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 Electrochemica l Analysis Laboratory Department of Chemical Metrology and Biometry Calibration and Maintenance of Conductivity Meter Create PDF files without this message by purchasing novaPDF printer ( http://www.novapdf.com)

Conductividad

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Conductividad eléctrica, metrologia

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  • Electrochemical Analysis LaboratoryDepartment of Chemical Metrology and Biometry

    Calibration and Maintenance of Conductivity Meter

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  • 2

    Outline

    What is Conductivity?

    How is Conductivity Measured?

    What is Conductive solution?

    Conductivity Meter

    Traceability

    Standard method

    Rules for reliable measurement

    Calibration

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  • 3What is Conductivity?Conductivity is the ability of a solution to pass an

    electric current. The current is carried by cations andanions.

    RG

    1

    The electrical conductance(G, Siemens) is thereciprocal of the resistance(R, Ohm).

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  • 4What is Conductivity?

    A

    lK

    K is the cell constant (m-1)

    l

    A

    l

    AG

    1

    A is the electrode area (m2)l is the electrode gap (m) is the specific conductivity (S/m) is the specific resistance (m)

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  • 5What is Conductivity?

    Solution conducts electricity depends on

    Concentration

    Mobility of ions

    Valence of ions

    Temperature

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  • 6How is Conductivity Measured?

    Conductivity may be measured by applying an

    alternating electrical current (I) to two electrodes

    immersed in a solution and measuring the resulting

    voltage (V).

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  • 7What is Conductive solution?

    Conductivity is measured in aqueous solutions of

    electrolytes.

    Electrolytes are substances containing ions or

    compounds that ionise in solution.

    Strong electrolytes: fully ionised in solution

    Weak electrolytes: not fully ionised in solution

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  • 8What is Conductive solution?

    nCC

    is molar conductance (S cm2 mol-1) is conductivity (S/m)C is concentrationn is charge of ion

    is equivalent conductivity of ion

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  • 9What is Conductive solution?Equivalent conductivity of various ions at 25 oC

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  • 10

    Conductivity value of solution

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  • 11

    What is Conductive solution?

    At the low electrolytic conductivity, the

    relationship between conductivity and concentration is

    linear.

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  • 12

    How is Conductivity Measured?

    The cell constant (K) cannot be determined by

    measuring the electrode gap and area.

    The cell constant is determined using a calibration

    solution with known conductivity (usually 0.01 mol/l

    KCl solution)

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  • 13

    Conductivity Meter

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  • 14

    Conductivity Meter

    The conductivity

    meter uses the conductance

    and cell constant to display

    the conductivity

    Conductivity = cell constant x conductance

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  • 15

    Conductivity Cell

    2 pole cell

    3 pole cell

    4 pole cell

    Platinised cell

    Flow through cell

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  • 16

    Conductivity Cell

    2 pole cell : universal used, interfere with

    polarization

    3 pole cell: better reproducibility

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  • 17

    Conductivity Cell

    4 pole cell: should measure with outer tube

    to minimize volume effect

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  • 18

    Conductivity Cell

    Platinised cell: coated electrode

    with platinum black to increase

    surface area and decrease

    polarization effect.

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  • 19

    Conductivity Cell

    Flow through cell: designed for flow

    system or small volume sample,

    suitable for measurement of

    conductivity of pure water (avoid

    carbon dioxide)

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  • 20

    Storage

    Before storing the cell, rinse with deionised water

    Short-term : deionised water

    Long-term : deionised water or store dry

    After long-term storage, condition the cell for 8 hours in

    deionised water before use.

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  • 21

    Selection of Conductivity Meter

    Factor affecting measurement accuracy

    Formats and units of reports results

    Suitability for the measuring environment

    features assisting ease of use

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  • 22

    Selection of Conductivity Cell

    Advantages Disadvantages

    - Easy to maintain - Field effect cell must be positioned in the middle of measuring vessel

    - Economic - Polarization in high conductivity sample

    - Recommended for viscous sample with suspension

    2 pole cell

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  • 23

    Selection of Conductivity Cell

    Advantages Disadvantages

    - Linear over a very large conductivity range

    - Unsuitable for micro samples

    - Calibration and measurement in different range

    - Ideal for high conductivity measurement

    4 pole cell

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  • 24

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  • 25

    Conductivity Measurement

    The accuracy of conductivity measurements can be influenced by

    Polarization

    Geometry

    Temperature

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  • 26

    Conductivity Measurement

    Polarization

    Polarization occurs on the electrode surface, which leads to errors on result.

