阅读说明：本技术 一种高含铜转炉氧化渣荧光分析标样制备及多元素快速分析方法 (Preparation and multi-element rapid analysis method of high-copper-content converter oxidation slag fluorescence analysis standard sample ) 是由 杨锐 陈全坤 张体富 杨应宝 叶钟林 宋银生 刘顺生 赵富江 姚依玲 于 2020-06-17 设计创作，主要内容包括：本发明涉及一种高含铜转炉氧化渣荧光分析标样制备及多元素快速分析方法,该标样制备方法包括以下步骤：样品筛选、样品处理、样品压制；对多元素快速分析的方法包括以下步骤：化学定值、条件设置、建立分析曲线、分析曲线验证。结合本发明的荧光分析标样制备及多元素快速分析方法,产生的有益效果为,1、分析元素范围广：可以实现高含铜氧化渣中多达16种元素分析；2、与化学分析相比,X射线荧光分析法测定高含铜氧化渣含铜准确性可以控制在1％以内,接收到样品后可以实现10分钟报出数据,对生产调控具有很好的指导作用和意义；3、每年可以减少外送化学分析费用20万元。(The invention relates to a preparation method of a standard sample for fluorescence analysis of high-copper-content converter oxidation slag and a rapid multi-element analysis method, wherein the preparation method of the standard sample comprises the following steps: sample screening, sample processing and sample pressing; the method for rapidly analyzing the multiple elements comprises the following steps: chemical value determination, condition setting, analysis curve establishment and analysis curve verification. The fluorescence analysis standard sample preparation and multi-element rapid analysis method provided by the invention has the beneficial effects that 1, the analysis element range is wide: the analysis of up to 16 elements in the high copper-containing oxidizing slag can be realized; 2. compared with chemical analysis, the accuracy of measuring the copper content of the high-copper-content oxidizing slag by using an X-ray fluorescence analysis method can be controlled within 1 percent, data can be reported in 10 minutes after a sample is received, and the method has good guiding effect and significance on production regulation and control; 3. the outward chemical analysis cost can be reduced by 20 ten thousand yuan each year.)

1. A preparation method of a standard sample for fluorescence analysis of high copper-containing converter oxidation slag is characterized by comprising the following steps:

1) sample screening

Counting the chemical analysis grades of the existing copper oxide slag, finding out the grades of the copper oxide slag with the lowest copper content and the highest copper content, carrying out sample combination according to the copper grade difference within 3 percent, and finding out 10 or more samples, wherein the weight of each sample is controlled to be 200g +/-5 g;

2) sample processing

The grinding disc is cleaned for the first time by quartz sand, the oxidation slag sample combined in the step 1 is cleaned for the second time, the rest oxidation slag sample is poured into the cleaned grinding disc, the grinding time is set to be 20s each time, the ground sample is screened by a 200-mesh standard sieve, and the oversize sample which cannot be screened is mixed into the unground sample to be continuously ground until all the samples pass through the 200-mesh standard sieve;

3) sample pressing

Filling the sample in the step 2 into a sample ring with the diameter of the sample ringAnd setting the pressure of the sample press to be 50 tons, and maintaining the pressure for 20s, and pressing the sample into a powder tabletting sample.

2. The method for rapidly analyzing multiple elements by using the preparation method of the standard sample for fluorescence analysis of the high-copper-content converter oxidation slag as defined in claim 1 is characterized in that: the method comprises the following steps:

A) chemical definite value

Carrying out chemical analysis and value determination on the contents of Cu, Fe and S elements in the oxidation slag;

B) condition setting

The fluorescence analysis conditions of each element are set as follows:

for Cu: calibration line Ka1, 2, detector: duplex xenon-sealed detector, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Fe: calibration line Ka1, 2, detector: duplex xenon-sealed detector, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for S: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: GE. A collimator: 300 μm, voltage: 36kV, Current: 100 mA.

3. The method for multiple element rapid analysis according to claim 2, characterized in that: the step A) also comprises the step of treating SiO in the oxidation slag₂、CaO、MgO、Al₂O₃And (5) carrying out chemical analysis and value determination.

