SSM INSTITUTE OF ENGINEERING AND

TECHNOLOGY

DEPARTMENT OF CIVIL ENGINEERING

CE – 6611 ENVIRONMENTAL ENGINEERING LABORATORY

LABORATORY MANUAL

NAME: ______________________

REG. NO: ____________________

YEAR/SEM: _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _

DEPT: _______________________
 INDEX

S.NO DATE LIST OFEXPREMENTS MARK SIGN

DETERMINATION OF AMMONIA
1.
NITROGEN IN WASTEWATER
DETERMINATION OF TURBIDITY OF THE
2. GIVEN WASTEWATER SAMPLE USING
NEPHELOMETER
COAGULATION AND PRECIPITATION
3. PROCESSFOR TREATING WASTEWATER

4. DETERMINATION OF HARDNESS IN WATER

5. DETERMINATION OF VOLATILE
ANDFIXED SOLIDS IN WASTEWATER
DETERMINATION OF SUSPENDED AND
6.
DISSOLVED SOLIDS IN WASTEWATER
DETERMINATION OF DISSOLVED
7.
OXYGEN

8. DETERMINATION OF CHEMICAL OXYGEN

DEMAND (C.O.D TEST)
DETERMINATION OF NITRATE IN THE
9.
GIVEN WASTEWATE SAMPLE
DETERMINATION OF BIOCHEMICAL
10. OXYGEN DEMAND (BOD TEST)

DETERMINATION OF PHOSPHATE IN
11.
THE GIVEN WASTEWATERSAMPLE

DETERMINATION OFPOTASSIUM IN
12.
THE GIVENWASTEWATERSAMPLE

DETERMINATIONOFSODIUMINTHEGIVEN
13. WASTEWATER SAMPLE
DETERMINATION OFCALCIUMIN
14.
THEGIVEN WASTEWATER SAMPLE
DETERMINATION OFHEAVYMETALS-
15.
DEMONSTRATION ONLY
 Laboratory Safety
1. State-approved safety goggles must be worn in the laboratory at all times.
This is required by state health regulation. Failure to observe this requirement will result in
your removal from the laboratory. The cost is approximately Rs100 (and trivial in comparison
to your eyesight). Safety glasses, etc. are not acceptable. If you already have goggles, you will
not be allowed in the laboratory and, consequently, will miss the experiment.
2. The use of contact lenses in the laboratory is absolutely prohibited. In the case of a splash
or other emergency, they may interfere with the flushing of the eye, you may not be in a
position to remove them, and those administering first aid may not know that you are wearing
them or might not be able to remove them easily.

3. You must dress appropriately for the laboratory. Lab coats are required to be worn. Bare
feet, sandals, or other open-toed shoes are not permitted in the laboratory. Shorts and short
skirts are likewise not permitted; legs must be covered to below the knees. Headphones are not
allowed in the laboratory.
Failure to observe these requirements will result in your removal from the laboratory. Cotton
clothing (including denim) is particularly susceptible to being eaten by acid solution. The
laboratory is not a good place to wear your favorite clothes. Long hair should be tied back.

4. The fire extinguishers should only be used for real emergencies since the chemicals they
contain can cause considerable damage. In any emergency that requires the assistance of the
fire department, aid car, or police, sends someone to the stockroom for assistance. Should
clothing catch on fire, remain as calm as possible. Walk (do not run) to the safety shower and
pull the ring to douse yourself with water. Alternatively, you may drop to the floor and roll to
extinguish the flames.

5. Become familiar with all of the exits from the laboratory. A repeating siren and flashing of the
FIRE indicator is the building evacuation signal. If this alarm goes off while you are in the lab,
turn off any open flames, grab your valuables, and leave the building as quickly as possible.
6. Never attempt any unauthorized or unassigned experiments. Follow the experimental
procedures explicitly, checking and double-checking the identity of all reagents before you use
them. There are potentially hazardous combinations of chemicals present in the laboratory. If
you have an idea for further investigation, discuss it with your instructor.
7. Clean up spills immediately. The next person to come along has no way of knowing if the
clear liquid or white powder on the lab bench is innocuous or hazardous. Neutralize acid spills
with sodium bicarbonate (baking soda) before cleaning them up. Spills of sulfuric acid
solutions are particularly hazardous since only the water will evaporate, thereby making the
 solution more concentrated upon standing.
8. Never return unused reagents to their storage container. If you take more than you need,
dispose of the excess in the appropriate manner. Use the reagents
sparingly—they are expensive and time-consuming to prepare. When taking
reagents, transfer the amount you need to a clean beaker or other suitable
container for taking the material back to your desk. Never insert a pipette or any
9. Keep coats, backpacks and other non-essential materials away from areas where people are
working.
10. Dispose of all broken glassware and other sharp objects in the cardboard glass disposal boxes.
Custodial personnel will stop collecting trash after they find broken glass in the trashcans.
11. Wash hands often when working in lab, and always wash thoroughly before leaving.
12. Use the hood for evaporation of anything other than water. The vapors from your procedure
alone may not present a problem but those from all the students in the lab could combine to
create a hazard.
13. Do not leave a Bunsen burner or other heated apparatus unattended. The person working
next to you may not know what is involved with your setup and may be working with a
flammable material. Turn off open flames if you must leave your area. Make sure the gas taps
are completely off whenever the Bunsen burner is not lit.
14. Waste Disposal Dispose of chemical reagents and other materials properly. The proper disposal
of chemical wastes is essential to the health and safety of Institute faculty, staff, students and
the surrounding community.
Tabulation

