Monday, December 1, 2008

Potentiometric Determination of the Perborates in Detergents

Cationic Surfactants in Fabric Softener

Potentiometric Determination of the Perborates in Detergents



Equipment
Potentiometer = 751 GPD Titrino / Titroprocessor
Electrodes =
6.0420.100 LL combined Pt electrode; input 1

Reagents
c
(KMnO4) = 0.02 mol/L; D0

Sample
5 mL sample solution
20 mL
w(H2SO4) = 0.30 (30%)

Remarks
Determination reaction:

5 NaBO2*H2O2 + 2 MnO4- + 6 H+2 Mn2+ + 5 O2 + 8 H2O + 5NaBO2

Calculations:

Perborat=EP1*C01*C02*C03*C04*C05/C00;2;%

Perborat = fraction of perborates in %
C01 = concentration of titrating agent (0.02 mol/L)
C02 = factor for “normality“ (5/2=2.5)
C03 = molecular mass of NaBO2*H2O2*3H2O (153.86 g/mol)
C04 = conversion mL L * factor for % (0.001*100 = 0.1)
C05 = factor for dilution (20)

Answer

Perborat = 1.289 x 0.02 x 2.5 x 153.86 x 0.1 x 20 / 2.5023 = 7.93 %

EP1 = 1.289 mL
C00 = 2.5023 g

Sample preparation:
Weigh 2.5 g in a measuring flask of 100 mL. Dissolve sample with
c(H2SO4) = 1 mol/L and wait for the reaction of the carbonate. When gas evolution has stopped, fill measuring flask to the mark. Pipette 5 mL of solution, add 20 mL of w(H2SO4) = 0.30 (30%) and titrate. The 6.0431.100 Pt Titrode may be used instead of the 6.0420.100 LL Pt electrode.

Literature
G. Jander, K.F.Jahr, “Massanalyse“, Sammlung Gröschen de Gruyter, Berlin, New York (1973), p. 67

Method documentation

'pa
751 GPD Titrino 15215 751.0010
MET U …Perborat
parameters
>titration parameters
V step …0.10 ml
dos.rate max…. ml/min
signal drift …OFF mV/min
equilibr.time …10 s
start V: ….abs.
start V ….0.5 ml
dos.rate max…. ml/min
pause …30 s
dos.element:…. internal D0
meas.input: ….1
temperature ….25.0 °C
>stop conditions
stop V: ….abs.
stop V ….5 ml
stop U ….OFF mV
stop EP ….9
filling rate max…. ml/min
>statistics
status: ….OFF
>evaluation
EPC ….30 mV
P recognition:…. all
fix EP1 at U ….OFF mV
pK/HNP: ….OFF
>preselections
req.ident: …OFF
req.smpl size:… OFF
activate pulse: …OFF
------------
'fm
751 GPD Titrino 15215 751.0010
MET U Perborat
>calculations

Perborat=EP1*C01*C02*C03*C04*C05/C00;2;%

C00= 2.5023
C01= 0.02
C02= 2.5
C03= 153.86
C04= 0.1
C05= 20
------------
'fr
751 GPD Titrino 15215 751.0010
U(init) 697 mV MET…. U Perborat
smpl size ….2.5023 g
EP1 ….1.289 ml 933 mV
Perborat…. 7.93 %
stop V reached
============
'cu
751 GPD Titrino 15215 751.0010
start V
...0.500 ml MET... U Perborat

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