HIRANUMA APPLICATION DATAPLATING &ETCHING
SOLUTION

Automatic Titrator

Data No. E10

Apr. 19,20182+

Quantitative determination of total nickel (Ni )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 byphotometric 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(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.

Indicator：MX indicator
0.1 g of murexide and 10 g of potassium sulfate are well-mixed by mortar.

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
Cnd. No.
Method ﾞ
Buret No.
Amp No.
D.UnitS- Timer
C.P. mL
T.Timer
D.P. mLEnd Sens
Over mLMax Vol.

1B cross
12T%
51500200
140sec
mL
sec
mL
mL
mL

Constant No.
SizeBlank
Morality
FactorKL
Unit
Formula10 g0 mL
0.1 mol/L
1.007
58.69
0g/L

(D-B)*K*F*M/SDigits4Auto input parameter

None

Mode No.
Pre Int
Del K
Del Sens
Int Time
Int Sens
Brt SpeedPulse

20
05050280

sec
mV
sec
mV

Measurement results
Number ofSize

Titrant

Total Nickel

Measurement(mL)

Volume (mL)Concentration (g/L)

1

119.093112.8412

119.003112.3093

118.970

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 thechange 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.
(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.
Nickel sulfamate tetrahydrate concentration (g/L)＝(CA – K × 0.247) × 5.502
CA： Measurement result of total nickel concentration (g/L)

K： Measurement result of nickel chloride hexahydrate (g/L)

0.247 ： Coefficient for converting from nickel chloride hexahydrate to nickel(Ni(58.69) / NiCl2･6H2O(237.69))
5.502 ： Coefficients for converting from nickel to nickel sulfamate tetrahydrate(Ni(NH2SO3)2･4H2O (322.93) / Ni (58.69))
When it is calculated as nickel sulfate hexahydrate concentration, change thecoefficient for converting from 5.502 to 4.479.(NiSO4･6H2O (262.85)／Ni (58.69))
Keywords：Nickel plating solution, Total nickel, Photometric titration, Chelatometric titration*Some measurement would not be possible depending on optional configuration of system.