Professional Documents
Culture Documents
I. The following areas (some may not be applicable to some parameters) are to
be discussed in the folders:
1. Aim
2. Principle
3. Sources and general theory
4. Standards for drinking water (as per BIS)
5. Removal methodologies
6. Equations of the titration
7. Formulae used in the calculation and explanation for the salient features of them
8. Procedure
9. Environmental Engineering Significance
10. Results and Comments on the results
11. Graphs
12. Questions and Answers
13. Observation Table
14. Calculations
It is customary to have 1 – 12 items on right hand side of the folder while the last
two on the left hand side
II. As far as possible, hand writing should be legible with neat presentation of figures and
tables.
III. Graphs should be clear. Scale used for drawing the graphs should be mentioned on
the graph itself clearly. The points marked for drawing graphs should be clear and
distinct from one another.
IV. All the observations and calculations should be carried in ink only and NOT with
pencil.
V. For every class (after the first one), folder of the previous class, observation book (in
ready condition with Observation and Calculation Tables for the day’s experiment),
calculator are must. Also, students would be asked some questions regarding the
procedure of the day’s experiment and one would be allowed to do the experiment only
if faculty are satisfied with the answers.
VI. Titrations should be carried till one gets two concurrent values (may or may not be
consecutively concurrent) and that value only should be taken into the consideration.
Hence, theoretically 2 is minimum and ∞ (may be 5 – 7) is the maximum number of
readings one should take.
2
Please verify and see that you are having the following items in your work space
corresponding to your respective experiment.
Sl.
No. Experiment Reagents Apparatus(Purpose)
1 Acidity N/50 NaOH
Methyl Orange Burette(Titration)
Phenolphthalein 25 ml Measuring cylinder(sampling)
2 Alkalinity N/50 H2SO4 100 ml Beaker (Reagent for Burette)
Phenolphthalein Conical Flasks – 2 ( Titration)
Methyl Orange Funnel (Taking reagent into burette)
3 Chlorides N/71 AgNO3
K2CrO4
N/71 NaOH
N/71 H2So4
4 Hardness Ammonia Buffer Burette(Titration)
0.01M EDTA 25 ml Measuring cylinder(sampling)
Eriochrome Black T indicator 100 ml Beaker (Reagent for Burette)
NaOH 2N Conical Flasks – 2 ( Titration)
Funnel (Taking reagent into burette)
Spoon (E B T)
10 ml Pipette (Buffer)
5 D.O. MnSO4 BOD Bottles – 3 (sampling)
Alk.KI 200/500 ml Measuring Cylinder
Conc. H2SO4 (Volume determinations)
Starch 25 ml Pipette – 2 (fixing DO)
N/40 Na2S2O3 10 ml Pipette (Acid)
Wash Water Beaker(Cleaning)
Burette(Titration)
100 ml Beaker (Reagent for burette)
Funnel (Taking reagent into burette)
Conical flasks – 3 (Titration)
6 B.O.D. Phosphate buffer solution 5 litre flask
Magnesium sulphate solution 1 ml Pipette (Standards)
Calcium chloride solution BOD Bottles – 2 (for each sampling)
Ferric chloride solution Incubator
Sodium thiosulphate solution Burette(Titration)
Distilled water 100 ml Beaker (Reagent for burette)
Funnel (Taking reagent into burette)
Conical flasks – 3 (Titration)
7 C.O.D. N/60 N K2Cr2O7 COD Digester
2Fe(SO4)2(NH4)6H2O 10ml Vial with cap
Conc. H2SO4 Conical flask – 1 (Titration)
Organics free water Burette(Titration)
Organic matter 100 ml Beaker (Reagent for burette)
Ferroin indicator Funnel (Taking reagent into burette)
5ml pipette
8 Fluorides 100 ppm stock solution 10 ml Pipette (Standards)
SPADNS solution 5 ml Pipette - 2 (1 – Standards and 1 –
Reference solution reagent)
Distilled Water 1 ml Pipette (Standards)
3
Beakers – 5 or more (standards and samples)
Spectrophotometer (Analysis)
9 Electrical Conductivity KCI 0.1N. Conductivity meter with measuring cell
Beaker
Thermometer.
10 Turbidity Hydrazine sulphate solution Nephelometric turbidmeter
Hexamethylene teramine solution
Sample tubes
11 Total Solids Evaporating dishes(Pyrex, porcelain or platinum
Oven
Desiccator
Water bath.
12 Total Dissolved Solids Evaporating dishes
Oven
Desiccator
Whatman filter paper No. 44
Water bath.
13 Total Fixed and Evaporating dish
Volatile Solids Oven 1030C
Muffle furnace 6000c
Desiccator
Water bath.
14 Total Settleable Solids Imhoff cone
Holding device
15 Total Suspended Solids Gooch crucible/glass fibre filter
Suction apparatus
Desiccator
16 Sulphates Hydroxylamine chloride Filter paper
Benzidine hydrochloride Beaker
NaOH(0.05N) Hot pan
Phenolpthalein indicator Burette
Pipettes
17 Residual Chlorine Orthotolidine reagent Chloroscope
18 Break Point Chlorination Six beakers of 1 litre capacity each
Stirrer
Chloroscope
19 Jar Test Alum solution (Synthetic coagulant)
Jar test apparatus
Nirmali solution(natural coagulant)
Beakers – 6
Pipette _1
Turbidity meter
PH meter
20 Available Chlorine Concentrated acetic acid Conical flask
Potassium iodide crystals Burette
Sodium thiosulphate 0.025 N Pipette
Starch Indicator
4
ACIDITY
OCCURRENCE AND TYPES
Most natural waters, domestic sewage and many industrial wastes are buffered
principally by a carbon dioxide – bicarbonate system. It is customary to consider that all
waters having pH lower that 8.5 contain acidity. The acidity of natural waters is caused by
carbon dioxide or by strong mineral acids, the former being the effective agent in waters
having pH values greater than 4.5 and the latter the effective agent in waters with pH
values less than 4.5.
