Method for measuring manganese content in copper concentrate

By optimizing the pretreatment process of copper concentrate samples and combining it with inductively coupled plasma optical emission spectrometry, the high cost and low accuracy problems of manganese content determination in copper concentrate were solved, low-cost, high-precision manganese element determination was achieved, and the technical level and product quality of copper smelting enterprises were improved.

CN120668644APending Publication Date: 2025-09-19CHIFENG YUNTONG NON FERROUS METAL CO LTD +1
View PDF 0 Cites 1 Cited by

Patent Information

Application Number
CN202510775535.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-11
Publication Date
2025-09-19

AI Technical Summary

Technical Problem

The existing technology for determining the manganese content in copper concentrate is costly and has low accuracy. X-ray fluorescence spectrometry is affected by matrix effects and spectral interference, resulting in inaccurate test results.

Method used

A mixed acid digestion system of nitric acid-hydrochloric acid-perchloric acid-hydrofluoric acid was used in combination with inductively coupled plasma optical emission spectrometry. The standard curve method and blank solution correction were used to optimize the sample pretreatment process, achieving complete dissolution and high-sensitivity analysis of manganese.

Benefits of technology

It significantly improves the accuracy and precision of manganese content determination in copper concentrate, reduces detection costs, meets the demand for trace manganese determination, optimizes smelting process parameters, and improves metal recovery rate and end product quality.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure SMS_1
    Figure SMS_1
  • Figure SMS_2
    Figure SMS_2
  • Figure SMS_3
    Figure SMS_3
Patent Text Reader

Abstract

The invention relates to the technical field of element detection, in particular to a method for measuring the manganese content in copper concentrate, which comprises the following steps: weighing a copper concentrate sample with the mass of m in a tetrafluoroethylene beaker, and adding a small amount of water to soak the sample; adding nitric acid and hydrochloric acid, and heating at 200-300 DEG C for 5-10 minutes; then adding perchloric acid and hydrofluoric acid, heating at 200-300 DEG C until the copper concentrate sample is completely dissolved, and cooling to room temperature; adding dilute nitric acid, and heating to dissolve the separated salt crystals to obtain a to-be-detected pre-solution; transferring the to-be-detected pre-solution to a volumetric flask, adding water to dilute the pre-solution to a scale line, and uniformly shaking to obtain a to-be-detected solution; according to the method, a nitric acid-hydrochloric acid-perchloric acid-hydrofluoric acid mixed acid digestion system is adopted, so that the manganese element in the copper concentrate is completely dissolved, and the interference of a complex matrix on manganese determination is effectively solved; by combining the high sensitivity and multi-element analysis capability of the inductively coupled plasma emission spectrometer, a linear standard curve of a manganese element characteristic spectral line and concentration is established, and the accuracy and precision of quantitative analysis are remarkably improved.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The present invention relates to the technical field of element detection, and in particular to a method for determining the manganese content in copper concentrate. Background Art

[0002] In the copper smelting industry, copper concentrate, a core raw material, requires precise chemical composition analysis, crucial for optimizing smelting processes, ensuring product quality, and achieving environmental protection. Manganese, a common impurity in copper concentrate, not only affects the efficiency and equipment life of the smelting process, but also the purity and performance of the final copper product. Therefore, establishing an accurate and reliable method for determining manganese content in copper concentrate is crucial for improving the overall technical level and economic efficiency of the copper smelting industry.

[0003] Currently, X-ray fluorescence spectrometry is the primary method for determining manganese content in copper concentrates. However, this method places high demands on instrumentation, requiring a high-precision X-ray fluorescence spectrometer and related auxiliary equipment. This leads to high testing costs and limits its widespread application. Furthermore, when measuring complex matrix samples, X-ray fluorescence spectrometry can be affected by factors such as matrix effects and spectral interference, which can compromise the accuracy of the results. Summary of the Invention

[0004] In view of the problems of high cost and low accuracy in the above-mentioned prior art for detecting manganese in copper concentrate, the present invention provides a method for determining the manganese content in copper concentrate.

