METTLER TOLEDO Application No.

M574

Content of Sulphate in Mineral Water

Sample: Mineral water, 5 mL Instruments: METTLER TOLEDO DL58

Sample Changer ST20A
Compound: Sulphate (SO42-) Balance METTLER AT 261
M = 96.06 g/mol; z = 1 Printer HP Deskjet 500

Preparations: See remarks Method: MT073

Titrant: Barium chloride Accessories: Titration beaker ME 101974

c(BaCl2) = 0.01 mol/L
Indication: Barium-selective electrode,
Standard: Ammonium sulphate (NH4)2SO4 e.g. DX337-Ba2+
DX200 reference electrode
(outer bridge sol.: 4 M KCl)

Results: METTLER TOLEDO DL58 Titrator V2.0 Mettler-Toledo GmbH

58 Market Support Laboratory

Method MT073 SO42--Determination 26-Mar-1997 18:59

Measured 26-Mar-1997 22:37
User K. Schaetti

ALL RESULTS

No. ID Sample size and results

1 Sulphate 3.0 mL
R1 = 0.932 g/L Content
R2 = 0.010 mol/L Concentration
R3 = 3.504 mL Consumption
2 Sulphate 3.0 mL
R1 = 0.904 g/L Content
R2 = 0.009 mol/L Concentration
R3 = 3.399 mL Consumption
3 Sulphate 3.0 mL
R1 = 0.937 g/L Content
R2 = 0.010 mol/L Concentration
R3 = 3.520 mL Consumption
4 Sulphate 3.0 mL
R1 = 0.811 g/L Content
R2 = 0.008 mol/L Concentration
R3 = 3.050 mL Consumption
5 Sulphate 3.0 mL
R1 = 0.894 g/L Content
R2 = 0.009 mol/L Concentration
R3 = 3.360 mL Consumption
6 Sulphate 3.0 mL
R1 = 0.898 g/L Content
R2 = 0.009 mol/L Concentration
R3 = 3.375 mL Consumption

STATISTICS
Number of results R1 n = 6
Mean value x = 0.896 mol/L Content
Standard deviation s = 0.04516 mol/L Content
Rel. standard deviation srel = 5.039 %

