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UNIVERSITY OF COLOMBO – SRI LANKA

FACULTY OF TECHNONOGY

BBST (Hons) Degree in Environmental Technology


Second Year – Semester I
Tutorial 1 – June 2021
ET 2301 Analytical Techniques for Water Studies (Theory)

Date: 27th July 2021 Index No: 2019t00572

1.
(i) Where is most of the fresh water on the Earth located?
In the frozen polar ice caps

(ii) Why water is defined as a fugitive resource?


Water is known as a fugitive resource because that means that-unlike land, food,
trees, minerals or even people-when left alone water is constantly on the run,
trying to escape and moves freely between properties and that may be claimed
by any property into which the resource moves.

(iii) Define the following terms given below.


a- Infiltration Capacity (F)
The maximum rate at which a soil is capable of absorbing water in a given condition.
b- Overland Flow
The movement of water over the land, downslope toward a surface water body.
c- Field Capacity
The water-retaining capacity of a soil usually including both the hygroscopic and
capillary water of the soil and being expressed as a percentage of the dry weight of
the soil.
d- Infiltration and Percolation
Infiltration is defined as the movement of water through the soil surface into the
soil profile. Percolation specifically refers to the movement of water within the soil,
while infiltration refers to water entering the soil surface.
e- Water Seepage
Water seepage is when water flows from one place to another via small holes or
porous material.

(iv) What is the difference between “Blue Water” and “Green Water”?
Blue Water Green Water
The surface water and groundwater which The water that is consumed by the vegetation
are intimately intertwined are the "blue through transpiration is called "green
water". water".

(v) Fill in the blank in below diagram.

(a) Green water

(b) Blue water

(c) Grey Water

2.
(i) What are the renewable water resources? Briefly explain.
Renewable water resources are computed on the basis of the water cycle. They represent
the long-term average annual flow of rivers (surface water) and groundwater. There is
two type of renewable water resources called Natural and actual renewable water
resources.
Natural renewable water resources are the total amount of a country’s water resources
(internal and external resources), both surface water and groundwater, which is
generated through the hydrological cycle. The amount is computed on a yearly basis.
Actual renewable water resources are defined as the sum of internal renewable
resources and external renewable resources, taking into consideration the quantity of
flow reserved to upstream and downstream countries through formal or informal
agreements or treaties and possible reduction of external flow due to upstream water
abstraction. Unlike natural renewable water resources, actual renewable water
resources vary with time and consumption patterns and, therefore, must be associated
to a specific year.

(ii) What are the factors that affect the total water quantity of a particular surface water
resource at a given time period.
• Storage Capacity
• Permeability
• Runoff Characteristics
• Timing of the Precipitation
• Local Evaporation rates.

(iii) What is meant by water resource management? What are the major issues/challenges of
the water resource management in Sri Lanka?
Water Resources Management is the process of planning, developing, and managing
water resources, in terms of both water quantity and quality, across all water uses.
It includes the institutions, infrastructure, incentives, and information systems that
support and guide water management.
Major issues/challenges of the water resource management in Sri Lanka
 Variability in water availability
 Climate change
 Water pollution and degradation of watersheds
 Water stress due to population growth
 Government influence (Government policy and budgeting)
 Water rights, trading and partnerships Severe deterioration of
infrastructure facilities
 Lack of community involvement and new technology

3.
(i) What are the preparations that needs to be performed prior to a water sampling field work?
Paperwork:
 Itinerary
 Inventory details of sampling stations; maps
 List of samples required at each sampling station
 List of stations where water level readings are to be recorded
Co-ordination:
 Local co-ordination, for example, to ensure access to sites on restricted or
private land
 Institutional co-ordination, for example, for travel arrangements or sample
transport
 Notify laboratories of expected date and time of sample arrival
 Check any available sources of information on local weather conditions and
feasibility of travel
For sampling:
 Sample bottles, preservatives, labels and marker pens
 Sample storage/transit containers and ice packs
 Filtering apparatus (if required)
 Samplers/sampling equipment
 Rubber boots, waders, etc.
 Standard operating procedures for sampling
 Spares of all above items if possible and when appropriate
For documentation:
 Pens/wax crayons
 Sample labels
 Field notebook
 Report forms
Safety:
 First-aid kit
 Waders, gloves, etc.
 Fire extinguisher (if appropriate)

