1

Name of the Experiments

1. Determination of pH of water sample
2. Determination of Solids of water sample
3. Observation of Coagulation and flocculation
of surface water
4. Determination of Dissolved Oxygen (DO) of
water sample
2
Determination of pH of water sample
Introduction: pH is the term used rather universally to
express the intensity of the acid or alkaline condition of a
solution. Mathematically pH is expressed as negative
logarithmic value of the concentration of hydrogen ions in a
solution.
pH = - log[H
+
]
The pH scale is usually represented as ranging from 0 to 14,
with pH 7 at 25
o
C representing absolute neutrality. For any
solution level of pH below 7 is considered acidic and above 7
basic.
3
Apparatus:
1. Beaker-100ml (01)
2. Beaker 50ml (03)
3. Thermometer (01)
4. Pocket Type pH Meter (01)

Reagents:
1. Standard pH-7 solution
2. Standard pH-4 solution
3. Standard pH-10 solution


4
Procedure: First of all the pH meter was calibrated. To do this job
about 30 ml of each standard pH solution were taken in the three
50 ml beakers individually. The pH meter was kept in each of the
beaker and tested the pH value of the standard solutions. Where
there was some discrimination found, the values were adjusted by
moving the calibration screws of the pH meter.
After standardization of the machine about 50 ml of water sample
was taken in a 100 ml beaker. First of all the the temperature of the
water sample was measured with thermometer. Then the electrodes
of pH meter was submerged in the beaker and reading of pH meter
was taken. By switching on and off reading was taken three times.
5
Results: the following pH values were found at the temperature of
33
O
C

No of Observation Reading of pH meter
01 5.6
02 5.8
03 5.5
Average pH value = (5.6+5.8+5.5)/3
= 5.63
6
Discussion: The average pH value of the supplied water
sample was found 5.6 which is below 7. The experiment
result revels the the nature of water sample is slide acidic.
Since the sample is acidic proper precaution should be
taken during supply of this water in metallic pipe.
Because acidic water is corrosive. If it is used for
drinking purpose pH should be raised up to 6.5.
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Precautions: Following precautions should be taken during this
experiment.
1. Before experiment all the glassware should be cleaned with
distilled water and dried in oven.
2. The electrodes of pH meter must be cleaned after use.
3. During calibration of machine care should be taken to avoid
contamination of different solutions.
4. Before pushing switch of pH meter it should be ensured that the
electrodes are submerged in the sample.
8
Determination of Solids of water sample

Introduction: Solids may affect water quality in number of ways.
Water with high dissolved solids generally are of inferior
palatability. A limit of 500 mg/L dissolved solids are desirable for
drinking purpose. Highly mineralized water is also unsuitable for
industrial applications.
Total Solids is the term applied to the material residue left in
the vessel after evaporation of a sample and its subsequent drying
in the oven at a defined temperature. Total solids includes total
suspended solids the portion of total solids retained by a filter
and total dissolved solids the portion passes through the filter of
2 micro meter.
9
Apparatus:
1. Glass fiber filter disks ( without organic binder)
2. Filtration Apparatus
3. Aluminium weighing-dish
4. Suction flask
5. Drying oven
6. Digital weighing balance
Glass fiber filter
disks
Filtration Apparatus
10
Procedure:
Preparation of glass-fibre disk: The disk was inserted with
wrinkled side up in filtration apparatus. Vacuum was applied and
the disk was washed with three successive 20 ml of deionised
water. Suction was continued until all traces of water was removed.
The filter was removed from filtration apparatus and transferred to
an inert aluminium weighing-dish. Care was taken to prevent the
dried filter from adhering to the weighing dish. The filter was dried
in an oven at 103-105 C for 1 hour. Then it was cooled and
weighted. The cycle of drying cooling and weighting was repeated
until a constant weight was obtained. The filter was stored in oven
until needed.
On the other hand a 100 ml capacity borosilicate glass beaker was
taken. The beaker was washed dried and weighted in the same
manner as described before.
11
Sample analysis: The filter was assembled with filtering
apparatus and suction was started. The filter was wetted with
small amount of deionised water to seat it. Then sample was
shaken vigorously, 100 ml volume of sample was piped onto the
seated glass fibre filter and suction was continued. The filter was
washed with 10 ml of deionised water successively three times.
Suction was also continued for about 3 minutes after filtration is
completed. Then the filter was removed from filtration apparatus
and transferred to an aluminium weighing-dish. The filter was
dried in an oven at 103-105 C for 1 hour. Then it was cooled and
weighted. The cycle of drying cooling and weighting was repeated
until a constant weight was obtained.
Next, the filtrated water sample was taken in the previously cleaned
and dried beaker. The beaker was dried and weighted in the same
manner as described incase of filter.
12
Results:

Total Suspended Solid = (Wt. of filter paper with soild Wt. of empty filter paper)
Volume of water sample
= (2.562 2.510) gm
100 ml
= 520 mg/L

Total Dissolved Solid = (Wt. of beaker with solid Wt. of empty beaker)
Volume of water sample
= (45.216 45.184) gm
100 ml
= 320 mg/L

Total Solid = Total Suspended Solid + Total Dissolved Solid
= 520 + 320
= 840 mg/L
13
Discussion: The above results show that the water sample contains
Total Suspended Solids (TSS) as 520 mg/L, Total Suspended Solids
(TDS) as 320 mg/L and Total Solids (TS) as 840 mg/L. For drinking
purpose water having TSS grater than 10 mg/L is not suitable for
drinking but the allowable TDS limit is up to 1000 mg/L. The results
of solids content of the supplied water sample reveals that the water
is not suitable for drinking purpose without removal of its
suspended materials.
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Precautions:
1. The glass fiber filter must be free from organic materials
2. Weight should be taken very carefully by the digital balance
because a simple carelessness may create a large error.
3. To reduce error weight should be taken several times repeatedly.
4. The temperature of oven must be kept within 103-105 C. If the
temperature is less moisture well not be removed fully and if the
temperature is higher then the volatile solids will be evaporated.
15
Determination of Total Hardness (TH) of water sample
Introduction: Hard water are generally considered to be those waters that
require considerable amounts of soap to produce a foam and that also
produce scale in hot-water pipes, heaters, boilers and other units in which
the temperature of water is increased materially. The hardness of waters
varies from place to place. Generally the surface waters are softer than
ground waters.
Water with hardness 0 - 75 mg/L is considered soft, 75 150 mg/L is
moderately hard, 150 300 mg/L is hard and above 300 mg/L is very hard.
But for drinking purpose up to 500 mg/L is allowable.
The principle cations causing hardness are Ca
2+
, Mg
2+
, Sr
2+
, Fe
2+
, and Mn
2+
; and the major anions are HCO
3
-
, SO
4
2-
, Cl
-
, NO
3
-
, SiO
3
2-

Hardness caused by carbonate or bi-carbonate ions are called temporary
hardness and it could be removed by boiling. And hardness caused by
sulfate, nitrate, chloride or silicate is called permanent hardness and it does
not remove by boiling.

16
Apparatus:
1. Pipette- 02 (2 ml and 25ml)
2. Burette with Stand 01 (50 ml)
3. Conical Flask 01 (250 ml)
4. Measuring Cylinder 01 (100 ml)
5. Dropper 01 (5 ml)
6. pH meter


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A. Reagents
(a) Buffer Solution: 1.179 gm di-sodium salt of ethylenediamine
tetraacetic acid di-hydrate and 0.780 gm magnesium sulphate (MgSO
4
.7H
2
O) was dissolved in 50 ml distilled water. 16.9 gm NH
4
Cl and 43 ml
conc NH
4
OH was added with the solution and diluted to 250 ml with
distilled water. The solution was stored in a plastic or borosilicate glass
container for no longer than 1 month.
(b) Indicator:
Eriochrome Black T: 0.5 gm dye (sodium salt of 1- (1-hydroxy-2-
naphthylazo) 5-nitro-2-naphthol-4-sulfonic acid; No. 203 in the Colour
Index) was dissolved in 100 gm 2-methoxymethanol (also called ethylene
glycol monomethyl ether).
(c) Standard EDTA titrant, 0.01M: 3.723 gm analytical reagent-grade
disodium ethylenediaminetetraacetate dihydrate was dissolved in distilled
water, and diluted to 1000 ml. It was standardized against standard calcium
solution.

