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Determination of Nickel Content in Iron-Nickel Alloys by Fully Automated Potentiometric Titration
I. Introduction
Permalloy, also known as iron-nickel alloy, has a wide range of nickel content, ranging from 35% to 90%. Based on composition, permalloy can be divided into four main categories: 35%–40% Ni-Fe alloy, 45%–50% Ni-Fe alloy, 50%–65% Ni-Fe alloy, and 70%–81% Ni-Fe alloy. Each category can be made into materials with circular, rectangular, or flat hysteresis loops.
This method uses the JH-T6 fully automated potentiometric titration method from Shanghai Jiahang to determine the nickel content. Ammonia water is used to shield the influence of iron ions to determine the nickel content.
II. Instruments and Reagents
2.1 Instruments
JH-T6 fully automated potentiometric titrator, copper ion selective electrode, analytical balance, etc.
2.2 Reagents
Ammonia water, EDTA standard solution (0.1 mol/L), etching solution (main components: hydrochloric acid, ferric chloride, ferrous chloride). III. Experimental Methods
3.1 Analytical Procedure
Accurately weigh 0.15g of sample and place it in a small beaker. Add 20ml of etching solution and stir magnetically for approximately 3 hours until the sample is completely dissolved. Transfer the solution to a 250ml volumetric flask and dilute to the mark with water. Let stand for 10 minutes.
Accurately transfer 20ml of the prepared sample to a small beaker and add primary water to make the volume approximately 50ml. Then add ammonia water and stir continuously until no more precipitate forms. Filter the solution through filter paper to remove the precipitate. Collect the filtrate and add a small amount of ammonia water to check for further precipitate formation. If no precipitate forms, collect the filtrate and dilute to the mark in a 250ml volumetric flask. If precipitate forms, repeat the previous steps until no more precipitate forms.
Transfer 20 ml of the diluted solution to a titration vessel, add 30 ml of water, place the vessel on the titration stand, and titrate with 0.1 mol/L EDTA standard titrant.
Titrate to the potential endpoint, while simultaneously performing a full-procedure blank experiment.
Set the titrator parameters as shown in Table 1:
Table 1 Titration Parameter Settings
3. Test Spectrum Example
IV. Results and Discussion
4.1 Experimental Results
The experimental results are shown in Table 2:
Table 2 Test Results
4.2 Conclusion
The test results showed that the nickel content in this iron-nickel alloy was 53.88%. The only drawback was the relatively high concentration of the titrant, which resulted in poor repeatability. It is recommended to reduce the titrant concentration or the sample size.
Keyword:
Automated Potentiometric Titration
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