Preparation method of X fluorescence analyzer drift correction sample for anode copper

Abstract

The invention discloses a preparation method of an X fluorescence analyzer drift correction sample for anode copper, and belongs to the technical field of X fluorescence analyzer drift correction. The method comprises the following steps: (1) processing anode copper until the size meets the size requirement of a drift correction sample of an X fluorescence analyzer to obtain an anode copper sample; (2) carrying out surface polishing treatment on the anode copper sample obtained in the step (1); and (3) heating the surface of the anode copper sample subjected to the polishing treatment in the step (2), so that a uniform and compact CuO oxide layer is formed on the surface of the anode copper sample. According to the method, the anode copper sample is treated to form a long-term stable oxide layer on the surface of the anode copper, so that the negative influence of random change of the properties of the sample on the drift correction of the X fluorescence analyzer is reduced, the drift correction accuracy is improved, the service life of the drift correction sample is prolonged, and the drift correction cost is reduced; and the drift correction efficiency is improved.

Description

Technical Field

[0001] This invention belongs to the field of X-ray fluorescence analyzer drift correction technology, and relates to a method for preparing a drift-corrected sample for an anode copper X-ray fluorescence analyzer. Background Technology

[0002] Copper electrolysis is a common production process in the copper smelting industry. During copper electrolysis, the quality of the anode copper used directly affects the quality of the cathode copper deposited. Therefore, before using anode copper to produce high-purity copper through copper electrolysis, it is necessary to determine the composition of the anode copper to ensure that qualified anode copper is used for the production of high-purity copper.

[0003] X-ray fluorescence (XRF) analyzers are non-destructive testing devices based on the principle of X-ray fluorescence. They are mainly used to determine the elemental content and composition of solid, liquid, and powder samples, and are widely used in non-ferrous mining, steel, cement, refractory materials, stainless steel, and alloy industries. Because they can accurately and quickly determine the elemental content and composition of anode copper, producers involved in copper electrolysis processes typically use XRF analyzers to analyze anode copper.

[0004] However, during the use of X-ray fluorescence analyzers, standard curve drift often occurs, leading to reduced accuracy of analytical results. Therefore, before using an X-ray fluorescence analyzer for detection and analysis, it is usually necessary to use drift-corrected samples to perform drift correction on the X-ray fluorescence analyzer to ensure more accurate analytical results, improve the reliability of the results, and safeguard copper smelting production.

[0005] Generally, to ensure the accuracy of X-ray fluorescence analysis results, the drift correction sample is the same as the analyte. Therefore, when the analyte is anodic copper, the drift correction sample must also be anodic copper. However, anodic copper correction samples have poor stability; when stored in air, their surface undergoes natural oxidation, which is highly random and easily leads to uneven composition. Storing them in a vacuum increases the difficulty of preservation, requires additional preservation costs, and cannot completely prevent oxidation. Currently, two methods are commonly used to solve these problems: using a lathe to remove the unevenly oxidized oxide layer (incomplete oxidation) from the surface of the drift correction sample, or directly purchasing a new drift correction sample for drift correction. However, when removing the surface oxide layer on a lathe, elemental segregation is unavoidable in the drift correction sample itself, making it difficult to ensure that the sample after lathe is exactly the same as the previous drift correction sample. When the differences between the two drift correction samples are large, the drift degree of the X-ray fluorescence analyzer will be increased due to the differences in the samples themselves. This part of the drift result does not belong to the actual drift degree of the X-ray fluorescence analyzer, thus increasing the error of the drift coefficient calculation result and the drift correction error. Ultimately, this results in inaccurate results when the X-ray fluorescence analyzer analyzes the anode copper sample. It is necessary to turn the surface of a series (usually 10) of anode copper standard samples, establish a new anode copper analysis method, and reselect an anode copper standard sample as the anode copper drift correction sample. As the oxide layer on the sample surface is continuously removed, the sample will be continuously consumed. When the sample size is consumed to the point that it does not meet the applicable size of the X-ray fluorescence analyzer, a new anode copper standard sample must be purchased. The commercial price of the sample is about 12,000 yuan / sample, and it is not possible to purchase an anode copper standard sample with suitable composition, which will undoubtedly increase the detection and analysis cost.