S.No Volume Initial Finalburette ConcurrentBur VolumeofSulp

buretteReadi Reading(ml) ettereading(ml) huric acid(ml)
ofwater ng
Sample (ml) (ml)

Calculation

NH3- N2mg/l =VolumeofH2SO4consumed x0.28 x1000

Volumeofsample taken
Exp No:
DETERMINATION OFAMMONIANITROGEN INWASTEWATER
Date:

Aim
To determine theamount of AmmoniaNitrogenpresent in the givenwastewatersample.

Principle
In theammoniatest, Nessler Reagent(K2HgI4)reacts with the ammoniapresent inthe
sample(under stronglyalkaline conditions) to produce ayellow-coloredspecies.
Theintensityof thecolor is indirectproportion to theammoniaconcentration..

Apparatusrequired
1. Measuringjar
2. Conical flask
3. Burette
4. Pipette

Reagents
1. Phosphatebuffer solution
2. Boricacid
3. Methylorange indicator
4. Sulphuric acid 0.02N (1 ml co n ta ins 0 . 2 8mgo f nitr ogen)

Procedure
1. Take 50ml of thesamplein a conical flask.
2. Add 5ml of phosphatebuffer solution and 10 ml ofboricacid solution.
3. Add 3 -5drops of methylorange indicator.
4. Titrateagainst0.02Nofsulphuricacidtilltheendpointischangesfromorangetoyellow.

Environmental Significance
1. Excess of ammonia in the form of nitrogen leads to Eutrophication in
lakes.2.Consumption of Nitrogengreaterthan 2mg/Iindrinkingwatermayleadto
mathemoglobonemia in children.

Application
1. Determination ofammoniacalnitrogenis usedforstandardizingthedrinking
watersupplyas perIS
2. Thedata is used in the treatment of waste waterbefore it is subjected to water-
courses.It is also used todetermine the extent of eutrophicationand possible methodsof removal ofNitrogen.
Further studies:
To removeexcess ofammonianitrogen thefollowingmethods areused
1. Ionexchange method
2. Biologicalremoval(nitrificationanddenitrification)
3. Airstrippingofammonia

Result
Theamount of AmmoniaNitrogenpresent in the given sample is------------mg/l.
Exp No: DETERMINATION OFTURBIDITYOFTHE GIVEN
Date: WASTEWATERSAMPLEUSINGNEPHELOMETER

Aim
To determine the turbidityofthegiven sample usingNephelometerin NTU.

Principle
Anephelometerisaninstrumentformeasuringconcentrationofsuspendedparticulatesinaliquid
orgascolloid.Anephelometermeasuressuspendedparticulatesbyemployingalightbeam(sourc
ebeam)andalightdetectorsettooneside(often90°)ofthesourcebeam.Nephelometryisconcerne
dwithmeasurementofscatteredlightfromacuvettecontainingsuspendedparticlesinasolution.
Theamountofscatteredlightdependsonthesizeandnumberof particles in suspension.

Apparatusrequired
1. Nephelo turbiditymeter
2. Cuvette
3. Standardmeasuringflask

Reagents
1. hydrazinesulphate(NH2)2H2SO4
2. hexamethylenetetramine(CH2)6N4(hexamine)

PreparationofFormazineTurbidity Concentrate
(a) Solution I
Weighaccurately5gof‘Anal–
R’qualityhydrazinesulphate(NH2)2H2SO4intoa500mLvolumetricflaskandadddistilled
watertomakeuptothemark.Leavethemixturetostandfor4 hours.

