Method for measuring manganese content of manganese ore

Abstract

The invention discloses a method for determining the manganese content of manganese ore, which realizes the accurate determination of the manganese content through the steps of accurate weighing, melting, dissolving, constant volume and the like in combination with an inductively coupled plasma spectrometer. The method comprises the step of performing curve correction by using a verification standard sample to ensure the measurement accuracy. The method has the beneficial effects that instrument analysis is adopted to replace traditional chemical analysis, the detection precision and speed are improved, personal errors are reduced, real-time remote monitoring is realized, skill requirements are reduced, and meanwhile, environmental pollution and occupational disease risks are reduced. The method is suitable for detection of manganese ores with different manganese contents, has the characteristics of high efficiency, accuracy and safety, and provides a new solution for analysis and determination of manganese ores.

Description

Technical Field

[0001] The invention relates to the field of measurement, and in particular to a method for determining the manganese content of manganese ore. Background Art

[0002] In the field of analysis and determination of manganese content in manganese ore, the national standard method GB / T 1506-2016 "Determination of manganese content in manganese ore by potentiometric titration and ammonium ferrous sulfate titration" is widely used. In particular, the ammonium ferrous sulfate titration method includes two technical paths: ammonium nitrate oxidation method and perchloric acid oxidation method. However, the perchloric acid oxidation method has significant safety hazards in actual operation. When using high-concentration and large-dose perchloric acid for testing in a fume hood, it is easy to cause high-concentration residual perchloric acid to accumulate in the fume hood, which may cause combustion, explosion or violent exothermic chemical reaction, posing a serious threat to laboratory safety.

[0003] On the other hand, although the ammonium nitrate oxidation method is suitable for large-scale manganese content detection, it is affected by the strict control of chemical reagents. Due to its unstable nature, ammonium nitrate is potentially dangerous during use and storage, and has become a key regulated hazardous chemical in recent years. Therefore, the use of ammonium nitrate is restricted, which limits the scope of application of the ammonium nitrate oxidation method in manganese ore determination.

[0004] In view of the safety risks and usage restrictions in the above-mentioned background technologies, this research field urgently needs to develop a new detection method to replace the existing measurement technology with safety hazards and high control risks. Summary of the invention

[0005] In order to solve the above technical problems, the present invention provides a method for determining the manganese content of manganese ore, aiming to provide a safer and more efficient solution for the accurate determination of manganese ore. The development of this new method is expected to fill the security loopholes in the current manganese content detection technology and provide important support for scientific research and technological progress in related fields.

[0006] The present invention is achieved through the following technical solutions: A method for determining the manganese content of manganese ore comprises the following steps: Step 1, weigh a manganese ore sample into a crucible, add an alkaline reagent and mix with the sample, cover it, put it into a high-temperature furnace and heat it to 600°C-800°C for melting treatment; Step 2, placing the molten sample in a container filled with hot ultrapure water and heating it until it is completely dissolved, and cleaning the crucible and the cover in the container to obtain a solution; Step 3, add nitric acid to the above solution, continue heating until the volume is reduced to about 45-55mL, dilute to a 100mL volumetric flask, shake well, and obtain a sample solution to be tested; Step 4, selecting several manganese ore standard samples with different manganese contents, treating the standard samples with the same method, and obtaining a plurality of standard solutions with different manganese contents as verification standards; Step 5, start the inductively coupled plasma spectrometer, establish an analysis method in the workstation, select an appropriate wavelength, perform quantitative detection of manganese, and set the manganese content of the standard solution; Step 6, analyzing the standard solutions with different manganese contents in sequence, and establishing a standard curve by detecting the absorbance thereof, and ensuring that the correlation coefficient is greater than or equal to 0.9990; Step 7: The solution of the sample to be tested is tested by the instrument, and the manganese content in the solution of the sample to be tested is calculated according to the standard curve.

[0007] This method ensures the standardization and consistency of sample processing through precise weighing, melting, dissolving and volume determination. Melting treatment converts the manganese element in manganese ore into soluble compounds, which is convenient for subsequent quantitative analysis. By utilizing the high sensitivity and accuracy of inductively coupled plasma spectrometer and establishing a standard curve, the accurate determination of manganese content is achieved. This method is applicable to manganese ores with different manganese contents and has broad application prospects.

