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Lab Manual
Submitted TO
Prof. Dr. Imran Hashmi
Submitted BY
Abid Hameed
IESE NUST
Islamabad
DO:
..
Keep only currently needed chemicals in the lab, and restricts lab work to the lab.
Know how to use emergency eyewash, safety shower, and fire extinguisher.
Keep food, food containers, or drinking glasses out of areas or refrigerators that
contain chemicals.
Wash thoroughly when leaving the lab and before eating, drinking, smoking,
chewing gum, or applying makeup.
DON'T:
Signature: _________________
Experiment No 1
Title:
Determination of alkalinity ?
Introduction:
Capacity of water to neutralize acid is called alkalinity. There are three types of
alkalinity which can be classified due to the presence of hydroxyl, carbonate and
bicarbonate ions.
i.
ii.
iii.
Principle of alkalinity is acid base titration in which standard (H2SO4 of 0.02N) acid is
used for titration. Phenolphthalein and methyl orange are used as indicator in this
regard.
Alkalinity of water may be due to the presence of carbonates, hydrogen carbonates,
silicates, borates, phosphates and hydroxyl ions in Free State. The primary source of
alkalinity in drinking water is due to carbonate containing rocks which come from lands
and mountains due to the erosion and weathering processes of rocks. Runoff of water
from agricultural land where lime is also applied contains carbonate which can cause
alkalinity in water. Phosphates and silicates are rarely found in natural supplies in
concentrations significant in the home.
Moderate concentration of alkalinity in water is also desirable so that corrosion of water
pipelines can be prevented and water can be prevented from contamination of copper
and lead because low alkalinity causes corrosion of pipelines. While high alkalinity
produces soda like taste in water. Water with low alkalinity is also not fit for bathing
purpose because it can remove too much oil from skin and causes dryness.
Alkalinity can be removed by reverse osmosis, distillation and softening.
Reagents:
Procedure:
1. Take 50ml of sample in a flask.
2. Add 2-3 drops of phenolphthalein indicator.
3. If a pink color appears titrate with 0.02 N H2SO4 until pink color disappears it will
give us phenolphthalein alkalinity.
4. Add 2-3 drops of methyl orange and titrate until yellow color changes to pink.
This is total alkalinity.
So ,
Phenolphthalein Alkalinity = Volume of Acid used X Normality X 50000
Vol. of sample
Experiment No 2
Title:
Determination of hardness in tap water.
Objectives:
To find out hardness in tap water.
Introduction:
Water having divalent (Ca+2, Mg+2, Fe+2, Mn+2 etc.) and trivalent (Al+3 etc.) cations is
called hard water. Major hardness is due to the presence of Ca +2 and Mg+2 ions. Rain
water is soft naturally but when falls on ground picks up natural hardness minerals like
calcium and magnesium and converts into hard water.
Principle:
Hardness of water is determined by using titrimitric method in which sample is titrated
against chelating agent Ethylene Diamine Tetra Acetic Acid (EDTA) while Eriochrome
Black Tea (EBT) is used as an indicator. Ca+2 and Mg+2 ions are chelated by EDTA and
complex componds are formed.
Impacts of Hardness (Draw backs):
Hard water causes scaling (CaCO3 & Mg(OH)2) in hot water systems, kettles, electric
irons and domestic appliances. Scaling of heating elements shortens their life and
makes appliances less efficient because high fuel/electricity is required to heat them.
Scaling also results the blockage of pipes which may cause huge security hazards.
Ca+2 + 2HCO3- CaCO3 + H2O +CO2
(scales)
Hard water produces less lather from soap, washing up liquid and washing powders. It
also leaves spots on basins, sinks, baths and toilets.
2C17H35COONa + Ca+2 (C17H35COO)2Ca + 2Na+
(water soluble)
(insoluble ppt)
Health Impacts:
Hard watre is not hazardous for health. Actually, hard water contributes a small amount
of Ca and Mg human dietry needs. In this regard, well known brands of bottled water
supplier maintain hardness of water upto some extant and this characteristic is also
important for the bright appearance of water as well.
Hardness Scale:
A scale is also developed known as hardness scale which is given below:
Hardness Description
Hardness mg/l
CaCO3
Soft
0-50
Moderately Soft
50-100
Slightly Hard
100-150
Moderately Hard
150-200
Hard
>200
Very Hard
>300
Reagents
Procedure
Sr.No
reading Volume
ml
ml
ml
17.5
17.5
17.5
33.2
15.7
16.2
16.2
Mean volume of EDTA used for Tap water sample is 16.3 ml.