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  • 27

    Conductivity Measurement

    Preventing polarization

    increasing the electrode area: coating platinum black on platinum electrode

    Selecting 4 pole conductivity cell

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  • 28

    Conductivity Measurement

    Geometry related errors field effect

    Field linesThese field lines can effect the

    measurement if something

    interferes with the field lines

    such as the sample vessel

    wall.

    This effect can be minimized

    by using 4-pole conductivity

    cell

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  • 29

    Conductivity Measurement

    Temperature

    Conductivity measurements are the temperature

    dependent, varying from 1.5 to 5.5 %/oC

    Temperature increasing - conductivity increasing

    Conductivity meter measures the actual

    conductivity and temperature and then converts

    it to reference temperature using temperature

    correction function

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  • 30

    Conductivity Measurement

    Temperature Temperature correction function

    Linear function

    Non-linear function

    User-Definable temperature compensation

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  • 31

    Temperature correction function

    Linear function

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  • 32

    Determination of the temperature coefficient

    The temperature coefficients of some electrolytes

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  • 33

    Temperature correction function

    Non-linear function

    Non-linear

    compensation data for

    variety of solutions is

    widely available such

    as ISO 7888-1985

    (natural waters)

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  • 34

    Traceability = G K

    Primary cell(defined dimension)

    Primary reference solution

    Secondary cell

    Secondary reference solution

    Electrolytic conductivity meter

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  • 35

    Standard method for Conductivity Measurement of Water

    ASTM D1195 95 (Reapproved 1999) Standard

    Test Methods for Electrical Conductivity and

    Resistivity of Water

    ISO 7888 1985 Water quality Determination of

    electrolytic conductivity

    OIML R 68 Calibration method for conductivity

    cells

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  • 36

    Rules for reliable measurements

    Calibrate frequently: cell constant is an important

    factor for conductivity measurement. Calibration

    interval for conductivity cell will depend on the

    application, sample and operating condition.

    Temperature and stirring conditions: For accurate

    measurement, recommended to use thermostat bath

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  • 37

    Rules for reliable measurements

    Position of conductivity cell: All the pole of

    conductivity cell are covered by the sample and stand

    at the center of sample vessel.

    Low conductivity measurement:

    use a flow through cell, to avoid CO2 from air

    use non-platinised and low cell constant (< 1 cm-1)

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  • 38

    Rules for reliable measurements

    High conductivity measurement:

    use platinised cells to prevent polarization error

    use high cell constant (> 1 cm-1)

    do not dilute sample (conductivity is not

    proportional to concentration at high levels)

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  • 39

    General Condition

    The conductivity of an electrolytic solution may be determined from the measured resistance of the cell, when it contains the solution, and the constant K of the cell

    The value of the cell constant K depends onthe construction of the cellthe temperature and concentration of the

    solutionthe measuring frequencyetc.

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  • 40

    Preparation for Calibration

    check the rigidity of the fixing of the electrode and

    the state of their surface

    the cell shall be degreased with the appropriate

    solvent according to the materials of which the cell

    and electrode are made and then wash with distilled

    water

    the standard solution shall be prepared in quantity

    sufficient for calibration

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  • 41

    Calibration

    the cell shall be washed with standard solution at

    least 5 times

    the solution of the last washing shall be left in the

    cell for 10 minutes

    the cell containing the solution shall be brought in

    thermostat bath at 25 0C and maintain at thermal

    equilibrium

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  • 42

    Calibration

    the cell shall be washed with standard solution at

    least 5 times

    the solution of the last washing shall be left in

    the cell for 10 minutes

    the cell containing the solution shall be brought

    in thermostat bath at 25 0C and maintain at thermal

    equilibrium

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  • 43

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