[0008] Furthermore, the method uses verification standards to perform curve calibration regularly to ensure the accuracy of the measurement results. Regularly using verification standards to perform curve calibration can effectively monitor and correct system errors and ensure the long-term stability and reliability of the measurement results. This step is an important part of quality control, ensuring the consistency and accuracy of the measurement results under different times and conditions.

[0009] Furthermore, the step 1 comprises the following steps: Weigh the sample: Use an analytical balance to accurately weigh 0.100g of manganese ore sample, ensuring that the weighing error is within the specified range; Adding alkaline reagent: adding 2.00 g of sodium hydroxide as an alkaline reagent; the addition of sodium hydroxide is to promote the dissolution and reaction of manganese ore; Mix and cover: Make sure the sodium hydroxide is completely mixed with the manganese ore sample to form a uniform mixture; then add it to the nickel crucible with a lid to avoid splashing or vapor escaping during heating; Place in a high-temperature furnace for heating: Place the nickel crucible containing the sample and sodium hydroxide in a muffle furnace for heating; Set the furnace temperature to 600°C-800°C and ensure that the temperature is stable; The heating process lasts for 10 minutes to ensure that the sample is fully melted; When heating, avoid excessively high temperatures to prevent excessive reaction of the sample or loss of volatiles during the melting process; Take out and cool slightly: After the melting process is completed, take out the nickel crucible and let it cool naturally to between 100℃ and 200℃ to avoid the container from breaking due to sudden temperature changes.

[0010] Accurately weighing and controlling the heating temperature and time are the key to ensuring that the sample is fully melted without over-reaction. Sodium hydroxide, as a flux, not only promotes the dissolution of manganese ore, but also avoids the loss of samples by volatilization at high temperatures. Control of the cooling process avoids the cracking of the crucible, ensuring the safety of the experiment and the integrity of the sample.

[0011] Further, the step 5 comprises the following steps: Turn on the instrument and preheat: Start the inductively coupled plasma spectrometer and preheat it according to the instrument's operating manual to ensure that the instrument reaches a stable working state; when starting the instrument, first turn on the voltage-stabilized power supply and water cooling system to ensure that the system is in a normal state; Start the workstation: turn on the computer connected to the spectrometer and start the control software; connect the instrument to the workstation and ensure that the connection between the instrument and the computer system is normal; New analysis method: Create a new analysis method in the workstation, select an appropriate preset template or create a new analysis method; Select wavelength setting: According to the emission spectrum of manganese, select the wavelength as 257.610 nm; Configure analysis parameters: Select instrument settings suitable for manganese analysis; Set the manganese content of the standard solution: Enter the manganese concentration corresponding to the standard solution into the software, set according to the actual concentration of the standard solution; make sure it is entered correctly and set up the analysis.

[0012] Instrument preheating and parameter setting are the prerequisites for ensuring measurement accuracy. The characteristic wavelength of 257.610 nm was selected for detection, which utilized the strong emission characteristics of manganese at this wavelength to improve the sensitivity and selectivity of detection. Correct instrument configuration and standard solution setting provide a reliable basis for subsequent standard curve establishment and sample analysis.

[0013] Further, the step 6 comprises the following steps: Prepare standard solutions: select manganese ores with manganese contents of 15.74%, 22.54%, and 36.99% as standard samples, prepare standard solutions respectively, and mix them thoroughly; ensure that the volume of the standard solutions is accurate and the concentrations have been calibrated; Injection and peak search: Use an injection tube to sequentially inject standard solutions with manganese contents of 15.74%, 22.54%, and 36.99% into the injection system of the spectrometer; The instrument automatically detects and identifies the absorbance of each standard solution; at this time, the sensitivity and stability of the instrument should be confirmed; Establish a standard curve: Draw a standard curve in the workstation based on the known concentration of the standard solution and the signal intensity measured by the spectrometer, the signal intensity includes absorbance or emission intensity; The workstation will automatically generate a graph of the relationship between concentration and absorbance or emission intensity, ensuring that the correlation coefficient R value of the standard curve is greater than or equal to 0.9990, indicating that the standard curve has a good fit; Check the curve quality: In the curve fitting interface of the workstation, check the linearity and correlation coefficient of the standard curve; if the correlation coefficient is lower than 0.9990, readjust the instrument settings or replace the standard solution; Once the curve is established and meets the quality criteria, save and confirm.