[0005] To achieve the above object, the technical solution of the present invention is as follows:

[0006] A method for determining the manganese content in copper concentrate comprises the following steps:

[0007] S1. Prepare the test solution: weigh a copper concentrate sample with a mass of m into a tetrafluoroethylene beaker, add a small amount of water to wet the sample; add nitric acid and hydrochloric acid, and heat at 200-300°C for 5-10 minutes; then add perchloric acid and hydrofluoric acid, and heat at 200-300°C until the copper concentrate sample is completely dissolved, and cool to room temperature; add dilute nitric acid and heat at 200-300°C for 5-10 minutes to dissolve the precipitated salt crystals, and cool to room temperature to obtain a pre-test solution; transfer the pre-test solution to a volumetric flask, add water to dilute to the scale line, and shake well to obtain the test solution;

[0008] S2. Prepare a blank solution: prepare a blank solution according to step S1, without adding the copper concentrate sample to the blank solution, and use the same amount of reagents, reaction time, and reaction temperature as in step S1;

[0009] S3. Pipette 0.00 mL, 0.50 mL, 1.00 mL, 5.00 mL, 10.0 mL, and 20.0 mL of manganese standard solution into a 100 mL volumetric flask, add 10 mL of nitric acid, dilute to the mark with water, and shake well to obtain manganese solutions with solubility of 0 μg / mL, 0.5 μg / mL, 1 μg / mL, 5 μg / mL, 10 μg / mL, and 20 μg / mL, respectively;

[0010] S4. Prepare a manganese standard curve: Place the manganese solutions obtained in step S3 into an inductively coupled plasma emission spectrometer, test according to the characteristic spectrum of manganese element, and prepare a standard curve; the abscissa of the standard curve is the concentration of manganese solution, and the ordinate is the emission peak intensity of manganese element;

[0011] S5. Place the test solution obtained in step S1 and the blank solution obtained in step S2 into an inductively coupled plasma optical emission spectrometer, respectively, and perform tests based on the characteristic spectrum of manganese to obtain the equivalent milligram amounts of manganese in the test solution and the blank solution;

[0012] S6. Calculate the percentage of manganese in the copper concentrate according to the following formula:

[0013]

[0014] Where ρ x is the mass concentration of manganese obtained from the standard curve based on the equivalent milligram amount of the test solution, in μg / mL; ρ0 is the mass concentration of manganese obtained from the standard curve based on the equivalent milligram amount of the blank solution, in μg / mL; V is the constant volume of the test solution, in mL; m is the mass of the copper concentrate sample weighed, in g; 10 -6 It is the conversion rate between μg / mL and g / L, mL and L; 100 is the percentage conversion rate.

[0015] Furthermore, in S1, the mass of the copper concentrate sample weighed is 0.2000±0.0001 g.

[0016] Furthermore, in S1, the particle size of the copper concentrate sample is less than 200 mesh.

[0017] Furthermore, in S1, dilute nitric acid is V 水 :V 酸 =1:1 nitric acid solution.

[0018] Furthermore, in S4 and S5, the operating parameters of the inductively coupled plasma emission spectrometer are plasma emission power 1300kW, cooling gas flow rate 12L / min, auxiliary gas flow rate 0.8L / min, nebulizing gas flow rate 0.8L / min, sample flow rate 2L / min, pump speed 45r / min, pre-flushing time 30s, detection time 15s, argon purity greater than 99.99%, argon pressure 0.6-0.8MPa, and the characteristic spectral line wavelength of manganese element is 294.92nm.

[0019] When preparing the test solution, nitric acid and hydrochloric acid are first added. Nitric acid is used to initially oxidize organic matter in the copper concentrate sample and dissolve heavy metal ions in the copper concentrate sample. Hydrochloric acid is used to dissolve and complex heavy metal ions in the copper concentrate sample. The nitric acid and hydrochloric acid work together to dissolve manganese into the liquid phase, forming manganese ions. Perchloric acid and hydrofluoric acid are then added. Perchloric acid is used to oxidize insoluble organic matter and accelerate the acid removal process at high temperature. Hydrofluoric acid is used to reduce the total solid weight in the solution, allowing manganese to be released from the lattice. The combined action of perchloric acid and hydrofluoric acid can dissolve manganese more completely.