(b) Solution II

Weighaccurately50gof‘Anal–
R’qualityhexamethylenetetramine(CH2)6N4(hexamine)intoa500mLvolumetricflaskan
dadddistilledwatertomakeuptothemark.MixequalvolumeofsolutionIandIItoformformazi
neturbidityconcentrate.Allowittostandinaclosedcontainerat25°Cto30°Cfor48hourstopro
duceinsolublewhiteturbiditycorrespondingto 4000 NTU.
Note:Onceprepared,formazineturbidityconcentrate(whichcorrespondsto10000ppmSiO2
)is stable for 2 to 3 months.
 TABULATION

S.No Sample Temperature(˚C) Turbidity (NTU)

1.

2.

3.

EnvironmentalSignificance:

1. Turbidityisthecloudinessorhazinessofafluidcausedbylargenumbersofindividu
alparticlesthataregenerallyinvisibletothenakedeye,similartosmokeinair.
Themeasurement ofturbidityisakeytest ofwaterquality.
2. Indrinkingwater,thehighertheturbiditylevel,thehighertheriskthatpeoplemayde
velopgastrointestinaldiseases

Applications:

1. To identifytheconcentration of suspended particles in drinkingwater and

wastewater
PreparationofFormazine Standard

Dilute25mLoftheformazineturbidityconcentrateto1litrewithturbidityfreedistilledwaterto
obtain 250 ppmor100 NTUfor setting‘100’ofthe instrument.
Note: Formazinestandard 100 NTU should be prepared weekly

Procedure

1. Switch the instrument on.

2. Open the lid of thesample compartment.
3. Insert atest tube filled with distilledwaterinto the sample compartment. Close the
lid.
4. Adjust ‘SET 0’control to get ‘0’ displayed on theread out.

5. Openthelid.Replacethetesttubefilledwithdistilledwaterwithatesttubefilledwit
h formazinestandardClose the lid.
6. Adjust the ‘SET 100’control to get ‘100’ displayed on the read out.
7. place the sample in thecuvette andread the correspondingNTU forthegiven
sample

Measurement of turbidityless than 100 NTU

1. Thoroughlyshakethesample.
2. Wait until air bubblesdisappearand pourthe sampleinto the nephelometer tube.
3. Read the turbiditydirectlyfrom the instrument.

Further studies:

1. Sodiumhypochloritesolution(chlorine)iseffectiveattreatingbothclearandturbi
d(dirty-looking)water.

2. Theotheravailableinexpensivemethodsare,Filtrationthroughacloth,Filtrationt
hroughsand, Settlingand decanting,Moringaseed flocculation, Alum
flocculation.

Result:

Theamount of turbiditypresent in thegiven water sample = ---------------------

Observations

Rawwaterturbidity(N
TU)=RawwaterpH=

S.No Sample details Dosage Residual pH

ofcoagula turbidity
nt
Exp No:
COAGULATION AND PRECIPITATION PROCESS
Date: FORTREATINGWASTEWATER

Aim

To find out the optimum coagulant dosage to treat the wastewater.

Principle
Inwatertreatment,coagulationistheresultoftheadditionofchemicalreagentstowatersus
pensionswherethedispersedcolloidalparticlesareassembledinlargeraggregatescalledfloc
sormicroflocs.Inotherwords,thedestabilizationofcolloidalparticlesbytheintroduction of
an opposite charge.

ApparatusRequired
1. Jars mixer
2. Turbidwater
3. Beakers
4. Pipettes
5. Turbiditymeter
6. pH meter
Reagents

Alum solution

Theory:

Theamountofcoagulantrequiredforcoagulationdependsontheturbidityofthewaste
water.Theuseofoptimumamountofcoagulantisindicatedbytheformationofthelargefeathe
ry flakes.Thiscanbeapproximately determinedinthelaboratory
byJartest.Thetestinvolvesrapidmixingtodispersethechemicals(coagulants)inthesamplea
ndslowmixingfor the floc formation.

Procedure

1. 200ml of watersample istaken in

eachjar.Increasingdoseofalum(1%)i.e.1gm/100ml of
 distilledwateradded toslowlyfor15min andallowed tostandfor15min.

