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EAA305 ENVIRONMENTAL ENGINEERING LABORATORY

EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES


EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

CONTENT:
EXPERIMENT 1 PAGE
a) USE OF pH METER 1
b) DETERMINATION OF ACIDITY 8
OF WATER SAMPLES
c) DETERMINATION OF 14
ALKALINITY OF WATER
SAMPLES
EXPERIMENT 2
a) DETERMINATION OF SOLIDS IN 21
WATER
b) DETERMINATION OF HARDNESS 28
IN WATER
REFERENCE 37
DECLARATION 38
APPENDIX 39

EAA 305 ENVIRONMENTAL ENGINEERING LABORATORY


EXPERIMENT 1 :-

GROUP 24 1 1
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY


WATER SAMPLES.

Experiment 1a :- Use of pH Meter

OBJECTIVES:

The objective of this test is determined pH of the given water samples by using pH
meter and pH paper.

THEORY:

pH
pH is a numerical representation of acidic or basic nature of solutions.
Water ionizes to a small degree. The ionization is represented by:

H2O H + + OH -

Equilibrium constant, K = [H +] [OH -]


[H2O]

Since ionization of water is very low, [H2O] is taken to be constant. Thus,

Ion product of water, Kw = [H +] [OH -]


= 1 10 -14 at 25 C

p Notation
pX = -log10 X

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EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

pH = -log [H+]
pH < 7 ; acidic solution
pH = 7 ; neutral solution
pH > 7 ; alkaline solution

In general,
pH + pOH = 14

APPARATUS:

o pH Meter,
o Volumetric Cone and
o Cylindrical

pH METER

PROCEDURES:

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EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

a) At first we calibrate the pH meter with buffer solutions (pH 4.01 and
7.01).
b) We have rinsed the electrode of the pH meter with distilled water and dry
it with a piece of tissue paper.
c) Then we determine the pH value for the following water samples by
immersing the pH meter electrode into them.

i) Distilled water
ii) Laboratory tap water
iii) Untreated sewage sample

Notes: Rinse your electrode with distilled water and dry it with a piece of tissue
paper before measuring each samples pH

a) We have compared the results with those obtained by using pH paper


b) The result we obtained recorded.

GROUP 24 4 4
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

RESULTS:

Experiment 1a: Use of pH Meter

pH meter reading
Sample
I II III Average

(a ) Tap water 6.26 6.46 6.53 6.42

(b ) Untreated sewage
sample 6.87 6.94 6.97 6.93

Experiment 1a : Use of pH Meter

The pH of tap water sample = 6.42


The pH of untreated sewage sample = 6.93

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EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

DISCUSSION:

Use of pH meter

pH-----The scientific definition is 'the negative logarithm of the Hydrogen ion


concentration'. OK - don't give up - its a very important concept. Lets get through to
that definition in every day terms.
First accept pH is a scale measuring the acidity or alkalinity of a solution. Squeezed
lemon and vinegar are sour or acidic. If we drank them we would take something
alkaline like bicarbonate of soda or magnesia to neutralise the acidity in our stomachs -
in other words raise the pH. The pH scale runs from 0 (highly acidic) to 14 (highly
alkaline) with distilled water being neutral at pH 7.
1. Why is the pH value of distilled water acidic?
The quality of reagents is strongly dependent upon the quality of water to prepare them.
There must be no detectable concentration of the substances to be analyzed, or of
anything which will react with that substances in the water. For use in a laboratory
where multiple analyses are being performed, a source of the purest water available is
needed; distilled water. The quality can be checks by measuring the electrical
conductivity (pure distilled water does not conduct electricity) at temperature 25 C.
Distilled water contained amount of free hydrogen more than ion hydroxide.
This special characteristic have make the distilled water became acidic samples.
At the temperature 25C the condition of distilled water is constant, since the density of
ion hydrogen more than ion hydroxide, when we expose the distilled water to the
atmosphere for a period, it will become more acidic.
The reaction can be shown from the equation below:
CO2 + H2O = H2CO3 H2CO3 is weak acid.
It will cause the density of ion hydrogen in distilled water higher than the ion
hydroxide:

2H2O + CO3 = H3O + HCO3-

2. What is the significance of pH in water/wastewater treatment?

GROUP 24 6 6
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

Aquatic organism treatment is sensitive to change of pH meter, and biology


treatment need for control of pH.
For the water treatment, pH also important to determine the chemical
treatment is successful to control disinfection and corrosion.
Also know that flowing water in mine usually yield the sulphuric acid
(concentration H+ is high) and hazardous to aquatic life.
The most important things to know the pH water is because to make sure
that we are drinking a safety water without any worried.

