ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) method for synchronously measuring contents of multiple components of primary quantity, secondary quantity, nickel, silicon, chromium, phosphorus, copper, lead and arsenic in
By dissolving nickel-iron alloy samples in batches using the ICP-AES method and measuring the emission line intensity using an ICP spectrometer, the difficult problem of simultaneous determination of multiple components in nickel-iron alloys was solved, rapid and accurate elemental analysis was achieved, and the gap in the determination of large-span elements was filled.
Patent Information
- Application Number
- CN202510722141.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-30
- Publication Date
- 2025-09-19
AI Technical Summary
Existing technologies make it difficult to simultaneously determine the content of elements with a large content span in nickel, silicon, chromium, phosphorus, copper, lead and arsenic in nickel-iron alloys. Traditional methods also have problems such as severe interference, complex separation process and long analysis cycle.
The ICP-AES method was used to dissolve the nickel-iron alloy sample in batches using concentrated nitric acid, concentrated hydrochloric acid and perchloric acid to prepare different solutions. The emission line intensity was measured using an ICP spectrometer, and a working curve was established to achieve simultaneous multi-component determination.
The rapid and accurate determination of major and minor elements in nickel-iron alloys is achieved, which shortens the analysis time, reduces the detection cost, and improves the detection efficiency and accuracy.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of chemical analysis, and particularly relates to an ICP-AES method for simultaneously determining the contents of major and minor components of nickel, silicon, chromium, phosphorus, copper, lead and arsenic in a nickel-iron alloy. Technical Background Ferronickel is a nickel-iron alloy with a nickel content of 20%-60%. Ferronickel is primarily composed of nickel and iron, but also contains impurities such as carbon, silicon, sulfur, phosphorus, chromium, copper, lead, and arsenic. It is primarily used as a nickel additive in steelmaking and cast iron. Ferronickel's primary application is as a nickel substitute in stainless steel furnaces. Generally, 200 series stainless steel can be made with low-grade ferronickel, while 300 series stainless steel requires ferronickel with a nickel content of 8% or higher. Ferronickel quality depends not only on its nickel content (commonly known as grade), but also on the presence of harmful impurities. Therefore, compositional analysis is a key indicator of product quality.
[0002] Traditional chemical analysis methods suffer from severe interference between elements, complex separation processes, long analysis cycles, and cumbersome and difficult-to-master procedures. Furthermore, existing techniques can only simultaneously measure the contents of low-level minor elements and lack the ability to simultaneously measure the relatively wide range of nickel, chromium, phosphorus, copper, lead, and arsenic components. Summary of the Invention
[0003] This invention addresses the shortcomings of current analytical methods and provides an ICP-AES method for the simultaneous determination of the major and minor components of nickel, silicon, chromium, phosphorus, copper, lead, and arsenic in nickel-iron alloys. By preparing different dissolving solutions for different components to be measured, the method enables simultaneous determination of multiple components with a wide range of content, shortening analysis and testing time.
[0004] An ICP-AES method for simultaneously determining the contents of major and minor components of nickel, silicon, chromium, phosphorus, copper, lead and arsenic in a nickel-iron alloy comprises the following steps: S1. Prepare sample solution: S101. Prepare nickel, phosphorus, lead, copper and arsenic sample solution to be tested: Weigh a nickel-iron alloy sample, add concentrated nitric acid, concentrated hydrochloric acid, and perchloric acid, and heat until the nickel-iron alloy sample is dissolved, wherein the volume ratio of the concentrated nitric acid, concentrated hydrochloric acid, and perchloric acid is 3:2:2; After the perchloric acid smoke has disappeared, cool the solution, add concentrated hydrochloric acid of equal volume to the perchloric acid, heat until the precipitated crystals dissolve, cool the solution, and adjust the volume to obtain a nickel, phosphorus, lead, copper, and arsenic sample solution. S102, prepare silicon chromium sample solution to be tested: Weigh a nickel-iron alloy sample, add water, concentrated nitric acid, and concentrated hydrochloric acid, and heat until the nickel-iron alloy sample is dissolved, keeping the solution volume constant. After dissolving until bubbling, cool and adjust the volume to obtain a silicon-chromium sample solution to be tested; the volume ratio of water, concentrated nitric acid, and concentrated hydrochloric acid is 25:10:4.
[0005] S2, preparing calibration curve solution; S3. ICP-AES detection.
[0006] In step S101, the mass volume ratio of the nickel-iron alloy sample to concentrated nitric acid is 1 g:150 mL.
[0007] In step S102, the mass volume ratio of the nickel-iron alloy sample to concentrated nitric acid is 1 g:100 mL.
[0008] The density of the concentrated hydrochloric acid is 1.16 g / mL to 1.19 g / mL, the density of the concentrated nitric acid is 1.42 g / mL, and the volume fraction of the perchloric acid is 70-72%.