[0014] The preparation and mixing of the standard solution ensures the accuracy of the standard curve. Through sample injection and peak search, the instrument automatically detects the absorbance of the standard solution and establishes the relationship between concentration and signal intensity. The correlation coefficient of the standard curve is greater than or equal to 0.9990, indicating a high degree of fit of the curve, ensuring the accuracy of sample measurement. The inspection and confirmation of the curve quality ensures the reliability of the analysis results.

[0015] Further, the step 7 comprises the following steps: Prepare the sample solution to be tested: Take out the dissolved and treated sample solution to be tested; ensure that the solution to be tested is fully mixed to avoid affecting the analysis results; Inject and measure: The sample solution to be tested is sent into the injection system of the spectrometer through the injection tube, and the samples are tested in turn; the instrument will automatically detect the signal intensity of manganese according to the characteristic wavelength 257.610nm emitted by the manganese element in the sample; Compare with the standard curve: The spectrometer will automatically convert the signal intensity of the sample to be tested into the corresponding manganese concentration according to the established standard curve; the instrument will calculate the manganese content in the sample and output the result in mg / L or ppm Result calibration and verification: Check the results of the samples to be tested; if necessary, use a verified standard solution, such as a 22.54% manganese standard solution, to calibrate the curve offset to ensure the accuracy of the results; if the standard curve is offset or there is a measurement error, make corrections in a timely manner; Recording and reporting: The instrument will output the concentration of manganese and record the analysis results; if necessary, the results will be compiled into a report with experimental conditions, standard curve, and concentration information of the samples to be tested.

[0016] The full mixing and injection measurement of the sample solution to be tested ensures the representativeness of the sample and the accuracy of the measurement results. The instrument automatically converts the signal intensity into manganese concentration according to the standard curve, realizing fast and accurate quantitative analysis. The result correction and verification links further ensure the accuracy of the measurement results. The arrangement of records and reports facilitates the preservation and transmission of experimental data. The whole process embodies scientific and rigorous experimental design and technical operation.

[0017] The beneficial effects of the present invention are: Technical breakthrough and innovation: This method uses instrumental analysis to replace traditional chemical analysis, realizing the technical transformation from chemical analysis to instrumental analysis. This innovation not only represents a technological breakthrough, but also brings revolutionary progress to the field of manganese content detection.

[0018] Improve detection precision and accuracy: Compared with traditional chemical analysis methods, this method significantly improves the detection precision and accuracy. The instrumental analysis is more accurate, reduces measurement errors, and ensures the reliability of the test results.

[0019] Speed ​​up the detection: This method is fast to operate and can obtain a large amount of data in a short time, which greatly improves the detection efficiency and is suitable for rapid analysis of large-scale samples.

[0020] Reduce human errors: Through automated and standardized operating procedures, this method minimizes human operating errors and ensures the stability of experimental results.

[0021] Realize real-time remote monitoring: This method supports real-time monitoring of remote data, making it easier for operators to monitor and manage the experimental process at different locations, thus improving the flexibility and convenience of the experiment.

[0022] Reduced skill requirements: This method has a high degree of automation, which reduces the impact of operator skills and experience on the experimental results, so that even operators without advanced skills can obtain reliable test results.

[0023] Simultaneous detection of multiple parameters: This method has the ability to detect multiple parameters simultaneously, which enhances the analytical capability and makes it possible to conduct comprehensive analysis of complex samples.

[0024] Convenient data recording and storage: The data recording and storage of instrument analysis are more convenient, which is convenient for subsequent data analysis and traceability.

[0025] Reduce environmental pollution and chemical risks: This method reduces the use of chemical reagents, thereby reducing the risk of environmental pollution and operator exposure to chemicals and improving laboratory safety.

[0026] Reduce the risk of occupational diseases: Since direct contact with chemical reagents is reduced, this method greatly reduces the possibility of laboratory workers suffering from occupational diseases, reflecting a high level of concern for the health of laboratory personnel.