(ii) What are precautions needed to be considered while collecting and transporting the water
sample?
 Before collecting sample, make sure that you are at the right place. This can be
determined by the description of the station, from the position of landmarks and,
in lakes, by checking the depth. If samples must be taken from a boat, a sampling
station may be marked by placing a buoy at the desired location; otherwise it is
necessary to identify the sampling station by the intersection of lines between
landmarks on the shore.
 Do not include large, non-homogeneous pieces of detritus, such as leaves, in the
sample. Avoid touching and disturbing the bottom of a water body when taking
a depth sample, because this will cause particles to become suspended. As an
example, the GEMS/WATER monitoring program sets the upper size limit of
particulate matter at 0.063 mm. To remove larger material pass the water
sample through a sieve and collect it in a bottle for transport.
 Sampling depth is measured from the water surface to the middle of the sampler.
 Samples taken to describe the vertical profile should be taken in a sequence that
starts at the surface and finishes at the bottom. When taking the sample at the
maximum depth it is important to ensure that the bottom of the sampler is at
least 1 m above the bottom.
 Do not lower a depth sampler too rapidly. Let it remain at the required depth
for about 15 seconds before releasing the messenger (or whatever other device
closes the sampler). The lowering rope should be vertical at the time of sampling.
In flowing water, however, this will not be possible and the additional lowering
necessary to reach the required depth should be calculated.
 A bottle that is to be used for transport or storage of the sample should be rinsed
three times with portions of the sample before being filled. This does not apply,
however, if the storage/transport bottle already contains a preservative
chemical.
 The temperature of the sample should be measured and recorded immediately
after the sample is taken.
 The sample to be used for dissolved oxygen determination should be prepared
immediately after the temperature is measured. If an electronic technique is
being used, a portion of the sample is carefully poured into a beaker for
measurement. If the Winkler method is being used, the chemical reagents are
added to the bottle in accordance with the directions contained in section 6.5.
 Separate portions of the sample should be set aside for pH and conductivity
determinations. The same portion must not be used for both determinations
because of the possibility of potassium chloride diffusing from the pH probe.
 At any time that the sample bottles are not closed, their tops must be kept in a
clean place. A small air space should be left in the sample bottle to allow the
sample to be mixed before analysis.
 All measurements taken in the field must be recorded in the field notebook
before leaving the sampling station.
 All supporting information should be recorded in the field notebook before
leaving the sampling station. Such conditions as the ambient air temperature,
the weather, the presence of dead fish floating in the water or of oil slicks, growth
of algae, or any unusual sights or smells should be noted, no matter how trivial
they may seem at the time. These notes and observations will be of great help
when interpreting analytical results.
 Samples should be transferred to sample bottles immediately after collection if
they are to be transported. If analysis is to be carried out in the field, it should
be started as soon as possible.
 Each sample bottle must be provided with an identification label.
 Sample bottles should be placed in a box for transport to the laboratory. Sturdy,
insulated wooden or plastic boxes will protect samples from sunlight, prevent the
breakage of sample bottles, and should allow a temperature of 4 °C to be attained
and maintained during transport. Figure 5.8 shows a suitable transport box.
Rapid cooling of samples for BOD and/or microbiological analyses requires that
the transport box should contain cold water in addition to ice or an “ice pack”.
The use of a solid coolant alone is inadequate because heat transfer and sample
cooling are too slow. Bottles containing samples for bacteriological analysis
should ideally be placed in clear plastic bags to protect them from external
contamination.
 If the delay between sample collection and bacteriological analysis will be less
than 2 hours, samples should simply be kept in a cool, dark place. When more
than 2 hours will elapse, samples should be chilled rapidly to about 4 °C by
placing them in a cold water/ice mixture (see above) in an insulated container,
where they should remain during shipment. If the time between collection and
analysis exceeds 6 hours, the report of the analysis should include information
on the conditions and duration of sample transport.
(iii) Draw an appropriate label for a water sample collected during a field visit.

Sample identification number


Name of the sample collector
Date
Time
Location
Sample type
Temperature
Weather condition
Volume

4.
(i) Compare and contrast different types of water samples by emphasizing the purpose of
them.
Grab samples Composite samples Integrated samples
Grab sampling is the most Provides a more Mixture of grab samples
often used method of representative sample of collected from different
sampling flowing water. heterogeneous matrices in points simultaneously, or as
Grab samples are single which the concentration of nearly so as possible, using
samples obtained at a the analyses of interest may discharge-weighed methods
specified location on a site in vary over short time and/or
a short period of time. space.

(ii) List down in situ and ex-situ water quality parameters.


In situ water quality parameters Ex-situ water quality parameters
 Temperature  pH
 Redox Potential  EC (Electrical conductivity)
 Dissolved Gases  Turbidity
 Alkalinity

(iii) Give appropriate methods to prevent following deteriorations that happen in water samples
during transportation.
Possible deterioration in water Prevention method
samples
1. Cations adsorption and Those are best collected in a separate clean
precipitation bottle and acidified with nitric acid to pH
below 2.0 to minimize precipitation and
adsorption on container walls.
2. Decreasing the values of Calcium Adding nitric acid to pH <2
and total hardness
3. Changing the oxidation state Changes caused by growth of microorganisms
are greatly retarded by keeping the sample at
a low temperature ( < 4C0 ) but above
freezing
4.Oxidation of Chlorine in to Cyanide De-chlorinate sample, add NaOH to pH >12,
And refrigerate in dark

5.
(i) Give three examples for each categories of water quality parameters.
a- Physical water quality parameters
 Taste
 Temperature
 Color
b- Chemical water quality parameters
 pH value
 Acidity
 Alkalinity
c- Biological water quality parameters
 Dissolved oxygen
 Chemical oxygen demand
 Coliforms, fecal and total.

