FACULTY : ENGINEERING

TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT:
DETERMINATION OF
ALKALINITY

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2016

AMENDMENT DATE:

FACULTY OF ENGINEERING TECHNOLOGY

DEPARTMENT OF CIVIL ENGINEERING TECHNOLOGY

INTRODUCTION TO ENVIRONMENTAL ENGINEERING

TECHNOLOGY LABORATORY
LABORATORY INSTRUCTION SHEETS
COURSE CODE

BNP 21403

EXPERIMENT CODE

EXPERIMENT 7

EXPERIMENT TITLE

DETERMINATION OF ALKALINITY

DATE
GROUP NO.
LECTURER/INSTRUCTOR/TUTOR

1)
2)

DATE OF REPORT SUBMISSION

DISTRIBUTION OF MARKS FOR

LABORATORY REPORT

EXAMINER COMMENTS:

ATTENDANCE/PARTICIPATION/DISIPLINE:

/5%

INTRODUCTION:

/5%

PROCEDURE:

/5%

RESULTS & CALCULATIONS

/15%

ANALYSIS

/15%

DISCUSSIONS:

/20%

ADDITIONAL QUESTIONS

/15%

CONCLUSION

/10%

SUGGESTIONS & RECOMENDATIONS

/5%

REFERENCES:

/5%

TOTAL:

/100%

RECEIVED DATE AND STAMP:

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT:
DETERMINATION OF
ALKALINITY

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2016

AMENDMENT DATE:

STUDENT CODE OF ETHICS

DEPARTMENT OF CIVIL ENGINEERING TECHNOLOGY

FACULTY OF ENGINEERING TECHNOLOGY

I hereby declare that I have prepared this report with my own efforts. I also admit to
not accept or provide any assistance in preparing this report and anything that is in it
is true.
1) Group Leader
Name
:
Matrix No. :

__________________________________________(Signature)
__________________________________
__________________________________

2) Group Member 1
Name
:
Matrix No :

__________________________________________(Signature)
__________________________________
___________________________________

3) Group Member 2
Name
:
Matrix No. :

__________________________________________(Signature)
__________________________________
__________________________________

4) Group Member 3
Name
:
Matrix No. :

__________________________________________(Signature)
__________________________________
__________________________________

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT:
DETERMINATION OF
ALKALINITY

1.0

EDITION:
2

REVISION NO:

FEB
2016

EFFECTIVE DATE:
AMENDMENT DATE:

OBJECTIVES
a)

To determine the alkalinity of a water sample using analytical method

(indicator method) double endpoint; phenolphthalein endpoint (pH 8.3)
and methyl orange endpoint (pH 4.5) titration.

2.0

LEARNING OUTCOMES
At the end of this course students are able to:
a) the student be able to describe the importance of alkalinity in the
environmental studies.
b) the students be able to measure the alkalinity of samples

3.0

INTRODUCTION

3.1 Alkalinity is a parameter that is measured on almost all environmental

samples -drinking water, natural waters, polluted waters, sewage, and
industrial wastes. Alkalinity refers to the buffering capacity of water samples
and to their ability to neutralize acidic pollution from rainfall or wastewater.
For municipal sewage or industrial wastes, the amount of alkalinity is
important in determining the type of treatment which should be employed.

3.2 Alkalinity is primarily caused by the presence of carbonate (C0 2-3) and
bicarbonate

(HCO-3)

ions,

although

hydroxide

(OH-)

ions

may

also

contribute, especially when there is industrial pollution. It is measured

volumetrically by titration with 0.05 N sulphuric acid and is reported in
terms of CaCO3 equivalent. For samples whose initial pH is above 8.3, the
titration is conducted in two steps.

3.3 In the first step, the titration is conducted until the pH is lowered to 8.2, the
point at which phenolphthalein indicator turns from pink to colourless. This
value corresponds to the points for conversion of carbonate to bicarbonate
ion.

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT:
DETERMINATION OF
ALKALINITY

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2016

AMENDMENT DATE:

3.4 The second phase of titration is conducted until the pH is lowered to 4.5,
corresponds to methyl orange end point, which corresponds to the
equivalence points for the conversion of bicarbonate ion to carbonic acid.