[0020] During the heating process, water from the mixed acid system continuously evaporates. As the solution nears dryness, certain metal salts precipitate due to reduced solubility, forming solid crystals. These precipitated salts may contain the element being analyzed. If not redissolved, the analysis result will be biased low. Therefore, dilute nitric acid must be added again to dissolve the precipitated salt crystals.

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] The present invention provides a method for determining the manganese content in copper concentrate. By optimizing the sample pretreatment process and adopting a mixed acid digestion system of nitric acid, hydrochloric acid, perchloric acid and hydrofluoric acid, the manganese element in the copper concentrate is completely dissolved, and the interference of a complex matrix on the manganese determination is effectively solved. The high sensitivity and multi-element analysis capability of an inductively coupled plasma emission spectrometer are combined to establish a linear standard curve between the characteristic spectrum line and the concentration of the manganese element, which significantly improves the accuracy and precision of the quantitative analysis. The blank solution correction is combined with the standard curve method to eliminate the interference of the reagent and the environmental background, and ensure the reliability of the manganese content determination result. The method has a standardized operating process and good repeatability, the detection limit can meet the determination requirements of trace manganese in copper concentrate, and the analysis efficiency is significantly improved. The method provides a low-cost, high-precision method for determining the manganese element for copper smelting enterprises, and is of great significance for optimizing smelting process parameters, improving metal recovery rate and ensuring the quality of end products. DETAILED DESCRIPTION

[0023] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below through specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0024] A method for determining the manganese content in copper concentrate comprises the following steps:

[0025] S1. Prepare the test solution: weigh a copper concentrate sample with a mass of m into a tetrafluoroethylene beaker, add a small amount of water to wet the sample; add nitric acid and hydrochloric acid, and heat at 200-300°C for 5-10 minutes; then add perchloric acid and hydrofluoric acid, and heat at 200-300°C until the copper concentrate sample is completely dissolved, and cool to room temperature; add dilute nitric acid and heat at 200-300°C for 5-10 minutes to dissolve the precipitated salt crystals, and cool to room temperature to obtain a pre-test solution; transfer the pre-test solution to a volumetric flask, add water to dilute to the scale line, and shake well to obtain the test solution;

[0026] S2. Prepare a blank solution: prepare a blank solution according to step S1, without adding the copper concentrate sample to the blank solution, and use the same amount of reagents, reaction time, and reaction temperature as in step S1;

[0027] S3. Pipette 0.00 mL, 0.50 mL, 1.00 mL, 5.00 mL, 10.0 mL, and 20.0 mL of manganese standard solution into a 100 mL volumetric flask, add 10 mL of nitric acid, dilute to the mark with water, and shake well to obtain manganese solutions with solubility of 0 μg / mL, 0.5 μg / mL, 1 μg / mL, 5 μg / mL, 10 μg / mL, and 20 μg / mL, respectively;

[0028] S4. Prepare a manganese standard curve: Place the manganese solutions obtained in step S3 into an inductively coupled plasma emission spectrometer, test according to the characteristic spectrum of manganese element, and prepare a standard curve; the abscissa of the standard curve is the concentration of manganese solution, and the ordinate is the emission peak intensity of manganese element;

[0029] S5. Place the test solution obtained in step S1 and the blank solution obtained in step S2 into an inductively coupled plasma optical emission spectrometer, respectively, and perform tests based on the characteristic spectrum of manganese to obtain the equivalent milligram amounts of manganese in the test solution and the blank solution;

[0030] S6. Calculate the percentage of manganese in the copper concentrate according to the following formula:

[0031]

[0032] Where ρ xis the mass concentration of manganese obtained from the standard curve based on the equivalent milligram amount of the test solution, in μg / mL; ρ0 is the mass concentration of manganese obtained from the standard curve based on the equivalent milligram amount of the blank solution, in μg / mL; V is the constant volume of the test solution, in mL; m is the mass of the copper concentrate sample weighed, in g; 10 -6 It is the conversion rate between μg / mL and g / L, mL and L; 100 is the percentage conversion rate.

[0033] In one embodiment of the present invention, in S1, the mass of the copper concentrate sample weighed is 0.2000±0.0001 g.