[0027] In summary, the method provided by the present invention has significant advantages in improving detection efficiency, accuracy and safety, and provides an efficient, accurate and safe solution for the analysis and determination of manganese content in manganese ore. DETAILED DESCRIPTION

[0028] The present invention will be further described below in conjunction with specific embodiments: Embodiment: A method for determining the manganese content of manganese ore comprises the following steps: Step 1, weigh a manganese ore sample into a crucible, add an alkaline reagent and mix with the sample, cover it, put it into a high-temperature furnace and heat it to 600°C-800°C for melting treatment; Step 2, placing the molten sample in a container filled with hot ultrapure water and heating it until it is completely dissolved, and cleaning the crucible and the cover in the container to obtain a solution; Step 3, add nitric acid to the above solution, continue heating until the volume is reduced to about 45-55mL, dilute to a 100mL volumetric flask, shake well, and obtain a sample solution to be tested; Step 4, selecting several manganese ore standard samples with different manganese contents, treating the standard samples with the same method, and obtaining a plurality of standard solutions with different manganese contents as verification standards; Step 5, start the inductively coupled plasma spectrometer, establish an analysis method in the workstation, select an appropriate wavelength, perform quantitative detection of manganese, and set the manganese content of the standard solution; Step 6, analyzing the standard solutions with different manganese contents in sequence, and establishing a standard curve by detecting the absorbance thereof, and ensuring that the correlation coefficient is greater than or equal to 0.9990; Step 7: The solution of the sample to be tested is tested by the instrument, and the manganese content in the solution of the sample to be tested is calculated according to the standard curve.

[0029] The method for determining manganese content combines chemical treatment with spectral analysis technology to provide an accurate and reliable method for analyzing the composition of manganese ore. In the melting process, high temperature helps to destroy the crystal structure of the ore and release manganese in the form of ions, while alkaline reagents such as sodium hydroxide promote this process and prevent the volatilization loss of manganese. The dissolution of the molten sample in hot ultrapure water ensures the complete extraction of manganese, and the subsequent nitric acid treatment not only helps to stabilize the solution, but also prepares the conditions for constant volume through precise volume control. The treatment of the standard sample is consistent with the sample to be tested, ensuring the consistency of the analysis process and the comparability of the results. The use of inductively coupled plasma spectrometer utilizes the high temperature excitation characteristics of plasma to make manganese emit light of a specific wavelength. By detecting this characteristic wavelength, the accurate determination of manganese content is achieved. The effectiveness of this method is guaranteed by the establishment of a standard curve and regular calibration. It is suitable for ores with different manganese contents from low grade to high grade, providing important technical support for the evaluation and utilization of manganese ore resources.

[0030] Furthermore, the method regularly uses verification standards to calibrate the curve to ensure the accuracy of the measurement results. Regularly using verification standards to calibrate the curve is a key step in ensuring the accuracy of the analysis results. This process involves analyzing a standard solution with a known manganese content and a sample to be tested under the same conditions, and identifying and correcting possible systematic errors by comparing the difference between the actual measured value and the standard value. The deviation of the calibration curve may be caused by factors such as instrument drift, environmental changes, or differences in reagent batches. The long-term stability of the measurement results and the consistency between different batches can be ensured through calibration. In addition, the calibration process is also a regular check of instrument performance, which helps to promptly discover and solve potential problems and ensure the continuity and reliability of the analysis work.

[0031] Furthermore, the step 1 comprises the following steps: Weigh the sample: Use an analytical balance to accurately weigh 0.100g of manganese ore sample, ensuring that the weighing error is within the specified range; Adding alkaline reagent: adding 2.00 g of sodium hydroxide as an alkaline reagent; the addition of sodium hydroxide is to promote the dissolution and reaction of manganese ore; Mix and cover: Make sure the sodium hydroxide is completely mixed with the manganese ore sample to form a uniform mixture; then add it to the nickel crucible with a lid to avoid splashing or vapor escaping during heating; Place in a high-temperature furnace for heating: Place the nickel crucible containing the sample and sodium hydroxide in a muffle furnace for heating; Set the furnace temperature to 600°C-800°C and ensure that the temperature is stable; The heating process lasts for 10 minutes to ensure that the sample is fully melted; When heating, avoid excessively high temperatures to prevent excessive reaction of the sample or loss of volatiles during the melting process; Take out and cool slightly: After the melting process is completed, take out the nickel crucible and let it cool naturally to between 100℃ and 200℃ to avoid the container from breaking due to sudden temperature changes.

