Experiment # 2

“How to determine the hardness of water and waste water”

Standard procedure:
APHA Standard Methods for Examination of Water and Waste Water- Method 2340 C

Method for Chemical Analysis of Water and Waste Water EPA 600/4-79-020 USEPA Method 130.2

Aim:
To determine the total hardness of given water sample as per standards

APPARATUS

 Wash bottle
 Pipettes
 Pipette bulb
 Conical flask
 250ml Graduated cylinder
 Standard flask
 Beaker
Chemical Required
 Ammonium Hydroxide
 EDTA
 Ammonium chloride
 Erichrome Black T
 Magnesium sulphate
PROCEDURE
 Take 50ml of water sample in conical flask.
 Add 1ml of buffer solution (Aluminum Hydroxide n Ammonium Chloride) of
hardness1.
 Add 3 drops of ferrochrome black T to the flask and shake well.
 Place the flask below the burette containing EDTA (Ethylene diamine tetra-acetic
acid) solution of 0.02 normality.
 Note the initial reading of the burette and open the tape of the burette to allow
the solution to flow in the flask.
 Note The Final Reading when the color of the water in the flask turn bluish

RESULTS AND CALCULATION

Total hardness= (IR-fR)*N*50*1000/50
Result is 266 mg/L
Hard water is classified as given in the table.
Description Hardness range (mg/L as CaCO3)
Soft <75
Moderately Hard 75‐100
Hard 100‐300
Very Hard >75
The common water treatment goal is to provide water with a hardness in the range of
75 to 120
Experiment # 02
“How to determine dissolved oxygen in Water and Wastewater”
Standard procedures:
APHA Standard Methods for the Examination of Water and Wastewater - 20th Edition. Method
4500
Methods for Chemical Analysis of Water and Wastes, EPA-600/4-79-020, USEPA, Method 360.1
REAGENT LIST
 2ml Manganese sulphate
 2ml alkali-iodide-azide
 2ml concentrated sulphuric acid
 2ml starch solution
 Sodium thiosulphate
ENVIRONMENTAL SIGNIFANCES
 Drinking water should be rich in dissolved oxygen for good taste.
 DO test is used to evaluate the pollution strength of domestic and industrial waste.
 Higher values of DO may cause corrosion of Iron and Steel.
 Algae growth in water may release oxygen during its photosynthesis and DO may even
shoot up to 30 mg/L.

WHY 201ml

Remember that in 200 mL sample, 1 mL of sodium thiosulfate of 0.025N equals to 1

mg/L dissolved oxygen.

 The sample is actually 201ml with ml starch indicator.

 We add starch to titration mixtures that involve iodine because the color change
is highly visible. Starch is a viable indicator in the titration process because it
turns deep dark blue when iodine is present in a solution. 
 Starch forms a complex with iodine. It is the complex which is the indicator.
RESULTS
Our water sample has DO=6.3mg/L
Experiment # 3 & 4
“How to determine total dissolved and suspended solids in Water and
Wastewater”
ENVIRONMENTAL SIGNIFICANCE
 Dissolved minerals, gases and organic constituents may produce aesthetically
displeasing color, taste and odor.
 Some dissolved organic chemicals may deplete the dissolved oxygen in the receiving
waters.
 Water with higher solids content often diarrhea and sometimes the reverse effect upon
people whose bodies are not adjusted to them.
 High concentration of dissolved solids about 3000 mg/L may also produce distress in
livestock. In industries, the use of water with high amount of dissolved solids may lead
to scaling in boilers, corrosion and degraded quality of the product.
Total Suspended Solids
Some suspended solids can settle out into sediment at the bottom of a body of water over a
period of time. Heavier particles, such as gravel and sand, often settle out when they enter
an area of low or no water flow. 
PROCEDURE
Determine by two methods
 By Gravimetric method
 By spectrophotometer

