24.10.2014 Views

Calibration and Maintenance of Conductivity Meter

Calibration and Maintenance of Conductivity Meter

Calibration and Maintenance of Conductivity Meter

SHOW MORE
SHOW LESS

You also want an ePaper? Increase the reach of your titles

YUMPU automatically turns print PDFs into web optimized ePapers that Google loves.

<strong>Calibration</strong> <strong>and</strong> <strong>Maintenance</strong><br />

<strong>of</strong> <strong>Conductivity</strong> <strong>Meter</strong><br />

Electrochemical Analysis Laboratory<br />

Department <strong>of</strong> Chemical Metrology <strong>and</strong> Biometry<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


อย่ากลัวทีจะก้าวไปใช้ชีวิตตามความใฝ่ ฝัน เราไม่ได้เกิดเป็นคนกันบ่อยครั งนัก ด้วยเหตุนั น จงใช้ศักยภา<br />

พของชีวิตนี ไปในทางสร้างสรรค์ให้คุ้มค่าทีสุด<br />

Outline<br />

What is <strong>Conductivity</strong>?<br />

How is <strong>Conductivity</strong> Measured?<br />

What is Conductive solution?<br />

<strong>Conductivity</strong> <strong>Meter</strong><br />

Traceability<br />

St<strong>and</strong>ard method<br />

Rules for reliable measurement<br />

<strong>Calibration</strong><br />

2<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


What is <strong>Conductivity</strong>?<br />

<strong>Conductivity</strong> is the ability <strong>of</strong> a solution to pass an<br />

electric current. The current is carried by cations <strong>and</strong><br />

anions.<br />

G <br />

1<br />

R<br />

The electrical conductance<br />

(G, Siemens) is the<br />

reciprocal <strong>of</strong> the resistance<br />

(R, Ohm).<br />

3<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


What is <strong>Conductivity</strong>?<br />

G<br />

<br />

K <br />

A<br />

l<br />

l<br />

A<br />

<br />

1<br />

<br />

<br />

K is the cell constant (m -1 )<br />

A<br />

l<br />

A is the electrode area (m 2 )<br />

l is the electrode gap (m)<br />

is the specific conductivity (S/m)<br />

is the specific resistance (m)<br />

4<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


What is <strong>Conductivity</strong>?<br />

Solution conducts electricity depends on<br />

• Concentration<br />

• Mobility <strong>of</strong> ions<br />

• Valence <strong>of</strong> ions<br />

• Temperature<br />

5<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


How is <strong>Conductivity</strong> Measured?<br />

<strong>Conductivity</strong> may be measured by applying an<br />

alternating electrical current (I) to two electrodes<br />

immersed in a solution <strong>and</strong> measuring the resulting<br />

voltage (V).<br />

6<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


What is Conductive solution?<br />

<strong>Conductivity</strong> is measured in aqueous solutions <strong>of</strong><br />

electrolytes.<br />

Electrolytes are substances containing ions or<br />

compounds that ionise in solution.<br />

• Strong electrolytes: fully ionised in solution<br />

• Weak electrolytes: not fully ionised in solution<br />

7<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


What is Conductive solution?<br />

<br />

<br />

C C n<br />

is molar conductance (S cm 2 mol -1 )<br />

is conductivity (S/m)<br />

C is concentration<br />

n is charge <strong>of</strong> ion<br />

<br />

<br />

<br />

<br />

<br />

is equivalent conductivity <strong>of</strong> ion<br />

<br />

8<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


What is Conductive solution?<br />

Equivalent conductivity <strong>of</strong> various ions at 25 o C<br />

9<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Conductivity</strong> value <strong>of</strong> solution<br />

10<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


What is Conductive solution?<br />

At the low electrolytic conductivity, the<br />

relationship between conductivity <strong>and</strong> concentration is<br />

linear.<br />

11<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


How is <strong>Conductivity</strong> Measured?<br />

The cell constant (K) cannot be determined by<br />

measuring the electrode gap <strong>and</strong> area.<br />

The cell constant is determined using a calibration<br />

solution with known conductivity (usually 0.01 mol/l<br />

KCl solution)<br />

12<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Conductivity</strong> <strong>Meter</strong><br />

13<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Conductivity</strong> <strong>Meter</strong><br />