[0032] In the melting process of samples, accurate weighing and control of heating temperature and time are the key to ensure the reproducibility of experimental results. The selection and pretreatment of crucibles, the purity and addition amount of alkaline reagents, and the constant temperature performance of high-temperature furnaces will affect the melting effect. As a flux, sodium hydroxide not only promotes the melting of ore, but also reacts with impurities in the ore to form soluble salts, thereby reducing the interference of impurities in the determination of manganese content. The control of the cooling process is not only for safety, but also to prevent the melt from forming difficult-to-dissolve particles during rapid cooling, affecting the subsequent dissolution steps. The entire melting process needs to be carried out in an oxygen-free or low-oxygen environment to prevent the oxidation of manganese and ensure the complete extraction of manganese.

[0033] Further, the step 5 comprises the following steps: Turn on the instrument and preheat: Start the inductively coupled plasma spectrometer and preheat it according to the instrument's operating manual to ensure that the instrument reaches a stable working state; when starting the instrument, first turn on the voltage-stabilized power supply and water cooling system to ensure that the system is in a normal state; Start the workstation: turn on the computer connected to the spectrometer and start the control software; connect the instrument to the workstation and ensure that the connection between the instrument and the computer system is normal; New analysis method: Create a new analysis method in the workstation, select an appropriate preset template or create a new analysis method; Select wavelength setting: According to the emission spectrum of manganese, select the wavelength as 257.610 nm; Configure analysis parameters: Select instrument settings suitable for manganese analysis; Set the manganese content of the standard solution: Enter the manganese concentration corresponding to the standard solution into the software, set according to the actual concentration of the standard solution; make sure it is entered correctly and set up the analysis.

[0034] The preheating and parameter setting of the instrument are the prerequisites for ensuring the accuracy of the measurement, which involves the wavelength calibration of the spectrometer, the inspection of the light source stability, and the adjustment of the detector sensitivity. The characteristic wavelength of 257.610 nm is selected for detection, based on the fact that manganese has the highest emission intensity and the smallest interference at this wavelength, which helps to improve the sensitivity and selectivity of the detection. The correct instrument configuration includes the optimization of parameters such as gas flow, power, and observation height to ensure the stability and excitation efficiency of the plasma. The setting of the standard solution includes the determination of the concentration range, the preparation and storage of the solution, and the calibration of the injection system, which provides a reliable basis for the subsequent establishment of the standard curve and sample analysis.

[0035] Further, the step 6 comprises the following steps: Prepare standard solutions: select manganese ores with manganese contents of 15.74%, 22.54%, and 36.99% as standard samples, prepare standard solutions respectively, and mix them thoroughly; ensure that the volume of the standard solutions is accurate and the concentrations have been calibrated; Injection and peak search: Use an injection tube to sequentially inject standard solutions with manganese contents of 15.74%, 22.54%, and 36.99% into the injection system of the spectrometer; The instrument automatically detects and identifies the absorbance of each standard solution; at this time, the sensitivity and stability of the instrument should be confirmed; Establish a standard curve: Draw a standard curve in the workstation based on the known concentration of the standard solution and the signal intensity measured by the spectrometer, the signal intensity includes absorbance or emission intensity; The workstation will automatically generate a graph of the relationship between concentration and absorbance or emission intensity, ensuring that the correlation coefficient R value of the standard curve is greater than or equal to 0.9990, indicating that the standard curve has a good fit; Check the curve quality: In the curve fitting interface of the workstation, check the linearity and correlation coefficient of the standard curve; if the correlation coefficient is lower than 0.9990, readjust the instrument settings or replace the standard solution; Once the curve is established and meets the quality criteria, save and confirm.