2. Thejars areobserved and the settlingof sedimentsarenoted.

Thequalityofalumadded to thejar containingtheclearest solution is
noted.
3. Take the sample out of beakerand test
forturbidityusingnephelometerineach trial,plot the curve on xandyaxis of
the graph sheet. Takethe alum dosagein ml alongxaxis and
turbidityalong-yaxis.
Environmentalsignificance and application
Thesuspendedmaterialinwatersandinwastewatersmostlyarisesfromlanderosion,th
edissolutionofminerals,thedecayofvegetationandfromseveraldomesticandindustrialwaste
discharges.Foragivenwaterorwastewater,suchmaterialmaycomprisesuspended,dissolved
organicand/orinorganicmatter,aswellasseveralbiologicalorganisms,suchasbacteria,algaeo
rviruses.Thismaterialhastoberemoved,asitcausesdeteriorationofwaterqualitybyreducingt
heclarity(e.g.causing turbidity or colour),causinginfection,andeventuallycarryingtoxic
compounds,adsorbed ontheir surfaces

Further studies

Acid washing(sulphuricacid) is an effective method to

removecoagulantsfromwastewater.ThepH level is between1-3.

Result
Theoptimum dosage ofcoagulantrequired to removeturbidityin thegivenwatersample is
……………
OBSERVATION :
Source of sample :
Date of collection :
Time :
Temperature :

Tabulation

Volume of
EDTA
water Hardness
S.No. Burette Reading (ml) Consumed
sample (mg/L)
(ml)
(ml)
Initial Final

Calculation

ml of EDTA used
Hardness in mg/1 of CaCO3 = x 1000
ml of water sample
Exp No:
DETERMINATION OF HARDNESS
Date:

Aim
To determine the total hardness present in the given sample

Apparatus Required
Burette, Pipette, Conical flask, measuring jar

Chemicals Required
Eriochrome Black-T (EBT) indicator, Ammonium chloride, Ammonium solution, EDTA

Reagents Preparation
EBT indicator
Dissolve 0.2 g of pure solid in 15 ml of distilled water
Standard EDTA Titrant
Take 0.5 g of EDTA. Heat it to 80oC for half an hour and cool it. Take 0.37 g of the
dissolve and add to get distilled water to make 100ml.
1 ml of exactly 0.02 N EDTA1mg of
CaCO3 Ammonia Buffer solution
Dissolve 0.7 g of ammonium chloride (NH4C1) in 5.7ml concentrate ammonia solution
and dilute to 100 ml.

Procedure

1. Take 20 ml of the sample in a conical flask.

2. Add 2ml of ammonia buffer to the flask.
3. Add 5 — 6 drops of EBT indicator to the flask wine red colour will be developed.
4. Titrate it with standard EDTA solution which is filled in the burette till the colour
changes from wine red to blue.
5. Repeat steps I to 4 for different samples with varying hardness and also for distilled
water (blank)
6. For determination of non-carbonate hardness the sample is to be boiled for 30
minutes. The procedure is the same as above.

Sanitary
7. Significance
Hard water has adverse action with soap since it allows less formation of leather. If hard
water is used in boilers, scaling problem occurs leading to the bursting of boilers, It
makes food tasteless. It affects the working of dyeing process. It is also precipitate
protein of meat and make tasteless.
Application of Hardness data in Environmental Engineering Practice
1. Hardness of water is important in determining the suitability of water for domestic and
industrial uses.
2. The relative amounts of calcium and magnesium hardness, carbonate and non-carbonate
hardness present in water are the factors while determining the most economical type of
softening process.

3. Determination of hardness serve as a basis for routine control of softening process.

Result
Hardness present in given semple ………………………………………………….
 Observation
Volume ofliquid sample taken = ml.
Emptyweightofcrucible(W1) = g.
Weight of crucible after
ovendrying(W2) = g.
Weight of crucible afterplacing
in mufflefurnace (W3) = g.

Calculation
Total Solids (TS) in the given sample (mg/l) = 𝑊2-𝑊1 x 10n
𝑉𝑜𝑙𝑢𝑚� 𝑜� 𝑠𝑎𝑚𝑝𝑙� 𝑡𝑎𝑘��

Total fixed Solids (TFS) in the given sample (mg/l) = 𝑊3-𝑊1 x 10

𝑉𝑜𝑙𝑢𝑚� 𝑜� 𝑠𝑎𝑚𝑝𝑙� 𝑡𝑎𝑘��

Total volatile Solids (TVS) in the given sample (mg/l) = 𝑊2-𝑊3 x 10

𝑉𝑜𝑙𝑢𝑚� 𝑜� 𝑠𝑎𝑚𝑝𝑙� 𝑡𝑎𝑘��
Exp
No: DETERMINATIONOFVOLATILEANDFIXEDSOLIDSINWASTEWA
TER
Date:

Aim:
Todeterminetheamountoftotal,fixedandvolatilesolidspresentinthegivenwastewater sample.