CONCLUSION:

The pH value is the negative logarithm to base 10 of the hydrogen ion


activity (mol/l) and is 7.0 in pure water (neutral point). This value changes in the
presences of acids and alkalis and through the hydrolysis of certain salts. In natural
water the pH ranged 6.5 to 8.5 the presence of free carbon dioxide or humus lowers the
pH. Biogenic decalcification in surface water, which occurs when there is high CO2
depletion by algae, can cause the pH to rise to 10.
pH Conc. H+ Example
0 10,000,000 Battery acid Most acidic
1 1,000,000 Hydrochloric acid
2 100,000 Lemon juice
3 10,000 Orange juice
4 1,000 Acid rain
5 100 Black coffee
6 10 Saliva
7 1 Distilled water Neutral
8 0.1 Salt water
9 0.01 Baking soda
10 0.001 Milk of magnesia
11 0.0001 Ammonia solution
12 0.00001 Soapy water
13 0.000001 Oven cleaner
14 0.0000001 Liquid drain cleaner Most
alkaline
The pH value we got in this experiment for samples laboratory tab water,
and untreated sewage sample were 6.42, and 6.93 respectively. So we can conclude that,

GROUP 24 7 7
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

laboratory tab water and untreated sewage sample are acidic. The standard value for
wastewater is 5.5 to 9 (standard A) and 5.0 to 9.0 (standard B) respectively.

Experiment 1b: Determination of acidity

OBJECTIVE:
To determine various forms of acidity in the given water samples.
THEORY:

Acidity

Both CO2 and mineral acidity can be measured by titration with a standard alkaline
solution. Mineral acids are measured by titration to a pH of 4.5. Titration to the pH 8.3
end point measures total acidity i.e. both mineral acidity as well as due to weak acids.

APPARATUS:

o pH Meter,
o Volumetric Cone,
o Cylindrical,
o Retort Stand and
o Burette.

GROUP 24 8 8
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

PROCEDURES:

a) For samples with pH 0 4.5 (i.e. mineral acidity), we take 50ml sample and
titrate it using N/50 NaOH and methyl orange as indicator (colour change from
red to orange).

b) For samples with pH 4.5 8.3 (i.e. CO2 acidity), we take 50ml sample and titrate
it using N/50 NaOH and phenolphthalein as indicator (colour change from
colourless to pink).
c) We have recorded the concentration and type of acidity.

RESULT:
Experiment 1b: Determination of Acidity Water Samples

i. Laboratory tap water

Sample Volume = 50 ml
pH value = 2.96

Burrete Reading
Type of Acidity
Volume of NaOH
Start ( 0.05 ml) End ( 0.05 ml)
(ml)

Mineral Acidity 16.10 27.60 11.50

Carbon Dioxide
Acidity 27.60 40.10 12.50

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EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

ii. Untreated sewage sample

Sample Volume = 50 ml
pH value = 6.93

Burrete Reading

Type of Acidity
Volume of N/50
Start ( 0.05 ml) End ( 0.05 ml)
NaOH (ml)

Mineral Acidity 40.10 43.50 3.40

Total Acidity 13.80 16.10 2.30

CALCULATION:

Determination of Acidity Water Samples

i ) Laboratory tap water


Sample volume = 50 ml
Mineral acidity = 230.00 mol/l
Total acidic = 250.00 mol/l
Type of acidity = -
pH value = 2.96

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EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

For Mineral acidity,


Volume of N/50 NaOH (ml) = End reading - Start Reading
= 27.60 16.10
= 11.5 ml

For Total acidity,


Volume of N/50 NaOH (ml) = End reading - Start reading
= 40.10 27.60
= 12.50ml
1000
Mineral acidity = ml of N/50 NaOH x mlsample
1000
= 11.50 x
50
= 230 mol/l

1000
Total acidity = ml of N/50 NaOH x mlsample
1000
= 12.50 x
50
= 250.00 mol/l

Carbon Dioxide acidity = Total acidity - Mineral acidity


= 250.00 230.00
= 20.00 mol/l

DISCUSSION:

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EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

Acidity
pH is a measure of a water sample's deviation from a neutral value of 7.00, it
provides little information about a water sample's ability to neutralize acids or bases.
The standard procedures for "acidity" and "alkalinity", which have been modified here
to fit the time and equipment requirements of a student laboratory,
quantitatively provide that information.
The acidity of a water sample is its capacity to neutralize hydroxide ions.
Acidity may be caused by mineral acids such as sulfuric acid or hydrochloric acid or by
dissolved carbon dioxide. Most commonly in drinking water, carbon dioxide is the
principal cause of acidity. Acidity increases the corrosive behavior of water. Drinking
water with a high acidity is likely to be corrosive to copper water pipes and to the solder
which joins those pipes. High levels of copper and lead in drinking water often occur
when acidic water stands in pipes for extended periods of time (such as over night). In
addition to creating a possible health hazard due to dissolved metal ions, acidity in
water can cause copper plumbing to develop pin hole leaks after a few years.
Acidity is generally measured by titration with sodium hydroxide to an accepted
pH value. Phenolphthalein is an acid-base indicator which changes from colourless to a
pink (magenta) at a pH of about 8.3.
Generally, acidity is measured by titration of a water sample to pH 8.3 with
NaOH titrant. Metacresol purple also changes color at pH 8.3, but gives a sharper color
change than phenolphthalein. If available, its use is recommended over phenolphthalein.
If a water sample is at the alkaline color of the indicator before any titrant is added, then
the acidity is zero and the alkalinity of the water should be tested.
Because CO2 is the most likely cause of acidity in water, the water sample
should be collected within a few hours of the time of analysis. The container used to
collect the water should be filled completely and closed with an air-tight seal. A clean
plastic soft drink bottle with screw cap is suitable for water samples tested in this
procedure.

