer, and particularly relates to a method for detecting multiple elements of the cold-plated zinc layer by using X-ray fluorescence without a standard sample.
Background
The national standard method for detecting the element content or thickness of the plating layer comprises the following steps: gravimetric method (GB/T1839-2008 steel product galvanized layer quality test method), coulombic method (GB/T15717-1995 vacuum metal coating thickness test method resistance method), magnetic method (GB/T4956-2003 magnetic method for measuring non-magnetic coating thickness on magnetic substrate), cross-sectional microscopy (also known as metallographic method (GB/T6462-2005 metal and oxide coating thickness measurement microscopy)), X-ray spectroscopic method (GB/T16921-2005 metal coating thickness measurement X-ray spectroscopic method). The method for detecting the content or thickness of zinc Zn, aluminum Al, silicon Si, calcium Ca and other components of the cold-plating zinc layer of the iron-based plate comprises the following steps: method 1, weight method: dissolving a galvanized layer on a known surface area in an experimental solution with a slow release effect, weighing the mass of the galvanized layer before and after the solution of a sample, and calculating the mass of the galvanized layer on a unit area according to the weighed difference and the area of the sample; method 2, metallographic method: after cutting a sample inlay from a designated location on the part to be tested, the cross section is suitably ground, polished and etched. Measuring the thickness of the cross section of the cover layer with a corrected scale; method 3, fluorescence correction curve method: the fluorescence intensity is a function of atomic numbers of elements, if the galvanized layer and the matrix are composed of different elements, the elements can generate respective radiation characteristics, a certain relation exists between the unit area mass of the covering layer (the linear thickness of the covering layer if the density is known) and the secondary radiation intensity, the fluorescence intensity of the element of the coating layer is measured, a standard correction curve of the fluorescence intensity and the thickness of the element is drawn, the fluorescence intensity of an unknown coating plate is measured under the same condition, and the composition and the thickness of the coating plate are obtained on the correction curve. However, the three methods have long detection period, use a large amount of chemical reagents, waste manpower and material resources, and only one element can be detected by one working curve, so that the three methods have the defects of large number of participating instruments, large demand and large consumption of standard samples.
Patent CN108918566a discloses a method for inspecting zinc-plated aluminum-magnesium plate coating, which is a fluorescence correction curve method, and uses a weight method fixed value to fix the internal control plating plate, so that the average thickness of the coating is complex in operation, elements except zinc Zn cannot be detected, and the penetration attenuation of fluorescence to thicker zinc layer is not considered. The method adopts an X-ray fluorescence spectrometry to measure the zinc layer quality of a hot-base galvanized plate and an electro-galvanized plate (2012, 32 nd stage, metallurgical analysis), improves some methods in X-ray fluorescence detection of cold-plated galvanized plates, and adopts an X-ray fluorescence correction curve method to detect the thickness of the galvanized layer, but firstly, the method determines the value of an internal control galvanized plate by means of a weight method and cannot detect secondary elements; and secondly, the weight method calibration is a destructive detection means which cannot be repeated, and over-peeling easily occurs, so that the analysis of the galvanized layer thickness is inaccurate.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for detecting multiple elements of a cold-galvanized layer by using X-ray fluorescence without a standard sample. The invention saves the raw materials for detection, reduces the production cost, improves the labor productivity, simplifies the previous work of a plurality of people into one person to finish, has high detection speed, less application reagent, improves the labor condition, reduces the environmental pollution, simultaneously expands the detection range, reduces the use of test articles, especially standard samples, and simultaneously lays a foundation for detecting more types of plating plates in the future as a scanning detection method.
