METTLER TOLEDO M569/570

Ascorbic Acid (Vitamin C): Voltametric Determination

Method for the determination of vitamin C content using voltametric indication and DPI as titrant.

Sample Various fruit samples Preparation and Procedures

The juice samples were weighed directly into the titration beaker,
without special treatment such as filtration. Even the relatively
high pulp content of the grapefruit juice did not disturb the
titration.
Substance L(+)-Ascorbic acid M = 176.13 The strawberries and kiwis were mashed with a mixer and then
g/mol; z = 2 weighed into the beaker.
After the addition of 50 mL deionised water the beaker is purged
Chemicals Water with nitrogen to avoid oxidation of the vitamin C.
Apple juice can be titrated without dilution because of its low
vitamin C content.
Prior to the analysis the pH of the sample solution has to be
adjusted by either oxalic acid (2 %) for samples with a higher
Titrant 2,6-Dichlorophenolindophenol (DPI), initial pH-value or with NaOH 0.1 mol/L for samples with an
initial pH lower than 3.0.
c (1/2 DPI) = 0.01 mol/L
Sample size: The sample size depends on the amount of
; vitamin C present in the sample. 1 - 15 mg of vitamin C lead to
a consumption of 0.5 - 8.5 mL DPI.
Standard L(+)-Ascorbic acid For automatic pH adjustment use the Special Method 91002,
which is already stored in every DL58 titrator.
Instruments DL58; Sample Changer ST20A,
Standard
Balance AT 200, Printer HP Deskjet 100 mg ascorbic acid is weighed into a 100 mL volumetric
500 flask and diluted with deionised water. The solution has to be
kept in the dark and should be prepared fresh daily.
Accessories Red titration beaker ME-25777, KF
option ME-51107269

Remarks
Indication DM142 The voltametric method
In voltametric titration a constant polarisation current is applied
to a double pin platinum electrode (DM142). Potential readings
Chemistry allow the indication of the equivalence point thanks to a rise in
potential after the EQP. Polarisation currents of -0.5 to -2.0 µA
were applied for the determinations.

Preparation of the titrant

0.36 g of 2,6-Dichlorophenolindophenol (DPI) sodium salt
monohydrate is weighed in a 250 mL volumetric flask, which is
Calculation filled up with deionised water to obtain a titrant concentration of
0.01 mol/L.
If 2,6-Dichlorophenolindophenol sodium salt dihydrate is used,
an excess has to be weighed in due to its bad solubility and the
titrant has to be filtrated prior to use.
The DPI titrant has to be prepared fresh daily. It has to be stored
in brown glass bottles.

Results Standardisation of DPI

The same parameters of the titration method should be used for
both standardisation and determination.
Waste No special treatment is necessary. 5 mL of standard solution are pipetted into a titration beaker,
disposal diluted with deionised water and the beaker is purged with
nitrogen to avoid oxidation of vitamin C. The pH is adjusted to
3.0 with oxalic acid (2 %).
A standard solution of ascorbic acid is produced to facilitate
sample entry. An aliquot of the solution is filtrated and the
Author A. Aichert, N. Spiru
sample size is entered as weight

1
Results
Vitamin C in apricot juice

METTLER TOLEDO DL58 Titrator V2.0 Mettler-Toledo GmbH

Market Support Laboratory

Method MT069 Vitamin C (voltam.) 17-Jul-1996 10:14

Measured 17-Jul-1996 11:23
User

RESULTS

No. ID Sample size and results

1 apricot juice 5.3814 g

R1 = 40.992 mg/100g Vitamin C
2 apricot juice 5.2443 g
R1 = 41.181 mg/100g Vitamin C
3 apricot juice 5.5123 g
R1 = 41.155 mg/100g Vitamin C

STATISTICS
Number of results R1 n = 3
Mean value x = 41.109 mg/100g Vitamin C
Standard deviation s = 0.10286 mg/100g Vitamin C
Rel. standard deviation srel = 0.250 %