GROUP 24 12 12
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

1. What are the source of acidity in waste water?

Acidity may be caused by mineral acids such as sulfuric acid or hydrochloric


acid or by dissolved carbon dioxide. Most commonly in drinking water, carbon
dioxide is the principal cause of acidity. Acidity increases the corrosive behavior
of water.
Carbon dioxide, the major acid components of all natural waters, enters surface
waters by absorption from the atmosphere, and from aerobic and anaerobic
bacterial action in water.
Sewage water become a little bit acidic if anaerobic process takes
place.Beacause of the fact that anaerobic process produces methane gas (CH 4),
carbon dioxide (CO2) and hydrogen sulphate (H2S). These gases can dissolve
into the water and decrease the pH value of sewage water making it more acidic.

Organic matter + Bacteria (CO2) + (CH4)


+ (H2S) +
(sewage water) (without the presence of oxygen) new cell

2. What is the significance of acidity in water/waste water treatment?


It is this CO2 acidity that is monitored in the acidity test, and it can exist in
natural waters which are under a pH of 8.3 (phenolphthalein endpoint ). It is of
no direct health significance in drinking waters. Our natural stomach acid is
concentrated HCL, with a pH between 0 and 1. The value of monitoring CO 2
content is in recognizing its capacity to react with other chemicals in the water.
If the waste water is either too acidic or too alkaline then further analysis will be
needed before any treatment is allowed. Thus, the lumping and flocking process
will not occur at an optimal rate. Besides, water with a high value of acidity may
be harmful to human health, therefore the magnitude of acidity in water is
important.

GROUP 24 13 13
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

CONCLUSION:

From the calculation based on the information we obtained, the result we get for
laboratory tap water sample:
Mineral acidity = 230 mol/l
Total acidity = 250 mol/l
Carbon Dioxide acidity = 20 mol/l
The acidity is quite high if we refer the data above, so the treatment is required upon the
water.

Experiment 1c : Determination of alkalinity

OBJECTIVE:

To determine various forms of alkalinity in the given water samples.

THEORY:

Alkalinity

Alkalinity of a water sample is defined as its capacity to neutralize acids. In natural


water alkalinity is generally due to the presence of the hydroxide (OH -), carbonate (CO3
2-
) and bicarbonate (HCO 3- ) ions.

Alkalinity is measured by titration with a standard acid solution. The end points of
importance for the titration are those of pH 8.3 and 4.5.

GROUP 24 14 14
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

APPARATUS:

o pH Meter,
o Volumetric Cone,
o Cylindrical,
o Retort Stand and
o Burette.

PROCEDURES:

a) We have taken 50ml of untreated sewage and add it with the appropriate
indicator.

b) (i) The pH of the sample is greater than 8.3, hence we titrate the sample by using
N/50 H2SO4 and phenolphthalein as indicator (colour change from pink
to colourless).

Phenolphthalein alkalinity (P) = ml H2SO4 (to pH 8.3) 1000


ml sample

To the same sample add methyl orange indicator to find total alkalinity (colour change
from orange to red).

Total alkalinity (M) = total ml H2SO4 (to pH 4.5) 1000


ml sample

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EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

(ii) For the sample pH lies between 4.5 and 8.3 that means only bicarbonate
alkalinity is present. We titrate the sample with N/50 H2SO4 using methyl orange as
indicator (colour change from orange to red).

Total alkalinity (i.e. bicarbonate) = total ml H2SO4 (to pH 4.5) 1000


ml sample

c) We have determine various forms of alkalinity with the help of following guide :

P=M ; all alkalinity is OH


P = M/2 ; all alkalinity is CO3 =
P > M/2 ; predominant species are OH and CO3 =
P < M/2 ; predominant species are CO3 = and HCO3
P=0 ; all alkalinity is HCO3

RESULT:
Experiment 1c : Determination of Alkalinity Water Samples

i) Laboratory tap water


Sample volume = 50 ml
pH value = 9.5

Burrete Reading
Type of Acidity
Volume of N/50
Start ( 0.05 ml) End ( 0.05 ml)
NaOH (ml)

P 33.1 38.3 5.2

M 38.3 48.4 10.1

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EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

ii) Untreated sewage sample


Sample volume = 50 ml
pH value = 6.43

Burrete Reading

Type of Acidity
Volume of N/50
Start ( 0.05 ml) End ( 0.05 ml)
NaOH (ml)