4. A method for multiple element rapid analysis according to claim 3, characterized in that: corresponding to SiO in the p-oxidation slag₂、CaO、MgO、Al₂O₃The fluorescence analysis conditions for each element for chemical analysis were set as follows:

for SiO₂: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: PE, collimator: 300 μm, voltage: 36kV, Current: 100 mA;

for CaO: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 36kV, Current: 100 mA;

for MgO: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: PX1, collimator: 700 μm, voltage: 36kV, Current: 100 mA;

for Al₂O₃: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 36kV, Current: 100 mA.

5. A method for multiple element rapid analysis according to claim 3, characterized in that: and the step A) also comprises the step of carrying out chemical analysis and value determination on Pb, Zn, As, Sb, Bi, Ni, Sn, Co and Cd in the oxidation slag.

6. The method for multiple element rapid analysis according to claim 5, characterized in that: correspondingly setting the fluorescence analysis conditions of the elements for carrying out chemical analysis and definite value on Pb, Zn, As, Sb, Bi, Ni, Sn, Co and Cd in the oxidation slag, wherein the conditions are As follows:

for Pb: correction line Lb1, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Zn: calibration line Kb1, 3, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for As: calibration line Kb1, 3, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Sb: calibration line Ka1, 2, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Bi: calibration line Ka1, 2, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Ni: calibration line Ka1, 2, detector: duplex xenon-sealed detector, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Sn: calibration line Ka1, 2, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 60kV, current: 60 mA;

for Co: calibration line Ka1, 2, detector: duplex xenon-sealed detector, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 60kV, current: 60 mA;

for Cd: calibration line Ka1, 2, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 60kV, current: 60 mA.

7. The method for multi-element rapid analysis according to any of claims 2, 4, 6, wherein: the method comprises setting after B) condition setting:

step C): establishing an analytical curve

And (3) carrying out element fluorescence analysis intensity test on the standard sample according to the condition setting, and establishing a relationship between light intensity and element concentration through an X-ray fluorescence spectrometer: performing fluorescence analysis quantitative analysis, wherein the element X-ray fluorescence analysis light intensity and the chemical concentration are in a linear relation; the calibration is carried out by an alpha empirical coefficient method, data points with more deviation curves are deleted, the linear correlation coefficient of the fluorescence analysis curve of each element is controlled to be more than 0.99, and the curve of each analysis element is built and corrected one by one according to the method;

qualitative and quantitative X-ray fluorescence analysis is based on Moseley's law, Bragg's equation and Lambert-Beer's law

1) Moseley's law: the square root of the spectral line frequency is linear with the number of the elements arranged in the periodic tableWherein λ is wavelength, Q is constant, and Z is atomic number; sigma is shieldingThe number of coefficients;

2) bragg equation: fundamental relations illustrating crystal diffraction: 2dsin θ ═ n λ

Wherein θ: incident angle d: the crystal spacing; λ: wavelength of light

3) Lambert-Beer's law, the sample absorption status involves the calculation of the relative intensity of theoretical X-ray fluorescence

I₀: the intensity of the incident ray; i: (ii) a transmission intensity; mu.s_m: a mass absorption coefficient; ρ: the density of the substance; t: the thickness of the substance;

4) derived from the above derivation: the intensity of the characteristic spectral line of X-ray is in linear relation with chemical concentration, namely: c + E R M, wherein C: chemical concentration; d, analyzing the intercept of the line; e, analyzing the slope of the line; r M is optical intensity;

step D) verification of analysis curves

Respectively checking whether each element analysis curve meets the requirements or not by carrying out chemical analysis and fluorescence analysis comparison on unknown samples; and if the requirements are not met, returning to the step C again, and adjusting and correcting the curve again.

8. The method for multi-element rapid analysis according to any of claims 2, 4, 6, wherein: the step A) is arranged after the step 2) and before the step 3) of the standard sample preparation method; the step B) is arranged after the step 3) of the standard sample preparation method.

Technical Field

The invention belongs to the technical field of element analysis methods, and particularly relates to the technical field of a fluorescence analysis method for multiple elements in high-copper-content converter oxidation slag used by copper processing enterprises.