Table of measured values Titration curve

2
Method
Method MT069 Vitamin C (voltam.) Method for the standardisation of DPI
Version 17-Jul-1996 10:14
Method MT070 Titer of DPI (voltam.)
Title Version 19-Jun-1996 11:21
Method ID . . . . . . . . . . . . . MT069
Title . . . . . . . . . . . . . . . Vitamin C (voltam.) Title
Date/time . . . . . . . . . . . . . 17-Jul-1996 10:14 Method ID . . . . . . . . . . . . MT070
Sample Title . . . . . . . . . . . . . . Titer of DPI (voltam.)
Sample ID . . . . . . . . . . . . . apricot juice Date/time . . . . . . . . . . . . 19-Jun-1996 11:21
Entry type . . . . . . . . . . . . . Weight Sample
Lower limit [g] . . . . . . . . . 5.0 Sample ID . . . . . . . . . . . . Vitamin C
Upper limit [g] . . . . . . . . . 7.0 Entry type . . . . . . . . . . . . Weight
Molar mass M . . . . . . . . . . . . 176.13 Lower limit [g] . . . . . . . . 0.0
Equivalent number z . . . . . . . . 2 Upper limit [g] . . . . . . . . 0.1
Titration stand . . . . . . . . . . Stand 1 Molar mass M . . . . . . . . . . . 176.13
Temperature sensor . . . . . . . . . Manual Equivalent number z . . . . . . . 2
Stir Titration stand . . . . . . . . . Stand 1
Speed [%] . . . . . . . . . . . . . 40 Temperature sensor . . . . . . . . Manual
Time [s] . . . . . . . . . . . . . . 10 Stir
EQP titration (Ipol/Upol) Speed [%] . . . . . . . . . . . . 40
Titrant/Sensor Time [s] . . . . . . . . . . . . . 10
Titrant . . . . . . . . . . . . . 1/2 DPI EQP titration (Ipol/Upol)
Concentration [mol/L] . . . . . . 0.01 Titrant/Sensor
Sensor . . . . . . . . . . . . . DM142 Titrant . . . . . . . . . . . . 1/2 DPI
Indication . . . . . . . . . . . . . Voltametric Concentration [mol/L] . . . . . 0.01
IPol [µA] . . . . . . . . . . . . -2.0 Sensor . . . . . . . . . . . . DM142
Predispensing . . . . . . . . . . . to volume Indication . . . . . . . . . . . . Voltametric
Volume [mL] . . . . . . . . . . . 2 IPol [µA] . . . . . . . . . . . -2.0
Wait time [s] . . . . . . . . . . 2 Predispensing . . . . . . . . . . to volume
Titrant addition Volume [mL] . . . . . . . . . . 4
dV [mL] . . . . . . . . . . . . . 0.1 Wait time [s] . . . . . . . . . 0
Measure mode . . . . . . . . . . . . Equilibrium controlled Titrant addition
dE [mV, µA] . . . . . . . . . . . 0.5 dV [mL] . . . . . . . . . . . . 0.1
dt [s] . . . . . . . . . . . . . 1.0 Measure mode . . . . . . . . . . . Equilibrium controlled
t(min) [s] . . . . . . . . . . . 3.0 dE [mV, µA] . . . . . . . . . . 0.5
t(max) [s] . . . . . . . . . . . 30.0 dt [s] . . . . . . . . . . . . 1.0
Recognition t(min) [s] . . . . . . . . . . 3.0
Threshold . . . . . . . . . . . . 400.0 t(max) [s] . . . . . . . . . . 30.0
Steepest jump only . . . . . . . No Recognition
Range . . . . . . . . . . . . . . No Threshold . . . . . . . . . . . 400.0
Tendency . . . . . . . . . . . . Positive Steepest jump only . . . . . . No
Termination Range . . . . . . . . . . . . . No
at maximum volume [mL] . . . . . 10.0 Tendency . . . . . . . . . . . None
at potential . . . . . . . . . . No Termination
at slope . . . . . . . . . . . . No at maximum volume [mL]. . . . . 10.0
after number EQPs . . . . . . . . Yes at potential . . . . . . . . . No
n = . . . . . . . . . . . . . 1 at slope . . . . . . . . . . . No
comb. termination conditions . . No after number EQPs . . . . . . . Yes
Evaluation n = . . . . . . . . . . . . 1
Procedure . . . . . . . . . . . . Standard comb. termination conditions . No
Potential 1 . . . . . . . . . . . No Evaluation
Potential 2 . . . . . . . . . . . No Procedure . . . . . . . . . . . Standard
Stop for reevaluation . . . . . . Yes Potential 1 . . . . . . . . . . No
Condition . . . . . . . . . . neq=0 Potential 2 . . . . . . . . . . No
Calculation Stop for reevaluation . . . . . Yes
Formula . . . . . . . . . . . . . . R1=Q*C1/m Condition . . . . . . . . . neq=0
Constant . . . . . . . . . . . . . . C1=M*100/z Calculation
Decimal places . . . . . . . . . . . 3 Formula . . . . . . . . . . . . . R1=m/(VEQ*c*C1)
Result unit . . . . . . . . . . . . mg/100g Constant . . . . . . . . . . . . . C1=M/(1000*z)
Result name . . . . . . . . . . . . Vitamin C Decimal places . . . . . . . . . . 3
Statistics . . . . . . . . . . . . . Yes Result unit . . . . . . . . . . .
Calculation Result name . . . . . . . . . . .
Formula . . . . . . . . . . . . . . Statistics . . . . . . . . . . . . Yes
Constant . . . . . . . . . . . . . . Titer
Decimal places . . . . . . . . . . . 0 Titrant . . . . . . . . . . . . . 1/2 DPI
Result unit . . . . . . . . . . . . Concentration [mol/L] . . . . . . 0.01
Result name . . . . . . . . . . . . Formula t = . . . . . . . . . . . x
Statistics . . . . . . . . . . . . . No Report
Calculation Output unit . . . . . . . . . . . Printer
Formula . . . . . . . . . . . . . . Results . . . . . . . . . . . . . No
Constant . . . . . . . . . . . . . . All results . . . . . . . . . . . Yes
Decimal places . . . . . . . . . . . 0
Result unit . . . . . . . . . . . .
Result name . . . . . . . . . . . .
Statistics . . . . . . . . . . . . . No
Report
Output unit . . . . . . . . . . . . Printer
Results . . . . . . . . . . . . . . No
All results . . . . . . . . . . . . Yes