[0009] In step S2, the preparation method of the calibration curve solution is as follows: Using the stepwise dilution method, add 5 mL of concentrated hydrochloric acid and 30 mL of iron standard solution (1000 μg / mL) to prepare 5 or more calibration curve solutions of different concentrations with the standard solutions of each component.
[0010] Preferably, the specific steps of step S3 are: S301, start the ICP-AES spectrometer and ignite the plasma until the instrument operates stably; S302, setting detection parameters and adjusting instrument working conditions; S303. Draw a calibration curve using the calibration curve solution and test the sample solution.
[0011] Preferably, the ICP-AES spectrometer is run for at least 1 h before testing.
[0012] Preferably, in step S302, the detection parameters include: matrix tube, sampling system, analysis spectrum line, background correction position, integration position, area, and time of the collected data signal.
[0013] Preferably, the analysis spectrum is as shown in Table 1.
[0014] Table 1 ICP-AES spectrometer analysis lines
[0015] Preferably, in step S302, the instrument working conditions include: pump speed, RF power, nebulizer gas flow rate, cooling gas flow rate, auxiliary gas flow rate, visible light chamber exposure and photocapture time, and ultraviolet light chamber exposure time.
[0016] Preferably, after the performance indicators of the instruments meet the requirements of Table 2, the sample solution is tested.
[0017] Table 2 ICP-AES spectrometer operating parameters
[0018] During the determination of the content of nickel-iron alloy components, it was found that the silicon-chromium component was difficult to be cleared up and interfered with the determination of other component elements. In addition, in nickel-iron alloy, the content span of each component of nickel, phosphorus, copper, lead and arsenic was larger, making it more difficult to achieve the complete clearing up of each component. Therefore, the present invention is based on the performance of each component of nickel-iron alloy, specifically dissolved in batches with concentrated nitric acid, concentrated hydrochloric acid and perchloric acid, and after being diluted to a certain volume, the emission line intensity of the component to be measured is measured by an ICP spectrometer, and the component content is calculated according to the working curve established by the calibration curve solution according to the characteristic line intensity. The present invention improves the precision and accuracy of analysis, and also greatly improves the speed of primary and secondary multi-component detection in nickel-iron alloy.
[0019] Beneficial effects: 1. The present invention dissolves the nickel-iron alloy sample in batches according to the difficulty of dissolving the major and minor elements, and then uses ICP for simultaneous determination and analysis. This technology is innovative and the measurement results are fast and accurate.
[0020] 2. The present invention provides a method for quickly and accurately determining the contents of multiple components of nickel, silicon, chromium, phosphorus, copper, lead and arsenic in nickel-iron alloys. Elements with higher contents can be directly determined without diluting the test solution, which not only greatly saves detection time and personnel energy and improves detection efficiency, but also saves electricity and gas costs and reduces detection costs. At the same time, it fills the gap in the lack of a method for quickly and accurately determining high and low content elements with a wide range in nickel alloys. It is an important innovation in the method for quickly and accurately determining the contents of multiple major and minor elements in nickel-iron alloys. DETAILED DESCRIPTION
[0021] The present invention will be further described below with reference to the examples, but is not limited thereto.
[0022] (1) Preparation of test and analysis samples Samples were taken and prepared according to "GB / T 20066-2006 Sampling and preparation of specimens for determination of chemical composition of steel and iron".
[0023] (2) Instruments and reagents Inductively coupled plasma atomic emission spectrometer (ICP-AES): Model: THERMO FISHER Icap7400.
[0024] Analytical balance: graduation value is not less than 0.0001 g.
[0025] Glass conical flask: 300mL.
[0026] Single-marked line volumetric flasks, graduated pipettes, and single-marked line pipettes should comply with the requirements of GB / T 12806-2011, GB / T12807-2021, and GB / T 12808-2015 respectively.
[0027] Hydrochloric acid, density 1.18 g / mL, high purity.
[0028] Nitric acid, density 1.42 g / mL, extra-pure.
[0029] Perchloric acid, HClO4 content 71%, high purity.
[0030] Nickel standard solution: Nickel standard solution 1000 μg / mL with standard substance certificate.
[0031] Iron standard solution: 1000 μg / mL iron standard solution with standard substance certificate.
[0032] Silicon standard solution (500 μg / mL): obtained by diluting the silicon standard solution (1000 μg / mL) with a standard substance certificate.
[0033] Phosphorus standard solution (100 μg / mL): prepared by diluting the phosphorus standard solution (1000 μg / mL) with a standard substance certificate.
[0034] Copper standard solution (20 μg / mL): obtained by diluting the copper standard solution (1000 μg / mL) with a standard substance certificate.
[0035] Lead standard solution (10 μg / mL): obtained by diluting the lead standard solution (1000 μg / mL) with a standard substance certificate.