[0034] In one embodiment of the present invention, in S1, the particle size of the copper concentrate sample is less than 200 mesh.

[0035] In one embodiment of the present invention, in S1, the dilute nitric acid is V 水 :V 酸 =1:1 nitric acid solution.

[0036] In one embodiment of the present invention, in S4 and S5, the operating parameters of the inductively coupled plasma optical emission spectrometer are as follows: plasma emission power 1300 kW, cooling gas flow rate 12 L / min, auxiliary gas flow rate 0.8 L / min, atomizing gas flow rate 0.8 L / min, sample flow rate 2 L / min, pump speed 45 r / min, pre-flushing time 30 s, detection time 15 s, argon purity greater than 99.99%, argon pressure 0.6-0.8 MPa, and the wavelength of the characteristic spectrum line of manganese element is 294.92 nm.

[0037] Example 1: Accuracy Test

[0038] In this embodiment, a purchased copper concentrate standard sample with a standard value is used as a sample, and the manganese content in the copper concentrate is determined by the method of the present invention, comprising the following steps:

[0039] S1. Prepare the test solution: weigh a copper concentrate sample with a particle size less than 200 mesh and a mass of 0.2000±0.0001g into a tetrafluoroethylene beaker, add a small amount of water to wet the sample; add 10mL nitric acid and 5mL hydrochloric acid, and heat at 200-300℃ for 5-10min; then add 2mL perchloric acid and 5-10mL hydrofluoric acid, and

[0040] Heat the copper concentrate sample at 200-300°C until it is completely dissolved, and cool to room temperature; add 10 mL of dilute nitric acid and heat at 200-300°C for 5-10 minutes to dissolve the precipitated salt crystals, and cool to room temperature to obtain a pre-test solution; transfer the pre-test solution to a volumetric flask, add water to dilute to the scale, and shake well to obtain a test solution;

[0041] S2. Prepare a blank solution: prepare a blank solution according to step S1, without adding the copper concentrate sample to the blank solution, and use the same amount of reagents, reaction time, and reaction temperature as in step S1;

[0042] S3. Pipette 0.00 mL, 0.50 mL, 1.00 mL, 5.00 mL, 10.0 mL, and 20.0 mL of manganese standard solution into a 100 mL volumetric flask, add 10 mL of nitric acid, dilute to the mark with water, and shake well to obtain manganese solutions with solubility of 0 μg / mL, 0.5 μg / mL, 1 μg / mL, 5 μg / mL, 10 μg / mL, and 20 μg / mL, respectively;

[0043] S4. Prepare a manganese standard curve: Place the manganese solutions obtained in step S3 into an inductively coupled plasma emission spectrometer, test according to the characteristic spectrum of manganese element, and prepare a standard curve; the abscissa of the standard curve is the concentration of manganese solution, and the ordinate is the emission peak intensity of manganese element;

[0044] S5. Place the test solution obtained in step S1 and the blank solution obtained in step S2 into an inductively coupled plasma optical emission spectrometer, respectively, and perform tests based on the characteristic spectrum of manganese to obtain the equivalent milligram amounts of manganese in the test solution and the blank solution;

[0045] S6. Calculate the percentage of manganese in the copper concentrate according to the following formula:

[0046]

[0047] Where ρ x is the mass concentration of manganese obtained from the standard curve based on the equivalent milligram amount of the test solution, in μg / mL; ρ0 is the mass concentration of manganese obtained from the standard curve based on the equivalent milligram amount of the blank solution, in μg / mL; V is the constant volume of the test solution, in mL; m is the mass of the copper concentrate sample weighed, in g; 10 -6 It is the conversion rate between μg / mL and g / L, mL and L; 100 is the percentage conversion rate.

[0048] In this embodiment, the operating parameters of the inductively coupled plasma emission spectrometer are as follows: plasma emission power 1300 kW, cooling gas flow rate 12 L / min, auxiliary gas flow rate 0.8 L / min, atomizing gas flow rate 0.8 L / min, sample flow rate 2 L / min, pump speed 45 r / min, pre-flushing time 30 s, detection time 15 s, argon purity greater than 99.99%, argon pressure 0.6-0.8 MPa, and the wavelength of the characteristic spectral line of manganese element is 294.92 nm.