(ii) Explain the procedure of total solid detection test


Heat a clean evaporating disc to 103 – 1050C
Evaporate a well-mixed sample of 100ml of water in the weighted dish.
Dry to constant weight in an oven at 103 – 1050C
Calculate the total solids in mg/l units by taking the differences in weight and divide
by the volume of the water sample.
Total dissolved solids - (Dried at 1800C)
Total suspended solids – (Dried at 103 – 1050C)

If a grouch crucible is used for this experiment remove the crucible from the filter
combination dry in an oven at 103 – 1050C for 1hr cool in a desiccator and weight.
Assemble the filter combination start succession wet the filter with a small volume of
regent-rate water. Transfer 100ml of the water sample collected through the filter
and wash with three successive 10ml volumes of regenerate water and continue
succession for three minutes after filtration is complete. Dry to constant weight in an
oven after calculate the total suspended solids in mg/l.

(iii) What are the two types of water hardness? Briefly Explain.
Temporary hardness
The presence of bicarbonate ions (Ca, Mg bicarbonates) in the water causes
Temporary hardness. It is possible to eliminate it by boiling the water.
Permanent hardness
The chlorides and sulfates of Ca2+, Mg+2, Fe3+, and SO4- ions cause permanent
hardness, which cannot be eliminated by boiling.

(iv) What is the most common instrument used for heavy metal analysis in water? Explain the
basic principle behind the instrument.
Atomic Absorption Spectrometry –AAS
In atomic absorption spectroscopy occurs the absorption of energy by the atom so
that the atom experiences an electronic transition from the ground state to the excited
state. In this method, the analysis is based on measuring the intensity of the light
absorbed by the atom so that excitation occurs.

(v) Name the methods utilized in analyzes of individual and total pesticides concentrations in
water samples.
Chromatographic techniques [Gas Liquid Chromatography (GLC) & High performance Liquid
Chromatography (HPLC)]

6. Choose the most suitable answer.


(i) Which oxidation state of nitrogen doesn’t have environmental concern for water?
(a) NH3
(b) NO2
(c) N2O5
(d) N2O3
(ii) …………………. method can be used for nitrite (NO2) analysis in water samples.
(a) Ultraviolet spectroscopy
(b) Cadmium reduction method
(c) Ion chromatography
(d) Cadmium reduction method

7. Below given flow chart is regarding the total phosphorus analysis. Fill in the blanks using
appropriate terms.

(a) Digesting
(b) Ascorbic acid method
(c) Dissolved phosphorus
(d) Insoluble phosphorus

8. A spike recovery for the analysis of chloride in well water was performed by adding 5.00 mL
of a 25 000 ppm solution of Cl– to a 50-mL volumetric flask and diluting to volume with the
sample. An unspiked sample was prepared by adding 5.00 mL of distilled water to a separate
50-mL volumetric flask and diluting to volume with the sample. Analysis of the sample and
the spiked sample return chloride concentrations of 18.3 ppm and 40.9 ppm, respectively.
Determine the spike recovery.
A=25000 ppm × (5.00 mL/50.0 mL)=2500ppm

Thus, the spike recovery is,

%R = (40.9−18.3) / 2500 ×100 = 0.904%


9. Calculate the standard deviation. Using the given formula.

Lead in Drinking Water


Replicate 1 2 3 4 5 6 7 8 9 10
ppm 2.002 1.996 2.000 1.995 1.999 1.987 2.010 2.014 2.007 2.004

Number of Values, n= 10
Mean, x’ = (2.002+1.996+2.000+1.995+1.999+1.987+2.010+2.014+2.007+2.004) / 10
= 20.014 / 10
= 2.0014 is the mean of the data set.