[0036] Arsenic standard solution (10 μg / mL): obtained by diluting the arsenic standard solution (1000 μg / mL) with a standard substance certificate.
[0037] Chromium standard solution (500 μg / mL): obtained by diluting the chromium standard solution (1000 μg / mL) with a standard substance certificate.
[0038] (3) Preparation of calibration curve solution Each calibration curve solution was added to a 100 mL single-marked volumetric flask according to the addition amount specified in Table 3. 5 mL of concentrated hydrochloric acid was then added, followed by 30 mL of iron standard solution (1000 μg / mL). The solution was then diluted to volume with water to prepare a series of calibration curve solutions. The concentrations of the calibration curve solutions are shown in Table 4.
[0039] Table 3 Amount of solution added for each calibration curve (in ml)
[0040] Table 4 Concentrations of calibration curve series solutions (unit: 10 μg / mL)
[0041] Example 1: ① Accurately weigh 0.1g of nickel-iron alloy 1# sample and place it in a 300mL conical flask. Add 15mL of concentrated nitric acid, 10mL of concentrated hydrochloric acid, and 10mL of perchloric acid. Place it in a low-temperature electric furnace and heat it at 150℃ until the sample is dissolved. After the concentrated perchloric acid smoke disappears, remove it and cool it. Add 10mL of concentrated hydrochloric acid and heat it at 150℃ to dissolve the salts. After cooling, transfer it to a 100mL volumetric flask and make up to volume with water to obtain the nickel, phosphorus, lead, copper and arsenic sample solution to be tested.
[0042] ② Accurately weigh 0.1g of nickel-iron alloy 1# sample and place it in a 300mL conical flask. Add 25mL of water, 10mL of concentrated nitric acid, and 4mL of concentrated hydrochloric acid. Place it in a low-temperature electric furnace and heat it to 150℃ until the sample is dissolved. Maintain the solution volume at 40mL by adding water. After dissolving until large bubbles appear in the test solution, remove it, cool it, transfer it to a 100mL volumetric flask, and make up the volume with water to obtain the silicon-chromium sample solution to be tested.
[0043] ③ICP-AES detection: Turn on the plasma spectrometer and its accessories according to the instrument operating procedures, ignite the plasma, and wait until the instrument runs stably. Run for at least 1 hour before taking measurements.
[0044] According to the instrument manufacturer's operating procedures and guidelines, select the appropriate matrix tube and sample introduction system. For each element to be analyzed, determine the appropriate analytical line (as shown in Table 1), background correction position, and detection parameters such as the integration position, area, and time for data signal acquisition. Then, adjust and set instrument operating conditions such as pump speed, RF power, nebulizer gas flow, cooling gas flow, auxiliary gas flow, visible light chamber exposure time, photoacquisition time, and UV chamber exposure time (as shown in Table 2). Once all instrument performance indicators meet the standards, construct a calibration curve using the calibration curve solution and conduct testing on the sample solution.
[0045] Example 2: ① Accurately weigh 0.1g of nickel-iron alloy 2# sample and place it in a 300ml conical flask. Add 15mL of concentrated nitric acid, 10mL of concentrated hydrochloric acid, and 10mL of perchloric acid. Place it in a low-temperature electric furnace and heat it at 150℃ until the sample is dissolved. After the concentrated perchloric acid smoke disappears, remove it and cool it. Add 10mL of concentrated hydrochloric acid and heat it at 150℃ to dissolve the salts. After cooling, transfer it to a 100mL volumetric flask and make up to volume with water to obtain the nickel, phosphorus, lead, copper and arsenic sample solution to be tested.
[0046] ② Accurately weigh 0.1g of nickel-iron alloy 2# sample and place it in a 300ml conical flask. Add 25ml of water, 10ml of concentrated nitric acid, and 4ml of concentrated hydrochloric acid. Place it in a low-temperature electric furnace and heat it at 150℃ until the sample is dissolved. Maintain the solution volume at 40ml by adding water. After dissolving until large bubbles appear in the test solution, remove it, cool it, transfer it to a 100ml volumetric flask, and make up the volume with water to obtain the silicon-chromium sample solution to be tested.
[0047] ③ICP detection: The plasma spectrometer and its accessories were turned on according to the instrument operating procedures, and the plasma was ignited until the instrument ran stably and ran for at least 1 hour before measurement.
[0048] Measure the calibration solution with the highest concentration of each element. According to the instrument manufacturer's operating procedures and guidelines, select the appropriate matrix tube and sample introduction system. For each element to be analyzed, determine the appropriate analytical line (as shown in Table 1), background correction position, and integration position, area, and time for data signal acquisition. Then, adjust and set instrument operating conditions such as pump speed, RF power, nebulizer gas flow, cooling gas flow, auxiliary gas flow, visible light chamber exposure time, photoacquisition time, and UV chamber exposure time (as shown in Table 2). Once all instrument performance indicators meet the standards, construct a calibration curve using the calibration curve solution and proceed with testing the sample solution.
