CN116794079A - Method for quantitatively analyzing main element of sinter by using X-ray fluorescence without standard sample - Google Patents

Method for quantitatively analyzing main element of sinter by using X-ray fluorescence without standard sample Download PDF

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CN116794079A
CN116794079A CN202310617209.1A CN202310617209A CN116794079A CN 116794079 A CN116794079 A CN 116794079A CN 202310617209 A CN202310617209 A CN 202310617209A CN 116794079 A CN116794079 A CN 116794079A
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sample
standard
ray fluorescence
analysis
standard sample
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张鲁宁
王亚朋
牟英华
唐语
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Bengang Steel Plates Co Ltd
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Bengang Steel Plates Co Ltd
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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
    • G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • 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
    • G01N1/44—Sample treatment involving radiation, e.g. heat
    • 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
    • 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
    • G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G01N2001/2866—Grinding or homogeneising

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Abstract

The invention belongs to the technical field of detection of elements in sinter, and particularly relates to a method for quantitatively analyzing main elements of sinter by using X-ray fluorescence without a standard sample. The method comprises the following steps: step one, sample drying: grinding the sample to a screen mesh of 160-200 meshes, uniformly mixing, and drying for later use; step two, tabletting: placing the dried sample into a PVC plastic ring, and tabletting by using a tablet press; setting detection conditions of an X-ray fluorescence spectrometer; and step four, 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