Standard Deviation,

S = √∑(X-2.0014)2 / (10- 1)
= √[(2.002 – 2.0014)2 + (1.996 – 2.0014)2 + (2.000 – 2.0014)2 + (1.995 – 2.0014)2 + (1.999 –
2.0014)2+(1.987 – 2.0014)2 + (2.010 – 2.0014)2 + (2.014 – 2.0014)2 + (2.007 – 2.0014)2 +
(2.004 – 2.0014)2] / 9
= √[3.6×10-7 + 296.6×10-7+ 19.6×10-7 +409.6×10-7 +57.6×10-7 +7290×10-7 +739.6×10-7
+1587.6×10-7 +313.6×10-7 +67.6×10-7] / 9
= √[(3.6+296.6+19.6+409.6+57.6+7290+739.6+1587.6+313.6+67.6)×10-7] / 9
= √[10785.4×10-7/ 9]
= √1198.378×10-7
= 0.0109470453
= 1.095

10. How many moles are there in 50 g of H2O? (MH20=18gmol-1)


Mass of the 1 mol of H2O = 18 g mol-1
Mols in 50 g of H2O = 50 g /18 g mol-1
= 2.778 mol

11. How many grams are there in 20.00 moles of H2O?


Mass of the 1 mol of H2O = 18 g mol-1
Mass of 20 mols of H2O =18 g mol-1 ×20 mol
=360 g
12. What is the percent composition of oxygen in water and of hydrogen in water? (O-16 H=1)
Oxygen % = (16 g / 18 g)×100%
= 88.889%
Hydrogen % = (2 g / 18 g)×100%
= 11.111%

13. You add 400 mL of water to 200 mL of a 3 mol/L solution of hydrogen peroxide. Calculate
the new concentration.
C1V1 =C2V2
3 mol/L×200mL = C2×600mL
(3 mol/L×200mL) / 600mL = C2
(C2) new concentration = 1 mol/L

14. You are supplied with a 200-mL plastic bottle filled to capacity with 6mol/L solution of KCN,
a poison. The plastic bottle is placed in a large beaker containing 1.0 L of water. The plastic
bottle leaks. What is the final concentration of the solution in the large beaker when the plastic
bottle is completely empty?
C1V1 =C2V2
6 mol/L×200mL = C2×1000mL
(6 mol/L×200mL) / 1200mL = C2
(C2) new concentration = 1 mol/L

15. What is the concentration of a solution made by diluting 8.00 mL of a 0.20 mol/L solution
with 12.0 mL water?
C1V1 =C2V2
0.2 mol/L×8 mL = C2× 20 mL
(0.2 mol/L×8 mL) / 20 mL = C2
(C2) new concentration = 0.08 mol/L

16. A particular water soluble fertilizer contains phosphorus in the form of phosphate ions, PO43-
. A student used the following procedure to determine the percentage of phosphorus in a
sample of soluble fertilizer.
5.17 g of fertilizer was added to a 250.0 mL volumetric flask and water was added to make
it up to the mark.
20.00 mL of this solution was pipetted into a conical flask.
A slight excess of precipitating agent was added to precipitate the phosphate ions as
MgNH4PO4.
The precipitate was filtered, washed with water and then converted by heating into
Mg2P2O7
The mass of Mg2P2O7 was 0.0312 g
Calculate the percentage by mass of phosphate in the fertilizer.
Mol of Mg2P2O7 = 0.0312g/ 222.6 g/mol
= 1.40 x 10-4mol
Moles of phosphorus in 200mL = 2 x n(Mg2P2O7)
=2 x 1.40x10-4
= 2.8 x 10-4mol
Moles in fertilizer sample = n(P) x in 250mL of solution,
= (2.8 x 10-4 /20) x 250
= 0.0035 mol
percentage of phosphorus ions,
n(PO43- ) = n(P)
phosphorus % = 0.0035 mol
= 0.0035 x 95.0
= 0.3325g
= (0.3325g/ 5.17g) x 100
= 6.43%

17. A student has been given 1 L of water and asked to determine the concentration of dissolved
calcium and magnesium ions in the water. Using a 0.010 mol L-1 standard solution of EDTA,
the student titrated 100.0 mL samples of the water using Eriochromshwartz-T as the indicator.
The student's titration results are shown below:
Titration No. volume EDTA (mL)
1 10.14
3 10.10
3 10.12
Determine the total concentration of calcium and magnesium ions in the water sample
The moles of EDTA required complex with calcium and magnesium ions in the water
Concentration of EDTA = 0.010mol/L
Volume of EDTA solution = (10.14 + 10.10 + 10.12) / 3
= 10.12mL
= 0.01012L
Moles of EDTA = 0.010 mol/L×0.01012L
= 0.0001012 mol
=1.012×10-4mol
Reactions between EDTA and calcium and magnesium ions
Ca2+ + H2 EDTA2 CaEDTA2- + 2H+
Mg2+ + H2 EDTA2 MgEDTA2- + 2H+
Let M2+ = Ca2+ + Mg2+, then
M2+ + H2EDTA 2- MEDTA2- +2H+
From the balanced chemical equation, a mole M2+ reacts with 1 mol EDTA so, 1.012×10-
4
moles of EDTA reacts with 1.012×10-4 moles of M2+
(M2+= Mg2+ + Ca2+ )
Concentration (M2+) = 1.012×10-4 mol/100×10-3L
=1.012×10-3mol/L

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