M 24.4 33.1 8.7

CALCULATION:
Experiment 1c: Determination of Alkalinity Water Samples
ii) Untreated sewage sample

Sample volume = 50 ml
pH value = 6.43
Total H2SO4 = 8.7 ml
Phenolftalein alkalinity (P) = 0
Total alkalinity (M) = total ml H2SO4 x 1000
ml sample
= 8.7 x 1000 / 50
= 174 mol/l

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EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

Types of alkalinity = HCO3- alkalinity (4.5 < pH < 8.3; all alkalinity is HCO3-)

DISCUSSION:

Alkalinity

Alkalinity is the measure of a water sample's ability to neutralize hydrogen ions


(its acid-neutralizing ability). Alkalinity may be caused by dissolved strong bases such
as sodium hydroxide or potassium hydroxide (and other hydroxide-containing
compounds), and it may also be caused by dissolved carbonates, bicarbonates, borates,
and phosphates. The measured alkalinity is the total of all of these species found in a
water sample. For the sake of simplicity, it is expressed in terms of mg CaCO3/L
although many species other than dissolved calcium carbonate may actually contribute
to the alkalinity.
One important environmental consequence of alkalinity is the ability of a body
of water to withstand acidification due to acidic precipitation or atmospheric deposition.
A body of water may have a fairly neutral pH, but if its alkalinity is low, it will be
readily acidified. A body of water with the same pH but with higher alkalinity will have
a greater buffer capacity and, consequently, a greater resistance to acidification.
The following figure shows the various combinations of alkalinity.

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EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

Representation of titration of samples

Determine various forms of alkalinity with the following guide:


If P=M ; Hydroxide = M, all alkalinity is OH-
If P<1/2M ; Carbonate = 2P
Bicarbonate = M-2P, predominant species are CO32-
and HCO3-
If P=1/2M ; Carbonate = 2P, all alkalinity is CO32-
If P>1/2M ; Hydroxide = 2P-M
Carbonate = 2 (M-P), predominant species are OH-
and CO32-
If P = 0 ; Bicarbonate alkalinity = M, all alkalinity is HCO3-

Since the total alkalinity = 174 mg/l as CaCO 3 and P = 0 and M = 8.7 ml. Therefore the
predominant species are bbicarbonate, HCO3-. Type of alkalinity is acid.

GROUP 24 19 19
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

1.Which ions other than hydroxide (OH-), carbonate (CO32-) and bicarbonate
(HCO3-)can cause alkalinity in water?
Alkalinity is defined as the ability of water to resist a change in pH when acid is
added; it relates to the pH buffering capacity of the water. Almost all natural
waters have some alkalinity. This is natures mean keeping the pH neutral, and
stable, so that life can exist there. Three major ions contribute to total alkalinity.
However other ions such as organic nitrogen, ammonia nitrogen, nitrite nitrogen,
nitrate nitrogen, phosphate PO42- , sulphate SO42- , chloride Cl- , fluoride F- , and
cyanide CN- can also cause alkalinity in water.

2.What is the significance of alkaliniy in water/waste water treatment?


Alkalinity is a beneficial feature of water, and does not necessarily indicate a
high pH. The amount of total alkalinity is just as important as the type of
alkalinity. Water with few thousand molecules of bicarbonates alkalinity has a
lot more buffering power than that same water with just a few molecules of
hydroxide alkalinity, and yet the pH of the water remains close to neutral.
Monitoring pH does not disclose much information about the amount of
alkalinity in water because basicity and alkalinity are not the same thing.
In the lumping and flocking process, alkalinity is an important factor because
the lumper agent, alum that is used will react with the alkalinity of water to form
a settlement of aluminium hydroxide. But, if this standard of alkalinity is not
reach then the settlement will not occur at its optimal rate. Water which have a
low value of alkalinity will show some behavior of erodibility

CONCLUSION:
Relative to the pH scale the various type of alkalinities reside. In other words,
these ions have the capacity to hold to the pH of the water at these ranges, depending on
how much of each is represent. Now picture titrating with an acid into a water with
carbonate alkalinity. By the time pH 8.3 is reached, exactly half the carbonate alkalinity
has been neutralized. This is always the case. One of the reasons that phenolphthalein

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EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

was chosen as a useful indicator for this method was that it does visually show this
point.
The total alkalinity of the effluent sample obtained from the experiment is 174
mg/l as CaCO3 with P = 0 and M = 8.7 ml. Therefore the only predominant species is
bicarbonate ions (HCO3-). Since the pH of the effluent sample is only 6.43 which does
not exceed 8.3, therefore the effluent alkalinity is at its required standards for alum to
react with suspended solid and settle as sludge. The alkalinity in water plays an
important role in waste water treatment especially in the lumping and flocking process.

EXPERIMENT 2 : DETERMINATION OF SOLIDS AND


HARDNESS IN WATER

Experiment 2a : Determination of solids in water

OBJECTIVES:

To determine the amount of total solids (TS), suspended solids (SS) and
volatile suspended solids (VSS) in the given wastewater samples.