Principle:
Gravimetricanalysisdescribesasetofmethodsinanalyticalchemistryforthequantitativedetermina
tionofananalytebasedonthemassofasolid.Asimpleexampleisthemeasurementofsolidssuspendedin
awatersample:Aknownvolumeofwaterisfiltered,and the collected solids areweighed.
ApparatusRequired:
1. Crucible
2. Weighingbalance
3. Hot airoven
4. Mufflefurnace
5. Desicator
Procedure:
1. Take the emptycrucible,cleanand dry. Takeemptyweightofcrucible (W1)g.
2. Add known quantityof liquid sample in the crucible
3. Heatthecrucibleinwaterbathat100°Ctilltheentireliquidinacrucibleevaporatesanddryresidue
remainsat thebottom thenplace the crucible in oven at 103°C for 1 hour.
4. Taketheweightofthecruciblewithresidueaftercoolingitinadesicatorfor20minutes.Let us
weightbe (W2)g.
5. Take thesamplecrucibleand keep it inamuffle
o for C
furnaceatatemperatureof650
30minutes.

6. Thevolatileandorganicmatterinthesolidsevaporatedandthecruciblecontains
onlyfixed solids.

7. Coolthecrucibleinadesicatorandweightitwiththefixedsolidsresidue.Letthe
weightbe (W3)g.
Environmental EngineeringSignificance:
Thewaterwhichcontainsofhighvolatilesolidsisnotsuitablefordrinkingpurposes.The
resultofhighvolatilesolidsindicatesthatthewatermayhavebeenpollutes
bydomesticwasteorotherorganicwaste.Ingeneral,groundwater
isfreefromvolatilesolidsunlesstheyhavebeenpollutedbywasteseepages.But,wellwatermayha
vehighvolatilesolidsduetolackofproperprotectionaroundwelltopreventseepageofusedwater.
Surfacewatermayalso havehigh volatilesolids duetodisposal of domestic and otherwastes.

Environmental Significanceand Applications

1. Volatile solids test is normallyapplied to sludges.

2. Itis indispensablein the designoperationof sludgedesicator,vacuum filter

andinfiltration plants.

3. BeforethedevelopmentofC.O.D.testitisusedtofindthestrengthofindustrialanddomestic
wastewater.

4. It is helpful in accessingtheamountbiologic allyinertorganic matter, such aslignin

inthe case ofwood pulping waste liquor.

Further studies:
Solids present in the wastewatercanbe removedusingfiltrationprocess.

Result
1. Total Solids (TS) in the givenwastewatersample =
2. Total fixed Solids (TFS) in the givenwastewater sample =
3. Totalvolatile Solids (TVS) in the givenwastewatersample =
Observation
Volume ofliquid sample taken = ml.

Total Solids (TS)

Emptyweight ofcrucible(W1) = g.
Weight of crucible with residue
afterwaterbath(W2) = g.

Total Dissolved Solids(TDS)

Emptyweight ofcrucible(W3) = g.
Weight of crucible with residue
afterwaterbath(W4) = g.

Calculation
Total Solids (TS) in the given sample (mg/l) = 𝑊2-𝑊1 x 10n
𝑉𝑜𝑙𝑢𝑚� 𝑜� 𝑠𝑎𝑚𝑝𝑙� 𝑡𝑎𝑘��

Total fixed Solids (TFS) in the given sample (mg/l) = 𝑊3-𝑊1 x 10

𝑉𝑜𝑙𝑢𝑚� 𝑜� 𝑠𝑎𝑚𝑝𝑙� 𝑡𝑎𝑘��

Total volatile Solids (TVS) in the given sample (mg/l) = 𝑊2-𝑊3 x 10

𝑉𝑜𝑙𝑢𝑚� 𝑜� 𝑠𝑎𝑚𝑝𝑙� 𝑡𝑎𝑘��
Exp No: DETERMINATION O FSUSPENDEDAND DISSOLVED
Date SOLIDS IN WASTEWATER
Aim:
To determine theamount of suspendedand dissolved solids present in thegiven
sampl
e.

Principle:
Gravimetricanalysisdescribesasetofmethodsinanalyticalchemistryforthequa
ntitativedeterminationofananalytebasedonthemassofasolid.Asimpleexampleisthem
easurementofsolidssuspendedinawatersample:Aknownvolumeofwaterisfiltered,an
d thecollectedsolids are weighed.

ApparatusRequired:
1. Crucible
2. Oven
3. Desiccator
4. Weighbalance.