Carbon dioxide is a normal component of all natural waters. It may enter surface
waters by absorption from the atmosphere, but only when the partial pressure of carbon
dioxide in the water is less than the partial pressure of the carbon dioxide in the
atmosphere, in accordance with Henry’s law. Carbon dioxide may also be produced in
waters through biological oxidation of organic matter, particularly in polluted water. In such
cases, if photosynthetic activity is limited, the partial pressure of carbon dioxide in the water
may exceed that of the atmosphere and carbon dioxide will escape from liquid. Thus it may
be concluded that surface waters are constantly absorbing or giving up carbon dioxide to
maintain equilibrium with the atmosphere. The amount the can exist at equilibrium is very
small because of the low partial pressure of carbon dioxide in the atmosphere.
Ground waters and waters form the of stratified lakes and reservoir often contain
considerable amount of carbon dioxide. This concentration results from bacterial oxidation
of organic matter with which the water has been in contact and under the conditions, the
carbon dioxide is not free to escape to the atmosphere. Carbon dioxide is an end product
of both aerobic and anaerobic bacterial oxidation; therefore its concentration is not limited
buy the amount of dissolved oxygen originally present. It is not uncommon to encounter
ground water with 30 to 50 mg/l of carbon dioxide. This is particularly true of waters that
have percolated through soils that do not contain enough calcium or magnesium carbonate
to neutralize the carbon dioxide through formation of bicarbonates.
Mineral acidity is present in many industrial wastes, particularly those of the
metallurgical industry and some from the production of synthetic organic materials. Certain
natural waters may also contain mineral acidity. The drainage from abandoned mines, lean
ore dumps will contain significant amounts of sulphuric acid or salts of sulphuric acid if
sulphur, sulphides, or iron pyrites are present. Conversion of these materials to sulphuric
acid and sulphates is brought about b sulphur – oxidizing bacteria under aerobic
conditions.
REAGENTS
PROCEDURE
OBSERVATIONS
CALCULATIONS
Mineral Acidity = V x1000 mg/l
VS
6
CO2 Acidity = VR x1000 mg/l
VS
RESULTS & DISCUSSIONS
ALKALINITY
OCCURRENCE AND TYPES
The alkalinity of the water is a measure of its capacity to neutralize acids. The
alkalinity of natural waters is due primarily to the salts of weak acids, although weak or
strong bases may also contribute. Bicarbonates represent the major form of alkalinity,
since they are formed in considerable amounts from the action of carbon dioxide upon
basic materials in the soil. Other salts of weak acids, such as borates, silicates and
phosphates, may be present in small amounts. A few organic acids that are quite resistant
to biological oxidation – for example, humic acid – form salts that add to alkalinity of natural
waters. In polluted or anaerobic waters, salts of weak acids such as acetic, propionic and
hydrosulphuric may be produced and would also contribute to alkalinity. In other cases,
ammonia or hydroxides may make a contribution to the total alkalinity of water.
Under certain conditions, ay contain appreciable amounts of carbonate and hydroxide
alkalinity. This condition is particularly true in surface waters where algae are flourishing.
The algae remove carbon dioxide, free and combined, from the water to such an extent
that pH values of 9 to 10 are often obtained. Boiler water always contain carbonate and
hydroxide alkalinity. Chemically treated waters, particularly those produced in lime or lime –
soda ash softening of water, contain carbonates and excess hydroxide.
Although many materials may contribute to the alkalinity of water, the major portion of
the alkalinity in natural water is caused by there major classes of materials which may be
ranked in order of their association with high pH value as follows: i) hydroxides, ii)
carbonates and iii) bicarbonates. For most practical purposes, alkalinity due to other
materials in natural waters is insignificant and may be ignored.
The alkalinity of waters is due principally to salts of weak acids and strong bases, and
such substances act as buffers to resist a drop in pH resulting from acid addition. Alkalinity
is thus a measure of the buffer capacity and in this used to a great extent in waste water
treatment practice.
PUBLIC HEALTH SIGNIFICANCE OF ALKALINITY
As far as is known, the alkalinity of water has little public health significance. Highly
alkaline waters are usually unpalatable and consumers tend to seek other supplies.
Chemically treated waters sometimes have rather high pH values which have met with
some objection on the part of consumers. For theses reasons, standards are sometimes
established on chemically treated waters.
APPLICATION OF ALKALINITY DATA
CHEMICAL COAGULATION
Chemicals used for coagulation of water and waste water react with water to form
insoluble hydroxide precipitates. The hydrogen ions released react with alkalinity of the
water. Thus the alkalinity acts to buffer the water in a pH range where the coagulant can be
effective. Alkalinity must be present in excess of that destroyed by the acid released by the
coagulant for effective and complete coagulation to occur.
WATER SOFTENING
7
Alkalinity is a major item that must be considered in calculating the lime and
soda – ash requirements in softening of water by precipitation methods. The alkalinity of
softened water is a consideration in terms of whether such waters meet drinking water
standards.
CORROSION CONTROL
Alkalinity is an important parameter involved in corrosion control. It must be known in
order to calculate the Langelier saturation index in the corrosion studies.
INDUSTRIAL WASTES
Many regulatory agencies prohibit the discharge of wastes containing caustic
(hydroxide) alkalinity to receiving waters. Municipal authorities usually prohibit the
discharge of wastes containing caustic alkalinity to sewers. Alkalinity as well as pH is an
important factor in determining the amenability of wastewater to biological treatment.