THEORY:
Solids in wastewater

Considerable information can be gained on a wastewater sample by determining its


various solid contents. Various types of solids in wastewater samples can be determined
gravimetrically.

Solids - Water normally contain solid material, both in dissolved and suspended forms.
Solids are also further classified as fixed or volatile. Fixed solids are basically the ash

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EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

left over after burning the dried solids; volatile solids are those that are lost in this
procedure. The sum of the two is referred to as total. Volatile solids are often used as an
estimate of the organic matter present.

Total solids (TS) are determined by drying a known amount of a sample at a


temperature of 103 to 105 C. Results can be expressed in mg/l or percent by weight.
If the sample is then burned in a furnace at about 500 C, cooled, and weighed,
the fixed (FS) or volatile solids (VS) can be determined.
If the original sample is filtered through a tared glass-fiber filter, which is then
dried, the weight of the material captured on the filter is used to figure the total
suspended solids (TSS). Burning the filter in the furnace allows measurement of
volatile suspended solids (VSS) or fixed suspended solids (FSS).
The dissolved solids (DS) can be estimated from the difference between the
total solids and the total suspended solids, but the official method calls for drying the
filtrate (the liquid which passes through the filter) in a dish at 180C. Of course, there are
TDS, FDS and VDS.

Suspended material can decrease the depth of the body of water. If there is a lot of
biodegradable organic material in the sediment, it will become anaerobic and contribute
to oxygen depletion. Toxic materials can also accumulate in the sediment and affect the
organisms which live there and can build up in fish that feed on them, and so be passed
up the food chain, causing problems all along the way . Also, some of the particulate
matter may be grease-- or be coated with grease, which is lighter than water, and float to
the top, creating an aesthetic nuisance.

APPARATUS:

o Volumetric Cone,
o Cylindrical,
o Filtration Unit,
o Vicar and
o Heat Bowl

PROCEDURE:

a) Total solids (TS)

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EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

(i) Dry a crucible in an oven at 104 C for one hour.

(ii) Cool the crucible in a desiccator and weight on an analytical balance to the
nearest 0.1 mg. (X)
(iii) Pour a suitable volume of sample into the crucible and evaporate the contents to
dryness on a steam bath.
(iv) Transfer to an oven at 104 C and dry to a constant weight (about 30 minutes).
(v) Cool the crucible in a desiccator and weight on an analytical balance to the
nearest 0.1 mg. (Y)

(vi) Calculate TS as:

Total solids (TS) (mg/l) = (Y X) 1000


volume of sample (ml)

b) Suspended solids (SS)

(i) Prepare glass fibre filters GF/C.


(ii) Dry in an oven at 104 C for 15 minutes.
(iii) Heat to constant weight at 550 C in a muffle furnace (about 15 minutes).
(iv) Cool in a desiccator and weight on an analytical balance to the nearest 0.1 mg.
(X)
(v) Filter a suitable volume of sample.
(vi) Dry at 104 C for an hour.
(vii) Cool in a desiccator and weight on an analytical balance to the nearest 0.1 mg.
(Y)
(viii) Calculate SS as:

Suspended solids (SS) (mg/l) = (Y X) 1000

GROUP 24 23 23
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

volume of sample (ml)

c) Volatile suspended solids (VSS)


(i) Ignite the glass fibre filters, from b) above, at 550 C for 15 minutes.
(ii) Cool in a desiccator and weight on an analytical balance to the nearest 0.1 mg.
(Z)
(iii) Calculate VSS as:

Volatile suspended solids (VSS) (mg/l) = (Y X) 1000


volume of sample (ml)

RESULT:

Determination Of Suspended Solids (SS)

Sample Volume = 100 ml

Sample weight (g)


Y (weight of filter paper A + dry sample) 0.3027
X (weight of filter paper A) 0.3368
Y - X (weight of dry sample) 0.0341
Suspended solids (mg/l)** 341.0000

Determination Of Volatile Suspended Solids (VSS)

Sample Volume = 100 ml

Sample weight (g)


Y (weight of filter paper B + dry sample
before ignite) 0.3339
X (weight of filter paper B) 0.3367
Z (weight of filter paper B + dry sample
after ignite) 0.0028

GROUP 24 24 24
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

Volatile suspended solids (mg/l)** 28.0000

Determination Of Total Solids (TS)

Sample Volume = 100 ml

Sample weight (g)


Y (weight of crucible) 91.4074
X (weight of crucible + dry sample) 91.4095
Y - X (weight of dry sample) 0.0048
Suspended solids (mg/l)** 21.0000

CALCULATION:

Suspended solids
Y X 1000
Suspended solids (SS) (mg/l) =
volumeofsample ml
= (0.3368 - 0.3027) x 1000
100
= 341.0000mg/l

Total Solids
Y X 1000
Total solids (TS) (mg/l) =
volumeofsample ml

= (91.4095 91.4074) x 1000


100

= 21.0000mg/l

Volatile Suspended Solids


Y Z 1000
Volatile suspended solids (SS) (mg/l) =
volumeofsample ml

= (0.3367 0.3339) x 1000


100
=28.0000 mg/l

GROUP 24 25 25
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

DISCUSSION:

1.What is the significance of various types of solids in water quality?