In order to achieve the above object, the technical scheme of the present invention is as follows:
a method for detecting multiple elements of a cold-galvanized layer by using an X-ray fluorescence non-standard sample, comprising the following steps:
step one, sample selection: selecting the area of the galvanized layer to be more than 2m 2 Is a cold-plated galvanized sheet;
step two, sample processing: processing the sample into a sample wafer according to the size of a sample box of the X-ray fluorescence spectrometer;
step three, setting detection conditions of an X-ray fluorescence spectrometer:
the spectral lines of the measurement elements and the measurement conditions are shown in Table 1:
TABLE 1 measurement element spectral lines and measurement conditions
Determining an internal standard value: detecting fluorescence intensity of the galvanized plate by using an X-ray fluorescence spectrometer, wherein the galvanized plate meeting the uniformity of fluorescence intensity is used as an internal standard plating plate, detecting the thickness of Zn element by using a weight method of the selected internal standard plating plate, detecting the thicknesses of Al, si and Ca element by using an ICP method, and taking the detection result as an internal standard value of the internal standard plating plate;
step five, detecting by an X-ray fluorescence spectrometer:
(1) Placing a sample wafer of the internal standard plating plate on a sample stage of an X-ray fluorescence spectrometer for fluorescence analysis to obtain the fluorescence intensity of a measuring element in the internal standard plating plate;
(2) Obtaining a fluorescence analysis value of each element of the internal standard plating plate by adopting a standard-sample-free analysis method, comparing the fluorescence analysis value with the internal standard value, and debugging and correcting the self-absorption/attraction effect coefficient of the measurement element until the fluorescence analysis value and the internal standard value meet the requirement of the reproducibility limit of the content of the analysis element;
(3) And placing the sample wafer of the sample to be detected on a sample table of an X-ray fluorescence spectrometer for fluorescence analysis to obtain a fluorescence analysis value of the content of the measuring element in the sample to be detected.
In the above technical solution, in the first step, at least 6 basic measurement surfaces are selected on the internal standard plating plate for detection.
In the above technical solution, in the first step, the basic measuring surface should be selected at least 10cm away from the edge of the plating plate.
In the above technical scheme, in the second step, the sample wafer has a square structure with a side length of 30-35 mm or a round structure with a diameter of 30-40 mm.
In the above technical solution, in the fourth step, the condition for evaluating uniformity of fluorescence intensity is: the ratio of the fluorescence intensity difference value of zinc Zn element to the average value of the zinc Zn element of the internal control standard plating plate is less than 3 percent.
The X-ray fluorescence spectrometer of the invention adopts a non-standard analysis method, opens non-standard software, and establishes an X-ray fluorescence non-standard method of the sinter in a 'method'/'kappa' list.
The simple calculation formula of each element component in the standard sample-free method is as follows:
C i ，C j -the content,%;
ω i ，ω j -fluorescence intensity of component i, j in the sample, kcps;
a, the ratio value of the detected area of the sample to the standard caliber is determined by the caliber of the collimator mask;
γ i -component i fluorescence sensitivity coefficient,%/kcps in the sample;
μ i -a weighted average mass attenuation coefficient of component i for the initial X-rays;
K i,i -self-priming/enhancement effect coefficient of component i;
K i,j absorption/enhancement effect coefficient of component i, j.
Detecting an internal control standard plating plate by using a fluorescent standard-free method of a cold-plated zinc layer, observing the difference between an analysis value and an internal standard value, and then manually adjusting the self-absorption/enhancement effect coefficient K in the method i,i Coefficient of attraction/enhancement effect K i,j Until the fluorescence analysis value and the internal standard value meet the requirement of the reproducibility limit of the content of the analysis element.
The beneficial effects of the invention are as follows:
1. the method is simple to operate, has short detection flow, and greatly improves the production efficiency;
2. under the condition of lacking a standard plating plate, the method establishes a method for selecting and preparing the internal control standard plating plate with higher precision, and uses other instrument methods with high precision and high accuracy to carry out value setting on the internal control standard plating plate;
3. compared with the national standard, the method has the advantages of less chemical used, less environmental pollution and saving the purchase cost of instruments and standard samples;
3. the detected multiple detection elements can be detected at one time, so that the detection efficiency is greatly improved, and the detection flexibility is far superior to that of the traditional X-ray fluorescence correction curve method.
In a word, the detection method saves raw materials for detection, reduces production cost, improves labor productivity, simplifies the work of a plurality of instruments into one person and one instrument to finish, has high detection efficiency and high speed, uses fewer reagents, reduces environmental pollution, and has greater flexibility compared with the traditional X-ray fluorescence detection method.
Drawings
FIG. 1 is a flow chart of the method of the present invention.
Detailed Description
The following examples will enable those of ordinary skill in the art to more fully understand the invention and are not intended to limit the invention in any way.
Example 1
The method comprises the steps of selecting an iron-based plate cold-plating galvanized plate internal control standard galvanized plate DC06-31, placing the iron-based plate cold-plating galvanized plate into a zinc-plating layer standard-free method for detection for 5 times, calculating the thickness of each element and calculating the relative standard deviation RSD, wherein the detection results of the front side and the back side of a DC06-31 sample are shown in tables 2 and 3 respectively.