[0036] The preparation and mixing of standard solutions are the basis for establishing an accurate standard curve. The concentration gradient of the standard solution should cover the expected concentration range of the sample to be tested to ensure the linear relationship of the curve. The mixing process needs to ensure the uniformity of the solution to avoid the uneven concentration gradient affecting the accuracy of the curve. Through sampling and peak searching, the instrument automatically detects the absorbance of the standard solution and establishes a calibration curve of concentration and signal intensity. The correlation coefficient of the standard curve is greater than or equal to 0.9990, indicating a high degree of fit of the data and reflecting the accuracy and repeatability of the measurement results. The inspection of the curve quality includes residual analysis, outlier identification, and curve smoothness assessment to ensure the reliability of the analysis results. The confirmation of the curve involves comparison with historical data and inter-laboratory comparison to verify the accuracy and applicability of the method.

[0037] Further, the step 7 comprises the following steps: Prepare the sample solution to be tested: Take out the dissolved and treated sample solution to be tested; ensure that the solution to be tested is fully mixed to avoid affecting the analysis results; Inject and measure: The sample solution to be tested is sent into the injection system of the spectrometer through the injection tube, and the samples are tested in turn; the instrument will automatically detect the signal intensity of manganese according to the characteristic wavelength 257.610nm emitted by the manganese element in the sample; Compare with the standard curve: The spectrometer will automatically convert the signal intensity of the sample to be tested into the corresponding manganese concentration according to the established standard curve; the instrument will calculate the manganese content in the sample and output the result in mg / L or ppm Result calibration and verification: Check the results of the samples to be tested; if necessary, use a verified standard solution, such as a 22.54% manganese standard solution, to calibrate the curve offset to ensure the accuracy of the results; if the standard curve is offset or there is a measurement error, make corrections in a timely manner; Recording and reporting: The instrument will output the concentration of manganese and record the analysis results; if necessary, the results will be compiled into a report with experimental conditions, standard curve, and concentration information of the samples to be tested.

[0038] The full mixing and injection measurement of the sample solution to be tested ensures the representativeness of the sample and the accuracy of the measurement results. The mixing process needs to avoid volatilization and contamination of the solution to ensure the uniformity of each injection. Cleaning and calibration of the injection system are important links to ensure measurement accuracy, avoiding cross-contamination and injection errors. The instrument automatically converts signal intensity into manganese concentration according to the standard curve, realizing fast and accurate quantitative analysis. The result correction and verification links, including the review of abnormal values, comparison of repeated measurements and backtesting of standard solutions, further ensure the accuracy of the measurement results. The arrangement of records and reports, including the recording of experimental data, the summary of analysis results, standard curves, and detailed descriptions of experimental conditions and analysis methods, facilitates the preservation, transmission and reproduction of experimental data. The entire process embodies scientific and rigorous experimental design and technical operations, and meets the requirements of the laboratory quality management system.

[0039] In summary, this method uses alkaline reagents as oxidants, and dissolves manganese ore into liquid samples under high temperature conditions by alkali fusion. Subsequently, an inductively coupled plasma emission spectrometer (ICP) is used to establish a standard curve for manganese content, and a comparative test is conducted with the standard sample. By repeatedly comparing and verifying with the national standard method (including ammonium ferrous sulfate titration method, ammonium nitrate oxidation method and perchloric acid oxidation method), the difference between the comparison test results and the accurate content of the known standard sample is analyzed to ensure that it is within the allowable deviation range. Therefore, this method can replace the traditional determination method of adding a strong oxidant (such as ammonium nitrate, perchloric acid) to an acidic medium to oxidize the manganese in the manganese ore to trivalent manganese after mixed acid dissolution.

[0040] The working example is as follows: Accurately weigh 0.1000g of manganese ore sample in a 30mL nickel crucible, add 2.00g of sodium hydroxide, mix thoroughly and cover. Place the crucible in a 700℃ muffle furnace to melt for 10 minutes, take it out and cool it slightly. Subsequently, place the nickel crucible in a 300mL beaker containing about 100ml of hot ultrapure water, and heat it on a hot plate until the frit is completely dissolved. Clean the crucible and lid, add 10mL of nitric acid to the beaker, continue heating until the solution volume is about 50mL, then dilute it to a 100mL volumetric flask and shake it well. Accurately transfer 5mL of the sample to another 100mL volumetric flask (pre-filled with a certain volume of ultrapure water), add 5mL of hydrochloric acid, dilute to volume, shake well, and wait for testing. The same method is used to treat standard manganese ore samples with manganese contents of 15.74%, 22.54%, and 36.99%, respectively, and dilute them into samples to be tested. Each time a sample is dissolved, standard manganese ore samples with different manganese contents can be carried as verification standards.