[0049] Table 1 Relative error and relative standard deviation of the determination results of this method and the standard value

[0050]

[0051] As shown in Table 1, the relative standard deviation of manganese tested by the present invention is less than 3.4%, and the precision is good, which meets the detection requirements of the sample.

[0052] Example 2: Spike recovery test

[0053] In this embodiment, a purchased copper concentrate standard sample with a standard value is used as a sample, and the manganese content in the copper concentrate is determined by the method of the present invention, comprising the following steps:

[0054] S1. Prepare the test solution: weigh a copper concentrate sample with a particle size of less than 200 mesh and a mass of 0.2000±0.0001g into a tetrafluoroethylene beaker, and add a small amount of water to soak the sample; pipette different volumes of manganese standard solution, add 10mL of nitric acid and 5mL of hydrochloric acid, and heat at 200-300°C for 5-10min; then add 2mL of perchloric acid and 5-10mL of hydrofluoric acid, heat at 200-300°C until the copper concentrate sample is completely dissolved, and cool to room temperature; add 10mL of dilute nitric acid and heat at 200-300°C for 5-10min to dissolve the precipitated salt crystals, and cool to room temperature to obtain a pre-test solution; transfer the pre-test solution to a volumetric flask, dilute to the scale with water, and shake well to obtain the test solution;

[0055] S2. Prepare a blank solution: prepare a blank solution according to step S1, without adding the copper concentrate sample to the blank solution, and use the same amount of reagents, reaction time, and reaction temperature as in step S1;

[0056] S3. Pipette 0.00 mL, 0.50 mL, 1.00 mL, 5.00 mL, 10.0 mL, and 20.0 mL of manganese standard solution into a 100 mL volumetric flask, add 10 mL of nitric acid, dilute to the mark with water, and shake well to obtain manganese solutions with solubility of 0 μg / mL, 0.5 μg / mL, 1 μg / mL, 5 μg / mL, 10 μg / mL, and 20 μg / mL, respectively;

[0057] S4. Prepare a manganese standard curve: Place the manganese solutions obtained in step S3 into an inductively coupled plasma emission spectrometer, test according to the characteristic spectrum of manganese element, and prepare a standard curve; the abscissa of the standard curve is the concentration of manganese solution, and the ordinate is the emission peak intensity of manganese element;

[0058] S5. Place the test solution obtained in step S1 and the blank solution obtained in step S2 into an inductively coupled plasma optical emission spectrometer, respectively, and perform tests based on the characteristic spectrum of manganese to obtain the equivalent milligram amounts of manganese in the test solution and the blank solution;

[0059] S6. Calculate the percentage of manganese in the copper concentrate according to the following formula:

[0060]

[0061] Where ρ x is the mass concentration of manganese obtained from the standard curve based on the equivalent milligram amount of the test solution, in μg / mL; ρ0 is the mass concentration of manganese obtained from the standard curve based on the equivalent milligram amount of the blank solution, in μg / mL; V is the constant volume of the test solution, in mL; m is the mass of the copper concentrate sample weighed, in g; 10 -6 It is the conversion rate between μg / mL and g / L, mL and L; 100 is the percentage conversion rate.

[0062] In this embodiment, the operating parameters of the inductively coupled plasma emission spectrometer are as follows: plasma emission power 1300 kW, cooling gas flow rate 12 L / min, auxiliary gas flow rate 0.8 L / min, atomizing gas flow rate 0.8 L / min, sample flow rate 2 L / min, pump speed 45 r / min, pre-flushing time 30 s, detection time 15 s, argon purity greater than 99.99%, argon pressure 0.6-0.8 MPa, and the wavelength of the characteristic spectral line of manganese element is 294.92 nm.

[0063] Table 2 Spike recovery test results

[0064]

[0065] As shown in Table 2, the recovery rate of the present invention is 99.07%-104.17%, which meets the requirements of the analysis test.