3.5

Living organisms, such as aquatic life, function best in a pH range of 5.0 to

9.0 and levels of 20 to 200 mg/L are typical alkalinity values for fresh water.
When the pH is above 8.3, carbonate (CO2-3) is the primary contributor to
alkalinity; when the pH is below 8.3, bicarbonate (HCO -3) becomes the
dominating factor. The values of alkalinity are reported in units of "mg
CaCO3/L" because of its relationship to hardness, which is reported using
the same unit.

4.0

INSTRUMENTS /APPARATUS / CHEMICAL / REAGENTS

This experiment consists of three parts:

Part A: Preparation of 0.05 M H2SO4 solutions
Part B: Preparation of phenolphthalein indicator solution
Part C: Preparation of methyl orange indicator solution
Part D: Alkalinity determination
Part A, B and C will be prepared by laboratory technician prior to the experiment
session.
Part A:
a. Chemicals
(i)
(ii)

Concentrated sulphuric acid

Distilled water

b. Equipments
(i)
(ii)
(iii)

1-litre volumetric flask

Digital pipette, and
1000-mL (1 L) Duran bottle

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT:
DETERMINATION OF
ALKALINITY

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2016

AMENDMENT DATE:

Part B:
This part must be conducted in area away from sources of ignition.
a. Chemicals
(i)
(ii)
(iii)

50 ml of ethanol
0.5 g of phenolphthalein
Distilled water

b. Equipments
(i)
Digital pipette
(ii)
Weighing boat
(iii)
100-ml volumetric flask
(iv)
small funnel
(v)
100-ml dropper bottle.
Part C:
a. Chemicals
(i)
0.1 g of methyl orange
(ii)
Distilled water
b. Equipment
(i)

100 ml beaker

(ii)

100 ml volumetric flask

(iii)

weighing boat

(iv)

small funnel

Part D:
a. Chemicals
(i)
(ii)

0.05 M H2SO4 solution (prepared from Part A)

Phenolphthalein indicator solution (prepared from Part B)

(iii)

Methyl orange indicator solution (prepared from Part C)

(iv)

Water sample

b. Equipments
(i)
(ii)
(iii)

Burette
Clamp stand
Volumetric flask

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT:
DETERMINATION OF
ALKALINITY

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2016

AMENDMENT DATE:

RESULTS CALCULATIONS

Part A: Preparation of 0.05 M H2SO4 solution

6.1. Half-fill a 1-litre volumetric flask with distilled water.

6.2. From a bench acid container of concentrated sulphuric acid, and using a

digital pipette, pipette 2.8 ml of acid into the flask. Swirl to mix. Rinse the
tip under running cold water immediately after use.
6.3. Make the solution up to 1-litre with distilled water.

6.4. Cap tightly and shake well to mix.

6.5. Pour into a 1-litre Duran bottle and label it.

Part B: Preparation of phenolphthalein indicator solution

6.1.

Using a digital pipette, pipette 50 ml of ethanol into a 100ml volumetric

flask.

6.2.

Weigh out 0.5 g of phenolphthalein into a weighing boat.

6.3.

Place a small funnel into the neck of the volumetric flask and tip the
powder into it.

6.4.

Wash the powder into the flask with distilled water, mix gently to dissolve.

6.5.

Make up to the 100 ml mark with distilled water. Cap tightly, shake to
mix.

6.6.

Using a small funnel, transfer to a 100ml, appropriately marked, dropper

bottle.

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT:
DETERMINATION OF
ALKALINITY

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2016

AMENDMENT DATE:

Part C: Preparation of methyl orange indicator solution

6.1.

Weigh out 0.1 g of methyl orange into a small beaker (100 ml).

6.2.

Add about 50ml of distilled water, stir to dissolve.

6.3.

Wash the contents of the beaker into a 100 ml volumetric flask and make
up to 100 ml with distilled water. Stopper and shake to mix. Using a
small funnel, transfer to an appropriately marked dropper bottle.

Part D: Alkalinity determination

6.1.

Clean burette with distilled water, allow to drain.

6.2.

Ensure burette is secure in the clamp stand.

6.3.

Pour about 40 ml of the 0.05 M acid into a small beaker very slowly.

6.4.

Insert the funnel into the top of the burette and pour in the contents of
the beaker very slowly.

