Analysis method for measuring copper content in copper tailings

Through precise pre-processing and spectral analysis methods, the problems of insufficient accuracy and precision in copper content detection in low-grade copper tailings were solved, and high-precision copper content determination was achieved.

CN120685576APending Publication Date: 2025-09-23JIANGXI COPPER
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Patent Information

Application Number
CN202510720640.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-30
Publication Date
2025-09-23

AI Technical Summary

Technical Problem

The existing technology has problems of insufficient accuracy and precision when measuring the copper content in low-grade copper tailings.

Method used

The sample amount was precisely controlled and pre-treatment was performed by adding specific amounts of hydrochloric acid and ammonium bifluoride to ensure complete dissolution of the sample. After dissolution with nitric acid, the sample was measured on an atomic absorption spectrometer. The most sensitive analytical line of copper element, 324.8 nm, was selected, and data processing was performed in combination with the working curve and calculation formula.

Benefits of technology

The analysis accuracy and precision of copper content in copper tailings are improved, ensuring the reliability and accuracy of the test results.

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Abstract

The invention discloses an analysis method for determining the copper content in copper tailings. According to the analysis method, the copper content in the copper tailings is finally obtained through pretreatment, complete dissolution, accurate volume determination, spectral analysis and data processing of the copper tailings, the accuracy and precision of determination are remarkably improved, and the analysis method is particularly suitable for detection of extremely-low-grade copper elements. According to the method, through a series of finely-regulated chemical treatment steps and an advanced spectrum analysis technology, the capability of accurately determining the copper content in a copper tailing sample is ensured.
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Description

Technical Field

[0001] The invention belongs to the technical field of metal analysis and detection, and particularly relates to an analysis method for determining the copper content in copper tailings. Technical Background

[0002] Copper tailings, a byproduct of copper ore smelting, contain various impurities. Accurately measuring their copper content is crucial for evaluating smelting efficiency and recovery rates. Existing technologies for processing low-grade copper elements suffer from insufficient accuracy and precision.

[0003] This method has the characteristics of high accuracy, good precision and wide detection range, providing guarantee for the improvement of copper smelting technology. Summary of the Invention

[0004] The invention discloses an analytical method for determining the copper content in copper tailings, so as to solve any of the above and other potential problems in the prior art.

[0005] In order to solve the above technical problems, the technical solution of the present invention is: an analytical method for determining the copper content in copper tailings, the analytical method specifically comprising the following steps:

[0006] S1) weighing a certain amount of copper tailings to be measured and carrying out pre-treatment;

[0007] S2) mixing the copper tailings treated in S1) with a certain amount of nitric acid to dissolve the copper tailings to obtain a mixed solution, transferring the obtained mixed solution to a volumetric flask and adding water to the volume to obtain a solution to be tested;

[0008] S3) starting the atomic absorption spectrometer and setting the measurement parameters;

[0009] S4) under the same conditions as those for measuring the test solution, a working curve is drawn with the copper concentration as the abscissa and the absorbance as the ordinate;

[0010] S5) obtaining the mass concentration of copper from the copper standard working curve, and calculating and obtaining the copper content in the copper tailings.

[0011] Furthermore, the copper content in the copper tailings in S1) is 0.10%-1.0%.

[0012] Furthermore, the specific steps of S1) are:

[0013] S1.1) Weigh 0.2000g-0.2500g of copper tailings into a beaker and blow 5ml of distilled water along the beaker wall to wet the sample.

[0014] S1.2) Add 20 ml of hydrochloric acid and 2-3 ml of saturated ammonium bifluoride solution, shake well, cover with a watch glass, and heat on a hot plate to 100-150°C for 5-8 minutes.

[0015] Further, the specific steps of S2) are:

[0016] S2.1) Add 10 ml of nitric acid to the copper tailings treated in S1) and heat until the copper tailings sample is completely dissolved. Boil gently for 4-6 minutes and then cool.

[0017] S2.2) Rinse the sides of the cup and watch glass with distilled water. Transfer the test solution to a 500ml volumetric flask as directed. Add distilled water to the flask, bring it to volume, and shake well to obtain the test solution.

[0018] Furthermore, the process parameters in S3) are: acetylene gas flow rate: 1.1 L / min, auxiliary gas flow rate: 0.26 MPa, measurement wavelength: 324.8 nm, lamp current: 4 mA, observation height: 7.0 mm, observation angle: 0 0 , slit: 0.5nm.