[0006] Therefore, it is necessary to provide a method for preparing drift-corrected samples for X-ray fluorescence analysis of anodic copper, so as to obtain drift-corrected samples whose composition remains stable over a longer period of time, thereby extending the service life of drift-corrected samples, improving drift correction efficiency, and reducing the analysis cost of anodic copper. Summary of the Invention

[0007] To overcome the problems in the prior art, this invention heats the surface of the anode copper produced during copper smelting, causing a stable oxide layer to form on the surface of the anode copper in a short time. This allows the X-ray fluorescence analyzer to only detect and analyze the elemental composition and content of the stable oxide layer (since the drift correction process mainly calibrates the X-ray fluorescence analyzer and does not involve formal detection and analysis, the drift correction work can be completed by using the X-ray fluorescence analyzer to detect and analyze the stable oxide layer). This reduces the negative impact of the difference in the properties of the drift correction sample itself on the increased error of drift correction in different drift correction processes, improves the accuracy of drift correction, extends the service life of drift correction samples, and effectively reduces the cost of drift correction.

[0008] To achieve the above objectives, the present invention is implemented through the following technical solution: This invention proposes a method for preparing a drift-corrected sample of anolyte copper using an X-ray fluorescence analyzer, the preparation method comprising the following steps: (1) The anode copper is processed to meet the size requirements of the X-ray fluorescence analyzer drift correction sample to obtain the anode copper sample. X-ray fluorescence analysis of anode copper is a routine method. Usually, an X-ray fluorescence analyzer with a scintillation detector is used to perform X-ray fluorescence analysis on anode copper. Therefore, X-ray fluorescence correction of anode copper is usually the same as X-ray fluorescence correction of scintillation detector. The size of anode copper sample can be determined according to the conventional drift correction sample size.

[0009] If the anode copper itself meets the size requirements of the drift correction sample, there is no need to process the anode copper; it can be directly used as the anode copper sample for subsequent processing. If the anode copper itself does not meet the size requirements of the drift correction sample, it can be processed by conventional methods such as casting or turning.

[0010] (2) Perform surface finishing on the anode copper sample obtained in step (1).

[0011] (3) Heat the surface of the anode copper sample after the machining treatment in step (2) to form a dense CuO layer on the surface of the anode copper sample.

[0012] Preferably, in step (1), the anode copper sample is cylindrical with a diameter of 34 mm and a height of 20-30 mm.

[0013] Preferably, in step (3), the heating temperature is controlled at 450℃~500℃ and the heating time is 60min.

[0014] Preferably, in step (2), the surface of the anode copper sample is machined to a surface roughness Ra≤3.0μm.

[0015] The beneficial effects of this invention are: 1. This invention processes the anolyte copper sample to form a dense and stable CuO layer on its surface, thereby ensuring that the surface of the anolyte copper drift correction sample remains stable throughout different drift correction processes. This eliminates errors caused by the inherent differences in the properties of the anolyte copper drift correction sample itself and improves the accuracy of drift correction.

[0016] 2. Since the CuO oxide layer on the surface of the drift-corrected sample can remain stable for a long time, it is not necessary to remove the surface due to the different degrees of oxidation of the anode copper drift-corrected sample surface over a longer period of time. This can effectively solve the problem of drift correction error caused by the segregation of different components of the anode copper at different levels, which leads to different positions / levels detected in different drift corrections.

[0017] 3. In the drift correction process, this invention does not require surface removal due to varying degrees of oxidation on the surface of the anode copper drift correction sample. It can effectively solve the problem of drift correction errors caused by component segregation at different layers of anode copper, which leads to different positions / layers detected in different drift corrections. Anode copper produced by the copper smelting company itself can be used directly as the substrate for treatment, eliminating the need to purchase expensive standard samples for drift correction, thus reducing drift correction costs.

[0018] 4. The oxide layer of the drift-corrected sample prepared by this invention can remain stable for a long time. Therefore, over a long period of time, it can be considered that the same drift-corrected sample is being used for X-ray fluorescence analysis and drift correction. This reduces the frequency of re-establishing the analytical method, reduces the consumption of anodic copper standard samples, and thus reduces the analysis cost of anodic copper samples.

[0019] 5. The oxide layer of the drift-corrected sample prepared by this invention can remain stable for a longer period of time, thus allowing it to be used for an extended period without the need for frequent replacement of the drift-corrected sample, which helps reduce the analysis cost of anodic copper samples.