REAGENTS
i. Phenolphthalein Indicator
ii. Methyl Orange Indicator
iii. N/50 Sulphuric Acid
PROCEDURE
1. Take 25 ml. of water sample (Vs) in a conical flask.
2. Add 2 – 3 drops of Phenolphthalein Indicator. If no colour is produced, the
phenolphthalein alkalinity is absent (Go to step no.5).
3. If the sample turns pink, titrate with N/50 H2SO4 till the pink colour
disappears.
4. Record the ml. of acid used (designate as P1).
5. Add 2 – 3 drops of methyl orange to the titrated mixture to get yellow colour.
6. Continue titration with N/50 H2SO4 until the first appearance pink red is noted.
7. Record the ml. of acid used (designate as T1).
OBSERVATIONS
Sl. Volume of sample Burette Readings
No. (ml.) Initial Final ml. of Reagent used
1
2
3
CALCULATIONS
Phenolphthalein Alkalinity = P1 x 1000 mg/l
Vs
Total Alkalinity = T1 x 1000 mg/l
Vs
Sl. No. If Alkalinity is due to
Bicarbonates Carbonates Hydroxides
1. P=0 T NIL NIL
2. P < (1/2) T T – 2P 2P NIL
3. P > (1/2) T NIL 2(T-P) 2P-T
4. P = (1/2/) T NIL T NIL
5. P=T NIL NIL T
8
Chlorides occur in all natural waters in widely varying concentration. The chloride
content normally increases as the mineral content increases. Upland and mountain
supplies usually are quite low in chlorides, whereas river and ground waters usually have a
considerable amount. Sea and ocean waters represent the residues resulting from partial
evaporation of natural waters that flow into them, and chloride levels are very high.
Chlorides gain access to natural waters in many ways. The solvent power of water
dissolves chlorides from top soil and deeper formations. Spray from the ocean is carried
inland as droplets or as minute salt crystals, which result from evaporation of the water in
the droplets. These sources constantly replenish the chlorides in inland areas where they
fall. Ocean and sea waters invade the rivers that drain into them, particularly the deeper
rivers. The salt water, being more dense, flows upstream under the fresh water which is
flowing downstream. There is a constant intermixing of the salt water with the fresh water
above.
Human excreta, particularly the urine contain chloride in an amount about equal to the
chlorides consumed with food and water. This amount averages about 6g of chlorides per
person per day and increases the amount of CI in sewage about 15 mg/l above that of the
carriage water. Thus sewage effluents add considerable chlorides to receiving streams.
Many industrial wastes contain appreciable amounts of chlorides. Control of contamination
of surface waters by chlorides contained in industrial wastes is a major consideration and
in all areas where oil field brines and other salt brines is allowed to reach receiving
streams.
REAGENTS
i. Potassium Chromate Indicator.
ii. N/71 Silver Nitrate Solution.
1
iii. N/71 Sodium hydroxide Solution
iv. N/71 Sulphuric acid
PROCEDURE
1. Take 25 ml. of sample (VS) in a conical flask.
2. Adjust the pH between 7.0 and 8.0 either with sulphric acid or sodium
hydroxide solution. Otherwise, AgOH is formed at high pH level or CrO-24 is
converted into Cr2O-27 at low pH levels.
3. Add 2 -3 drops of Potassium Chromate Indicator.
4. Titrate with Standard N/71 Silver Nitrate solution till colour changes from
light yellow to brick red (or brown).
5. Note the amount of titrant used (RS).
6. Repeat the procedure with chloride free water and note the amount of titrant
used (RB).
OBSERVATIONS
CALCULATIONS
PSEUDO HARDNESS
Sea, brackish and other waters that contain appreciable amounts of Na interfere with
the normal behaviour of soap because of the common ion effect. Sodium is not a hardness
causing cation, and so this action which it exhibits when present in high concentration is
termed pseudo hardness.
PROCEDURE
1. Take 25 ml. of sample (VS) in a conical flask.
2. Add 1 ml. of Ammonia Buffer solution and few crystals (a Pinch) of Erio-
chrome Black T Indicator.
3. Titrate with standard 0.01 M EDTA Solution till the colour changes from
wine red to blue.
4. Note the reading (VR).
5. Repeat the procedure by taking fresh sample and after boiling it.
OBSERVATIONS
CALCULATIONS
DISSOLVED OXYGEN
REAGENTS
i. Manganous Sulphate
ii. Alkaline Potassium Iodide
iii. N/40 Sodium Thiosulphate
iv. Conc. Sulphuric Acid
v. Starch Indicator
PROCEDURE
1. Find out the exact capacity of the bottle in ml.
2. Collect the sample in a narrow mouth flat stoppered through D.O. sampler to
avoid contact with air. The bottle should be completely filled.
3. Add 1.0 ml. of Manganous Sulphate solution by a 10/20ml. pipette, dipping the
end below the surface. Some water would overflow. Transfer back the
remaining Manganous Sulphate solution into its respective bottle without
dipping the pipette in to the solution and place the pipette in a glass of beaker
kept for washing.
4. Add 1.0 ml. of Alkaline Potassium Iodide solution also in the same manner by
using a separate 10/20 ml. pipette. Transfer back the remaining Alkaline
Potassium Iodide, solution into its respective bottle without dipping the pipette
in to the solution.
5. Place the pipettes in a glass of water kept for washing.
6. Insert the stopper and mix thoroughly (white precipitate indicates absence of
dissolved oxygen). Let the brown precipitate settle.
7. Add 2.0 ml. of H2So4 and mix thoroughly.
8. Take the calculated amount of decoction (VS = 201ml.) worked out as below:
200 * 300
201 mL
300 2
1
9. Titrate with N/40 Sodium Thiosulphate using Starch as indicator till
the blue colour disappears.