6.5.

Allow the acid to flow through the burette, top up as necessary.

6.6.

Place 100ml (or record another known volume as V) of sample in a 250

ml conical flask.

6.7.

Add 2-3 drops of phenolphthalein indicator.

6.8.

If no pink colour is produced, record the titre as A= 0ml.

6.9.

If the sample turns pink, titrate with the standard acid solution until the
pink colour just disappears. Note down the volume of acid used as A
(ml).

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT:
DETERMINATION OF
ALKALINITY

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2016

AMENDMENT DATE:

6.10.

To the same sample, add a few drops of methyl orange indicator.

6.11.

If the sample turns red, record the titre as B=0ml.

6.12.

If the sample turns yellow, titrate with the standard acid until the colour
just changes to red. Note down the volume of acid used as B (ml).

(Repeat the same procedures using different samples)

ANALYSIS
Please show the calculation for each of the plating method and fill in the above
table. Analyze the results by using appropriate method. Explain your findings.

If the amount of acid recorded as A was zero, then phenolphthalein

alkalinity is 0 mg CaCO3/L.

If the amount acid recorded as A was > zero, then calculate

phenolphthalein alkalinity as follows:
Phenolphthalein alkalininty (mg/L as CaCO3)= A x C x 1000 x100
V

If the amount of acid recorded as B was zero, then total alkalinity is 0 mg

CaCO3/L.

If the amount of acid recorded as B was > zero, then calculate total
alkalinity as follows:

Total alkalininty (mg/L as CaCO3) = B x C x 1000 x100

V
Where:

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT:
DETERMINATION OF
ALKALINITY

EDITION:
2

REVISION NO:
EFFECTIVE DATE:

FEB
2016

AMENDMENT DATE:

A = volume of standard acid titrated to reach phenolphthalein endpoint

(pH 8.3) [ml]
B = volume of standard acid solution required to reach methyl orange
endpoint (pH 4.5) [ml]
C = concentration of acid [0.05 M]
V = volume of sample used [usually 100 ml].
Table 1: Alkalinity data (Sample 1: tap water )

Sample ID

A (ml)

B (ml)

Phenolphthalein
Alkalinity (mg
CaCO3/L)

Total Alkalinity
(mg CaCO3/L)

Sample 1
Sample 1
Sample 1
Average
Conc. of acid, C [M]

0.05

vol. of sample used, V (ml)

100

Table 2: Alkalinity data (Sample 2: wastewater effluent )

Sample ID

A (ml)

B (ml)

Phenolphthalein
Alkalinity (mg
CaCO3/L)

Total Alkalinity
(mg CaCO3/L)

Sample 1
Sample 1
Sample 1
Average
Conc. of acid, C [M]

0.05

vol. of sample used, V (ml)

100

Table 3: Alkalinity data (Sample 3: lake wastewater )

FACULTY : ENGINEERING
TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT:
DETERMINATION OF
ALKALINITY
Sample ID

A (ml)

B (ml)

EDITION:
2

REVISION NO:
EFFECTIVE DATE:

FEB
2016

AMENDMENT DATE:

Phenolphthalein
Alkalinity (mg
CaCO3/L)

Total Alkalinity
(mg CaCO3/L)

Sample 1
Sample 1
Sample 1
Average

Conc. of acid, C [M]

0.05

vol. of sample used, V (ml)

100

DISCUSSIONS
State the systematic bias error that could occur during this experiment and
readings for different samples.

ADVANCED QUESTIONS

8.1

What is alkalinity?

8.2

What is relationship between alkalinity and hardness?

8.3

Define equivalent weight and determine equivalent of CaCO3.

8.4

Discuss the importance of alkalinity to the environment.

CONCLUSION
Conclusion is merely a summary, presented in a logical order, of the
important findings already reported in the discussion section. It also relates to
the objectives stated earlier.

Prepared by/Disediakan oleh :

Approved by/Disahkan oleh :

Signature/Tandatangan :
Name/Nama : DR. NOR HASLINA HASHIM

Signature/Tandatangan :
Name/Nama : DR. SURAYA HANI ADNAN

Date/Tarikh :

FEBRUARY 2016

Date/ Date/Tarikh : FEBRUARY 2016