| HIRANUMA APPLICATION DATA | Automatic Titrator | Data No. | E10 | Apr. 19,2018 |
| PLATING & ETCHING SOLUTION | Quantitative determination of total nickel (Ni²⁺) in nickel plating solution |
1. Abstract
The control and analysis of nickel plating solution is very important process for the product quality. Analytical components of the general nickel plating solution are 1) nickel sulfamate, 2) nickel chloride, and 3) boric acid. The example of quantitative determination for total nickel which is total amount of nickel chloride and nickel sulfamate in nickel plating solution is introduced in this report. The total nickel is determined by photometric titration with EDTA standard solution using indicator MX.
| Ni(II) ＋ EDTA → Ni-EDTA |
2. Configuration of instruments and Reagents
| (1) | Configuration | ||
| Main unit | : | Hiranuma Automatic Titrator COM series (Photometric titrator unit type M) with 530 nm optical filter |
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| (2) | Reagents | ||
| Titrant | : | 0.1 mol/L EDTA standard solution | |
| Buffer solution | : | Diluted ammonia solution (1:1, v/v) Mix 28 ~30 % ammonia solution and DI water with 1:1 volume ratio. |
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| Indicator | : | MX indicator 0.1 g of murexide and 10 g of potassium sulfate are well-mixed by mortar. |
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3. Measurement procedure
| (1) | Dispense 1 mL of sample with volumetric pipette into a 100 mL beaker. |
| (2) | Add 60 mL of DI water. |
| (3) | Add 20 mL of diluted ammonia solution. |
| (4) | Add 0.2 g of MX indicator. |
| (5) | Immerse photometric probe into sample solution and titrate with 0.1 mol/L EDTA standard solution. |
4. Measurement conditions and results
Examples of titration conditions
Measurement results
| Number of measurement |
Size (mL) |
Titrant volume (mL) |
Total Nickel Concentration (g/L) |
|---|---|---|---|
| 1 | 1 | 19.093 | 112.841 |
| 2 | 1 | 19.003 | 112.309 |
| 3 | 1 | 18.970 | 112.114 |
| Statistic calculation |
Average | 112.4 g/L | |
| Standard deviation | 0.376 g/L | ||
| Coefficient of variation | 0.33 % | ||
Example of titration curve
5. Note
| (1) | Measurement condition “Method” on condition parameter is set to “B Cross” because the endpoint is defined as the point where the change in color of the indicator is completed. The titrant is continuously added by using the function “CP mL”. This function is useful to add titrant until just before it reaches endpoint when the titrated volume is relatively large as described in this report. The measurement time can be reduced by “CP mL” function. |
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| (2) | Calculation of nickel sulfamate Nickel sulfamate concentration can be calculated by the subtraction of nickel chloride from total nickel. Calculation of nickel sulfamate concentration is possible by the following formula.
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| Keywords： | Nickel plating solution, Total nickel, Photometric titration, Chelatometric titration |
*Some measurement would not be possible depending on optional configuration of system.