16.3
Sr.No
reading Volume
ml
ml
ml
0.1
0.1
0.1
0.2
0.1
0.2
0,3
0.1
0.1
Mean volume of EDTA used for Distilled water sample is 0.1 ml.
Formula
Hardness of water as mg/l CaCO3 = A B 1000 / Volume of Sample (ml)
Where,
A= Mean volume of EDTA used for Tap water sample
B= Mean volume of EDTA used for Distilled water sample
So by putting values
= (16.3 0.1) X 1 X 1000
50
= 324 mg / L
Result
So the hardness in tap water is 324 mg / L.
Discussion:
Above calculations show that tap water sample is hard water but may be used for
drinking purpose because National Standards for Drinking Water Quality (NSDWQ) for
Pakistan provides maximum limit of 500mg/l as CaCO3 for drinking water. So, water is
not hazardous for human health.
Reference:
http://dwi.defra.gov.uk/consumers/advice-leaflets/hardness.pdf
http://www.environment.gov.pk/act-rules/DWQStd-MAY2007.pdf
http://www.water-research.net/hardness.htm
National Standards for Drinking Water Quality (NSDWQ), June, 2008, Government of
Pakistan, Pakistan Environmental Protection Agency.
Experiment No 3
Title:
Determination of Total Chlorine in Water Sample.
Objectives:
Core objective of the analysis is to find out the concentration of total chlorine in water
sample and recommend some mitigation measures to reduce excessive amount of free
chlorine in sample. Importance of free chlorine for disinfection of water will also be
explored.
Introduction:
Chlorine is one of the most widely used disinfectants for water. It is very effective for the
deactivation of pathogenic organisms and makes water fit for human consumption. This
process is also known as chlorination. It is also used for disinfection of pathogens in
swimming pools.
Chlorine forms hypochloric acid on dissolution in water which further dissociates into
HCl and nascent oxygen. Nascent oxygen is a strong oxidizing agent as well as a
disinfectant.
Cl2 + H2O HOCl + HCl
HOCl HCl + [O]
Mainly chlorine gas and hypochlorites (NaOCl and Ca(OCl)2) are used for chlorination in
water.
NaOCl + H2O OCl- + Na+
Ca(OCl)2 + H2O 2OCl- + Ca+2
Different forms of chlorine in water:
Free Chlorine
Free chlorine may be available in water in three forms at different pH (Cl2 at pH < 5,
HOCl and OCl- at pH 5-8, OCl- at pH > 10). Best pH range for disinfection is 5-6.
Combined Chlorine
Chlorine combines with organic compounds and forms chlorinated organic compounds
like in the case of alkyl, amine etc. Chloramines are produced when NH3 and
corresponding chloramines react with HOCl.
NH3 + HOCl H2O + NH2Cl (Monochloramine)
NH2Cl+ HOCl H2O + NHCl2 (Dichloramine)
NHCl2 + HOCl H2O + NCl3 (Trichloramine)
Principle:
Total chlorine is determined by using titrimetric method where sample is titrated against
Sodium Thiosulphate (Na2S2O3) of 0.01 Normality. Starch solution is used as an
indicator.
Advantages:
Highly effective against most pathogens.
Provides a residual to protect against recontamination and to reduce bio-film
growth in the distribution system.
Easily applied, controlled, and monitored.
Strong oxidant meeting most pre-oxidation objectives.
Operationally the most reliable.
The most cost-effective disinfectant.
Limitations:
Byproduct formation (THMs, HAAs) which are toxic for aquatic life.
Will oxidize bromide to bromine, forming brominated organic byproducts.
Not effective against Cryptosporidium.
Requires transport and storage of chemicals.
Reagents
Procedure
1. Take 5 ml of conc. Acetic acid in conical flask.
2. Add one gram of Potassium iodide in a conical flask.
3. Add 100 ml water sample in conical flask yellow or brown color will appear if cl2
is present.
4. Titrate against STD Na2SO3 (0.01M) Solution.
5. Titrate until yellow color becomes light yellow.
6. Add 1 ml of starch solution. The solution will become blue.
7. Titrate until blue color disappears. Take total volume of Na2SO3.
Total chlorine =
(A+B) N35450
Vol of sample
Final reading
Difference
1.1
1.1
Initial reading
Final reading
Difference
1.1
1.5
0.4
Discussion:
Result from above calculation show that sample contain 5.31 mg/l total chlorine which is
beyond limit as prescribed in National Standards for Drinking Water Quality, Pakistan.