Background

The converter of the existing copper processing enterprise adopts a high-grade (Cu: 70-75%) matte one-step converting method, the copper-containing grade of the produced oxidation slag is 10-50% (chemical analysis), the fluctuation range is large, the components are relatively complex, the existing X-ray fluorescence rapid analysis curve is not suitable for the production requirement, and a new standard sample needs to be prepared again and a new analysis curve needs to be established. In the copper smelting process, low-grade (Cu: 50-60%) matte is blown into blister copper by a converter, a large amount of converter slag is generated in the slagging process, the slag mainly contains three components of copper, iron and silicon, the copper grade is mainly concentrated between 3-5%, the component fluctuation is not large, and the copper slag can be directly subjected to flotation recovery because the copper slag has low grade; the high-grade (70-80 percent of Cu) matte is blown without a slagging stage, copper is smelted in one step, converter oxidation slag with high copper content (10-50 percent of Cu) is generated, the copper slag has a large fluctuation range and relatively complex components, and the copper slag can be directly returned to the furnace for smelting as a cold charge due to high grade of the copper slag. In order to guide production, most of the low-grade copper converter slag at present adopts a fluorescence rapid analysis method, while the high-copper-content oxidation slag is difficult to prepare for analyzing standard samples due to complex components and large grade fluctuation range, and is mainly dependent on chemical analysis at present.

The main problems existing in the analysis of the high copper-containing converter oxidation slag are as follows: 1. the currently produced converter oxidation slag has high copper content, large component fluctuation and poor analysis accuracy, and an analysis result has no guiding effect on production; 2. most elements need to be sent out for chemical analysis, the detection period is long, the data reporting is relatively delayed, and the test cost needs to be additionally increased when the production guidance is not in time; 3. the sample amount of each oxidation slag sample is small, a plurality of oxidation slag samples are required to be combined to prepare a fluorescence analysis standard sample, the manual sample mixing time is long, and the sample uniformity is difficult to ensure.

Examples are for evidence: a certain copper smelting enterprise adopts a bottom blowing furnace and converter blowing process to smelt and produce blister copper, mainly uses low raw material coarse impurities, the bottom blowing furnace is smelted to produce high-grade (75% -80%) matte, the converter is smelted and produces blister copper in one step, high-grade (Cu: 15% -50%) oxidation slag is generated along with the smelting and producing process of the converter, at present, the high-copper-containing converter oxidation slag has large copper-containing grade fluctuation, a fluorescence analysis standard sample is difficult to prepare, and the method also depends on chemical analysis, but the chemical analysis period is long, the data report is relatively lagged, and the method has low guidance on smelting and producing.

Disclosure of Invention

The invention aims to solve the defects of the problems and provides a method for preparing a fluorescence analysis standard sample of the high-copper-content converter oxidation slag and quickly analyzing multiple elements.

The invention is realized by adopting the following technical scheme.

A preparation method of a standard sample for fluorescence analysis of high copper-containing converter oxidation slag comprises the following steps:

1) sample screening

Counting the chemical analysis grades of the existing copper oxide slag, finding out the grades of the copper oxide slag with the lowest copper content and the highest copper content, carrying out sample combination according to the copper grade difference within 3 percent, and finding out 10 or more samples, wherein the weight of each sample is controlled to be 200g +/-5 g;

2) sample processing

The grinding disc is cleaned for the first time by quartz sand, the oxidation slag sample combined in the step 1 is cleaned for the second time, the rest oxidation slag sample is poured into the cleaned grinding disc, the grinding time is set to be 20s each time, the ground sample is screened by a standard sieve of 200 meshes (0.074mm), and the oversize sample which cannot be screened is mixed into the unground sample to be continuously ground until all the samples pass through the standard sieve of 200 meshes;

3) sample pressing

Filling the sample in the step 2 into a sample ring with the diameter of the sample ringAnd setting the pressure of the sample press to be 50 tons, and maintaining the pressure for 20s, and pressing the sample into a powder tabletting sample.

The method for rapidly analyzing the multiple elements by using the preparation method of the fluorescence analysis standard sample of the high-copper-content converter oxidation slag comprises the following steps:

A) chemical definite value

Carrying out chemical analysis and value determination on Cu, Fe and S in the oxidation slag;

B) condition setting

The fluorescence analysis conditions of each element are set as follows:

for Cu: calibration line Ka1, 2, detector: duplex xenon-sealed detector, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Fe: calibration line Ka1, 2, detector: duplex xenon-sealed detector, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for S: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: GE. A collimator: 300 μm, voltage: 36kV, Current: 100 mA.