10. Note the ml. of titrant used (VR) and the room temperature.
OBSERVATIONS
CALCULATIONS
However, in the present experiment, since the Normality of Na2S2O4 is 1/40 (and 1 ml.
of N/40 Sodium Thiosulphate = 1 mg/l of the sample), the ml. of the titrant used is
equivalent to mg/l of DO.
D.O. = VR X 1000 X 1 X8
VS 40
AIM:
To determine Biochemical oxygen demand (BOD) exerted by the given waste water
sample.
PRINCIPLE:
The BOD is an empirical biological test. This BOD test may be considered as wet
oxidation procedure in which the living organisms serve as the medium for oxidation of the
organic matter to carbon-dioxide and water.
CnHaObNc +[n+a-b-3c]O2Bacteria nCO2 +[a-3c]H2O +cNH3
424 2 2
On the basis of the above relationship, it is possible to interpret BOD data in terms of
organicmatter as well as the amount of oxygen used during its oxidation.
INTERFERENCE:
An undesirable oxygen consumption via nitrification can be prevented by addition of 1
ml of an N-allyl thourea solution. Free chlorine, present in some waste waters after
chlorination reacts with organic components within about 2 hours and does not interfere.
Compounds which use up oxygen without the presence of micro-organisms (e.g. iron (ll),
sulphite of sulphide ions) are oxidized by leaving the orginal sample for 2 hours with
occasional shaking. Lack of nutrient in dilution water, lack of an acclimated seed organisms
and the presence of toxic substances can result in very low BOD values despite the
presence of sufficient degradable organic materials. In such cases, a series of
measurements should be carried out at greater dilutions.
REGENTS:
1. Distilled water
2. Phosphate buffer solution
3. Magnesium sulphate solution
4. Calcium chloride solution
5. Ferric chloride solution
6. Sodium thiosulphate solution.
PROCEDURE:
1. Place the desired volume of distilled water in a 5 litre flask. Aeration is done by
bubbling compressed air through water.
2. Add 1 ml of phosphate buffer, 1 ml of magnesium sulphate solution, 1 ml of
calcium chloride solution and 1 ml of ferric chloride solution for every litre of
distilled water (dilution water).
3. In the case of the waste waters which are not expected to have sufficient bacterial
population, add seed to the dilution water. Generally, 2 ml of settled sewage is
sufficient for 1000 ml of dilution water.
4. Highly acidic or alkaline samples are to be neutralized to a pH of 7.
5. Add 2 or 3 ml of sodium thiosulphate solution to destroy residual chlorine if any.
6. Take the sample as follows:
Strong wastes: 0.1, 0.5 or 1%
1
Settle domestic sewage: 1, 2.5 or 5%
Treated effluents: 5, 12.5 or 25%
River water 25% to 100%
7. Dilution the sample with the distilled water and mix the contents well.
8. Take diluted sample into 2 BOD bottles.
9. Fill another two BOD bottles with diluted (distilled) diluted water (distilled water).
10. Immediately find D.O. of a diluted waste water and diluted water (distilled water).
11. Incubate the other two BOD bottles at 20oC for 5 days. They are to be tightly
stoppered to prevent any air entry into the bottles.
12. Determine D.O. content in the incubated bottles at the end of 5 days (120 hours).
CALCULATIONS:
REAGENTS
I. K2Cr2O7 of N/60 N
II. 2Fe(SO4)2(NH4)6H2O
III. Conc. H2SO4
IV. Organics free water
V. Organic matter
VI. Ferroin indicator
PROCEDURE
1. Take 2.5 ml of sample into the vial.
2. Add 1ml of potassium dichromate solution.
3. Carefully add 3.5ml of Conc.H2SO4.
4. Digest the mixture (7.5ml) after capping the vial tight in the COD digester
for 24 hours.
5. Cool the vial and transfer the contents to a conical flask.
6. Add 1 or 2 ml drops of Ferroin Indicator
7. Titrate the excess dichromate with 0.1M Ferrous ammonium sulphate till
the colour changes from blue – green to reddish brown.
8. Repeat the procedure from step 2- 7 for blank with 2.5 ml distilled water.
9. Designate the titration for the sample as Rs and for the blank i.e distilled
water as RB
OBSERVATIONS
CALCULATIONS
1
Procedure:
Standards:
1.Pipette 0.0, 0.5, 1.0, 2.0, 3.0, 4.0, 5.0, 6.0, and 7.0, ml. fluoride standard
solution into 50 ml. Nessler tubes and make up to the mark with
distilled water.
2. Add exactly 10.0-ml. acid-zirconyl-SPADNS reagent to each tube and
mix well.
3. Set the spectrophotometer or filter photometer to zero absorbance
using reference solution at 570 mμ and measure the absorbance of the
standards immediately.
4. Plot a calibration curve.
Samples:
Place 50.0 ml. Of the sample or an aliquot diluted to 50.0 ml. in a Nessler tube. If
the sample contains any residual chlorine add 1 drop of sodium arsenite solution
for each 0.1mg CI2 and mix well. Add exactly 10.0-ml. of the acid-zirconyl-
SPADNS reagent and mix well. After setting the spectrophotometer to zero-
absorbance with the reference solution, measure the absorbance of the sample.
Find out the mg fluoride of the sample equivalent to the observed optcal density
from the calibration graph.
Express the result as mg fluoride (as F-) per liter of the sample.
2
FLUORIDES
REAGENTS
i. Fluoride Stock Solution of 100 ppm
ii. Colour Reagent
PROCEDURE
1. Prepare 20ml. of 10 ppm stock solution from given 100 ppm stock solution.
2. Prepare 10ml. of different standards (Eg: 1 ppm, 2 ppm, 3 ppm, ….) from this 10
ppm stock solution prepared in the previous step.