[0049] Table 5 Test results
[0050] Table 5 shows the test results of various components of the nickel-iron alloy obtained by testing in Examples 1 and 2. It can be seen from the table that the results obtained by testing in Examples 1 and 2 have high accuracy.
Claims
1. An ICP-AES method for simultaneously determining the contents of major and minor components of nickel, silicon, chromium, phosphorus, copper, lead and arsenic in nickel-iron alloy, characterized in that: The following steps are involved: S1. Prepare sample solution: S101. Prepare nickel, phosphorus, lead, copper and arsenic sample solution to be tested: (1) Weigh a nickel-iron alloy sample, add concentrated nitric acid, concentrated hydrochloric acid, and perchloric acid, and heat until the nickel-iron alloy sample is dissolved. The volume ratio of the concentrated nitric acid, concentrated hydrochloric acid, and perchloric acid is 3:2:
2. After the perchloric acid smoke has disappeared, cool the solution, add concentrated hydrochloric acid of equal volume to the perchloric acid, heat until the precipitated crystals dissolve, cool, and dilute to obtain a nickel, phosphorus, lead, copper, and arsenic sample solution; S102, prepare silicon chromium sample solution to be tested: Weigh a nickel-iron alloy sample, add water, concentrated nitric acid, and concentrated hydrochloric acid, and heat until the nickel-iron alloy sample is dissolved, keeping the solution volume constant. After dissolving until bubbling occurs, cool and adjust the volume to obtain a silicon-chromium sample solution to be tested; the volume ratio of water, concentrated nitric acid, and concentrated hydrochloric acid is 25:10:4; S2, preparing calibration curve solution; S3. ICP-AES detection.
2. The ICP-AES method for synchronously determining the multi-component content of nickel, silicon, chromium, phosphorus, copper, lead and arsenic in the nickel-iron alloy according to claim 1, is characterized in that: In step S101, the mass volume ratio of the nickel-iron alloy sample to concentrated nitric acid is 1 g:150 mL.
3. The ICP-AES method for synchronously determining the multi-component content of nickel, silicon, chromium, phosphorus, copper, lead and arsenic in the nickel-iron alloy according to claim 1, is characterized in that: In step S102, the mass volume ratio of the nickel-iron alloy sample to concentrated nitric acid is 1 g:100 mL.
4. The ICP-AES method for synchronously determining the multi-component content of nickel, silicon, chromium, phosphorus, copper, lead and arsenic in nickel-iron alloy according to claim 1, is characterized in that: The density of the concentrated hydrochloric acid is 1.16 g / mL to 1.19 g / mL, the density of the concentrated nitric acid is 1.42 g / mL, and the mass fraction of the perchloric acid is 70-72%.
5. The ICP-AES method for synchronously determining the multi-component content of nickel, silicon, chromium, phosphorus, copper, lead and arsenic in nickel-iron alloy according to claim 1, is characterized in that: In step S2, the preparation method of the calibration curve solution is as follows: Using the stepwise dilution method, add 5 mL of concentrated hydrochloric acid and 30 mL of iron standard solution (1000 μg / mL) to prepare 5 or more calibration curve solutions of different concentrations with the standard solutions of each component.
6. The ICP-AES method for synchronously determining the multi-component contents of nickel, silicon, chromium, phosphorus, copper, lead and arsenic in nickel-iron alloy according to claim 1, wherein: The specific steps of step S3 are: S301, start the ICP-AES spectrometer and ignite the plasma until the instrument operates stably; S302, setting detection parameters and adjusting instrument working conditions; S303. Draw a calibration curve using the calibration curve solution and test the sample solution.
7. The ICP-AES method for synchronously determining the multi-component contents of nickel, silicon, chromium, phosphorus, copper, lead and arsenic in nickel-iron alloy according to claim 6, is characterized in that: The ICP-AES spectrometer was run for at least 1 h before testing.
8. The ICP-AES method for synchronously determining the content of the major and minor components of nickel, silicon, chromium, phosphorus, copper, lead and arsenic in the nickel-iron alloy according to claim 6 is characterized in that: In step S302, the detection parameters include: matrix tube, sample injection system, analysis spectrum line, background correction position, integration position, area and time of collected data signal.
9. The ICP-AES method for synchronously determining the multi-component contents of nickel, silicon, chromium, phosphorus, copper, lead and arsenic in nickel-iron alloy according to claim 6, is characterized in that: In step S302, the instrument working conditions include: pump speed, RF power, nebulizer gas flow, cooling gas flow, auxiliary gas flow, visible light chamber exposure and light capture time, and UV chamber exposure time.