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FACULTY : ENGINEERING

TECHNOLOGY
LABORATORY: CIVIL
ENGINEERING TECHNOLOGY
EXPERIMENT:
DETERMINATION OF
ALKALINITY

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2015

AMENDMENT DATE:

FACULTY OF ENGINEERING TECHNOLOGY


DEPARTMENT OF CIVIL ENGINEERING TECHNOLOGY

ENVIRONMENTAL ENGINEERING TECHNOLOGY


LABORATORY
LABORATORY INSTRUCTION SHEETS
COURSE CODE

BNP 20503

EXPERIMENT CODE

EXPERIMENT 7

EXPERIMENT TITLE

DETERMINATION OF ALKALINITY

DATE
GROUP NO.
LECTURER/INSTRUCTOR/TUTO
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DATE OF REPORT SUBMISSION

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LABORATORY REPORT

ATTENDANCE/PARTICIPATION/DISIPLINE:

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INTRODUCTION:

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PROCEDURE:

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RESULTS & CALCULATIONS

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ANALYSIS

/15%

DISCUSSIONS:

/20%

ADDITIONAL QUESTIONS

/15%

CONCLUSION

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SUGGESTIONS & RECOMENDATIONS

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REFERENCES:

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

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2015

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)
__________________________________
__________________________________

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

EDITION:
REVISION NO:
EFFECTIVE DATE:

2
FEB
2015

AMENDMENT DATE:

1.0 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.

2.0LEARNING 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

3.0INTRODUCTION
3.1Alkalinity 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.

3.2Alkalinity 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 CaCO 3
equivalent. For samples whose initial pH is above 8.3, the titration is
conducted in two steps.

3.3In 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.
1

3.4The 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.

4.0INSTRUMENTS /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)

Concentrated sulphuric acid

(ii)

Distilled water

b. Equipments
(i)

1-litre volumetric flask

(ii)

Digital pipette, and


2

(iii)

1000-mL (1 L) Duran bottle

Part B:
This part must be conducted in area away from sources of ignition.

a. Chemicals
(i)

50 ml of ethanol

(ii)

0.5 g of phenolphthalein

(iii)

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)

0.05 M H2SO4 solution (prepared from Part A)

(ii)

Phenolphthalein indicator solution (prepared from Part B)

(iii)

Methyl orange indicator solution (prepared from Part C)

(iv)

Water sample
3

b. Equipments

(i)

Burette

(ii)

Clamp stand

(iii)

Volumetric flask

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.

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).

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
6

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:
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 )


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

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

ADVANCED QUESTIONS
8

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 2015

Date/ Date/Tarikh : FEBRUARY 2015