METTLER TOLEDO

M574

Content of Sulphate in Mineral Water

Method for the determination of sulphate content in water by precipitation titration with BaCl2 using a Barium selective electrode Sample
Mineral water, 5 mL

Preparation and Procedures

The sample is placed in an ultrasonic bath during 30 minutes to degas the mineral water. Then it is passed through a strong acid cation exchanger (Merck LAB ion exchanger I) to remove the ions that might interfere. 5 mL of the prepared mineral water are mixed with 40 mL deionised water, 8 mL isopropanol and 2 mL lithium acetate buffer. Preparation of the lithium acetate buffer: Dissolve 10.2 g lithium acetate dihydrate (analytical reagent grade) in approx. 500 mL H2O in a beaker. Add 5.7 mL glacial acetic acid while stirring. Transfer the solution to a 1 L-measuring flask and fill up to the mark with water.

Substance Chemicals

Sulphate (SO42-) z=2 Water

M = 96.06 g/mol;

Titrant

Barium chloride mol/L;

c(BaCl2) = 0.01

Standard Instruments

Ammonium sulphate (NH4)2SO4 DL58; Sample Changer ST20A, Balance AT 261, Printer HP Deskjet 500 Titration beaker ME 101974

Accessories

Remarks Indication Chemistry

Barium-selective electrode DX200 reference electrode
This method allows the determination of the sulphate concentration in mineral water. When all the sulphate is precipitated as BaSO4, the barium-selective electrode registers the free Ba2+-ions in the solution with a potential change. Predispensing is not always possible as it may lead to disturbances of the signal and hence generate problems in the recognition of the equivalence point. Maintenance Since a fine layer of BaSO4 is formed during titration, the electrode must be conditioned in H2O after each titration. In addition to that, the electrode was cleaned in HCl 0.1 mol/L after each series of titration. DX200 reference electrode outer bridge solution: 0.1 M NaNO3

Calculation

Results

Waste disposal

The precipitate (BaSO4) has to be classified as special waste.

Author

K. Schaetti

Results
METTLER TOLEDO DL58 Titrator 58 V2.0 Mettler-Toledo GmbH Market Support Laboratory 26-Mar-1997 18:59

Method Measured User RESULTS No. 1 ID

MT073 SO42--Determination 26-Mar-1997 22:37 K. Schaetti

Sample size and results 3.0 R1 = 0.932 R2 = 0.010 R3 = 3.504 3.0 R1 = 0.904 R2 = 0.009 R3 = 3.399 3.0 R1 = 0.937 R2 = 0.010 R3 = 3.520 3.0 R1 = 0.811 R2 = 0.008 R3 = 3.050 3.0 R1 = 0.894 R2 = 0.009 R3 = 3.360 3.0 R1 = 0.898 R2 = 0.009 R3 = 3.375 mL g/L mol/L mL mL g/L mol/L mL mL g/L mol/L mL mL g/L mol/L mL mL g/L mol/L mL mL g/L mol/L mL Content Concentration Consumption Content Concentration Consumption Content Concentration Consumption Content Concentration Consumption Content Concentration Consumption Content Concentration Consumption

Sulphate

Sulphate

Sulphate

Sulphate

Sulphate

Sulphate

STATISTICS Number of results R1 Mean value Standard deviation Rel. standard deviation

n x s srel

= = = =

6 0.896 mol/L 0.04516 5.039 %

Content mol/L Content

Table of measured values

Titration curve

Method
Method MT073 Version SO42--Determination 26-Mar-1997 18:59 . MT073 . SO42--Determination . 26-Mar-1997 18:59 . . . . . . . . . . . . . . Sulphate Fixed volume 3.0 96.06 1 ST20A No No No Yes 10 1 No Manual Title Method ID . . . . . . . . . . Title . . . . . . . . . . . . Date/time . . . . . . . . . . Sample Sample ID . . . . . . . . . . Entry type . . . . . . . . . . Volume [mL] . . . . . . . . Molar mass M . . . . . . . . . Equivalent number z . . . . . Titration stand . . . . . . . Pump . . . . . . . . . . . Pump . . . . . . . . . . . Rinse . . . . . . . . . . . Conditioning . . . . . . . Time [s] . . . . . . . . Interval . . . . . . . . Rinse . . . . . . . . . Temperature sensor . . . . . . Stir Speed [%] . . . . . . . . . . . Time [s]. . . . . . . . . . . . EQP titration Titrant/Sensor Titrant. . . . . . . . . . . Concentration [mol/L]. . . . Sensor . . . . . . . . . . . Unit of meas . . . . . . . . Predispensing . . . . . . . . . Titrant addition. . . . . . . . dV [mL]. . . . . . . . . . . Measure mode. . . . . . . . . . dE [mV]. . . . . . . . . . . dt [s] . . . . . . . . . . . t(min) [s] . . . . . . . . . t(max) [s] . . . . . . . . . Recognition Threshold. . . . . . . . . . Steepest jump only . . . . . Range. . . . . . . . . . . . Tendency . . . . . . . . . . Termination at maximum volume [mL] . . . at potential . . . . . . . . at slope . . . . . . . . . . after number EQPs. . . . . . comb. termination conditions Evaluation Procedure. . . . . . . . . . Potential 1. . . . . . . . . Potential 2. . . . . . . . . Stop for reevaluation. . . . Calculation Formula . . . . . . . . . . . . Constant. . . . . . . . . . . . Decimal places. . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics. . . . . . . . . . . Calculation Formula. . . . . . . . . . . . . Constant. . . . . . . . . . . . Decimal places. . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics. . . . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant. . . . . . . . . . . . Decimal places. . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics. . . . . . . . . . . Report Output. . . . . . Results . . . . . All results . . . Raw results . . . Table of measured Sample data . . . E - V curve . . . . . . . . . . . . . . . . . . . values. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Printer No Yes No Yes No Yes

. 50 . 600 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . BaCl2 0.01 Barium-ISE mV No Incremental 0.05 Equilibrium controlled 0.25 2.0 15.0 60.0 5.0 Yes No None 6.0 No No No No Asymmetric No No No R1=Q*C1/m C1=M/z 3 g/L Content Yes

. R2=Q/m . . . . 3 mol/L Concentration No

. R3=VEQ . . . . 3 mL Consumption No