There are few types of solids in water. Total Dissolved Solids (TDS) consist mainly of
carbonates, bicarbonates, chlorides, sulfates, phosphates, nitrates, calcium, magnesium,
sodium, potassium, iron, manganese, and a few others. Total Suspended Solids (TSS) is
comprised of organic and mineral particles that are transported in the water column.
Total suspended solids (TSS) gives a measure of the turbidity of the water.

Solids in water are harmless to people, unless they exist in high amounts. Small
amounts of chlorides are necessary for normal cell functions in plant and animal life.
However, fish and aquatic animals can not live in high levels of chlorides. Phosphorus
is a necessity for all plant life, and nearly all fertilizers contain phosphates.

Suspended solids (SS) cause the water to be milky or muddy looking due to the light
scattering from very small particles in the water. Sometimes it is mixed with color, but
colored waters can also be clear. Normally, we notice suspended solids before we notice
anything else.

GROUP 24 26 26
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

Suspended solids reduce light penetration and submersed plant productivity. Suspended
solids also affect organisms that live in the water. Those organisms that depend on
plants for food and predators that rely on their visual abilities to hunt are adversely
affected. Suspended solids in a body of water also accelerate the process of
eutrophication. Eutrophication is the process whereby bodies of water become
fertilized. This fertilization causes a significant increase in the growth rate of algae and
other aquatic plants. With continued eutrophication, dissolved oxygen levels become
depleted further accelerating the process of eutrophication leading to eventual aquatic
collapse.

High levels of total dissolved solids can adversely industrial applications requiring the
use of water such as cooling tower operations; boiler feed water, food and beverage
industries, and electronics manufacturers. High levels of chloride and sulfate will
accelerate corrosion of metals.

2.What precaution must be taken in VSS determination? Why?

The main function of the desiccator is to remove all the moisture exist on the surface of
the filter paper. Therefore the ignited filter paper should be put into the desiccator
before we weighing it, as the moisture exist on the surface of the ignited filter paper
may bring significant affection to the final weighing result.

CONCLUSION:

From the experiment, the effluent sample solid component comprises of suspended
solid and volatile suspended solid. The suspended solid content must be acknowledged
to simplify the waste water treatment process. Parameter values from the experiments
are as below.

Suspended solid = 341mg/l

GROUP 24 27 27
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

Volatile suspended solid =21 mg/l


Total solid = 28mg/l

The allowed suspended solid in waste water is only 100 mg/l as stated in Environmental
Quality Act 1974. This is because suspended solid contains organic substances that are
the main parameter of wastewater.

Experiment 2b : Experiment of hardness

OBJECTIVES:
To determine total, Ca and Mg hardness in the given wastewater samples.

THEORY:
Hardness

Hardness is the presence of multivalent metallic cations in solution. Metal ions like Ca
2+
, Mg 2+, Fe 2+, Mn 2+, Sr 2+ and Al 3+ would all contribute hardness.
However, in natural waters the major hardness contributing ions are Ca2+
and Mg 2+. Thus, generally total hardness is taken as the sum of Ca and Mg hardness.
Hardness of a water sample is determined by titration with ethylenediaminetetraacetic
acid (EDTA).

The amount of dissolved calcium and magnesium in water determines its "hardness."

Water hardness can be calculated as shown in the equation :

GROUP 24 28 28
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

Hardness (mg/l) = 2,5 [conc. of Ca2+ (mg/l)] + 4,1 [conc. of Mg2+ (mg/l)]

The most frequently used standard classifies water supplies is shown in the following
table.

Hardness Scale

Classification Range of hardness (ppm)


Soft 0 - 60
Moderately Hard 61 - 120
Hard 121 - 180
Very Hard >180

APPARATUS:

o Volumetric Cone,
o Cylindrical, Vicar,
o Heat Bowl

Filtration unit heat bowl

GROUP 24 29 29
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

Volumetric Cone, Cylindrical and beaker

PROCEDURES:

a) Total hardness

i) We have measured 100 ml of sample diluted to 100ml with distilled water into a
250 ml conical flask (hardness between 10 200 mg/l as CaCO3).
ii) 2 ml of ammonia buffer solution added in sample to get pH 10.
iii) 1 drop of Eriochrome Black T (EBT) added as indicator and mix it with the
sample.
iv) Then we titrate the sample with M/100 EDTA (colour change from red to
blue/grey).
v) The total hardness calculated as:

Total hardness (mg/l as CaCO3) = ml EDTA 1000


ml sample

b) Ca hardness

GROUP 24 30 30
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

(i) We measure 100 ml of sample or a suitable volume diluted to 100ml with


distilled water into a 250 ml conical flask (hardness between 10 200 mg/l as
CaCO3).
(ii) 1 ml of 4 N NaOH added into sample and stirs it. The pH of the solution should
be 12 13.
(iii) 1 spatula of murexide added as indicator and mix it.
(iv) We titrate the sample with M/100 EDTA (colour change from red
to blue).
(v) Ca hardness calculated as:

Ca hardness (mg/l as CaCO3) = ml EDTA 1000


ml sample

c) Mg hardness;
The Mg hardness calculated as:
Mg hardness = Total hardness Ca hardness

RESULT:

Total Hardness

Sample volume = 100 ml


Indicator = EBT

Burette Reading

End Start Volume of


Type of sample (0.05 ml) (0.05 ml) EDTA (ml)
Untreated water 12.10 7.50 4.60

Colour of indicator change from : red to blue

Calcium Hardness

GROUP 24 31 31
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

Sample volume = 100 ml


Indicator = murexide

Burette Reading

End Start Volume of


Type of sample (0.05 ml) (0.05 ml) EDTA (ml)
Untreated water 15.30 12.10 3.20

Colour of indicator change from: purple to dark purple

CALCULATION:

For Total Hardness,


Volume of EDTA (ml) = End reading - Start Reading
= 12.10 7.50
= 4.60 ml
For Calcium Hardness,
Volume of EDTA (ml) = End reading - Start reading
= 15.30 12.10
= 3.20 ml

1000
Total hardness (mg/l as CaCO3) = mlEDTA
mlsample
= 4.60 x 1000
100
= 46.00 mg/l as CaCO3
1000
Calcium hardness (mg/l as CaCO3) = mlEDTA
mlsample
= 3.20 x 1000
100

= 32.00 mg/l as CaCO3

Magnesium hardness = Total Hardness - Ca Hardness


= 46.00 32.00

GROUP 24 32 32
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

= 14.00 mg/l as CaCO3

DISCUSSION:
Hardness
Hardness is defined as the sum of the concentrations of calcium and magnesium
ions dissolved in water. These two ions are the major hardness constituents, and though
some other metals contribute to hardness, their concentrations in natural waters are so
much smaller that their significance as hardness is negligible.
Calcium is the most abundant dissolved cationic constituent of natural fresh
waters, and is widely distributed in the minerals of rocks and soil. It is fifth most
abundant element on earth and is found in every major land area of the world.
Magnesium is also a major constituents of rocks, in abundance second to
calcium ( about fifth as much ), and is usually found in occurrence with calcium.
The carbonate salts of calcium are the major source of dissolved calcium and are
generally referred to as limestone or calcite. They include Iceland spar ( pure ), marble
and alabaster ( less pure and more compressed ), and chalk. They can be white or
colorless. Calcium carbonate is quite isoluble in pure water and dissolves only up to 15
mg/l, but if CO2, is represent, this natural acidity make the lime stones much more
soluble. This often occurs in groundwater; bacterial action in the soil release CO2,

GROUP 24 33 33
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

changing the carbonates to bicarbonates, and dissolving large amounts of calcium into
the water. Because of this, groundwater is generally harder waters than surfaces water.
Hard water typically contains high concentration of Ca , Mg (and other) cations
which interfere with the use of the water for many application .(For example the ions
diminish the effectiveness of soaps and detergens for cleansing operations , they
diminish the drinking quality of water and contribute to accumulation of insoluble salt
deposit in storage vessels or plumbing.)

1.What are problems associated with hardness in water?


Hardness in the waters effect on scaling, corrosion, and soap. With hard water it
is difficult to produce a soap lather.
Hard waters leave spot on glasess, digny film on laundry and hair and crusty
deposits on bathroom fixtures.
The hardness will obstruct the soap bubbling and will cause sediment of ion
carbonate precipitate in the pipe and cause the pipe to be choked. It will cause
the escalating of the cost of curing the wastewater.

2.Differentiate between carbonate and non-carbonate hardness?


Carbonate hardness the hardness ion associated with carbonates and
bicarbonates ( CaCO3, Ca(HCO3)2, Mg(HCO3)2 ). A consumer term, temporary
hardness was formerly used for this type of hardness ( it precipitates when the
water was boiled, and therefore, is temporary ). It is of interest to all utilities to
keep track how much of the hardness is carbonate hardness, for this is the
component that is associated with scaling tendency in distributions piping. It
relates to the amount of alkalinity in the water.

Carbonate hardness is hardness combined with the waters alkalinity.

GROUP 24 34 34
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

Noncarbonate hardness The hardness ions associated with other anions


(CaSO4,MgSO4,MgCI2). Previously termed permanent hardness because it could
not be made to precipate by boiling the water.
The major significance in separating carbonate from nancarbonate hardness is for water-
softening calculations. Lime and soda ash dosage will depend upon the concentrations
of each two types of hardness.
If the total hardness is greater than the total alkalinity, then the difference
between them is the nocarbonate hardness.

