Experiment No.

1
Aim
Calibration of pH meter, TDS and conductivity meter and determination of pH, TDS and
conductivity of a given water sample.

The Experiment No: 1 has been divided into three distinct sections based on their measurable
parameters. The Sections are: Experiment No: 1A, 1B & 1C.

Experiment No. 1A

Aim
To ensure calibration of pH meter and measurement of pH of given water sample.

Principle
Measurement of pH is one of the most important and frequently used tests in water chemistry.
The pH of a solution is measured as negative logarithm of hydrogen ion concentration (Eq.1).
pH= -log [H+] Eq. (1)
Where {H+} is the concentration (or activity) of hydrogen ion (or photon) in moles per liter
(M). At a given temperature, the intensity of the acidic or basic character of a solution is
indicated by pH or hydrogen ion concentration. pH values from 0 to 7 are diminishing acidic,
7 to 14 increasingly alkaline and 7 is neutral. The basic principle of electrometric pH
measurement is determination of the activity of the hydrogen ions by potentiometric
measurement using a standard hydrogen electrode and a reference electrode. Majority of
modern pH electrodes are combination pH electrodes rather than a set of two separate
electrodes. The combination pH electrode is virtually a tube within a tube arrangement. The
inner tube housing the pH indicator electrode (pH sensing membrane, Ag/AgCl reference
electrode, and HCl) and the outer one housing the reference electrode (Ag/AgCl) and its salt
bridge. The pH sensing component of the indicator electrode is a glass bulb. When a pH probe
is immersed in a sample solution, an electrical potential is developed inside and another
electrical potential is developed outside, the difference in the potential is measured and is given
as the pH of the sample.

Calibration of pH meter
To be certain of accurate and reliable measurements, you need to perform pH meter calibration.
This is generally done by measuring different buffer solutions with standardized, well-defined
values, and then adjusting the pH meter based on any deviations from the buffer’s known pH
value. Buffers are solutions that resist changes in pH when small amounts of a strong acid or a
base are added. Because they maintain a constant pH, buffers are good reference solutions.
Calibration should be performed periodically to maintain the pH data quality.

Apparatus
pH meter, Glassware (Beaker)

Reagents

1
Buffer Solutions
• pH 4: It is prepared by dissolving buffer tablet of pH 4 in a 100 mL volumetric flask
and diluting it up to the mark with deionized water. Alternatively, it may be prepared
by dissolving 1.021 g of potassium hydrogen phthalate (KHC8H4O4) in fresh 100 mL
deionized water.
• pH 7: Dissolve a buffer tablet of pH 7 in deionized water in a
100 mL volumetric flask and make up to the mark. Alternatively, dissolve 0.340 g of
potassium hydrogen phosphate (KH2PO4) and 0.355 g disodium hydrogen phosphate
(Na2HPO4) in distilled water in a 100 mL volumetric flask and make up the solution to
the mark.

Procedure
Calibration of pH meter

1. Plug in the meter and let it warm up for five to ten minutes.
2. Put the selector knob to zero pH mode.
3. Rinse the electrode with de-ionized water and blot dry using a piece of tissue.
4. Allow all of the buffers to reach the same temperature, since pH readings are
temperature dependent. If the buffers are not at 25 °C, temperature compensation is
recommended. Measure the temperature of the buffers using thermometer and manually
adjust the “temperature compensation knob” to this temperature. Where, ATC probe is
available the system automatically transmit the temperature of the buffers to the meter.
5. Place the electrode in the solution of pH 7 buffer. It should be ascertained that the glass
electrode membrane is completely immersed in the solution. Electrode should not
touch the sides or the bottom of the beaker. Allow the pH value to stabilize and adjust
'set buffer knob' in a manner that the reading matches with buffer pH. Remove the
electrode from the buffer.
6. Rinse the electrode with de-ionized water and blot dry using a piece of tissue.
7. Place the electrode in the solution of next buffer i.e. pH 4. Follow the step no. 4 until
pH value reaches pH 4. Remove the electrode from the buffer. Similarly, other pH
standard such as 10.1 can be used, depending on the expected sample pH range.
Generally for groundwater sample pH 7.0 and 10.0 should be used for calibration
purpose.
8. Rinse the electrode with de-ionized water and blot dry using a piece of tissue.
9. Now, the instrument is ready to measure pH of unknown sample.

pH Measurement of samples

1. Make sure that the meter is set to the pH mode.

2. Place the electrode in the sample (30-50 mL) to be tested.
3. The pH of the solution appears in the display. Allow the display to stabilize before
taking your reading.
4. Note down the pH and temperature reading.
5. Rinse the pH electrode and place it back in the storage solution.