Procedure:
1. Take the crucible,cleananddry. Takeemptyweight of crucible (W1)g.
2. Add known quantityof liquid sample in the crucible
3. Heat the crucible in water bath at 100°C till the entireliquid in a crucible
evaporates
anddryresidue remainsat thebottom thenplace the crucible in oven at
103°C for 1hour.
4. Taketheweightofthecruciblewithresidueaftercoolingitinadesiccatorfor20mi
nutes.Let us weightbe(W2)g
5. Knownquantityofsampleisfilteredthroughwattmanfilterpaper.Thedissolved
solids go in solution through the filterpaper.
6. Thenproceed theabove steps 1 to 4 forthe filteredsample.

EnvironmentalSignificance:
1. Waterwithhighdissolvedsolidsgenerally isofinferiorpolatibility
andmakesituseanunfavorablephysiologicalreaction in a transit consumer.
2. SuspendedSolids
containingmuchorganicmattermakeaspurificationandconsequentlythismaybe
dividingofdissolvedoxygenloadingtodestructionofplantand human life.

Application:
1. Dissolvedsolidsdeterminationgivesanideaabouttheformationofscalescauseoffoa
minginboilers,accelerationofcorrosionandinterferencewiththecolourandtasteof
manyfinishesproducts.
2. Thesuspended solid determination is particularlyuseful in the analysis of sewageand
otherwastewater.It is used to evaluate the strength of waste waterand to determine
theefficiencyof treatment units.

Further studies:
Solids present in the wastewatercanbe removedusing filtrationprocess.

Totalsuspended Solids (TSS) in the givensample(mg/l) = TS -TD

Result
1. Total Solids (TS) in the givenwastewatersample =
2. TotalSuspended Solids (TSS) in the givenwastewatersample =
3. Total Dissolved Solids (TDS) in the givenwastewatersample =
AIM
Exp No: DETERMINATION OF DISSOLVED OXYGEN
Date
To determine dissolved oxygen(DO) in the given water sample with the stipulations.

PRINCIPLE
Dissolved Oxygen can be measured either by titrimetric or electrometric method.
TitrimetricMethod
TitrimetricmethodisbasedontheoxidizingpropertyofDOwhiletheelectrometricmeth
od(usingmembraneelectrodes)isbasedontherateofdiffusionofmolecularoxygenacro
ssamembrane.It ismost accuratemethod todetermineDO.

Therearedifferenttitrimetricmethodsbasedon thenatureofsample tobetested.

(a) WinklerMethod
(b) AzideModification
(c) AlumFlocculationModification
(d) PermanganateModification
TheTitrimetricprinciple:
DivalentManganesesaltinsolutionisprecipitatedbystrongalkalitodivalentmanganesehydroxi
de.

AdditionofPotassiumiodideorPotassiumhydroxideisaddedtocreateapinkishbrownprecipitate
.
Inthealkalinesolution,dissolvedoxygenpresentinthesamplerapidlyoxidizedtoformtrivalentor
highervalencyhydroxide.

MnO(OH)2appears asabrownprecipitate.Thereis someconfusionabout

whethertheoxidisedmanganeseistetravalentor
trivalent.SomesourcesclaimthatMn(OH)3isthebrownprecipitate,buthydratedMnO2mayalsog
ivethebrowncolour.
Iodideionsareaddedandacidified(acidfacilitatestheconversionbythebrown),whichreducestet
ravalenthydroxidesbacktotheirstabledivalentstatetherebyliberatingequivalent
amountofiodine.

Thiosulphatesolutionis used, with a starchindicator, totitratetheiodine.

This iodineis equivalent todissolvedoxygenpresentinthesample.

.
APPARATUS REQUIRED

1. Burette
2. Burettestand
3. 300mLglassstoppered BODbottles
4. 500mLconicalflask
5. Pipetteswith elongatedtips
6. Pipette bulb
7. 250mLgraduatedcylinders
8. Washbottle
CHEMICALS REQUIRED

1. Manganoussulphatesolution
2. Alkaline iodide-azide solution
3. Sulfuricacid,Concentrated
4. Starchindicatorsolution
5. Sodium thiosulphate
6. Distilled or deionized water
7. PotassiumHydroxide
8. PotassiumIodide
9. SodiumAzide
i. PRECAUTIONS