Method for quantitatively analyzing main element of sinter by using X-ray fluorescence without standard sample
Technical Field
The invention belongs to the technical field of detection of elements in sinter, and particularly relates to a method for quantitatively analyzing main elements of sinter by using X-ray fluorescence without a standard sample.
Background
The iron ore sintering is a process of mixing and pelletizing various powdery iron-containing raw materials, then making the materials undergo a series of physical and chemical changes on sintering equipment, and binding mineral powder particles into blocks, wherein the sintered ore is a product thereof, and belongs to artificial block ores. The prior art for detecting the main element content of the sinter is aimed at: the national Standard GB/T6730 iron ore refers to the silica SiO in iron ore 2 Calcium oxide CaO, magnesium oxide MgO, aluminum oxide Al 2 O 3 Manganese oxide MnO and titanium oxide TiO 2 The detection method of the components comprises the following steps: method 1, capacity method: adding hydrochloric acid, nitric acid or perchloric acid for dissolution and filtration according to different chemical properties of elements, separating other elements, adding an indicator, and titrating to a constant volume by using a standard titration solution; method 2, atomic absorption spectrometry: dissolving with hydrochloric acid-nitric acid, evaporating to dryness, treating the residue with hydrofluoric acid, melting with sodium carbonate, adding proper release agent under certain acidity, and measuring with air-acetylene flame under specific wavelength of atomic absorption spectrophotometer; method 3, X-ray fluorescence correction curve method: and dissolving a sample by using borate, measuring the X-ray fluorescence intensity of the element to be detected, deducting the background intensity, correcting the matrix effect to prepare a correction curve between the fluorescence intensity and the element concentration, detecting the fluorescence intensity of the measured sample, and carrying the fluorescence intensity into the correction curve to obtain a result. The three methods have long detection period, use a large amount of chemical reagents, waste manpower and material resources, and have limited number of detection elements, and need to participate in a large amount of instruments.
Patent CN101526488A discloses a method for analyzing iron ore components by X-ray fluorescence spectrum, which is an internal standard calibration curve method, and has the advantages of complex operation and limited measurement elements. The paper (powder tabletting method for determining main elements in the sinter, third period 2019, tianjin metallurgy) discloses that X-ray fluorescence is used for detecting the tabletting of the sinter, and although the sample preparation is simple, a plurality of elements are detected simultaneously, firstly, the method is still a correction curve method, the detection range is limited, secondly, the mutual absorption/enhancement effect among the elements in the sinter is underestimated, and if unusual elements such as barium, nickel and the like can influence the detection result.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for quantitatively analyzing main elements of a sinter by using X-ray fluorescence without a standard sample. The method has the advantages of saving raw materials for detection, reducing production cost, improving labor productivity, simplifying the previous work of a plurality of people into one person for completion, shortening manufacturing time, detecting speed, reducing application reagents, improving labor conditions, reducing environmental pollution, expanding detection range, reducing the use of test products, particularly standard samples, and laying a foundation for increasing the detection quantity of elements 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 quantitatively analyzing main elements of a sinter by using an X-ray fluorescence standard-free sample, comprising the following steps:
step one, sample drying: grinding the sample to a screen mesh of 160-200 meshes, uniformly mixing, and drying for later use;
step two, tabletting:
placing the dried sample into a PVC plastic ring, and tabletting by using a tablet press;
step three, setting detection conditions of an X-ray fluorescence spectrometer:
analytical elemental lines and measurement conditions are shown in table 1:
table 1 analysis of elemental lines and measurement conditions
Fourth, detection by an X-ray fluorescence spectrometer:
(1) Selecting a standard sample, and placing the standard sample on a sample stage of an X-ray fluorescence spectrometer for fluorescence analysis to obtain the fluorescent X-ray measurement intensity of an analysis element in the standard sample;
(2) Obtaining a fluorescence analysis value of each element of the standard sample by adopting a standard sample-free analysis method, comparing the fluorescence analysis value with a standard value, and debugging and correcting the self-absorption/attraction effect coefficient of the analysis element until the fluorescence analysis value and the standard value meet the requirement of the reproducibility limit of the content of the analysis element;
(3) And placing the sample to be detected on a sample stage of an X-ray fluorescence spectrometer for fluorescence analysis to obtain a fluorescence analysis value of the content of the analysis element in the sample to be detected.
In the above technical solution, further, in the first step, the sample grinding time is 180±20s.
In the above technical scheme, in the first step, the drying temperature is 105±5 ℃, and the drying time is 1±0.1h.
In the above technical scheme, in the second step, the pressing time is kept for 20s on a tablet press at a rated pressure of 30 tons, and the wafer with the outer diameter of 40+/-2 mm and the inner diameter of not less than 32mm is prepared.
In the above technical solution, further, in the step (2), the content of each component in the standard sample needs to satisfy a normalization condition.
In the above technical solution, further, the standard sample is a sample consistent with the production condition of the sample to be tested.
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;
the content of each detected element meets the normalization condition:
C 1 +C 2 +…+C i …+C FIX +C REST ＝1(100％)
C i -the content,%;
C FIX -the content,%;
C REST -content of fixed component in the sample,%.
Scanning a standard sample by using an X-ray fluorescence spectrometer, detecting the intensity of the standard sample, and adding the standard sample into a detection software standard sample list; entering a standard sample list, inputting the content of each component in a standard sample, calculating the addition of each element, and judging whether the addition is close to 100% (normalization condition); loading standard value and fluorescence analysis value of standard sample under X-ray fluorescence standard-free method of sinter, and debugging self-absorption/enhancement effect coefficient K of each element in correction method i,i Coefficient of attraction/enhancement effect K i,j Until the fluorescence analysis value and the 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. 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 standard sample sintered ore Wk88306c-1 is selected to be made into tablets for 5 times, the tablets are put into a fluorometer to be detected by a sintered ore standard-free method, the relative standard deviation RSD of the measured results of each element is calculated, and the results are shown in Table 2:
TABLE 2 precision of agglomerate non-standard method
As can be seen from Table 3, the RSD of each component is less than 5%, and the precision of the method of the present invention is good.
Example 2
Standard samples 02-31B, GBW07220a, W88306b, wk88306c-1, GSB03-1807, YSBC13702, GBW 07226a, GBW 07226 were tested using the sinter no-standard method, and the results and standard values are shown in tables 3-5:
TABLE 3 sinter SiO 2 And Al 2 O 3 Comparison of detection results and standard values by standard-sample-free method
TABLE 4 comparison of test results and standard values of CaO and MgO of agglomerate by no-standard method
TABLE 5 sinter MnO and TiO 2 Comparison of detection results and standard values by standard-sample-free method
Note that: -this means that the component is in trace amounts.
As shown in tables 3-5, the standard-free method of the sintered ore has high conformity with the standard value result and no deviation, and meets the chemical inspection requirement.
Example 3
Silica SiO for sintered ore samples HB2208017, HB2208018, HB2208019, HB2208020, HB2208021 to be tested 2 Calcium oxide CaO, magnesium oxide MgO, aluminum oxide Al 2 O 3 Manganese oxide MnO and titanium oxide TiO 2 The ingredients were measured and compared with the calibration curve results, see tables 6-8:
TABLE 6 sinter SiO 2 And Al 2 O 3 Result comparison of standard-free method and correction curve method
TABLE 7 comparison of test sample and calibration curve method results for CaO and MgO agglomerate in no-standard method
TABLE 8 sinter MnO and TiO 2 Comparison of the results of the sample to be measured without standard sample method and the calibration curve method
The measurement results of the two methods are high in conformity and do not exceed the allowable error, and the method has feasibility.
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 (6)