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(d) Standard calcium solution: 1 gm anhydrous CaCO
3

powder was weighted into a 500-mL Erlenmeyer flask. A funnel
was placed in the flask neck and 1 + 1 HCI was added, a little at
a time, until all CaCO
3
had been dissolved. 200 ml distilled
water was added and boiled for a few minutes to expel CO
2
. The
solution was cooled and a few drops of methyl red indicator was
added to adjust the intermediate orange colour by adding 3N
NH
4
OH or 1 + 1 HCI, as required. Finally it was diluted to 1000
ml with distilled water; 1 ml = 1.00 mg CaCO
3
.

(f) Sodium hydroxide: NaOH, 0.1N.
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B. Procedure:

Titration of Sample: The volume of sample was selected which requires
less than 15 ml EDTA titrant and complete titration within 5 min,
measured from time of buffer addition.
25 ml sample was diluted to about 50 ml with distilled water in a
porcelain casserole or other suitable vessel. Then 1 to 2 ml buffer solution
was added. Usually 1 ml is sufficient to give a pH of 10.0 to 10.1. Then 2
drops indicator solution was added. The standard EDTA titrant was slowly
added, with continuous stirring, until the last reddish tinge disappeared.
The last few drops were added at 3 to 5 second intervals. At the end point
the solution became blue.
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Results:
Hardness as mg CaCO
3
/L
= (ml of EDTA titrant x mg CaCO
3
equivalent to 1 ml EDTA tirant) x 1000
ml of sample


Observation
No
Burette Reading

Difference
ml
Initial Final
1 0.0 5.20 5.20
2 5.20 10.40 5.20
3 10.40 15.55 5.15
Average value 5.18 ml
Hardness of the sample is
= 5.15 x1 x 1000
25
= 206 mg/L as CaCO
3

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Discussion: The hardness of the supplied water sample was found as 206
mg/L as CaCO
3
. The characteristics of the water sample is hard. The degree
of hardness falls within the allowable limit of drinking water but it will not
be suitable to use in laundry purpose or other industrial purpose like boiler
feed water. To make it useable for those purposes removal of hardness is
must.

The hard water some times good for drinking purpose because it contains
calcium, magnesium, iron etc. which makes the water testy as well as
contribute as a source of minerals. But for industrial purpose it is always
undesirable.
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Precautions:
1. Test should be performed within 5 minutes.
2. How much dilution of sample is required should be measured
first.
3. Special attention should be given for taking burette reading
4. The last few drops of titrant should be added very slowly and
carefully to fix the correct end point.
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Determination of Dissolved Oxygen (DO) of water sample

Introduction: The analysis of Dissolved Oxygen (DO) content is a key test in
water pollution and waste treatment process control. All living organisms are
dependent upon oxygen in one form or another to maintain the metabolic
processes that produce energy for growth and reproduction. All the gases of the
atmosphere are soluble in water to some degree. Both nitrogen and oxygen are
classed as poorly soluble and since they do not react with water chemically. Their
solubility is directly proportional to their partial pressure. Solubility of oxygen also
varies greatly with the temperature. The solubility of atmospheric oxygen in fresh
waters ranges from 14.6 mg/L at 0
o
C to about 7 mg/L at 35
o
C under 1
atmospheric pressure. The solubility of oxygen also depends upon contents of
some chemicals in water. DO is one of the indicators of pollution.
To maintain a healthy aquatic environment at least 4 mg/L of dissolved oxygen is
required. On the other hand in the boiler feed water removal of oxygen is required
as much as possible. For drinking water 6 mg/L of dissolved oxygen is standard.
The requirement of DO in water varies according to its purpose of use.
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Apparatus:
1. DO Bottle- 01 (300 ml)
2. Pipette- 02 (1 ml)
3. Burette with Stand 01 (50 ml)
4. Conical Flask 01 (500 ml)
5. Measuring Cylinder 01 (250 ml)
6. Dropper 01 (5 ml)