The conductivity<br />

meter uses the conductance<br />

<strong>and</strong> cell constant to display<br />

the conductivity<br />

<strong>Conductivity</strong> = cell constant x conductance<br />

14<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Conductivity</strong> Cell<br />

• 2 – pole cell<br />

• 3 – pole cell<br />

• 4 – pole cell<br />

• Platinised cell<br />

• Flow through cell<br />

15<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Conductivity</strong> Cell<br />

• 2 – pole cell : universal used, interfere with<br />

polarization<br />

• 3 – pole cell: better reproducibility<br />

16<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Conductivity</strong> Cell<br />

• 4 – pole cell: should measure with outer tube<br />

to minimize volume effect<br />

17<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Conductivity</strong> Cell<br />

• Platinised cell: coated electrode<br />

with platinum black to increase<br />

surface area <strong>and</strong> decrease<br />

polarization effect.<br />

18<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Conductivity</strong> Cell<br />

• Flow through cell: designed for flow<br />

system or small volume sample,<br />

suitable for measurement <strong>of</strong><br />

conductivity <strong>of</strong> pure water (avoid<br />

carbon dioxide)<br />

19<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


Storage<br />

Before storing the cell, rinse with deionised water<br />

• Short-term : deionised water<br />

• Long-term : deionised water or store dry<br />

After long-term storage, condition the cell for 8 hours in<br />

deionised water before use.<br />

20<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


Selection <strong>of</strong> <strong>Conductivity</strong> <strong>Meter</strong><br />

• Factor affecting measurement accuracy<br />

• Formats <strong>and</strong> units <strong>of</strong> reports results<br />

• Suitability for the measuring environment<br />

• features assisting ease <strong>of</strong> use<br />

21<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


Selection <strong>of</strong> <strong>Conductivity</strong> Cell<br />

• 2 – pole cell<br />

Advantages<br />

Disadvantages<br />

- Easy to maintain - Field effect – cell must<br />

be positioned in the middle<br />

<strong>of</strong> measuring vessel<br />

- Economic - Polarization in high<br />

conductivity sample<br />

- Recommended for<br />

viscous sample with<br />

suspension<br />

22<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


Selection <strong>of</strong> <strong>Conductivity</strong> Cell<br />

• 4 – pole cell<br />

Advantages<br />

- Linear over a very large<br />

conductivity range<br />

- <strong>Calibration</strong> <strong>and</strong><br />

measurement in different<br />

range<br />

- Ideal for high<br />

conductivity measurement<br />

Disadvantages<br />

- Unsuitable for micro<br />

samples<br />

23<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)<br />

24


<strong>Conductivity</strong> Measurement<br />

The accuracy <strong>of</strong> conductivity measurements can be<br />

influenced by<br />

• Polarization<br />

• Geometry<br />

• Temperature<br />

25<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Conductivity</strong> Measurement<br />

• Polarization<br />

Polarization occurs on the electrode surface,<br />

which leads to errors on result.<br />

26<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Conductivity</strong> Measurement<br />

Preventing polarization<br />

• increasing the electrode area: coating platinum<br />

black on platinum electrode<br />

• Selecting 4 – pole conductivity cell<br />

27<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Conductivity</strong> Measurement<br />

• Geometry related errors – field effect<br />

Field lines<br />

These field lines can effect the<br />

measurement if something<br />

interferes with the field lines<br />

such as the sample vessel<br />

wall.<br />

This effect can be minimized<br />

by using 4-pole conductivity<br />

cell<br />

28<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Conductivity</strong> Measurement<br />

• Temperature<br />

<strong>Conductivity</strong> measurements are the temperature<br />

dependent, varying from 1.5 to 5.5 %/ o C<br />

Temperature increasing - conductivity increasing<br />

<strong>Conductivity</strong> meter measures the actual<br />

conductivity <strong>and</strong> temperature <strong>and</strong> then converts<br />

it to reference temperature using temperature<br />

correction function<br />

29<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Conductivity</strong> Measurement<br />