[0019] Further, the specific steps of S4) are:

[0020] S4.1) Pipette 0.00 mL, 0.50 mL, 1.00 mL, 3.00 mL, and 5.00 mL of a 500 μg / mL copper standard solution into a 500 mL volumetric flask pre-filled with 25 mL of nitric acid and shaken well. Dilute to the mark with water, mix well, and label the solution.

[0021] S4.2) Under the same conditions as for measuring the test solution, measure its absorbance intensity according to the instrument operating procedures, subtract the absorbance intensity of the "zero" concentration standard solution, and draw a working curve with copper concentration as the horizontal axis and absorbance intensity as the vertical axis.

[0022] Further, the copper content in the tailings can be calculated according to the following formula in S5):

[0023]

[0024] Where: is the measured concentration, ug / ml;

[0025] V is the sample measurement volume, ml;

[0026] m is the mass of the copper tailings sample, g.

[0027] Pretreatment: By precisely controlling the sample amount and adding specific amounts of hydrochloric acid and ammonium bifluoride, the sample dissolution process is optimized, preventing the loss or adsorption of copper at high temperatures, and ensuring the representativeness of the sample and the accuracy of the analysis.

[0028] 1. Complete dissolution: Use nitric acid to ensure that the sample is completely dissolved, converting the elements to be tested into an ionic state that is easy to detect, thereby improving the sensitivity of the analysis.

[0029] 2. Accurate volume determination: Accurate volume determination using a 500mL volumetric flask reduces errors during operation and improves the accuracy of analysis results.

[0030] 4. Spectral analysis: The most sensitive analytical line of copper element was selected and measured at a wavelength of 324.8nm. Air-acetylene flame atomic absorption spectrometry was used to improve the sensitivity and accuracy of detection.

[0031] 5. Data processing: By establishing a working curve and a specific calculation formula, the copper content in the tailings can be accurately calculated. The formula takes into account the sample measurement volume and sample mass to ensure the accuracy of the results.

[0032] The innovations are as follows:

[0033] 1. Optimized sample processing: Through precise chemical treatment steps, the dissolution quality of the sample and the extraction efficiency of copper are improved.

[0034] 2. Accurate spectral analysis: Select specific wavelengths and flame conditions, optimize for copper elements, and improve the sensitivity and accuracy of analysis.

[0035] 3. Innovation in data processing: By establishing precise working curves and calculation formulas, accurate determination of copper content in complex samples is ensured. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] Figure 1 The present invention is a schematic flow chart of an analytical method for determining the copper content in copper tailings. DETAILED DESCRIPTION

[0037] The present invention will be further explained and illustrated below through specific implementation plans. It should be understood that the purpose of the following implementation plans is to make the technical solutions of the present invention clearer and easier to understand, and is not limited to the scope of protection of the claims.

[0038] The present invention provides an analytical method for determining the copper content in copper tailings, comprising the following steps:

[0039] Step a: Weigh 0.2000g-0.2500g of copper tailings sample, place it in a 200ml beaker, and blow a small amount of water along the wall of the beaker;

[0040] Step b: Add 20 ml of hydrochloric acid, then add 2-3 ml of saturated ammonium bifluoride solution, shake well, cover with a watch glass, and heat on a hot plate at low temperature (100°C-150°C) for 5-8 minutes;

[0041] Step c: Add 10 ml of nitric acid, heat until the sample is completely dissolved, boil slightly for about 5 minutes, and then cool;

[0042] Step d: Rinse the cup wall and watch glass with distilled water, pour into a 500ml volumetric flask, dilute to the mark with distilled water, and shake well;

[0043] Step e: According to the operating conditions of the instrument, at a wavelength of 324.8 nm, using an air-acetylene flame and zeroing with water, a working curve was drawn with the copper concentrations of 0, 0.5, 1, 3, and 5 μg / mL as the abscissa and the absorbance as the ordinate;

[0044] Step f: Based on the data obtained during the experiment, the copper content in the tailings can be calculated according to the following formula:

[0045]

[0046] Where: ρ---measured concentration, ug / ml;

[0047] V---sample measurement volume, ml;

[0048] m---mass of the sample, g;