3. Add to each of these standards 2 ml. of colour reagent.
4. Take 10ml. of the sample and add 2 ml of colour reagent.
5. Keep them for about an hour for the colour development.
6. Record the absorbance for all the standards and for the sample as well in an U V
Spectrophotometer at 570nm.
7. Prepare the calibration chart for the standards with the help of the concentration
and their corresponding absorbance values.
8. Back read the concentration of Fluoride of the sample from this calibration chart
with the help of the absorbance of the sample recorded.
OBSERVATIONS
ELECTRICAL CONDUCTIVITY
PRINCIPLE:
The electrical conductivity is a total parameter for dissolved, dissociated substances.
Its value depends on the concentration and degrees of dissociation of the ions as well as
the temperature and migration velocity of the ions in the electric field.
APPARATUS:
1. Conductivity meter with measuring cell.
2. Beaker
3. Thermometer.
REAGENTA:
1. KCL 0.1N.
PROCEDURE:
1. Calibrate the cell with standard 0.1 N. KCL solution of conductivity 14.12 mmhos
at 30oC.
2. Rinse the cell thoroughly with deionized distilled water and carefully wipe with a
tissue paper.
3. Dip the cell into the sample solution, swirl the solution and wait upto 1 minute for
a steady reading.
4. Note down the Instrument reading and also temperature by a thermometer.
TURBIDITY
AIM:
To find out Turbidity of the given samples.
PRINCIPLE:
When light is passed through a sample having suspended particles, some of the light
is scattered by the particles. The scattering of the light is generally proportional to the
turbidity. The turbidity of sample is thus measured from the amount of light scattered by the
sample taking a reference with standard turbidity suspension.
APPARATUS:
1. Nephelometric turbidimeter
2. Sample tubes.
INTERFERENCES:
The determination of turbidity is interfered by the presence of debris and other rapidly
settleable matter. The true colour in the sample reduces the values of turbidity.
REAGENTS:
1. Dissolve 1.0 gm Hydrazine sulphate and dilute to 100 ml.
2. Dissolve 10 gm Hexamethylene Tetramine and dilute to 100 ml.
3. Mix 5 ml of each of the above solution (1 and 2) in a 100 ml volumetric flask and
allow to stand for 24 hours at 25+ 3oC and dilute to 1000 ml. this solution has a
turbidity of 40 NTU.
4. This solution can be kept for about a month.
PROCEDURE:
1. SWITCH ON Nephelometric turbidimeter and wait for few minutes till it warms up.
2. Set the instrument at 100 on the scale with a 40 NTU standard suspension. In this
case, evey division on the scale will be equal to 0.4 NTU turbidity.
3. Shake thoroughly the sample, and keep it for sometime to eliminate the air bubbles.
4. Take sample in Nephelometer sample tube and put the sample in sample chamber
and find out the value on the scale.
5. Dilute the sample wqith turbidity free water and again read the turbidity.
TOTAL SOLIDS
AIM:
To determine the Total Solids of the given sample.
PRINCIPLE:
Total solidas are determined as the residule left after evaporation and drying of the
unfiltered sample.
APPARATUS:
1. Evaporating dishes (pyres, porcelain or platinum)
2. Oven
3. Desiccators
4. Water bath.
PROCEDURE:
1 A clean porcelain dish is ignited in a muffle furnace and after partial cooling in the
air, it is cooled in a desiccators and weighed.
2 A 100 ml of well mixed sample (graduated cylinder is rinsed to ensure transfer of all
suspend matter) is placed in the dish and evaporated at 100oC for 1 hour.
3 Dry to a constant weight at 103oC, cool ina desiccators and weigh.
CALCULATIONS:
Total solids (mg/l) = (A-B) X 1000
V
A = Final weight of the dish in mg.
B = Initial weight of the dish in mg.
V = Volume of sample taken in ml.
Sample details Volume of Initial weight of the Final weight of the Total solids
sample (ml) Dish (mg) Dish (mg) (mg/l)
2
PRINCIPLS:
Total dissolved solids are determined as the residue left after evaporation and drying
of the filtered sample.
APPARATUS:
1. Evaporating dishes
2. Oven
3. Desiccators
4. Whatman filter paper No. 44
5. Water bath.
PROCEDURE:
1. A clean porcelain dish is ignited in muffle furnace and after partial cooling in the
air, it is cooled in a desiccators and weighed.
2. A 100 ml of filtered sample is placed in the dish and evaporated at 100oC on
water bath followed by drying in oven at 103oC for 1 hour.
3. Dry to a constant weight at 103oC, cool in a desiccators and weigh.
CALCULATIONS:
Total
volatile
solids
2
PRINCIPLE:
The particles in suspension whose specific gravity great than that of water will settle
under quiescent conditions.
APPARATUS:
1. Imhoff cone
2. Holding device
PROCEDURE:
1. Gently fill the Inhoff cone with the thoroughly wel mixed sample usually one litre
and allow it to settle.
2. After 45 minutes, gently rotate the cone between hands to ensure that all solids
adhering to the sides are loosened.
3. Allow the solids to settle for 15 minutes more, to make up for a total period of 1
hour.
4. Read the volume of the sludge which has settled the apex.
5. Express the results in ml settleable solids per litre of sample per hour.
CALCULATIONS:
Total settleable solids (ml/l) = ml of solids X 1000
ml of sample
PRECAUTIONS:
1. The Imhoff cones must be cleaned with a strong soap and hot water using a brush.
2. Wetting the cone with water before use, helps in preventing adherence of the solids
to the sides.
3. The method is subjected to considerable in accuracy if the solids contain large
fragments.
4. The determination of total settleable solids should be carried out soon after
sampling in order to avoid errors through flocculation.
PRINCIPLE:
Total suspended solids are determined as the residue left on gooch cruchible or a
glass fibre filter after drying in oven.