[0020] 6. The present invention reduces the Cu content in the anode copper-corrected sample by forming an oxide layer, so that the fluorescence intensity of Cu is controlled at about 77% of the detector's full intensity during the drift correction process. This ensures a sufficient count rate (high signal-to-noise ratio) and avoids nonlinear response caused by excessive signal saturation. As a result, the X-ray fluorescence analyzer is in its optimal working state during the drift correction process, with better drift correction sensitivity and better drift correction effect. Attached Figure Description

[0021] Figure 1 Image of the sample without oxidation drift correction; Figure 2 This is a physical image of the drift correction sample prepared according to the present invention. Detailed Implementation

[0022] The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments, but the scope of protection of the present invention is not limited to the content described.

[0023] Example 1 This embodiment prepares the drift-corrected sample using the following method: (1) Select self-produced anode copper with the required size directly as the anode copper sample.

[0024] (2) The surface of the anode copper sample is machined until the surface roughness of the anode copper does not exceed 3μm.

[0025] (3) Place the machined anode copper sample in a muffle furnace that has been heated to 500°C, open the muffle furnace door to allow oxygen to enter the furnace, and control the temperature to fluctuate between 450°C and 500°C (close the muffle furnace door when the temperature is close to 450°C). After heating for 60 minutes, take out the anode copper sample to obtain the drift correction sample.

[0026] The oxide layer of the drift-corrected sample prepared in this embodiment was observed to be uniform and dense.

[0027] X-ray fluorescence analysis was performed on the oxide layer of the drift-corrected sample prepared in this embodiment (X-ray tube power was 50 kV / 40 mA, which is also the X-ray tube power used in our unit's routine X-ray fluorescence analysis of Cu elemental anode copper). The results showed that the X-ray fluorescence intensity of Cu was 770.25 kcps, approximately 77.02% of the detector's full intensity. Eighteen months later, the same anode copper drift-corrected sample was analyzed again using the same method and X-ray fluorescence analyzer. The results showed that the X-ray fluorescence intensity of Cu was 769.36 kcps, which was about 76.94% of the detector's full intensity.

[0028] The X-ray fluorescence intensity analysis results from the two analyses show that the oxide layer can maintain high stability over a long period of time, which can effectively reduce the degree of error in the two drift correction processes. It can also be used for a long time, which is beneficial to reducing analysis costs.

[0029] Meanwhile, the X-ray fluorescence intensity analysis results from the two tests also show that the CuO layer thickness of the drift-corrected sample prepared by the method of this invention is sufficient, and X-rays will hardly penetrate the CuO layer.

[0030] In summary, this invention treats the anolyte copper sample to form a long-term stable and dense oxide layer on its surface, thereby reducing the negative impact of sample property fluctuations or variability on the accuracy of drift correction. When X-ray fluorescence analyzers perform drift correction, significant differences in the X-ray fluorescence intensity of the same element can occur between two correction processes. Fluorescence and variability in the sample's properties also cause significant differences in X-ray fluorescence intensity. Therefore, if the drift correction sample itself has poor stability, it can easily lead to increased errors in determining the degree of drift by the X-ray fluorescence analyzer, resulting in inaccurate correction. High sample stability reduces the influence of the sample itself on the error in determining the degree of drift, making the drift determination results more accurate and thus improving correction accuracy. Furthermore, the anolyte copper samples used in this invention are widely available, eliminating the need for frequent replacements and re-establishment of analytical methods, effectively reducing drift correction costs and improving drift correction efficiency.

[0031] Finally, it should be noted that the above preferred embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail through the above preferred embodiments, those skilled in the art should understand that various changes can be made to it in form and in detail without departing from the scope defined by the claims of the present invention.

Claims

1. A method for preparing a drift-corrected sample of anolyte copper using an X-ray fluorescence analyzer, characterized in that: The preparation method includes the following steps: (1) The anode copper is processed to meet the size requirements of the X-ray fluorescence analyzer for drift correction, and an anode copper sample is obtained; (2) Perform surface finishing on the anode copper sample obtained in step (1); (3) Heat the surface of the anode copper sample after the machining treatment in step (2) to form a dense CuO layer on the surface of the anode copper sample.

2. The preparation method according to claim 1, characterized in that: In step (1), the anode copper sample is cylindrical with a diameter of 34 mm and a height of 20-30 mm.

3. The preparation method according to claim 1, characterized in that: In step (3), the heating temperature is controlled at 450℃~500℃ and the heating time is 60min.

4. The preparation method according to claim 1, characterized in that: In step (2), the surface of the anode copper sample is machined to a surface roughness Ra≤3.0μm.

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