TABLE 2 front side of DC No. 06-31 sample wafer
TABLE 3 reverse side of DC No. 06-31 sample
As can be seen from tables 3 to 4, the RSD of each component is less than 5%, and the precision of the method of the present invention is good.
Example 2
Random samples with the numbers of DC 04-12, DC 04-16, DC 04-11, DC 06-21, DC 06-25, DC 06-32 and DC04 NE-5 are detected by a standard-free method, and compared with a chemical weight method and an ICP method, the following table (the front side and the back side are detected except for a sample with the number of DC04NE 5):
table 4 comparison of X-ray fluorescence non-standard sample method and chemical weight method and ICP method for cold-plating zinc coating on iron-based sheet material
Representing the composition as trace or unexplained
Table 4 shows that the fluorescent standard-free method and the gravimetric method and the ICP method for detecting zinc Zn, calcium Ca, aluminum Al and silicon Si have high coincidence degree: the relative difference between the result of detecting Zn element by fluorescence method and weight method is less than 3%; the relative difference between the results of detecting the aluminum Al and silicon Si elements by the fluorescence method and the ICP method is respectively less than 5%, 5% and 10%. The main elements of the galvanized layer of the iron-based plate detected by the fluorescent standard-free method accord with the chemical detection requirement.
The above examples are only preferred embodiments of the present invention and are not limiting of the implementation. The protection scope of the present invention shall be subject to the scope defined by the claims. Other variations or modifications may be made in the various forms based on the above description. Obvious variations or modifications of the embodiments are within the scope of the invention.
Claims (5)
1. A method for detecting multiple elements of a cold-galvanized layer by using an X-ray fluorescence non-standard sample, which is characterized by comprising the following steps:
step one, sample selection: selecting the area of the galvanized layer to be more than 2m 2 Is a cold-plated galvanized sheet;
step two, sample processing: processing the sample into a sample wafer according to the size of a sample box of the X-ray fluorescence spectrometer;
step three, setting detection conditions of an X-ray fluorescence spectrometer:
the measurement element spectral lines and measurement conditions are shown in the following table:
determining an internal standard value: detecting fluorescence intensity of the galvanized plate by using an X-ray fluorescence spectrometer, wherein the galvanized plate meeting the uniformity of fluorescence intensity is used as an internal standard plating plate, detecting the thickness of Zn element by using a weight method of the selected internal standard plating plate, detecting the thicknesses of Al, si and Ca element by using an ICP method, and taking the detection result as an internal standard value of the internal standard plating plate;
step five, detecting by an X-ray fluorescence spectrometer:
(1) Placing a sample wafer of the internal standard plating plate on a sample stage of an X-ray fluorescence spectrometer for fluorescence analysis to obtain the fluorescence intensity of a measuring element in the internal standard plating plate;
(2) Obtaining a fluorescence analysis value of each element of the internal standard plating plate by adopting a standard-sample-free analysis method, comparing the fluorescence analysis value with the internal standard value, and debugging and correcting the self-absorption/attraction effect coefficient of the measurement element until the fluorescence analysis value and the internal standard value meet the requirement of the reproducibility limit of the content of the analysis element;
(3) And placing the sample wafer of the sample to be detected on a sample table of an X-ray fluorescence spectrometer for fluorescence analysis to obtain a fluorescence analysis value of the content of the measuring element in the sample to be detected.
2. The method for detecting multiple elements of a cold-galvanized coating according to claim 1, wherein in the first step, at least 6 basic measuring surfaces are selected for detection on an internal standard coating.
3. The method for detecting multiple elements of a cold-galvanized coating according to claim 1, wherein in the first step, the basic measuring surface is selected at least 10cm from the edge of the coating.
4. The method for detecting multiple elements of a cold-galvanized layer by using an X-ray fluorescence non-standard sample according to claim 1, wherein in the second step, the sample wafer is in a square structure with a side length of 30-35 mm or in a round structure with a diameter of 30-40 mm.
5. The method for detecting multiple elements of a cold-galvanized layer by using an X-ray fluorescence non-standard sample according to claim 1, wherein in the fourth step, the fluorescence intensity uniformity evaluation condition is: the ratio of the fluorescence intensity difference value of the zinc element to the average value of the zinc element which meets the internal control standard plating plate is less than 3 percent.
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