APPARATUS:
1. Gooch crucible/glass fibre filter
2. Suction apparatus
3. Desiccators
PROCEDURE:
1. A clean gooch crucible is ignited in a muffle furnace and after partial cooling in the
air, cool in deciccator and weigh (W1).
2. Pour 100ml of well mix sample on gooch crucible or glass fibre filter which is kept
on filter flask and apply suction.
3. Wash the gooch crucible with 100ml of distilled water to remove all soluble salts.
4. Carefully remove the glass fibre filter paper or gooch crucible and dry in a oven at
105oC for one hour.
5. Cool in a desiccators and weigh(W2).
6. Ignite gooch crucible in a muffle furnace at 600oC for 15-20 minutes.
7. Cool the crucible partially in air until most of heat has been dissipated and then in a
desiccators and record final weigh(W3).
CALCULATIONS:
Sulphate ions are precipitated as barium sulphate crystals of uniform size in acid
medium. Light absorbed by the precipitate is measured using a spectrophotometer.
Turbidimetric analysis is based on measuring the weakening of intensity of luminous flux
when it passes through a solution containing particles in suspension. The intensity
decreases owing to absorption and scattering of light.
Reagents:
1. BaCl2 Crystals
2. Stabilizing reagent: mix 20 ml of glycerol with 80 ml of alcohol
3. 200 ppm 'Standard' solution
Calibration curve:
SULPHATES
AIM:
To find the amount of Sulphates in the given sample.
PRINCIPLE:
Benzidine hydrochloride reacts with sulphates in HCL solution to form a slightly soluble
compound of benzidine sulphuric acid.
CaSO4 + C12 H8 (NH2)2 2 HCl ------>C12 H8 (NH2)2 H2SO4 Benzidine Sulphuric acid + Ca++ +
Mg+++ Cl2
MgSO4
The compound is filtered and washed entirely free of HCL. The amount of H2SO4 in the
compound is determined by titration with standard NaOH(0.05N)
REAGENTS:
1. Hydroxylamine chloride
2. Benzidine hydrochloride
3. NaOH (0.05N)
4. Phenolphthalein indicator
APPARATUS:
1. Filter paper
2. Beaker
3. Hot pan
4. Burette
5. Pipettes.
PROCEDURE:
1. Take 125ml of sample in a 4ooml beaker.
2. Add 5 ml of hydroxylamine chloride and then add 10 ml of benzidine
hydrochloride.
3. Stir the mixture vigorously and allow the precipitate to settle.
4. Filter the solution and wash the beaker and the filter paper with cold distilled
water.
5. Pierce the filter paper in the funnel and wash the precipitate formed on the filter
paper to the original beaker with 100 to 150 ml distilled water.
6. Heat the beaker to dissolve the contents for 20 to 30 minutes.
7. Add 2 drops of phenolphthalein indicator and titrate with 0.05N NaOH until pink
colour is developed.
CALCULATIONS:
Concentration of sulphates (mg/l)= Vol. of 0.05N NaOH X 38.4
Volume of the sample taken
3
RESIDUAL CHLORINE
AIM:
To find out the amount of Residual chlorine available in the given sample.
PRINCIPLE
Ortholidine is an aromatic organic compound that is oxidized in acid solution by
chlorine, chloramines, and other oxidizing agents to produce a yellow coloured compound
called Holoquinone. Intensity of yellow colour of holoquinone is proportional to the amount
of chlorine present.
INTERFERENCE:
Oxidising agents such as ferric compounds, manganic salts, nitrites etc.
APPARATUS:
Chloroscope.
REAGENTS:
Orthotolidine reagent.
PROCEDURE:
1. Take the water sample under question into one of the cylinders of the comparator
and distilled water into the other.
2. Add 5 drops of orthotolidine solution to both the cylinders and put them in the
comparator.
3. The colour which matches in both the cylinders directly gives the ‘residual chlorine’.
APPARATUS:
1. Six beakers of 1 litre capacity each
2. Stirrer
3. Chloroscope.
PRINCIPLE:
Chlorine combines with water to form hypochlorous and hydrochloric acid.
Hypochlorous acid dissociates to give the OCI- ion. Quantities of OCI- and HOCI rupture the
cell membrane of impurities like ammonia, oxidisable inorganic matter like ferrous ions,
nitrites etc. to form chloramines and stable ions of the latter respectively.
PROCEDURE:
1. Take 1000 ml of water sample in six different beakers.
2. Prepare a stock solution of 0.1 g/l by dissolving 0.5 g of bleaching powder in 100
ml of distilled water. Each ml of stock solution gives a dosage of 0.5 mg.
3. Add varying does of bleaching powder to each beaker. This amount may be
2.0,3.0,4.0,5.0 till 8.0 mg. (The dosage may be raised by 10 times in the case of
polluted waters.)
4. Stir the sample with a glass rod so that bleaching powder gets dissolved into water.
5. Necessary contact period of 20 minutes is given for bleaching powder to oxidize
chloro-organic compounds and form free available chlorine.
6. After the required contact period, the residual chlorine in each sample is
determined.
7. The first beaker which gives the residual chlorine between 0.1 to 0.2 mg/l that will
be the required dose for disinfection.
PRECAUTIONS:
1. The beakers should not be disturbed during its contact period.
2. The bleaching powder should be allowed to dissolve completely.
3. As far as possible, bleaching powder should be applied in solution form.
JAR TEST
AIM:
To find the optimum amount of coagulant required to treat the turbid waters.
PRINCIPLE:
Metal salts hydrolyse in presence of the natural alkalinity to form metal hydroxides.
The div alent cations can reduce the zeta-potential, while the metal hydroxides are good
absork=bents and hence remove the suspended particles by enmeshing them.