[0066] Example 3: Detection limit test

[0067] In this embodiment, a blank solution is used as a sample, and the manganese content in the blank solution is determined by the method of the present invention, comprising the following steps:

[0068] S1. Prepare the test solution: weigh a copper concentrate sample with a particle size of less than 200 mesh and a mass of 0.2000±0.0001g into a tetrafluoroethylene beaker, and add a small amount of water to soak the sample; pipette different volumes of manganese standard solution, add 10mL of nitric acid and 5mL of hydrochloric acid, and heat at 200-300°C for 5-10min; then add 2mL of perchloric acid and 5-10mL of hydrofluoric acid, heat at 200-300°C until the copper concentrate sample is completely dissolved, and cool to room temperature; add 10mL of the solution and heat at 200-300°C for 5-10min to dissolve the precipitated salt crystals, and cool to room temperature to obtain a pre-test solution; transfer the pre-test solution to a volumetric flask, dilute to the scale with water, and shake well to obtain the test solution;

[0069] S2. Prepare a blank solution: prepare a blank solution according to step S1, without adding the copper concentrate sample to the blank solution, and use the same amount of reagents, reaction time, and reaction temperature as in step S1;

[0070] S3. Pipette 0.00 mL, 0.50 mL, 1.00 mL, 5.00 mL, 10.0 mL, and 20.0 mL of manganese standard solution into a 100 mL volumetric flask, add 10 mL of nitric acid, dilute to the mark with water, and shake well to obtain manganese solutions with solubility of 0 μg / mL, 0.5 μg / mL, 1 μg / mL, 5 μg / mL, 10 μg / mL, and 20 μg / mL, respectively;

[0071] S4. Prepare a manganese standard curve: Place the manganese solutions obtained in step S3 into an inductively coupled plasma emission spectrometer, test according to the characteristic spectrum of manganese element, and prepare a standard curve; the abscissa of the standard curve is the concentration of manganese solution, and the ordinate is the emission peak intensity of manganese element;

[0072] S5. Place the blank solution obtained in step S2 into an inductively coupled plasma optical emission spectrometer and perform a test based on the characteristic spectrum of manganese element. The test is repeated 11 times to obtain the equivalent milligram amount of manganese element in the blank solution.

[0073] S6. Calculate the detection limit using the three-times standard deviation method based on the mass concentration of manganese obtained from the standard curve using the equivalent milligram amount measured in the blank solution.

[0074] In this embodiment, the operating parameters of the inductively coupled plasma emission spectrometer are as follows: plasma emission power 1300 kW, cooling gas flow rate 12 L / min, auxiliary gas flow rate 0.8 L / min, atomizing gas flow rate 0.8 L / min, sample flow rate 2 L / min, pump speed 45 r / min, pre-flushing time 30 s, detection time 15 s, argon purity greater than 99.99%, argon pressure 0.6-0.8 MPa, and the wavelength of the characteristic spectral line of manganese element is 294.92 nm.

[0075] Table 3 Detection limit determination results

[0076]

[0077] As can be seen from Table 3, the detection limit of the present invention is 0.00033%, which meets the requirements of the analysis test.

[0078] The present invention provides a method for determining the manganese content in copper concentrate. By optimizing the sample pretreatment process and adopting a mixed acid digestion system of nitric acid, hydrochloric acid, perchloric acid and hydrofluoric acid, the manganese element in the copper concentrate is completely dissolved, and the interference of a complex matrix on the manganese determination is effectively solved. The high sensitivity and multi-element analysis capability of an inductively coupled plasma emission spectrometer are combined to establish a linear standard curve between the characteristic spectrum line and the concentration of the manganese element, which significantly improves the accuracy and precision of the quantitative analysis. The blank solution correction is combined with the standard curve method to eliminate the interference of the reagent and the environmental background, and ensure the reliability of the manganese content determination result. The method has a standardized operating process and good repeatability, the detection limit can meet the determination requirements of trace manganese in copper concentrate, and the analysis efficiency is significantly improved. The method provides a low-cost, high-precision method for determining the manganese element for copper smelting enterprises, and is of great significance for optimizing smelting process parameters, improving metal recovery rate and ensuring the quality of end products.