• Temperature<br />

Temperature correction function<br />

• Linear function<br />

• Non-linear function<br />

• User-Definable temperature compensation<br />

30<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


Temperature correction function<br />

• Linear function<br />

31<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


Determination <strong>of</strong> the temperature coefficient<br />

The temperature coefficients <strong>of</strong> some electrolytes<br />

32<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


Temperature correction function<br />

• Non-linear function<br />

Non-linear<br />

compensation data for<br />

variety <strong>of</strong> solutions is<br />

widely available such<br />

as ISO 7888-1985<br />

(natural waters)<br />

33<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


Traceability<br />

= G K<br />

Primary reference solution<br />

Primary cell<br />

(defined dimension)<br />

Secondary cell<br />

Secondary reference solution<br />

Electrolytic conductivity meter<br />

34<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


St<strong>and</strong>ard method for <strong>Conductivity</strong><br />

Measurement <strong>of</strong> Water<br />

• ASTM D1195 – 95 (Reapproved 1999) St<strong>and</strong>ard<br />

Test Methods for Electrical<br />

Resistivity <strong>of</strong> Water<br />

<strong>Conductivity</strong> <strong>and</strong><br />

• ISO 7888 – 1985 Water quality – Determination <strong>of</strong><br />

electrolytic conductivity<br />

• OIML R 68 <strong>Calibration</strong> method for conductivity<br />

cells<br />

35<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


Rules for reliable measurements<br />

• Calibrate frequently: cell constant is an important<br />

factor for conductivity measurement. <strong>Calibration</strong><br />

interval for conductivity cell will depend on the<br />

application, sample <strong>and</strong> operating condition.<br />

• Temperature <strong>and</strong> stirring conditions: For accurate<br />

measurement, recommended to use thermostat bath<br />

36<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


Rules for reliable measurements<br />

• Position <strong>of</strong> conductivity cell: All the pole <strong>of</strong><br />

conductivity cell are covered by the sample <strong>and</strong> st<strong>and</strong><br />

at the center <strong>of</strong> sample vessel.<br />

• Low conductivity measurement:<br />

• use a flow through cell, to avoid CO 2 from air<br />

• use non-platinised <strong>and</strong> low cell constant (< 1 cm -1 )<br />

37<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


Rules for reliable measurements<br />

• High conductivity measurement:<br />

• use platinised cells to prevent polarization error<br />

• use high cell constant (> 1 cm -1 )<br />

• do not dilute sample (conductivity is not<br />

proportional to concentration at high levels)<br />

38<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


General Condition<br />

• The conductivity <strong>of</strong> an electrolytic solution may be<br />

determined from the measured resistance <strong>of</strong> the cell,<br />

when it contains the solution, <strong>and</strong> the constant K <strong>of</strong><br />

the cell<br />

• The value <strong>of</strong> the cell constant K depends on<br />

the construction <strong>of</strong> the cell<br />

the temperature <strong>and</strong> concentration <strong>of</strong> the<br />

solution<br />

the measuring frequency<br />

etc.<br />

39<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


Preparation for <strong>Calibration</strong><br />

check the rigidity <strong>of</strong> the fixing <strong>of</strong> the electrode <strong>and</strong><br />

the state <strong>of</strong> their surface<br />

the cell shall be degreased with the appropriate<br />

solvent according to the materials <strong>of</strong> which the cell<br />

<strong>and</strong> electrode are made <strong>and</strong> then wash with distilled<br />

water<br />

the st<strong>and</strong>ard solution shall be prepared in quantity<br />

sufficient for calibration<br />

40<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Calibration</strong><br />

the cell shall be washed with st<strong>and</strong>ard solution at<br />

least 5 times<br />

the solution <strong>of</strong> the last washing shall be left in the<br />

cell for 10 minutes<br />

the cell containing the solution shall be brought in<br />

thermostat bath at 25 0 C <strong>and</strong> maintain at thermal<br />

equilibrium<br />

41<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


<strong>Calibration</strong><br />

the cell shall be washed with st<strong>and</strong>ard solution at<br />

least 5 times<br />

the solution <strong>of</strong> the last washing shall be left in<br />

the cell for 10 minutes<br />

the cell containing the solution shall be brought<br />

in thermostat bath at 25 0 C <strong>and</strong> maintain at thermal<br />

equilibrium<br />

42<br />

Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)


Create PDF files without this message by purchasing novaPDF printer (http://www.novapdf.com)<br />

43

Hooray! Your file is uploaded and ready to be published.

Saved successfully!

Ooh no, something went wrong!