APPARATUS:
1. Jar test apparatus
2. Beakers
3. Pipettes
4. Turbidity meter
5. pH meter.
REAGENTS:
1. Alum solution (synthetic coagulant)
2. Nirmali solution (natural coagulant).
PROCEDURE:
1. Take 1 litre of sample into each of the 6 beakers.
2. Switch on the motor and adjust the speed of paddles to 100 rpm.
3. Add varying doses of alum solution i.e., 1 ml, 2 ml, 3ml, 4ml or 6ml to different
beakers simultaneously. (The doses varies with turbidity in water sample.)
4. Allow flash mix (at 100rpm) for 1 minute.
5. Reduce the speed of paddles to 40 rpm and continue mixing for 10
minutes.
6. Switch off the motor and allow 20 minutes for settling .
7. Collect the supernatant without disturbing the sediment and find the turbidity of
each.
8. Also record pH, colour, alkalinity. CO2 and temperature.
9. Repeat the experiment with high doses of alum, if satisfactory results are not
obtained.
10. The experiment may be repeated for different pH ranges.
11. Note the ideal (optimum) dose of the coagulant for excellent floc formation.
OBSERVATIONS:
1. Raw water turbidity (NTU) =
RESULT:
Ideal dose fo coagulant(mg/l) =
3
AVAILABLE CHLORINE
AIM
PRINCIPLE:
Chlorine is a strong oxidizing agent and liberates iodine from iodide ion.
CI2 + 2KI--------- I2 + 2KCI
Starch give blue colour with iodine
I2 + Starch -------- Blue colour.
The liberated iodine is titrated with standard sodium thiosulphate – a reducing agent.
I2 + 2Na2 S2O3 ----------- Na2S4O6 + 2Nal.
The disappearance of blue colour indicates the completion of reaction with free iodine is
converted back to iodide.
INTERFERENCE:
APPARATUS:
1. Conical flask
2. Burette
3. Pipette.
REAGENTS:
PROCEDURE:
1. Take 5 gm of fresh bleaching powder. Adding small quantity of water to it, and
prepare fine paste. Add some more water, stir and allow to settle for a few minutes.
Dilute it with distilled water to make upto 1 litre and stopper the container.
2. Take 25ml of the bleaching powder solution in a conical flask and add a pinch of Kl.
3. Add 10 ml of acetic acid and allow the reaction to complete.
4. Titrate the sample with standard sodium thiosulphate solution until the yellow colour
of the liberated iodine is almost faded out.
5. Add 1 ml of starch solution and titrate until the blue colour disappears.
6. Note down the quantity of sodium thiosulphate added (V1).
7. Repeat the same procedure fro distilled water.
8. Note down the volume of sodium thiosulphate added (V2).
3
CALCULATIONS:
Concentration of chlorine = (V1 –V2) X N X 35.45 X 1000
Vol. of bleaching powder solution.
burette burette
Readings readings
3
APPENDIX
APPENDIX A
PREPARATION OF STANDARD SOLUTIONS AND REAGENTS
1. Aluminium hydroxide suspension:
Dissolve 500 gm NaOH (or 700 gm of KOH) and 150 gm of Kl (or 135 gm of Nl) in
distilled water and dilute to one litre. Dissolve 10 gm of NaN3 in 40 ml of distilled
water separately and pour it into the above solution. This solution should not give
colour with starch solution when diluted and acidified.
Dissolve 250 gm of NH4C2H3O2 in 150 ml distilled water. Add 700 ml of glacial acetic
acid and the solution is diluted to 1 litre with distilled water.
(b) Dilute 112 ml of concentrated hydrochloric acid to 500 ml with ditilled water. Also
add 37 ml of concentrated sulphuric acid to 400 ml of distilled water and then dilute
to 500 ml. mix the two diluted acids when cool.
(c) Dilute the clear zirconium prepared in (a) to 1000 ml with mixed acid solution
prepared in (b). The reagent is at first red, but within an hour it changes to orange –
3
yellow and is ready for use. The solution shall be stored in the dark; if
kept in a refrigerator it is stable for 2 to 3 months.
6. Buffer solution:
7. Calcium chloride:
Mix 0.5 gm of eriochrome black T, with 100 gm NaCl (A.R.) to prepare dry powder.
9. Ferrion chloride:
12. Inhibitor:
Prepare a grind mixture of 0.2 gm of murexide with 100 gm of solid NaCl (A.R.).
Since this indicator is unstable under high pH, titration must start immediately after
adding this indicator powder to the sample under test.
Dissolve 50 gm K2Cr2O4 in a small quantity of distilled and add AgNO3 till definite
red precipitate is formed. Allow to stand for 24 hours. Filter and dilute to 1000 ml
with distilled water.
200 ml of 1M CH3COOH is mixed with 100 ml 1 M NaOH and 700 ml distilled water.
3
24. pH 7.0 buffer solution:
(a) Dissolve 12.40 gm H3BO3 in 100 ml NaOH and make it 1 litre with distilled water.
Weight accurately 1.0 gm AR grade CaCO3 and transfer to 250 ml conical flask.
Place a funnel in the neck of a flask and add 1 + 1 HCl till CaCO3 dissolves
completely. Add 200 ml distilled water and boil for 20 – 30 minutes to expel CO2.
Cool and add few drops of methyl red indicator. Add 3N NH4OH dropwise till
intermediate orange colour develops. Dilute to 1000 ml to obtain 1 ml = 1 mg Ca
CO3.
3
31. Sodium hydroxide 2N:
0.8 gm of NaOH is dissolved in CO2 free distilled water and diluted to 1000 ml. It is
standardized against 0.02 N potassium biopthalate, KHC3H4O4. Store in air tight,
rubber stoppered pyrex/coring glass bottle to protect from atmospheric CO2.