Further, the step A) of the invention also comprises the step of adding SiO in the oxidation slag₂、CaO、MgO、Al₂O₃And (5) carrying out chemical analysis and value determination.

Further, the invention corresponds to SiO in the p-oxidation slag₂、CaO、MgO、Al₂O₃The fluorescence analysis conditions for each element for chemical analysis were set as follows:

for SiO₂: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: PE, collimator: 300 μm, voltage: 36kV, Current: 100 mA;

for CaO: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 36kV, Current: 100 mA;

for MgO: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: PX1, collimator: 700 μm, voltage: 36kV, Current: 100 mA;

for Al₂O₃: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 36kV, Current: 100 mA.

Further, the step A) of the invention also comprises the step of carrying out chemical analysis and value determination on Pb, Zn, As, Sb, Bi, Ni, Sn, Co and Cd in the oxidation slag.

Further, the invention sets the fluorescence analysis conditions of each element for carrying out chemical analysis and definite value on Pb, Zn, As, Sb, Bi, Ni, Sn, Co and Cd in the oxidation slag, and the conditions are As follows:

for Pb: correction line Lb1, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Zn: calibration line Kb1, 3, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for As: calibration line Kb1, 3, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Sb: calibration line Ka1, 2, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Bi: calibration line Ka1, 2, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Ni: calibration line Ka1, 2, detector: duplex xenon-sealed detector, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Sn: calibration line Ka1, 2, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 60kV, current: 60 mA;

for Co: calibration line Ka1, 2, detector: duplex xenon-sealed detector, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 60kV, current: 60 mA;

for Cd: calibration line Ka1, 2, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 60kV, current: 60 mA.

Further, the method of the present invention includes setting after setting the condition of B):

step C): establishing an analytical curve

And (3) carrying out element fluorescence analysis intensity test on the standard sample according to the condition setting, and establishing a relationship between light intensity and element concentration through an X-ray fluorescence spectrometer: performing fluorescence analysis quantitative analysis, wherein the element X-ray fluorescence analysis light intensity and the chemical concentration are in a linear relation; the calibration is carried out by an alpha empirical coefficient method, data points with more deviation curves are deleted, the linear correlation coefficient of the fluorescence analysis curve of each element is controlled to be more than 0.99, and the curve of each analysis element is built and corrected one by one according to the method;

qualitative and quantitative X-ray fluorescence analysis is based on Moseley's law, Bragg's equation and Lambert-Beer's law

1. Moseley's law: the square root of the spectral line frequency is linear with the number of the elements arranged in the periodic table(where λ is the wavelength, Q is a constant, Z is the atomic number, and σ is the number of shielding coefficients)

2. Bragg equation: fundamental relations illustrating crystal diffraction: 2dsin θ ═ n λ (where θ: incident angle d: crystal spacing; λ: wavelength)

3. Lambert-Beer's law, the sample absorption status involves the calculation of the relative intensity of theoretical X-ray fluorescence(I₀: the intensity of the incident ray; i: (ii) a transmission intensity; mu.s_m: a mass absorption coefficient; ρ: the density of the substance; t: the thickness of the substance);

4. derived from the above derivation: the intensity of the characteristic spectral line of X-ray is in linear relation with chemical concentration, namely: c + E R M, wherein (C: chemical concentration; D: intercept of analytical line; E: slope of analytical line; R M: optical intensity);

step D) verification of analysis curves

Respectively checking whether each element analysis curve meets the requirements or not by carrying out chemical analysis and fluorescence analysis comparison on unknown samples; and if the requirements are not met, returning to the step C again, and adjusting and correcting the curve again.

Further, the step A) is arranged after the step 2) and before the step 3) of the standard sample preparation method; the step B) is arranged after the step 3) of the standard sample preparation method.