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Reagents:
(a) Manganous sulphate solution: 480 gm MnSO
4
.4H
2
O was dissolved in
distilled water, filtered and diluted to 1 L.
(b) Alkaline iodide azide reagent: 700 gm KOH and 150 gm KI was
dissolved in distilled water. 10 gm NaN
3
was dissolved in 40 ml distilled water
and was added to the solution and diluted to 1 L.
(a) Sulphuric acid, conc H
2
SO
4
: One millilitre is equivalent to about 3 ml
alkali-iodide-azide reagent.
(b) Starch: To prepare an aqueous solution, 2 gm laboratory grade soluble
starch and 0.2 gm salicylic acid, as a preservative, was dissolved in 100 ml hot
distilled water.
(c) Standard sodium thiosulphate titrant: 6.205 gm Na
2
S
2
O
3
.5H
2
O was
dissolved in distilled water. 0.4 gm solid NaOH was added and diluted to 1000
ml. It was standardized with bi-iodate solution.
(d) Standard potassium bi-iodate solution, 0.0021M: 0.8124 gm KH(IO
3
)
2

was dissolved in distilled water and diluted to 1000 ml.

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Standardization: Approximately 2 gm KI (free from iodate)
was dissolved in an Erlenmeyer flask with 100 to 150 ml
distilled water. A few drops of conc H
2
SO
4
and 20 ml standard
bi- iodate solution was added and diluted to 200 ml. Then
liberated iodine was titrated with thiosulphate titrant in presence
of starch. At the end point of titration a pale straw colour was
reached. When the solutions were of equal strength, 20 ml
0.025 M Na
2
S
2
O
3
was required. If not, adjustment was required
to make the concentration of Na
2
S
2
O
3
solution to 0.025 M.
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Procedure:
(a) Sample preparation: The sample was collected in a 300 ml bottle; 1 ml
MnSO
4
solution was added and followed by 1 ml alkali-iodide-azide
reagent. The pipet tips were hold just above liquid surface when adding
reagents. The bottles were stoppered and mixed thoroughly by inverting.
Thus the dissolved oxygen was fixed and samples were taken to the
laboratory. When precipitate had been settled sufficiently to leave clear
supernatant above the manganese hydroxide flocs, 1.0 ml conc H
2
SO
4
was
added. Again the bottle was stoppered and mixed by inverting several times
until dissolution was completed. A volume corresponding to 200 ml
original sample after correction for sample loss by displacement with
reagents was taken for titration. For a total of 2 ml of MnSO
4
and alkali-
iodide azide reagents in a 300 ml bottle, 200*300/(300-2)=201 ml sample
was taken in a conical flask for titration.
Three bottle samples were collected from the same source.
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(b) Titration: 0.025 M N
2
S
2
O
3
solution was used as a titrant.
A few drops of starch solution were added to the sample and
the straw colour was changed to blue. The titration was
continued to first disappearance of blue colour.

29
Results:
For titration of 200 ml sample, 1 ml 0.025 M N
2
S
2
O
3
= 1 mg DO/L.
Average Value = 6.1 ml
So, Dissolved Oxygen of the supplied sample is 6.1 mg/L

Observation
No
Burette Reading

Difference
ml
Initial Final
1 0 6.15 6.15
2 6.15 12.2 6.05
3 12.2 18.3 6.10
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Discussion: The dissolved oxygen level of the supplied water sample was
found 6.1 mg/L. This level of oxygen meet the drinking water standard as
well as very much fit for aquatic creatures. It also indicates that water is
free from biological pollution or less polluted. Because where DO level is
high generally there BOD and COD level is low.
But if it is used as boiler feed water, DO must be reduced. Because excess
DO is corrosive for the metals.
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Precautions:
1. During collection of the sample care should be taken so that no
external oxygen can mix with the sample.
2. The sample bottles should be air tight .
3. At the time of mixing oxygen fixing chemicals pipette should be
submerged enough into the sample.
4. Burette reading should be taken carefully.
5. To determine accurate end point last few drops of titrant should be
added very slowly and carefully.