2
Precautions
1. Make sure to store a pH electrode in its wetting cap containing electrode fill solution (3
M KCl, purchased or prepared by dissolving 22.37 g KCl into 100 mL DI water). Do
not store electrode in DI water.
2. Never touch the membrane of the glass electrode with anything else except soft tissue
paper since it is fragile and is easily ruined if scratched or bumped.
3. Always bring the standards and the sample to the same temperature before
measurement (preferably room temperature).

Observation Table:
Sample No. pH of the sample Temperature of the sample

Results:

Home Work
1. Write down the environmental significance of pH measurement of water samples.

3
 Experiment No. 1B

Aim
To calibrate conductivity meter and measure conductivity of given water sample

Principle
Conductivity, k, is a measure of the ability of an aqueous solution to carry an electric current.
This ability depends on the presence of ions; on their total concentration, mobility, valence and
on the temperature of measurement. Conductivity is customarily reported in micromhos per
centimeter (μmho/cm). Freshly distilled water has a conductivity of 0.5-2 μmho/cm.

Apparatus

Conductivity meter

Reagents
• Conductivity water: Pass distilled water through a mixed bed deionizer and discard first
1000 mL of water. Conductivity of this water should be less than 1 μmho/cm.
• Standard potassium chloride solution, KCl, 0.0100M: Dissolve 745.6 mg anhydrous
KCl in conductivity water and dilute to 1000 mL at 25°C. This is the standard reference
solution, which at 25°C has a conductivity of 1412 μmhos/cm.

Procedure
Calibration and measurement of sample
1. Rinse the electrode thoroughly blot and dry.
2. Immerse the electrode in 0.01M KCL solution and the conductivity should be 1413
micro mhos at 25°C Temperature.
3. Now the instrument is calibrated.
4. Remove the cell from KCL solution and wash it thoroughly with distilled water.
5. Immerse the electrode/cell in the unknown sample whose conductivity is to be
determined.
6. Note down the instrument reading. If the cell constant is given on the cell itself, then
the measured value of conductivity = Cell Constant C × reading of instrument.

Calculation

Conductivity (k) at 25°C

(𝑘𝑚 )
𝑘, μmho/cm =
1 + 0.0191 (𝑡 − 25)

Where,
km = measured conductivity in units of μmho/cm at t °C
t = temperature of measurement

4
Observation Table:
Sample No. Conductivity Temperature

Results:

Home Work
1. Write down the environmental significance of measuring the conductivity water samples.

5
 Experiment No. 1C

Aim
To calibrate TDS meter and measure TDS of given water sample

Principle

Although the basis for testing ppm of total dissolved solids is the conductivity of the solution,
it is not correct to assume that this measurement is absolute. It is always necessary to calibrate
all total dissolved solids meters with a parts per million total dissolved solids standard
calibration solution that contains the same type of salts or mixtures of salts as the solution to
be tested. Failure to do this will result in serious errors in the measurement of total dissolved
solids.

Reagents

Deionised water, NaCl stock solution

Procedure

• Take certain amount (3 g) of NaCl in watch glass and dry it in oven at 120 C for 45
minutes.
• Cool it, and make 20 and 342 ppm solution of NaCl solution (Commercially available
standard solution can also be used).
• Rinse the electrode with deionised water.
• Dip the electrode in 20 ppm solution and wait for the reading to stabilize.
• Next, use 342 ppm solution and adjust the knob to the correct value.
• Rinse the electrode with deionised water and wipe with tissue paper.
• Instrument is calibrated now and ready to be used.
• Now check the TDS of given sample and record the value.

*Alternatively, TDS content can be approximated by multiplying the specific conductance in

micro-Siemens per cm (µS/cm) by an empirical factor varying from 0.55 to 0.90 depending on
the chemical composition of the TDS.

Observation Table:
Sample No. TDS Temperature

6
Results:

Home Work
1. Write down the environmental significance of measuring the TDS of water samples.