[0049] Example 1

[0050] Step a: Weigh 6 portions of 0.2000g-0.2500g copper tailings samples, place them in a 200ml beaker, and blow a small amount of water along the wall of the beaker;

[0051] Step b: Add 20 ml of hydrochloric acid to a beaker, then add 2-3 ml of saturated ammonium bifluoride solution, shake well, cover with a watch glass, and heat on a hot plate at low temperature (100°C-150°C) for 5-8 minutes;

[0052] Step c: Add 10 ml of nitric acid to a beaker, heat until the sample is completely dissolved, boil slightly for about 5 minutes, and then cool;

[0053] Step d: After the sample has cooled to room temperature, rinse the cup wall and watch glass with distilled water, transfer to a 500ml volumetric flask, dilute to the mark with distilled water, and shake well;

[0054] Step e: According to the operating conditions of the instrument, at a wavelength of 324.8 nm, using an air-acetylene flame and zeroing with water, a working curve was drawn with the copper concentrations of 0, 0.5, 1, 3, and 5 μg / mL as the abscissa and the absorbance as the ordinate;

[0055] Step f: Determine the sample. Based on the data obtained during the experiment, the copper content in the tailings can be calculated according to the following formula:

[0056]

[0057] Where: ρ---measured concentration, ug / ml;

[0058] V---sample measurement volume, ml;

[0059] m---mass of the sample, g;

[0060] Through Example 1, the test results are shown in Table 1:

[0061] Table 1

[0062]

[0063] From the data in the table above, we can see that the RSD of the copper multi-cup results in copper tailings is 0.73, indicating that the sample results have good precision.

[0064] Example 2

[0065] Select a reference copper sheet (Cu ≥ 99.999%) and two copper tailings samples. Add different amounts of the reference copper sheet to the copper tailings samples and determine the copper content according to the following steps:

[0066] Step a: Weigh 12 portions of 0.2000g-0.2500g copper tailings sample into a 200ml beaker, then weigh 12 portions of different amounts of reference copper sheets, and blow a small amount of water along the wall of the beaker;

[0067] Step b: Add 20 ml of hydrochloric acid to a beaker, then add 2-3 ml of saturated ammonium bifluoride solution, shake well, cover with a watch glass, and heat on a hot plate at low temperature (100°C-150°C) for 5-8 minutes;

[0068] Step c: Add 10 ml of nitric acid to a beaker, heat until the sample is completely dissolved, boil slightly for about 5 minutes, and then cool;

[0069] Step d: After the sample has cooled to room temperature, rinse the cup wall and watch glass with distilled water, transfer to a 500ml volumetric flask, dilute to the mark with distilled water, and shake well;

[0070] Step e: According to the operating conditions of the instrument, at a wavelength of 324.8 nm, using an air-acetylene flame and zeroing with water, a working curve was drawn with the copper concentrations of 0, 0.5, 1, 3, and 5 μg / mL as the abscissa and the absorbance as the ordinate;

[0071] Step f: Determine the sample. Based on the data obtained during the experiment, the copper content in the tailings can be calculated according to the following formula:

[0072]

[0073] Where: ρ---measured concentration, ug / ml;

[0074] V---sample measurement volume, ml;

[0075] m---mass of the sample, g;

[0076] The recovery rate test results obtained by Example 2 are shown in Table 2:

[0077] Table 2

[0078]

[0079] The method for determining the copper content in copper tailings of the present invention, through a series of innovative technical means, fills the gap that traditional detection methods cannot determine low-grade copper tailings, significantly improves the accuracy and precision of the determination, and provides important technical support for the optimization of copper smelting technology.

[0080] The above describes in detail an analytical method for determining the copper content in copper tailings provided in the examples of this application. The description of the above examples is intended only to facilitate understanding of the method and core concept of this application. Furthermore, those skilled in the art will appreciate that variations in the specific implementation and scope of application may occur based on the concepts of this application. In summary, this description should not be construed as limiting this application.

[0081] For example, certain words are used in the specification and claims to refer to specific components. Those skilled in the art should understand that hardware manufacturers may use different nouns to refer to the same component. This specification and claims do not use differences in names as a way to distinguish components, but use differences in the functions of components as the criteria for distinction. For example, "including" and "comprising" mentioned throughout the specification and claims are open-ended terms, so they should be interpreted as "including / including but not limited to". "Approximately" means that within an acceptable error range, those skilled in the art can solve the technical problems within a certain error range and basically achieve the technical effects. The subsequent description in the specification is a preferred embodiment of the present application, but the description is for the purpose of illustrating the general principles of the present application, and is not used to limit the scope of the present application. The scope of protection of the present application shall be as defined in the attached claims.