Theexperimentinvolveslotofsolutionsandadditionsofstrongacidandalkaliandhence
careshouldbetaken.
 Dissolvedoxygenconcentrationsmaychangedrasticallydependingupondepth,distance,
temperature andperiodofsampling.
 Ifthesamplewasobtainedbyasamplingdeviceofsomekind,thewatercannotbesimplypou
redintoaBODbottle,sincethiswouldcauseaerationofthesample.Instead,thesamplemus
tbedrawnofffromatubelocatednearthebottomofthesamplingdevice.Placetherubbertu
beintothebottomoftheBODbottleandfillthebottle,againallowingthebottletooverflow.
 Forshallowdepthusenormalwatersamplers.Howeverfordepthgreaterthan150cm(5ft),u
seKemmererSampleBottles.
ENVIRONMENTALSIGNIFICANCE

 Drinkingwatershouldbe richindissolvedoxygenforgoodtaste.
 DOtestisusedtoevaluatethepollutionstrengthofdomestic and
industrialwaste.Highervalues of DO maycause corrosionof IronandSteel.
 AlgaegrowthinwatermayreleaseoxygenduringitsphotosynthesisandDOmayeven
shoot upto30mg/L.
 Oxygenispoorlysolubleinwater.Itssolubilityisabout14.6forpurewaterat0°Cundernorm
al atmosphericpressureandit drops to7mg/lat 35°C.
  Highertemperature,biologicalimpurities,Ammonia,Nitrates,ferrousiron,chemicals
suchashydrogensulphideandorganicmatter reduceDOvalues.
 Aerobicbacteriathrivewhenoxygenisavailableinplenty.Aerobicconditionsdoprevailw
hensufficientDOisavailablewithinwater.Endproductsofaerobiosisarestableandarenot
foulsmelling.
 ItisnecessarytoknowDOlevelstoassessqualityofrawwaterandtokeepacheckon
streampollution.
 DOtestisthebasisforBODtestwhichisanimportantparametertoevaluateorganicpollutio
n potentialofa waste.
 DOtestisnecessaryforallaerobicbiologicalwastewatertreatmentprocessestocontrolther
ateofaeration.

PREPARATION OFREAGENTS
a) ManganousSulphateSolution
DissolveManganese Sulphate
480gof (or)
400gof (or)
364gof
infreshlyboiledandcooleddistilledwater,filterthesolutionandmakeupto1000mL(Onel
itre).Inthisexperiment,weareusingManganesesulphateMonohydrate,

Take364gManganesesulphateMonohydrate( )andtransferitto
thebeaker.Todissolvethe content,placeitinthemagneticstirrer.

Thesolutionshouldnotgivebluecolorbyadditionofacidifiedpotassiumiodide
solutionandstarch.
b) Alkaline IodideSodiumAzideSolution
Topreparethis reagentwearegoingtomixthreedifferentchemicals
Dissolveeither
500gofSodiumHydroxide(or)
700gofPotassiumHydroxideand
135gofSodiumIodide(or)
150 gof PotassiumIodide
Topreparethisreagent,take700gofPotassiumhydroxideandadd150gofpotassiumiodid
eanddissolveitinfreshlyboiledandcooledwater,andmakeupto1000mL (Onelitre).

Dissolve10gofSodiumAzide in40mLofdistilledwaterandaddthiswithconstan
t stirringto thecoolalkalineiodidesolutionprepared.
c) SodiumThiosulphateStockSolution
Weighapproximately25g ofsodiumthiosulphate and
dissolveitinboileddistilledwaterandmakeupto1000mL.Add1gofSodiumHydroxide
topreserveit.

TABLE
 BuretteReadi Volumeof
Temper VolumeofSam DissolvedOxyge
S. ng(mL SodiumThiosulp
atu ple(mL) hate(mL) n(mg/L)
No. )
re Initial Final
(ºC)
1
.
2
.
3
.

BuretteSolution:SodiumThiosulphateP
ipetteSolution:Sample
Volume of Sodium Thiosulphate V1= ml
Normality of Sodium Thiosulphate N1= N
Volume of sample V2 = ml
Indicator:Starch
 d) StarchIndicator
Weigh2gofstarchanddissolvein100mLofhotdistilledwater.Incaseifyouaregoingtopre
servethestarchindicatoradd0.2gofsalicylicacidaspreservative.
e) Sulphuric Acid

PROCEDURE:

 Taketwo300-
mLglassstopperedBODbottleandfillitwithsampletobetested.Avoidanykindofbubbling
andtrappingofairbubbles.Remember–nobubbles!
(Or)
 Takethesamplecollectedfromthefield.ItshouldbecollectedinBODbottlefilleduptotheri
m.

 Add2mLofmanganesesulfatetotheBODbottlebyinsertingthecalibratedpipettejustbelow
thesurfaceoftheliquid.