The invention has the beneficial effects that 1, the analysis element range is wide: the analysis of up to 16 elements in the high copper-containing oxidizing slag can be realized; 2. compared with chemical analysis, the accuracy of the copper-containing X-ray fluorescence analysis in the high-copper-containing oxidizing slag can be controlled within 1 percent, data can be reported in 10 minutes after a sample is received, and the method has good guiding effect and significance on production regulation and control; 3. after the sample is received, the fluorescence analysis of the high copper-containing oxidation slag can be realized for 10 minutes, and the outgoing chemical analysis cost can be reduced by 20 ten thousand yuan each year.

The invention is further explained below with reference to the drawings and the detailed description.

Drawings

FIG. 1 is a diagram showing the relationship between the concentration of the element in the high-grade converter oxidation slag and the optical intensity.

FIG. 2 is a graph showing the X-ray fluorescence analysis of copper in the oxidized slag of the converter.

The content concentration of the copper element and the optical intensity are in a linear relation, the linear correlation coefficient is good and is 0.996, the root mean square RMS is 0.33%, and the quality factor K is 0.07, so that the requirements can be met.

Detailed Description

A preparation method of a standard sample for fluorescence analysis of high copper-containing converter oxidation slag comprises the following steps:

1) sample screening

Counting the chemical analysis grades of the existing copper oxide slag, finding out the grades of the copper oxide slag with the lowest copper content and the highest copper content, carrying out sample combination according to the copper grade difference within 3 percent, and finding out 10 or more samples, wherein the weight of each sample is controlled to be 200g +/-5 g;

2) sample processing

The grinding disc is cleaned for the first time by quartz sand, the oxidation slag sample combined in the step 1 is cleaned for the second time, the rest oxidation slag sample is poured into the cleaned grinding disc, the grinding time is set to be 20s each time, the ground sample is screened by a standard sieve of 200 meshes (0.074mm), and the oversize sample which cannot be screened is mixed into the unground sample to be continuously ground until all the samples pass through the standard sieve of 200 meshes;

3) sample pressing

Filling the sample in the step 2 into a sample ring with the diameter of the sample ring

And setting the pressure of the sample press to be 50 tons, and maintaining the pressure for 20s, and pressing the sample into a powder tabletting sample.

The method for rapidly analyzing the multiple elements by using the preparation method of the fluorescence analysis standard sample of the high-copper-content converter oxidation slag comprises the following steps:

A) chemical definite value

Carrying out chemical analysis and value determination on Cu, Fe and S in the oxidation slag; the basic analysis comprises three elements of Cu, Fe and S in the high-copper-content converter oxidation slag, and can basically meet the basic characteristics and elements of the analysis.

B) Condition setting

The fluorescence analysis conditions of each element are set as follows:

for Cu: calibration line Ka1, 2, detector: duplex xenon-sealed detector, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Fe: calibration line Ka1, 2, detector: duplex xenon-sealed detector, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for S: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: GE. A collimator: 300 μm, voltage: 36kV, Current: 100 mA.

Further, the step A) of the invention also comprises the step of adding SiO in the oxidation slag₂、CaO、MgO、Al₂O₃And (5) carrying out chemical analysis and value determination. The middle-level analysis comprises SiO in the oxidized slag of the converter with high copper content₂、CaO、MgO、Al₂O₃The four compounds can deeply analyze substances in a sample on the premise of basic analysis, and have a chronological sequence, namely, under the action of a certain time, the surface or internal elements of the high-copper-content converter oxidation slag can generate a certain oxidation effect.

Further, the invention corresponds to SiO in the p-oxidation slag₂、CaO、MgO、Al₂O₃The fluorescence analysis conditions for each element for chemical analysis were set as follows:

for SiO₂: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: PE, collimator: 300 μm, voltage: 36kV, Current: 100 mA;

for CaO: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 36kV, Current: 100 mA;

for MgO: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: PX1, collimator: 700 μm, voltage: 36kV, Current: 100 mA;

for Al₂O₃: calibration line Ka1, 2, detector: flow gas, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 36kV, Current: 100 mA.

Further, the step A) of the invention also comprises the step of carrying out chemical analysis and value determination on Pb, Zn, As, Sb, Bi, Ni, Sn, Co and Cd in the oxidation slag. The high-level analysis comprises trace elements of Pb, Zn, As, Sb, Bi, Ni, Sn, Co and Cd in the high-copper content converter oxidation slag, can deeply analyze substances in a sample on the premise of medium-level analysis, is more systematic and comprehensive, basically relates to all element components in the high-copper content converter oxidation slag, thoroughly solves the defects in the background technology, and meets all the advantages in the beneficial effects of the invention.

