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Titrimetric Determination of Free Boric Acid and Tetrafluoroboric Acid in Nickel Plating Baths

This bulletin describes a potentiometric titration method for simultaneously determining the concentrations of free boric acid and tetrafluoroboric acid in nickel plating baths. The method involves adding mannitol to the sample, which forms complexes that are then titrated with sodium hydroxide solution. This gives two equivalence points, with the first corresponding to tetrafluoroboric acid concentration and the difference between the two points corresponding to boric acid concentration. The determination is direct and is not interfered with by nickel or other metal ions in the plating bath sample.

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193 views3 pages

Titrimetric Determination of Free Boric Acid and Tetrafluoroboric Acid in Nickel Plating Baths

This bulletin describes a potentiometric titration method for simultaneously determining the concentrations of free boric acid and tetrafluoroboric acid in nickel plating baths. The method involves adding mannitol to the sample, which forms complexes that are then titrated with sodium hydroxide solution. This gives two equivalence points, with the first corresponding to tetrafluoroboric acid concentration and the difference between the two points corresponding to boric acid concentration. The determination is direct and is not interfered with by nickel or other metal ions in the plating bath sample.

Uploaded by

Dang Thinh
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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No.

195/2 e

Application Bulletin
Of interest to: Metals, electroplating A 10

Titrimetric determination of free boric acid and tetra-


fluoroboric acid in nickel plating baths

Summary
This bulletin describes the simultaneous potentiometric titration of free boric acid
and free tetrafluoroboric acid in nickel plating baths. After addition of mannitol, the
formed mannitol complexes are titrated with sodium hydroxide solution. The deter-
mination is carried out directly in the plating bath sample; nickel and other metal
ions do not interfere.

Instruments and accessories

• 702 SET/MET Titrino, 716 DMS Titrino, 736 GP Titrino, 751 GPD Titrino or 785
DMP Titrino or
796 Titroprocessor with 700 Dosino or 685 Dosimat
• 2.728.0040 Magnetic Stirrer
• 6.3014.223 Exchange Unit
• 6.0222.100 combined LL pH glass electrode with 6.2104.020 electrode cable

Reagents

• Titrant: sodium hydroxide solution, c(NaOH) = 0.1 mol/L (or more diluted)
• D-Mannitol solution, w(mannitol) = 10% in dist. water

Analysis
Pipet a defined volume of the sample into a plastic beaker, add 30 mL dist. water
and 10 mL w(mannitol) = 10% and titrate with c(NaOH) = 0.1 mol/L.
Application Bulletin No. 195/2 e
Titrimetric determination of free boric acid and tetrafluoroboric acid Page 2

Calculation
Two equivalence points are obtained, the first of which corresponds to the HBF4
content and the difference between the second and the first equivalence point to
the H3BO3 content.
1 mL c(NaOH) = 0.1 mol/L corresponds to 8.781 mg HBF4 or 6.183 mg H3BO3

g/L HBF4 = EP1 * C01 / C00


g/L H3BO3 = (EP2 – EP1) * C02 / C00

EP1 = titrant consumption to reach the first EP in mL


EP2 = titrant consumption to reach the second EP in mL
C00 = sample volume in mL
C01 = 8.781
C02 = 6.183

Figures
'pa
736 GP Titrino 04268 736.0011
date 99-12-17 time 14:56 9
DET pH AB 195
parameters
>titration parameters
meas.pt.density 4
min.incr. 10.0 µl
titr.rate max. ml/min
signal drift 20 mV/min
equilibr.time 38 s
start V: OFF
pause 0 s
dos.element: internal D0
meas.input: 1
temperature 25.0 °C
>stop conditions
stop V: abs.
stop V 4 ml
stop pH OFF
stop EP 9
filling rate max. ml/min
>statistics
status: OFF
>evaluation
EPC 5
EP recognition: all
fix EP1 at pH OFF
pK/HNP: OFF
>preselections
req.ident: OFF
req.smpl size: value
activate pulse: OFF
============

'fm
736 GP Titrino 04268 736.0011
date 99-12-17 time 14:56 9
DET pH AB 195
>calculations
HBF4=EP1*C01/C00;2;g/l
H3BO3=(EP2-EP1)*C02/C00;2;g/l
C00= 0.250
C01= 8.781
C02= 6.183
============

Fig. 1: Parameter settings and calculation formulae for the determination of free
boric acid and tetrafluoroboric acid.
Application Bulletin No. 195/2 e
Titrimetric determination of free boric acid and tetrafluoroboric acid Page 3

'fr
736 GP Titrino 04268 736.0011
date 99-12-17 time 14:56 9
pHc(init) 3.10 DET pH AB 195
smpl size 0.250 ml
EP1 0.834 ml 4.19
EP2 2.786 ml 8.34
HBF4 29.29 g/l
H3BO3 48.28 g/l
stop V reached
============

AB 195
11

10

9
EP2
8

7
pH

EP1
4

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0


V [ml]

Fig. 2: Result block and titration curve for the determination of free boric acid and
tetrafluoroboric acid in a nickel plating bath.

Literature

• E. Scholz
Die Analyse von Fluoroboratbädern und anderen Fluoroboratlösungen
Galvanotechnik 66 (1975) 811–819.
• D. Strohm
Automation komplexer Titrationen am Beispiel eines galvanischen Nickelbades
GIT 32 (1988) 369–373.

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