[0041] Analytical determination: (1) Start the voltage-stabilized power supply, circulating water cooling tank, ICP power supply and computer in sequence, and connect to the workstation after ignition is successful.

[0042] (2) Create a new analysis method: First, perform the zero search operation. After finding the zero aurora, create a new analysis method. Add the manganese element detection line (wavelength Mn: 257.610nm), and then add standard quantity points in sequence. Take three standard quantity points as an example, marked as STD1, STD2, and STD3, and the corresponding contents are 15.74%, 22.54%, and 36.99% respectively. Set the number of tests, the number of significant digits, and the digital unit, and then save the method.

[0043] (3) Analyze samples: Place the injection capillary into STD3, find the center of the peak, then perform attenuation operation, find the peak again, and ensure that the highest point of the peak overlaps with the theoretical value. Analyze the standard samples from low to high, check the correlation coefficient R value in the curve fitting interface, and ensure that it is greater than or equal to 0.9990. After saving the standard curve, test the sample to be tested, and at the same time test the 22.54% verification standard to correct the curve offset and ensure the accuracy of the test results.

[0044] After the establishment and verification of the standard curve, move the injection capillary to the sample solution to be tested and determine the manganese content according to the preset method. The instrument automatically records the signal intensity of each sample and calculates the corresponding manganese content based on the standard curve. To ensure the accuracy and reliability of the data, each sample is measured multiple times and the average value is taken as the final result.

[0045] During the measurement process, the operating status of the instrument needs to be closely monitored. If abnormal fluctuations or unstable signals are found, the problem should be promptly investigated and solved. At the same time, verification standards should be used regularly for intermediate checks to verify the stability of the standard curve and the accuracy of the test results.

[0046] After the determination is completed, the obtained data is imported into professional analysis software for processing to generate a detailed analysis report. The report should include sample number, determination date, instrument parameters, standard curve, determination results and uncertainty assessment, etc. Finally, the experimental data is archived for subsequent query and verification.

[0047] Through the above rigorous analysis and determination process, the scientificity, accuracy and operability of the manganese content determination method of manganese ore are ensured, providing reliable technical support for the grade assessment and resource utilization of manganese ore.

[0048] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for determining the manganese content of manganese ore, characterized in that: The following steps are involved: Step 1, weigh a manganese ore sample into a crucible, add an alkaline reagent and mix with the sample, cover it, put it into a high-temperature furnace and heat it to 600°C-800°C for melting treatment; Step 2, placing the molten sample in a container filled with hot ultrapure water and heating it until it is completely dissolved, and cleaning the crucible and the cover in the container to obtain a solution; Step 3, add nitric acid to the above solution, continue heating until the volume is reduced to about 45-55mL, dilute to a 100mL volumetric flask, shake well, and obtain a sample solution to be tested; Step 4, selecting several manganese ore standard samples with different manganese contents, treating the standard samples with the same method, and obtaining a plurality of standard solutions with different manganese contents as verification standards; Step 5, start the inductively coupled plasma spectrometer, establish an analysis method in the workstation, select an appropriate wavelength, perform quantitative detection of manganese, and set the manganese content of the standard solution; Step 6, analyzing the standard solutions with different manganese contents in sequence, and establishing a standard curve by detecting the absorbance thereof, and ensuring that the correlation coefficient is greater than or equal to 0.9990; Step 7: The solution of the sample to be tested is tested by the instrument, and the manganese content in the solution of the sample to be tested is calculated according to the standard curve.

2. A method for determining the manganese content of a manganese ore as claimed in claim 1, characterized in that: The method was regularly calibrated using verification standards to ensure the accuracy of the measurement results.