Page 32/40 METTLER TOLEDO Beverage Determinations with Standard Methods

Method
Method MT073 SO42--Determination Report
Version 26-Mar-1997 18:59 Output. . . . . . . . . . . . . Printer
Results . . . . . . . . . . . . No
Title All results . . . . . . . . . . Yes
Method ID . . . . . . . . . . . MT073 Raw results . . . . . . . . . . No
Title . . . . . . . . . . . . . SO42--Deter- Table of measured values. . . . Yes
mination Sample data . . . . . . . . . . No
Date/time . . . . . . . . . . . 26-Mar-1997 E - V curve . . . . . . . . . . Yes
18:59 dE/dV - V curve . . . . . . . . No
Sample d2E/dV2 - V curve . . . . . . . No
Sample ID . . . . . . . . . . . Sulphate
Entry type . . . . . . . . . . . Fixed volume
Volume [mL] . . . . . . . . . 3.0
Molar mass M . . . . . . . . . . 96.06
Equivalent number z . . . . . . 1
Remarks
Titration stand . . . . . . . . ST20A
Pump . . . . . . . . . . . . No Method
Pump . . . . . . . . . . . . No
Rinse . . . . . . . . . . . . No This method allows the determination of the sulphate
Conditioning . . . . . . . . Yes
Time [s] . . . . . . . . . 10 concentration in mineral water. When all the sulphate
Interval . . . . . . . . . 1 is precipitated as BaSO4, the barium-selective elec-
Rinse . . . . . . . . . . No
Temperature sensor . . . . . . . Manual trode registers the free Ba2+-ions in the solution with
Stir a potential change.
Speed [%] . . . . . . . . . . . . 50
Time [s]. . . . . . . . . . . . . 600 Predispensing is not always possible as it may lead to
EQP titration
Titrant/Sensor
disturbances of the signal and hence generate prob-
Titrant. . . . . . . . . . . . BaCl2 lems in the recognition of the equivalence point.
Concentration [mol/L]. . . . . 0.01
Sensor . . . . . . . . . . . . Barium-ISE Maintenance
Unit of meas . . . . . . . . . mV
Predispensing . . . . . . . . . . No Since a fine layer of BaSO4 is formed during titration,
Titrant addition. . . . . . . . . Incremental
dV [mL]. . . . . . . . . . . . 0.05 the electrode must be conditioned in H2O after each
Measure mode. . . . . . . . . . . Equilibrium
controlled
titration. In addition to that, the electrode was cleaned
dE [mV]. . . . . . . . . . . . 0.25 in HCl 0.1 mol/L after each series of titration.
dt [s] . . . . . . . . . . . . 2.0
t(min) [s] . . . . . . . . . . 15.0
t(max) [s] . . . . . . . . . . 60.0
Preparation
Recognition
Threshold. . . . . . . . . . . 5.0
The sample is placed in an ultrasonic bath during 30
Steepest jump only . . . . . . Yes minutes to degas the mineral water.
Range. . . . . . . . . . . . . No
Tendency . . . . . . . . . . . None
Then it is passed through a strong acid cation exchang-
Termination er (Merck LAB ion exchanger I) to remove the ions
at maximum volume [mL] . . . . 6.0
at potential . . . . . . . . . No that might interfere.
at slope . . . . . . . . . . . No 5 mL of the prepared mineral water are mixed with
after number EQPs. . . . . . . No
comb. termination conditions . No 40 mL deionised water, 8 mL isopropanol and 2 mL
Evaluation lithium acetate buffer.
Procedure. . . . . . . . . . . Asymmetric
Potential 1. . . . . . . . . . No Preparation of the lithium acetate buffer:
Potential 2. . . . . . . . . . No
Stop for reevaluation. . . . . No Dissolve 10.2 g lithium acetate dihydrate (analytical
Calculation reagent grade) in approx. 500 mL H2O in a beaker.
Formula . . . . . . . . . . . . . R1=Q*C1/m
Constant. . . . . . . . . . . . . C1=M/z Add 5.7 mL glacial acetic acid while stirring. Trans-
Decimal places. . . . . . . . . . 3
Result unit . . . . . . . . . . . g/L
fer the solution to a 1 L-measuring flask and fill up to
Result name . . . . . . . . . . . Content the mark with water.
Statistics. . . . . . . . . . . . Yes
Calculation Waste disposal
Formula. . . . . . . . . . . . . . R2=Q/m
Constant. . . . . . . . . . . .
Decimal places. . . . . . . . . . 3
The precipitate (BaSO4) has to be classified as special
Result unit . . . . . . . . . . . mol/L waste.
Result name . . . . . . . . . . . Concentration
Statistics. . . . . . . . . . . . No
Calculation
Other titrators
Formula . . . . . . . . . . . . . R3=VEQ Method MT073 also works with the following titra-
Constant. . . . . . . . . . . .
Decimal places. . . . . . . . . . 3 tors:
Result unit . . . . . . . . . . . mL
Result name . . . . . . . . . . . Consumption
DL50, DL53, DL55, DL67, DL70ES, DL77.
Statistics. . . . . . . . . . . . No
Author: K. Schaetti

Beverage Determinations with Standard Methods METTLER TOLEDO Page 33/40

METTLER TOLEDO Application No. M575

Titer Determination of BaCl2 0.1 mol/L

Sample: Ammonium sulphate, 40 mg Instruments: METTLER TOLEDO DL58

Sample Changer ST20A
Compound: Sulphate (SO42-) Balance METTLER AT 261
M = 96.06 g/mol; z = 1 Printer HP Deskjet 500

Preparations: See remarks Method: MT074

Titrant: Barium chloride Accessories: Titration beaker ME 101974

c(BaCl2) = 0.1 mol/L
Indication: Barium-selective electrode,
e.g. DX337-Ba2+
DX200 reference electrode
(outer bridge sol.: 4 M KCl)

Results: METTLER TOLEDO DL58 Titrator V2.0 Mettler-Toledo GmbH

58 Market Support Laboratory

Method MT074 Titer Determination BaCl2 09-Apr-1997 11:47

Measured 09-Apr-1997 14:18
User K. Schaetti

ALL RESULTS

No. ID Sample size and results

1 Sulphate 0.0351 g
R1 = 1.3048 Titer
2 Sulphate 0.0424 g
R1 = 1.1931 Titer
3 Sulphate 0.0352 g
R1 = 1.1701 Titer
4 Sulphate 0.0351 g
R1 = 1.1783 Titer
5 Sulphate 0.0348 g
R1 = 1.1328 Titer
6 Sulphate 0.0427 g
R1 = 1.1954 Titer

STATISTICS
Number of results R1 n = 6
Mean value x = 1.1957 Titer
Standard deviation s = 0.05802 Titer
Rel. standard deviation srel = 4.852 %