A=weight of the filter paper, g

B=weight of filter paper + residue dried at 105C
C=weight of filter paper + residue upon ignition at 550C
RESULT
Our sample contain 47mg/l TSS (spectrophotometer)
Experiment#6
To Determine the Alkalinity of Water
Definition
Alkalinity of a water is its acid-neutralizing capacity

Environmental Significance
 The alkalinity of a body of water provides information about how sensitive that water
body will be to acid inputs such as acid rain.
 Turbidity is frequently removed from drinking water by coagulation and flocculation.
This process releases H+ into the water. Alkalinity must be present in excess for effective
and complete coagulation to occur.
 Hard waters are frequently softened by precipitation methods. The alkalinity of the
water must be known in order to calculate the lime (Ca(OH)2) and soda ash (Na2CO3)
requirements for precipitation.
 Alkalinity is important to control corrosion in piping systems.
 Bicarbonate (HCO3) and carbonate (CO3) may complex with other elements and
compounds, altering their toxicity, transport, and behavior in the environment.
In the lab we will assume that the entire alkalinity is attributed to bicarbonate, carbonate,
and hydroxide. According to this scheme.
 Carbonate (CO3) alkalinity is present when phenolphthalein alkalinity is not zero but
is less than total alkalinity.
 Hydroxide (OH–) alkalinity is present if phenolphthalein alkalinity is more than half
the total alkalinity.
 Bicarbonate (HCO3) alkalinity is present if phenolphthalein alkalinity is less than half
the total alkalinity.

Phenolphthalein Alkalinity = Amount of acid used to reach pH 8.3 (ml) * Normality

of acid (eq/L) * 100,000 (mg CaCO3/eq) / sample volume (ml)

Total Alkalinity = Amount of acid used to reach pH 4.5 (ml) * Normality of acid
(eq/L) * 50,000 (mg CaCO3/eq) / sample volume (ml)
‘‘Phenolphthalein alkalinity’’
Is the term traditionally used for the quantity measured by titration to pH 8.3?
Procedure
 Measure 50 ml or 100 ml of your sample into a 250 mL beaker or flask. Place your
sample onto a stir plate (make sure to put a bar magnet in the flask).
 Measure initial pH of your sample. If the sample pH is below 8.3 (if above 8.3, do step 3
first), add several drops of bromcresol green indicator. If the color of the solution turned
blue, titrate your sample with 0.02 N H2SO4 or HCl (you may need to dilute the acid
provided in the lab) until the color changes to yellow (pH 4.5). Record the total volume
of acid used for the titration.
 Measure initial pH of your sample. If the sample pH is above 8.3, add several drops of
phenolphthalein indicator. If the color of the solution turned pink, titrate your sample
with 0.02 N H2SO4 or HCl (you may need to dilute the acid provided in the lab) until
color changes from pink to clear (pH 8.3). Record the volume of acid used for the
titration.
 Calculate both Phenolphthalein Alkalinity and Total Alkalinity using the formula.

TYPES OF ALKALINITY
Titrations can distinguish between three types of alkalinity; carbonate, bicarbonate, and total
alkalinity.
Carbonate alkalinity is determined by titration of the water sample to the phenolphthalein
indicator endpoint, or approximately a pH of 8.3.
Total alkalinity is determined by titration of the water sample to the endpoint of the methyl
orange indicator, or an approximate pH of 4.5.
The difference between the two is the bicarbonate alkalinity
RESULT
Our water sample contain total alkalinity of 180mg/l
Phenolphthalein alkalinity 337mg/l
 Experiment # 7
“How to determine chlorides in Water and Wastewater”