3. A method for determining the manganese content of a manganese ore as claimed in claim 1, characterized in that: The step 1 comprises the following steps: Weigh the sample: Use an analytical balance to accurately weigh 0.100g of manganese ore sample, ensuring that the weighing error is within the specified range; Adding alkaline reagent: adding 2.00 g of sodium hydroxide as an alkaline reagent; the addition of sodium hydroxide is to promote the dissolution and reaction of manganese ore; Mix and cover: Make sure the sodium hydroxide is completely mixed with the manganese ore sample to form a uniform mixture; then add it to the nickel crucible with a lid to avoid splashing or vapor escaping during heating; Place in a high-temperature furnace for heating: Place the nickel crucible containing the sample and sodium hydroxide in a muffle furnace for heating; Set the furnace temperature to 600°C-800°C and ensure that the temperature is stable; The heating process lasts for 10 minutes to ensure that the sample is fully melted; When heating, avoid excessively high temperatures to prevent excessive reaction of the sample or loss of volatiles during the melting process; Take out and cool slightly: After the melting process is completed, take out the nickel crucible and let it cool naturally to between 100℃ and 200℃ to avoid the container from breaking due to sudden temperature changes.

4. A method for determining the manganese content of a manganese ore as claimed in claim 1 or 2, characterized in that: The step 5 comprises the following steps: Turn on the instrument and preheat: Start the inductively coupled plasma spectrometer and preheat it according to the instrument's operating manual to ensure that the instrument reaches a stable working state; when starting the instrument, first turn on the voltage-stabilized power supply and water cooling system to ensure that the system is in a normal state; Start the workstation: turn on the computer connected to the spectrometer and start the control software; connect the instrument to the workstation and ensure that the connection between the instrument and the computer system is normal; New analysis method: Create a new analysis method in the workstation, select an appropriate preset template or create a new analysis method; Select wavelength setting: According to the emission spectrum of manganese, select the wavelength as 257.610 nm; Configure analysis parameters: Select instrument settings suitable for manganese analysis; Set the manganese content of the standard solution: Enter the manganese concentration corresponding to the standard solution into the software, set according to the actual concentration of the standard solution; make sure it is entered correctly and set up the analysis.

5. A method for determining the manganese content of a manganese ore as claimed in claim 1 or 2, characterized in that: The step 6 comprises the following steps: Prepare standard solutions: select manganese ores with manganese contents of 15.74%, 22.54%, and 36.99% as standard samples, prepare standard solutions respectively, and mix them thoroughly; ensure that the volume of the standard solutions is accurate and the concentrations have been calibrated; Injection and peak search: Use an injection tube to inject standard solutions with manganese contents of 15.74%, 22.54%, and 36.99% into the injection system of the spectrometer in sequence; The instrument automatically detects and identifies the absorbance of each standard solution; at this time, the sensitivity and stability of the instrument should be confirmed; Establish a standard curve: Draw a standard curve in the workstation based on the known concentration of the standard solution and the signal intensity measured by the spectrometer, the signal intensity includes absorbance or emission intensity; The workstation will automatically generate a graph of the relationship between concentration and absorbance or emission intensity, ensuring that the correlation coefficient R value of the standard curve is greater than or equal to 0.9990, indicating that the standard curve has a good fit; Check the curve quality: In the curve fitting interface of the workstation, check the linearity and correlation coefficient of the standard curve; if the correlation coefficient is lower than 0.9990, readjust the instrument settings or replace the standard solution; Once the curve is established and meets the quality criteria, save and confirm.

6. A method for determining the manganese content of a manganese ore as claimed in claim 1 or 2, characterized in that: The step 7 comprises the following steps: Prepare the sample solution to be tested: Take out the dissolved and treated sample solution to be tested; ensure that the solution to be tested is fully mixed to avoid affecting the analysis results; Inject and measure: The sample solution to be tested is sent into the injection system of the spectrometer through the injection tube, and the samples are tested in turn; the instrument will automatically detect the signal intensity of manganese according to the characteristic wavelength 257.610nm emitted by the manganese element in the sample; Compare with the standard curve: The spectrometer will automatically convert the signal intensity of the sample to be tested into the corresponding manganese concentration according to the established standard curve; the instrument will calculate the manganese content in the sample and output the result in mg / L or ppm Result calibration and verification: Check the results of the samples to be tested; if necessary, use a verified standard solution, such as a 22.54% manganese standard solution, to calibrate the curve offset to ensure the accuracy of the results; if the standard curve is offset or has a measurement error, calibrate it in time; Recording and reporting: The instrument will output the concentration of manganese and record the analysis results; if necessary, the results will be compiled into a report with experimental conditions, standard curve, and concentration information of the samples to be tested.