1. A method for quantitatively analyzing main elements of a sintered ore by using X-ray fluorescence without a standard sample, which is characterized by comprising the following steps:
step one, sample drying: grinding the sample to a screen mesh of 160-200 meshes, uniformly mixing, and drying for later use;
step two, tabletting:
placing the dried sample into a PVC plastic ring, and tabletting by using a tablet press;
step three, setting detection conditions of an X-ray fluorescence spectrometer:
the analytical element spectral lines and measurement conditions are shown in the following table:
fourth, detection by an X-ray fluorescence spectrometer:
(1) Selecting a standard sample, and placing the standard sample on a sample stage of an X-ray fluorescence spectrometer for fluorescence analysis to obtain the fluorescent X-ray measurement intensity of an analysis element in the standard sample;
(2) Obtaining a fluorescence analysis value of each element of the standard sample by adopting a standard sample-free analysis method, comparing the fluorescence analysis value with a standard value, and debugging and correcting the self-absorption/attraction effect coefficient of the analysis element until the fluorescence analysis value and the standard value meet the requirement of the reproducibility limit of the content of the analysis element;
(3) And placing the sample to be detected on a sample stage of an X-ray fluorescence spectrometer for fluorescence analysis to obtain a fluorescence analysis value of the content of the analysis element in the sample to be detected.
2. The method for quantitative analysis of main elements of sintered ore according to claim 1, wherein in the first step, the sample grinding time is 180+ -20 s.
3. The method for quantitative analysis of main elements of sintered ore with no standard sample by X-ray fluorescence according to claim 1, wherein in the first step, the drying temperature is 105+ -5deg.C and the drying time is 1+ -0.1 h.
4. The method for quantitatively analyzing main elements of sintered ore by using X-ray fluorescence non-standard sample according to claim 1, wherein in the second step, the pressing time is kept for 20s at the rated pressure of 30 tons on a tablet press, and a wafer with the outer diameter of 40+/-2 mm and the inner diameter of not less than 32mm is prepared.
5. The method for quantitative analysis of elements in sintered ore by X-ray fluorescence according to claim 1, wherein in the step (2), the content of each component in the standard sample is required to satisfy the normalization condition.
6. The method for quantitatively analyzing main elements of sintered ore by using X-ray fluorescence non-standard sample according to claim 1, wherein the standard sample is a sample consistent with the production conditions of the sample to be measured.
CN202310617209.1A 2023-05-29 2023-05-29 Method for quantitatively analyzing main element of sinter by using X-ray fluorescence without standard sample Pending CN116794079A (en)

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