[0082] It should also be noted that the terms "include," "comprises," or any other variations thereof are intended to encompass non-exclusive inclusion, such that a product or system comprising a series of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such product or system. In the absence of further limitations, an element defined by the phrase "comprises a..." does not exclude the presence of other identical elements in the product or system comprising the element.

[0083] It should be understood that the term "and / or" as used herein is merely a description of the relationship between associated objects, indicating that three possible relationships exist. For example, "A and / or B" can represent: A exists alone, A and B exist simultaneously, or B exists alone. Furthermore, the character " / " in this document generally indicates that the associated objects are in an "or" relationship.

[0084] The above description shows and describes several preferred embodiments of the present application. However, as previously mentioned, it should be understood that the present application is not limited to the form disclosed herein and should not be construed as excluding other embodiments. Instead, the present application can be used in various other combinations, modifications, and environments and can be modified within the scope of the application concept described herein through the above teachings or technology or knowledge in the relevant field. Modifications and variations made by those skilled in the art that do not depart from the spirit and scope of the present application should be protected by the claims appended hereto.

Claims

1. An analytical method for measuring the copper content in copper tailings, characterized in that, The analytical method specifically comprises the following steps: S1) weighing a certain amount of copper tailings to be measured and carrying out pre-treatment; S2) mixing the copper tailings treated in S1) with a certain amount of nitric acid to dissolve the copper tailings to obtain a mixed solution, transferring the obtained mixed solution to a volumetric flask and adding water to the volume to obtain a solution to be tested; S3) starting the atomic absorption spectrometer and setting the measurement parameters; S4) under the same conditions as those for measuring the test solution, a working curve is drawn with the copper concentration as the abscissa and the absorbance as the ordinate; S5) obtaining the mass concentration of copper from the copper standard working curve, and calculating and obtaining the copper content in the copper tailings.

2. The analysis method according to claim 1, characterized in that The copper content in the copper tailings in S1) is 0.10%-1.0%.

3. The analysis method according to claim 1, characterized in that The specific steps of S1) are: S1.1) Weigh 0.2000g-0.2500g of copper tailings into a beaker and blow 5ml of distilled water along the beaker wall to wet the sample. S1.2) Add 20 ml of hydrochloric acid and 2-3 ml of saturated ammonium bifluoride solution, shake well, cover with a watch glass, and heat on a hot plate to 100-150°C for 5-8 minutes.

4. The analysis method according to claim 1, characterized in that The specific steps of S2) are: S2.1) Add 10 ml of nitric acid to the copper tailings treated in S1) and heat until the copper tailings sample is completely dissolved. Boil gently for 4-6 minutes, then remove and cool. S2.2) Rinse the sides of the cup and watch glass with distilled water. Transfer the test solution to a 500ml volumetric flask as directed. Add distilled water to the flask, bring it to volume, and shake well to obtain the test solution.

5. The analysis method according to claim 1, characterized in that The process parameters in S3) are: acetylene gas flow rate: 1.1 L / min, auxiliary gas flow rate: 0.26 MPa, measurement wavelength: 324.8 nm, lamp current: 4 mA, observation height: 7.0 mm, observation angle: 0 0 , slit: 0.5nm.

6. The analysis method according to claim 1, characterized in that The specific steps of S4) are: S4.1) Pipette 0.00 mL, 0.50 mL, 1.00 mL, 3.00 mL, and 5.00 mL of a 500 μg / mL copper standard solution into a 500 mL volumetric flask pre-filled with 25 mL of nitric acid and shaken well. Dilute to the mark with water, mix well, and label the solution. S4.2) Under the same conditions as for the test solution, measure its absorbance according to the instrument operating procedures, subtract the absorbance of the "zero" concentration standard solution, and plot a working curve with copper concentration as the horizontal axis and absorbance as the vertical axis.

7. The analysis method according to claim 1, characterized in that The copper content in the tailings can be calculated according to the following formula in S5): Where: ρ is the measured concentration, ug / ml; V is the sample measurement volume, ml; m is the mass of the copper tailings sample, g.