3.Why are samples adjusted to different pH values for total and Ca hardness
determination?
The unit of the hardness is stated in CaCO3 equivalent . The water is defined as
Hard water if the hardness of the water is more than 150 mg/l as CaCO3
equivalent.And the value of soft water have the hardness in between 50-60
mg/l as CaCO3 equivalent.

4.Briefly describe the methods for hardness removal?


Process of removing hardness from water is called softening. Water softening is
a measurement of calcium and magnesium are needed to determine chemical
dosage for lime/ soda ash softening plants and the size of ion exchange softening
units.
Hardness is mainly caused by the presence of calcium and magnesium salts.The
lenght of time that water is in contact with the hardness producing material is
one factor that determines how much hardness there is in the raw water.The
soften water by the lime or soda-ash method , its degree of alkalinity has to be
considered.
The alkalinity of a water is a measure of the waters capacity to neutraliza
acids.Many of the chemical used in water treatment , such as alum , chlorine or
lime, cause changes in alkalinity.

GROUP 24 35 35
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

Two basic methods of softening water are chemical precipitation and ion
exchange.Other methods can also be used to soften water such as
electrodialysis , distillation , freezing and reverse osmosis.
Chemical precipitation is one of the more common methods used to soften
water.The chemical normally used are lime ( calcium hydroxide , Ca(OH) 2 ) and
soda ash ( sodium carbonate , Na2CO3).
Lime is used to remove the chemical that cause the carbonate and magnesium
non-carbonate hardness.Soda ash is used to remove the chemical that cause the
non-carbonate hardness.
When the lime and soda ash are added , the hardness-causing minerals form
nearly insoluble precipitates.When calcium hardness is removed in a chemical
softener , it is precipitates as calcium carbonate (CaCO 3).When magnesium
hardness is removed is a chemical softener , it is precipitated as magnesium
hydroxide (Mg(OH)2.

CONCLUSION:

From our experiment, we discover that our sample is good for experiment. From
calculation, we got very high notes for effluent sample that we used for experiment. The
result is:

Total hardness: 46.00 mg/l as CaCO3

Calcium hardness: 32.00 mg/l as CaCO3

Magnesium hardness: 14.00 mg/l as CaCO3

Weve learnt that from our syllabus, those water need to recycle to be drink or for
housework to be done. The data shows that the total hardness is more that it should be.
From books, we already know that total hardness for water is given the value of 500 and
below. So, the sample is totally can be drink daily as the experiment show. After all, we
just have to remove the colour and the water is ready to be drink. Weve refer to the
Malaysian Standard for water drinking to determine total hardness that the water should

GROUP 24 36 36
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

have. Finally, it is shown that hardness is a factor, besides other factor as pH, the colour
and minerals in the sample

REFERENCE:

1. Introduction To Environmental Engineering,


3rd Edition, Mackenzie L.Davis,
McGraw-Hill, ms 133-160

2. Water & Wastewater Engineering Volume 2,


Gordon Maskew, John Charles Geyes & Daniel Alexander Okun,
John Wiley & sons

3. Kejuruteraan Air Sisa, Kualiti Air dan Air Sisa, Hamidi Abdul Aziz (1999),
Utusan Publication & Distributors Sdn Bhd, ms 19-30

4. Kejuruteraan Air Sisa, Modul 1, Dini Ramya Hasan Basri, ms 15-20

5. Bekalan Air, Pembetungan dan Pengiran, Nik Ahmad Fuaad Nik Abillah, ms 61-
74.

GROUP 24 37 37
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

DECLARATION

E1 USE OF pH METER, DETERMINATION OF ACIDITY


AND ALKALINITY WATER SAMPLES, DETERMINATION OF
SOLIDS AND HARDNESS IN WATER
8 JULY 2004

WE, hereby make the declaration that we have successfully carry out
the experiment with cooperation from each member in the group. In order
to complete this lab report we have equally divided the jobs to every
member in the group.

NAME MATIRC NUM. JOB SIGNATURE


TING PING WANG 70260 EDIT, REFERENCE,
DECLARATION
IVAN LASANUL 70178 PROCEDURE,
TSEN SAM PAK TEORY,
APPARATUS
MOHD. MAZRI BIN 72917 CALCULATION
ZAHARI
MOHD. OZAIRIEE 70210 RESULT

GROUP 24 38 38
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

ABDUL AZIZ
MARSHIDAH 70195 DISCUSSION,
MUSTAPA CONCLUSION

APPENDIX
GROUP 24 39 39
EAA305 ENVIRONMENTAL ENGINEERING LABORATORY
EXPERIMENT 1 USE OF pH METER, DETERMINATION OF ACIDITY AND ALKALINITY WATER SAMPLES
EXPERIMENT 2. DETERMINATION OF SOIL AND HARDNESS IN WATER

GROUP 24 40 40

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