Further, the invention sets the fluorescence analysis conditions of each element for carrying out chemical analysis and definite value on Pb, Zn, As, Sb, Bi, Ni, Sn, Co and Cd in the oxidation slag, and the conditions are As follows:

for Pb: correction line Lb1, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Zn: calibration line Kb1, 3, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for As: calibration line Kb1, 3, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Sb: calibration line Ka1, 2, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Bi: calibration line Ka1, 2, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Ni: calibration line Ka1, 2, detector: duplex xenon-sealed detector, optical filter: no need, spectroscopic crystal: LiF200, collimator: 150 μm, voltage: 60kV, current: 60 mA;

for Sn: calibration line Ka1, 2, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 60kV, current: 60 mA;

for Co: calibration line Ka1, 2, detector: duplex xenon-sealed detector, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 60kV, current: 60 mA;

for Cd: calibration line Ka1, 2, detector: hipercint high energy scintillation, optical filter: no need, spectroscopic crystal: LiF200, collimator: 300 μm, voltage: 60kV, current: 60 mA.

Table for setting conditions of all elements or compounds of the present invention

Further, the method of the present invention includes setting after setting the condition of B):

step C): establishing an analytical curve

And (3) carrying out element fluorescence analysis intensity test on the standard sample according to the condition setting, and establishing a relationship between light intensity and element concentration through an X-ray fluorescence spectrometer: performing fluorescence analysis quantitative analysis, wherein the element X-ray fluorescence analysis light intensity and the chemical concentration are in a linear relation; the calibration is carried out by an alpha empirical coefficient method, data points with more deviation curves are deleted, the linear correlation coefficient of the fluorescence analysis curve of each element is controlled to be more than 0.99, and the curve of each analysis element is built and corrected one by one according to the method;

qualitative and quantitative X-ray fluorescence analysis is based on Moseley's law, Bragg's equation and Lambert-Beer's law

1. Moseley's law: the square root of the spectral line frequency is linear with the number of the elements arranged in the periodic table

(where λ is the wavelength, Q is a constant, Z is the atomic number, and σ is the number of shielding coefficients)

2. Bragg equation: fundamental relations illustrating crystal diffraction: 2dsin θ ═ n λ (where θ: incident angle d: crystal spacing; λ: wavelength)

3. Lambert-Beer's law, the sample absorption status involves the calculation of the relative intensity of theoretical X-ray fluorescence

(I₀: the intensity of the incident ray; i: (ii) a transmission intensity; mu.s_m: a mass absorption coefficient; ρ: the density of the substance; t: the thickness of the substance);

4. derived from the above derivation: the intensity of the characteristic spectral line of X-ray is in linear relation with chemical concentration, namely: c + E R M, wherein (C: chemical concentration; D: intercept of analytical line; E: slope of analytical line; R M: optical intensity);

step D) verification of analysis curves

Respectively checking whether each element analysis curve meets the requirements or not by carrying out chemical analysis and fluorescence analysis comparison on unknown samples; and if the requirements are not met, returning to the step C again, and adjusting and correcting the curve again.

Further, the step A) is arranged after the step 2) and before the step 3) of the standard sample preparation method; the step B) is arranged after the step 3) of the standard sample preparation method.

The present valve methods involve equipment including, but not limited to: a sealed test sample preparation crusher (for grinding and mixing samples), a 200-mesh standard sieve (for sieving samples and detecting sample granularity), a 60-ton sample press (for pressing powder samples), a sample ring (for pressing powder samples) and an X-ray fluorescence spectrometer; and so on.

The above description is only a part of specific embodiments of the present invention (since the formula of the present invention belongs to the numerical range, the embodiments are not exhaustive, and the protection scope of the present invention is subject to the numerical range and other technical point ranges), and the detailed contents or common knowledge known in the schemes are not described too much. It should be noted that the above-mentioned embodiments do not limit the present invention in any way, and all technical solutions obtained by means of equivalent substitution or equivalent transformation for those skilled in the art are within the protection scope of the present invention. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.