Dissolve 2.395 gm of dry AgNO3 in distilled water and dilute 1000 ml. Standardize
against NaCI. 1 ml. of 0.0141 N AgNO3 = 0.5 mg CI.
Completely dissolve 0.60 gm of sulphanilic acid in 70 ml. of hot distilled water, after
cooling, add 20 ml. of concentrated hydrochloric acid and dilute to 1000 ml. with
distilled water.
Dissolve 16.4 gm of an hydrous sodium acetate in distilled water and dilute to 100
ml. Filter if necessary.
Dissolve 0.246 gm of anhydrous sodium nitrite in nitrite – free distilled water and
dilute to 1 litre. Preserve by adding 1 ml of chloroform. One mililitre of the solution
contains 0.05 mg of nitrite nitrogen.
Dilute 10 ml of stock nitrite solution to 1 litre with nitrite free distilled water.
Preserve by adding 1 ml of chloroform and store in a sterilized bottle. One ml of
this solution contains 0.0005 mg of nitrite nitrogen (as N).
4
41. Standard phosphate solution:
Add 300ml concentrated H2SO4 to 600 ml distilled water. Add 4 ml conc. HNO3,
cool the solution and dilute to 1000 ml.
Dissolve 0.2 gm of NaOH in distilled water and dilute to 100 ml with distilled water.
Dissolve 2 gm of L.R. grade soluble starch in distilled water and pour this emulsion
into 100 ml of boiling water. Allow to boil for few minutes, add 0.2 gm of salicyclic
acid or toluene as preservative. Cool this solution and then use.
Dissolve 12.259 gm of K2Cr2O7 dried at 103oC for 24 hours in distilled water and
make upto 1000ml.
Add 100 gm of Ag2SO4 to 1000 ml of concentrated H2SO4 and keep over night for
dissolution.
4
50. Standard ferrous ammonium sulphate (0.1N):
Dissolve 0.221 gm of dry sodium fluoride in distilled water and make upto 1000 ml.
dilute 100 ml of the solution to 1000 ml. One milliliter of this diluted solution
contains 0.01 mg of fluoride (as F). The solution shall be kept in polyethylene or
wax-lined glass bottles.
Dissolve 721.8 gm anhydrous potassium nitrate and dilute to 1000 ml with distilled
water. 1 ml = µg NO3.
PREPATION OF STANDARD
SOLUTIONS AND REAGENTS
1. ACIDITY
Standard sodium hydroxide (0.02 N): 0.8 gm of NaOH is dissolved in CO2 free
distilled water and diluted to 1000 ml. It is standardized against 0.02 N potassium
biopthalate, KHC3H4O4. Store in air tight, rubber stoppered pyrex/coring glass bottle to
protect from atmospheric CO2.
Methyl orange indicator: 0.5 gm of methyl orange powder is dissolved in CO2 free
distilled water and diluted to one litre.
2. ALKALINITY
Standard sulphuric acid 0.02 N: Prepare 0.1 N H2SO4 by diluting 3 ml conc. H2SO4 to
1000ml. standardizes against standard Na2CO3 0.1 N. Take appropriate volume of
H2SO4 (approximatels 0.1N) and dilute with distilled weater to make upto 1 litre to
obtain standard 0.02N H2SO4
3. CHLORIDIES
Standard silver nitrate solution 0.0141 N: Dissolve 2.395 gm of dry AgNO3 in distilled
water and dilute 1000 ml. Standardize against NaCI. 1 ml. of 0.0141 N AgNO3 = 0.5
mg CI.
HARDNESS
Standard EDTA solution 0.01M: Dissolve 3.723 gm of EDTA sodium sald in distilled
water to prepare 1 litre of solution. Standardized against standard calcium solution such
that 1.0 ml of the EDTA titrant is equivalent to 1.0 mg CaCO3.
Eriochrome black T indicator: Mix 0.5 gm of eriochrome black T, with 100 gm NaCl
(A.R.) to prepare dry powder.
DO
4
Standard sodium thiosulphate (0.025 N): Dissolve 1.575 gm of Na2S2O3
in distilled water and make upto 1 litre (OR) Dissolve 6.205 gm of Na2S2O3 5H2O in
1000 ml(1 LItre) of water
Alkali iodide – azide reagent: Dissolve 500 gm NaOH (or 700 gm of KOH) and 150
gm of Kl (or 135 gm of Nl) in distilled water and dilute to one litre. Dissolve 10 gm of
NaN3 in 40 ml of distilled water separately and pour it into the above solution. This
solution should not give colour with starch solution when diluted and acidified.
Starch Indicator: Dissolve 2 gm of L.R. grade soluble starch in distilled water and pour
this emulsion into 100 ml of boiling water. Allow to boil for few minutes, add 0.2 gm of
salicyclic acid or toluene as preservative. Cool this solution and then use.
6. COD
7. FLUORIDE
Acid zirconium alizarin solution: (a) Dissolve 0.3 gm of zirconium oxychloride or 0.25
gm of zirconium oxynitrate in 50 ml of distilled water. Dissolve 0.07 gm of alizarin
sodium monosulphonate in another 50 ml of distilled water and add the latter solution
slowly to the zirconium solution with continuous stirring. The resulting solution clears on
standing for a few minutes.
(b) Dilute 112 ml of concentrated hydrochloric acid to 500 ml with ditilled water. Also
add 37 ml of concentrated sulphuric acid to 400 ml of distilled water and then dilute to
500 ml. mix the two diluted acids when cool.
(c) Dilute the clear zirconium prepared in (a) to 1000 ml with mixed acid solution
prepared in (b). The reagent is at first red, but within an hour it changes to orange –
4
yellow and is ready for use. The solution shall be stored in the dark; if kept
in a refrigerator it is stable for 2 to 3 months.
4