 Chloride, in the form of the Cl– ion, is one of the major negative ions, in saltwater and
freshwater. It originates from the dissociation of salts.
Sources of chloride in water
The Sources of chloride in water may be natural or human beings. The natural sources are
surrounding rock or soil or seawater intrusion in coastal areas. Whereas, various human
sources are fertilizers, road salting, wastewater from industries, animal feeds, septic tank
effluents etc.
Environmental Significance
 Chlorides associated with sodium (Sodium Chloride) exert salty taste when its
concentration is more than 250 mg/L. These impact a salty taste to water.
 Chlorides are generally limited to 250 mg/L in water supplies intended for public water
supply.
 In many areas of the world where water supplies are scarce, sources containing as much
as 2000 mg/L are used for domestic purposes without the development of adverse
effect, once the human system becomes adapted to the water.
Procedure
 Measure the pH of the water sample.
 Take a 25 ml collected water sample into a conical flask.
 Add 2-3 drops potassium chromate (K2CrO4) indicator. The color of the water sample is
turn into light yellow.
 Add standard silver nitrate solution (0.0141N) from the burette and shake well. Titrate
until the light yellow color changes to permanent brownish-red color (bricks-red color).
 Note the volume of silver nitrate added.
 Repeat the titration.
 Calculate chloride ion concentration
Formula
Chloride= (IR-fR)*N*35.45*1000/volume of sample
 From reading we subtract (.2-.4) blank.
 Our sample contain 41mg/l of chloride.
Experiment # 8
“How to determine Sulphites in Water and Wastewater”
Environmental significance
 Sulphates are of considerable concern because they are indirectly responsible for two
serious problems often associated with the handling and treatment of wastewater. They
are bad smell and sewer corrosion problem result from the reduction of sulphates to
hydrogen sulphide.
 The amount of sulphates in wastewater is a factor of concern in determining the
magnitude of problems that can arise from reduction of sulphates to hydrogen sulphide.
 For example knowledge of the sulphites content of the sludge or waste fed to digestion
units provides a means of estimating the hydrogen sulphide gas produced.
Iodometric titration
 Iodometry, also known as Iodometric titration, is a method of volumetric chemical
analysis, where the appearance or disappearance of elementary iodine indicates the
end point.
Reagents
 Hydrochloric acid
 Standard iodine solution (0.025N)
 Standard sodium thiosulphate solution (0.025N)
 Starch solution
Procedure
 Take 200ml of water sample under the surface.
 Add Iodine solution.
 On disappearance of color add some more iodine solution
 Add 2 mL of 6 N HCl.
 . Titrate with sodium thiosulphate solution, adding a few drops of starch solution, as the
end point is approached and continuing until the blue color disappears.
Calculation
Mg/L sulphide = (a – b) x Eq wt x1000/ vol of sample
Where, a = mL 0.025 x N iodine used
b = mL 0.025 x N sodium thiosulphate solution used.
Result our sample contain 7.2mg/l of sulphide

Experiment # 10
“How to determine chemical oxygen demand”