TITER
Titrant BaCl2 0.1 mol/L
New Titer t = 1.19568

Page 34/40 METTLER TOLEDO Beverage Determinations with Standard Methods

Method for the standardisation of BaCl2
Method MT074 Titer Determination BaCl2 Report
Version 09-Apr-1997 11:47 Output . . . . . . . . . . . . . Printer
Results . . . . . . . . . . . . No
Title All results . . . . . . . . . . Yes
Method ID . . . . . . . . . . . MT074 Raw results . . . . . . . . . . No
Title . . . . . . . . . . . . . Titer Table of measured values . . . . Yes
Determina- Sample data . . . . . . . . . . No
tion BaCl2 E - V curve . . . . . . . . . . Yes
Date/time . . . . . . . . . . . 09-Apr-97 dE/dV - V curve . . . . . . . . No
11:47 d2E/dV2 - V curve . . . . . . . No
Sample log dE/dV - V curve . . . . . . No
Sample ID . . . . . . . . . . . Sulphate E - t curve . . . . . . . . . . No
Entry type . . . . . . . . . . . Weight V - t curve . . . . . . . . . . No
Lower limit [g] . . . . . . . 0.0 dV/dt - t curve . . . . . . . . No
Upper limit [g] . . . . . . . 2.0
Molar mass M . . . . . . . . . . 96.06
Equivalent number z . . . . . . 1 Remarks
Titration stand . . . . . . . . ST20A
Pump . . . . . . . . . . . . No
Pump . . . . . . . . . . . . No
Preparations
Rinse . . . . . . . . . . . . No
Conditioning . . . . . . . . Yes
Approx. 40 mg ammonium sulphate are diluted
Time [s] . . . . . . . . . 10 in 40 mL deionised water. After adding 8 mL iso-
Interval . . . . . . . . . 1
Rinse . . . . . . . . . . No
propanol and 2 mL lithium acetate buffer (see
Temperature sensor . . . . . . . Manual p. 33) the solution is titrated with BaCl2 (c(BaCl2)
Stir
Speed [%] . . . . . . . . . . . 50
= 0.1 mol/L) to determine the titer factor.
Time [s] . . . . . . . . . . . . 600
EQP titration Method
Titrant/Sensor
Titrant . . . . . . . . . . . BaCl2 This standardisation is carried out with a barium-
Concentration [mol/L] . . . . 0.1 selective electrode.
Sensor . . . . . . . . . . . Barium-ISE
Unit of meas. . . . . . . . . mV The mean value of the titer is automatically stored
Predispensing . . . . . . . . . No as part of the setup data by the function TITER.
Titrant addition . . . . . . . . Incremental
dV [mL] . . . . . . . . . . . 0.1 Asymmetric evaluation is used, as the titration
Measure mode . . . . . . . . . . Equilibr. forms a typical asymmetric curve.
controlled
dE [mV] . . . . . . . . . . . 0.25
dt [s] . . . . . . . . . . . 2.0
Titration curve
t(min) [s] . . . . . . . . . 15.0
t(max) [s] . . . . . . . . . 60.0
Recognition
Threshold . . . . . . . . . . 5.0
Steepest jump only . . . . . Yes
Range . . . . . . . . . . . . No
Tendency . . . . . . . . . . None
Termination
at maximum volume [mL] . . . 6.0
at potential . . . . . . . . No
at slope . . . . . . . . . . No
after number EQPs . . . . . . No
comb. termination conditions No
Evaluation
Procedure . . . . . . . . . . Asymmetric
Potential 1 . . . . . . . . . No Waste disposal
Potential 2 . . . . . . . . . No
Stop for reevaluation . . . . No The precipitate (BaSO4) must be treated as spe-
Calculation cial waste.
Formula . . . . . . . . . . . . R=m/(VEQ*c*C)
Constant . . . . . . . . . . . . C=M/(1000*z)
Decimal places . . . . . . . . . 4 Other titrators
Result unit . . . . . . . . . .
Result name . . . . . . . . . . Titer
Method MT074 also works with the following ti-
Statistics . . . . . . . . . . . Yes trators:
Titer
Titrant . . . . . . . . . . . . . BaCl2
DL50, DL53, DL55, DL67, DL70ES, DL77.
Concentration [mol/L] . . . . . . 0.1
Formula t = . . . . . . . . . . . x
Author: K. Schaetti

Beverage Determinations with Standard Methods METTLER TOLEDO Page 35/40

Literature

[1] Fundamentals of Titration, Mettler-Toledo GmbH, ME-704153A, 1993

[2] Standardization of Titrants, Mettler-Toledo Applications Brochure No. 8 (ME-51724650) and 9
(ME-51724652)
[3] Primary volumetric standards, E. Merck, Darmstadt, D
[4] Encyclopedia of Weighing, Mettler-Toledo GmbH, ME-720113
[5] Swiss Food Manual, 5th Ed., Eidg. Drucksachen- und Materialzentrale Bern, 1993

Page 36/40 METTLER TOLEDO Beverage Determinations with Standard Methods