[0079] Some exemplary embodiments of the present invention are described above. It will be understood that the above embodiments are only used to explain the present invention and do not constitute a limitation on the scope of protection of the present invention. The features in these embodiments can be recombined in an appropriate manner, and the solutions obtained thereby are still within the scope of protection claimed by the present invention. Based on the above embodiments, all other embodiments obtained by those skilled in the art without making creative work, that is, all modifications, equivalent substitutions and improvements made within the spirit and principles of this application, fall within the scope of protection claimed by the present invention.

Claims

1. A method for determining the manganese content in copper concentrate, characterized in that: The following steps are involved: S1. Prepare the test solution: weigh a copper concentrate sample with a mass of m into a tetrafluoroethylene beaker, add a small amount of water to wet the sample; add nitric acid and hydrochloric acid, and heat at 200-300°C for 5-10 minutes; then add perchloric acid and hydrofluoric acid, and heat at 200-300°C until the copper concentrate sample is completely dissolved, and cool to room temperature; add dilute nitric acid and heat at 200-300°C for 5-10 minutes to dissolve the precipitated salt crystals, and cool to room temperature to obtain a pre-test solution; transfer the pre-test solution to a volumetric flask, add water to dilute to the scale line, and shake well to obtain the test solution; S2. Prepare a blank solution: prepare a blank solution according to step S1, without adding the copper concentrate sample to the blank solution, and use the same amount of reagents, reaction time, and reaction temperature as in step S1; S3. Pipette 0.00 mL, 0.50 mL, 1.00 mL, 5.00 mL, 10.0 mL, and 20.0 mL of manganese standard solution into a 100 mL volumetric flask, add 10 mL of nitric acid, dilute to the mark with water, and shake well to obtain manganese solutions with solubility of 0 μg / mL, 0.5 μg / mL, 1 μg / mL, 5 μg / mL, 10 μg / mL, and 20 μg / mL, respectively; S4. Prepare a manganese standard curve: Place the manganese solutions obtained in step S3 into an inductively coupled plasma emission spectrometer, test according to the characteristic spectrum of manganese element, and prepare a standard curve; the abscissa of the standard curve is the concentration of manganese solution, and the ordinate is the emission peak intensity of manganese element; S5. Place the test solution obtained in step S1 and the blank solution obtained in step S2 into an inductively coupled plasma optical emission spectrometer, respectively, and perform tests based on the characteristic spectrum of manganese to obtain the equivalent milligram amounts of manganese in the test solution and the blank solution; S6. Calculate the percentage of manganese in the copper concentrate according to the following formula: Where ρ x is the mass concentration of manganese obtained from the standard curve based on the equivalent milligram amount of the test solution, in μg / mL; ρ0 is the mass concentration of manganese obtained from the standard curve based on the equivalent milligram amount of the blank solution, in μg / mL; V is the constant volume of the test solution, in mL; m is the mass of the copper concentrate sample weighed, in g; 10 -6 It is the conversion rate between μg / mL and g / L, mL and L; 100 is the percentage conversion rate.

2. The method for determining the manganese content in copper concentrate according to claim 1, wherein: In S1, the mass of the copper concentrate sample weighed is 0.2000±0.0001 g.

3. The method for determining the manganese content in copper concentrate according to claim 1, wherein: In S1, the particle size of the copper concentrate sample is less than 200 mesh.

4. The method for determining the manganese content in copper concentrate according to claim 1, wherein: In S1, dilute nitric acid is V 水 :V 酸 =1:1 nitric acid solution.

5. The method for determining the manganese content in copper concentrate according to claim 1, wherein: In S4 and S5, the operating parameters of the inductively coupled plasma emission spectrometer are as follows: plasma emission power 1300kW, cooling gas flow rate 12L / min, auxiliary gas flow rate 0.8L / min, nebulizing gas flow rate 0.8L / min, sample flow rate 2L / min, pump speed 45r / min, pre-flushing time 30s, detection time 15s, argon purity greater than 99.99%, argon pressure 0.6-0.8MPa, and the characteristic spectral line wavelength of manganese element is 294.92nm.

Citation Information

Cited By

  • Method for measuring contents of copper and manganese in Hopcalite

    CN121703074A