As mentioned in NSDWQ that concentration of chlorine at consumers end should be
0.5-0.2 ppm while at source concentration of chlorine in drinking water should be 1.50.5 ppm. As mentioned earlier, concentration of chlorine in sample is beyond limit so it
has to be lowered within prescribed limits so that no health hazard can occur. For this
purpose aeration has to be done to lower the value of chlorine.
References:
http://www.lenntech.com/processes/disinfection/chemical/disinfectants-chlorine.htm
http://www.waterandhealth.org/drinkingwater/wp.html
Chemistry for Environmental Engineers by Dr. Ishtiaq A. Qazi
National Standards for Drinking Water Quality (June, 2008), Ministry of Environment,
Pakistan.
Experiment:
Determination of Total Dissolved and Suspended Solids in Water
Objective
To characterize the water sample with respect to total solids, total dissolved solids and
suspended solids in the given water samples
Introduction
The total dissolved solids are defined as solids that are filterable in nature and are completely
dissolved in water. After evaporation of filterable sample the residue left is termed as Dissolved
Solids.
Suspended Solids are non-filterable in nature and are not dissolved in water. It is residue of
non-filterable sample upon evaporation.
Principle
A properly mixed sample is filtered through a Glass Fiber Filter paper. Filtrate is dried in a
weighted porcelain china dish to constant weight at 179-181 0C in the oven or on the burner.
Weigh the china dish, increase in weight represents the Dissolved Solids.
A properly mixed sample is weighted through a preweighted glass fiber and the residue
retained on filter paper is dried at constant weight 103-105 0C. The increase in the weight of
filter represents the weight of Suspended Solids.
A properly mixed sample is added in pre weighted china dish. It is evaporated in water bath
and dried in oven 103-105 0C for one hour. Weigh the china dish, increase in weight represents
Total Solids
Sample Handling and Preservation
Sample preservation is necessary because biological activity will continue after collection of
sample and changes may occur during handling and storage. These things may change the
characteristics of amount of solids.
To avoid the change certain measures are taken which are as follows
Precautions
Water or waste water samples which contain high amount of chlorides, magnesium
or sulfate rapidly absorbs moisture from air. Therefore, samples are kept in
desiccators to achieve reasonable constant weight
Samples with high concentration of bicarbonates need additional drying at 180 0C to
ensure all bicarbonates to carbonates
Prolong drying may lose constituents from samples particularly nitrates or chlorides
0.0178mg/l
Discussion
The Total Dissolved Solids of the given sample (614mg/l) is under the permissible limit of the
National Environmental Quality Standards (1000mg/l). There are no available quality
standards for Total Suspended Solids and Total solids in National Environmental Quality
Standards and World Health Organizations. Reliable data on possible health effects associated
with the ingestion of TDS in drinking water are not available. The results of early
epidemiological studies suggest that even low concentrations of TDS in drinking-water may
have beneficial effects, although adverse effects have been reported in two limited
investigations.
Water containing TDS concentrations below 1000 mg/liter is usually acceptable to consumers,
although acceptability may vary according to circumstances. However, the presence of high
levels of TDS in water may be objectionable to consumers owing to the resulting taste and to
excessive scaling in water pipes, heaters, boilers, and household appliances. Water with low
concentration of TDS is also unacceptable for consumers because of its flat and insipid taste
Environmental Significance
Dissolved mineral , gases and organic constituents may produce displeasing taste,
odor or color
Dissolved organic chemicals may deplete the dissolved oxygen in receiving water
and may be inert to biological oxidation
High concentration of dissolved solids may produce distress in livestock.
Estimation of total dissolved solids is useful to determine the quality of drinking
water
Suspended organic solids which are degraded anaerobically may release obnoxious
odor
Biological active suspended solids may include disease causing organisms as well as
organisms such as toxic producing strains of algae
Suspended solids exclude light, thus reducing growth of oxygen producing plants
References
Hydrology project; World Band and Government of Netherlands funded. 1999. How to
measure dissolved suspended and total solids. Training module. New Delhi. India
APHA Standard Methods of Examination for water and waste water- 20th Edition.
Method 2540 C and 2540 D
Tihansky DP. Economic damages from residential use of mineralized water supply.
Water resources research, 1974, 10(2):145
International Organization for Standardization. Water qualitydetermination of
electrical conductivity. Geneva, 1985 (ISO 7888:1985).