 COD determines the quantity of oxygen required to oxidize the organic matter in water
or waste water.
 The chemical oxygen demand (COD) test is commonly used to indirectly measure the
amount of organic compounds in water.
Environmental Significance
 COD values are particularly important in the surveys designed to determine and control
the losses to sewer systems.
 The ratio of BOD to COD is useful to assess the amenability of waste for biological
treatment.
 Ratio of BOD to COD greater than or equal to 0.8 indicates that wastewater highly
polluted and amenable to the biological treatment.
 It is useful to assess strength of wastes, which contain toxins and biologically resistant
organic substances.
 BOD value is always lower than COD value. For domestic and some industrial
wastewater, COD value is about 2.5 times BOD value.
Relationship between BOD and COD
 There are not ratio between COD and BOD which correspond with all type of
wastewater.
 The quality of wastewater is different from a source of discharge to another and from a
region to another.
 However, for exemple in France, one usually assumes that, for domestic wastewater, 2 <
COD/BOD5 < 3; for wastewater from food-industries, 1,5 3.
 It varies for different wastewaters, the ratio commonly being 25-75% of COD
Interrelationship between BOD, COD
 Typical values for the ratio of BOD/COD for untreated municipal wastewater are in
the range from 0.3 to 0.8 (see in table 3). If the BOD/COD ratio for untreated
wastewater is 0.5 or greater, the waste is considered to be easily treatable by
biological means. If the ratio is below about 0.3, either the waste may have some
toxic components or acclimated micro-organism’s may be required in its
stabilization.
Procedure
  Prior to completing the COD test, a series of known standards are prepared using
KHP (potassium hydrogen phthalate). Most wastewater samples will fall in the high
range, so standards of 100, 250, 500 and 1000 mg/L are typically prepared. COD
standards can also be purchased.
 A COD reactor/heating (150°C) block and a colorimeter are turned on so that both
instruments are allowed to stabilize.
 Pre-prepared low-range (3-50 ppm) or high-range (20-1500 ppm) vials are selected
for the COD test based on expected results. Both ranges can be used if expected
results are unknown.
 One vial is marked as a “blank,” and three or four vials are marked with known
standard levels. Two vials are then marked for the wastewater sample to make a
duplicate run. Note: If multiple wastewater samples are being run, at least 10% of
samples are duplicated.
 2 mL of liquid are added to each vial. In the case of the “blank,” 2 mL of DI water are
added. 2 mL of each standard are added to the corresponding vials. If the
wastewater sample is tested at full strength, then 2 mL is added to the
corresponding vial. If dilution is required, then serial dilutions are performed and 2
mL of the diluted sample are added to the corresponding vial.
 Each vial is mixed well and placed into the reactor block for two hours. After two
hours, the vials are removed from the block to a cooling rack for about 15 minutes.
 The colorimeter is set and calibrated per the specific instructions for that unit (i.e.,
proper wavelength, blank and standards) and each vial is placed in the unit and the
COD concentration read.
 If the sample was diluted, the corresponding multiplication is made.
Blank solution
 A Blank solution is one that do not have any chemical that you are looking for or
measuring or detecting. Usually, it can be as simple as just plain distilled water if you are
measuring an aqueous solution.
 The BLANK is all those items EXCEPT your desired chemical. 
Sometimes, a blank MAYBE loosely called a "control" solution. 
Experiment # 1
Turbidity of water
Water is said to turbid when it is seen containing materials of suspension inside it. While
turbidity may be defined as the measure of visible material in suspension in water, turbidity
may be caused by algae or other organisms. It is generally caused by silt or clay.
There are various units for the measurement of turbidity which are
 Standard turbidity unit[mg/lit or ppm]
 Jackson turbidity unit [J.T.U]
 Nephelometric turbidity unit [N.T.U]
 A device called nephelometric turbidity measures the turbidity of water in N.T.U the
intensity of light after passing through the water gives a measure of turbidity of water.
WHO guideline value:
 WHO suggested a guideline value for turbidity as [N.T.U]for disinfection the turbidity of
water should be less than 1 N.T.U
Apparatus:
W.H.O Nephelometric turbidity meter for mazine solution of the sample by multiplying the
scale reading by 0.9 N.T.U, 9 N.T.U, 99 N.T.U, test tubes and water sample’s.
Procedure:
 Switch on the power supply and check the battery of the turbidimeter,
 Press the 1 N.T.U button and coincide the scale with zero by using focusing template.
 Again press 1 N.T.U button and coincide the scale with zero using the focusing template.
 A Standard formazine solution of N.T.U is placed on tubidimeter in the path of rays and
scale is brought 9 n.t.u
 The Water sample is taken in a test and is placed in turbidimeter.
 Use a Cell rise if the turbidity is more than 100 N.T.U and get the turbidity dilution
factor.
The dilution factor to calculate the turbidity of the original sample 31.
NTU = (A * (B + C)) / C
A = NTU found in diluted sample
B = volume of dilution water, mL
C = sample volume taken for dilution, mL