Introduction
COD test is widely used to measure the organic strength of domestic & industrial
wastewater [1]. Chemical oxygen demand (COD) is defined as a measure of the oxygen
equivalent of the organic matter content of a sample that is susceptible to oxidation by a
strong chemical oxidant [2]. COD, which can indicate the level of pollution for water
contaminated by reductive pollutants, is the main determinant used to assess organic
pollution in aqueous systems and is one of the most important parameters in water
monitoring.
Blank
Synthetic Waste
Water Sample
2.5
1.4
2.5
0.9
2.5
0.92
2.5
0.9
= 0.9
REFERENCES
1- Standard Methods for the Examination of Water and Wastewater. (1989),
American Public Health Association, Washington, DC, 17th Edition, p. 510.
2- Alexandra M.E. Viana da Silva, Ricardo J.N. Bettencourt da Silva, M. Filomena,
G.F.C. Camoes. (2011), Optimization of the determination of chemical oxygen
demand in wastewaters, Analytica Chimica Acta.
OBJECTIVE
Determination of number of colonies of E.coli present in tap water sample by using Membrane
Filtration Technique.
INTRODUCTION
Escherichia coli, also referred to as E. coli, is a type of fecal coliform bacteria that is found in the
intestines of healthy warm-blooded animals and humans. Most E. coli strains are harmless and
serve a useful function in the body by stopping the growth of harmful bacteria species and by
making necessary vitamins. However, some strains can be opportunistic pathogens, while others
can cause gastrointestinal illness in healthy humans when ingested. An opportunistic pathogen is
an organism that normally lives inside a host without causing injury, but can cause infection in
people with weakened immune systems. E. coli is present in the large intestine, so it will be
present in fecal matter from humans and animals. If recent contamination of water sources with
sewage or animal waste has occurred, E. coli will be present [1].
OBSERVATIONS AND CALCULATIONS
Calculate the number of E.coli count (CFU) per 100ml of sample according to the following
general rule.
Total number of E.coli colonies found: 10
E.coli/100ml = Number of E.coli colonies 100
Volume of sample filtered (ml)
= 10 100
100
= 10 E.coli/100 ml
DISCUSSION
The discharge of municipal wastes is one of the most important water quality issues world-wide
that results in contamination of drinking water. The sewage contains human feces and water
contaminated with these effluents may contain pathogenic organisms which are hazardous to
human health if used as drinking-water or in food preparation. Fecal contamination of water is
routinely detected by microbiological analysis. For this purpose membrane filter technique is
used for the analysis of water samples. It gives a direct count of total coliforms and fecal
coliforms present in a given sample of water. The organisms used most commonly as indicator
organisms for the detection of the recent contamination are E.coli and coliform group (bacteria
having fecal origin) as whole, as they are easy to detect. By using membrane filtration technique,
10 E.coli colonies per 100ml are found in the tap water sample.
According to National Standards for Drinking Water Quality (NSDWQ) the number of colonies
should be zero per 100ml of the water so that it could be fit and safe for drinking water [2].
Similarly World Health Organization (WHO) guidelines give the same standard for drinking
water [3]. It shows that the sample we have tested is not fit for the drinking purpose as it contains
10 E.coli per 100ml of water which is far exceeding the standard value. The presence of E.coli in
water sample is a strong indication of recent sewage or animal waste contamination. Some E.coli
outbreaks are also caused by some lakes and private wells. These bacteria are capable of causing
illness. The presence of total coliform bacteria may also indicate a breakdown in the treatment
process, or growth in the distribution system. So it is important to discover and remove the
source of pollution for safe drinking water purpose. That is why tap water contains chlorine and
has undergone ozone or ultraviolet treatment [4] .
REFRENCES
1. http://www.safewater.org/PDFS/resourcesknowthefacts/Detailed_Escherichia_Coli.
pdf
2. National Standards for Drinking Water Quality. (2008), Pakistan Environmental
Protection Agency (Ministry of Environment), Government of Pakistan.
3. European standards for drinking water, second edition, World Health Organization
Geneva, 1970.
4. "What Is E. Coli? (Escherichia Coli)." Medical News Today. MediLexicon, Intl., 8 Jun.
2011. Web.
Discussion:
Elements
Percentage
Si
66.02
3.69
Ca
16.06
Ti
1.34
0.036
Cr
0.0425
Mn
0.2478
Fe
12.3651
Rb
0.0373
Sr
0.0572
Zr
0.0866