 Add2mLofalkali-iodide-azidereagentinthesamemanner.

 Squeezethepipetteslowlysonobubblesareintroducedviathepipette(Thepipetteshouldbe
dippedinsidethesamplewhileaddingtheabovetworeagents.Ifthereagentisaddedabovethe
samplesurface,youwillintroduceoxygenintothesample).

 If oxygenispresent,a brownish-orangecloudofprecipitateorflocwillappear.
 Allowit tosettleforsufficienttimeinorderto reactcompletelywithoxygen.

 Add2mLofconcentratedsulfuricacidviaapipetteheldjustabovethesurfaceofthesample.
 Carefullystopperandinvert several times todissolvethefloc.
 Atthispoint,thesampleis"fixed"andcanbestoredforupto8hoursifkeptin acool,
darkplace.

 Rinsetheburettewithsodiumthiosulphateandthenfill
itwithsodiumthiosulphate.Fixtheburettetothe stand.

 Measureout203mLofthesolutionfromthebottleandtransfertoanconicalflask.

 Titrationneedstobestartedimmediatelyafterthetransferofthecontentstoconicalflask.
 Titrateitagainstsodiumthiosulphateusingstarchasindicator.(Add3-4dropsof
starchindicatorsolution)

 Endpointof thetitrationisfirstdisappearanceof thebluecolortocolorless.

 Notedownthevolumeofsodiumthiosulphatesolutionaddedwhichgivesthedissolvedoxyg
envalue
 Repeat thetitrationforconcordant values.

RESULT
Dissolved oxygen present in given waste water sample is ………………………….
 Observations

S.NO Volume of Burette Reading(ml) Volume of CODofthe

Sample FAS
sample consumed Sample
Initial Final
(ml) (ml) mg/l

1. Blank

2.
Sample 1

Sample 1
3.

Calculation
A−B ×N ×8 xV
TotalChemicalOxygenDemand(mg/L) =
1000

Where,

A – Volume ofFerrous Ammonium Sulphateused for blank solution

B – Volume ofFerrous Ammonium Sulphateused for sample titration

N – NormalityofFerrous Ammonium Sulphate solution

V – Volume ofwastewatersample taken

Exp No: DETERMINATIONOFCHEMICALOXYGENDEMAND(C.O
.DTEST)
Date
 Ai
m
To determine thechemicaloxygendemand in thewastewatersample.

Principle
TheorganicmatterpresentinsamplegetsoxidizedcompletelybyK2Cr2O7int
hepresenceofH2SO4toproduceCO2andH2O.TheexcessK2Cr2O7remainingafter
thereactionistitratedwithFe(NH4)2(SO4)2(Ferrousammoniumsulphate).Thedic
hromateconsumedgives the O2required to oxidation of the organicmatter.

ApparatusRequired
1. COD Digester
2. Burettewith stand
3. Pipette
4. Measuringjar
5. Tiles
6. Beakers
7. Conical flask

ChemicalsRequired:

1. Potassium dichromate
2. Sulfuricacid
3. Ferrousammoniumsulphate
4. Silversulphate
5. Mercurysulphate
6. Ferroinindicator
7. Organicfree distilled water

ReagentsPrepar
ation:
1. StandardPotassiumDichromateReagent-Digestion Solution
Weighaccurately4.913gofpotassiumdichromate,previouslydriedat103ºCfor2-
4hoursandtransferittoabeaker.Weighexactly33.3gofmercuricsulphateandaddtot
hesamebeaker.
Measureaccurately167mLofconcentratedsulphuricacidusingcleandrymeasurin
gcylinderandtransferittothebeaker.Dissolvethecontentsandcooltoroomtemperat
ure.
(Ifnotdissolvedkeepitovernight).Take1000mLstandardmeasuringflaskandplaceafunnelover
it.Carefullytransferthecontentstothe1000mLstandardflaskandmakeupto1000mL
usingdistilledwater.Thisisthestandardpotassiumdichromatesolutiontobeusedfordigestion.
2. SulphuricAcidReagent - Catalyst Solution
Weighaccurately5.5gsilversulphatecrystalstoadryclean1000mLbeaker.Tothiscare
fully addabout500mLof concentratedsulphuric
acidandallowtostandfor24hours(so that the silversulphatecrystals
dissolvecompletely).
3. StandardFerrous AmmoniumSulphate solution
Weighaccurately39.2gofferrousammoniumsulphatecrystalsanddissolveitindistille
dwater.Take1000mLstandardmeasuringflaskandplaceafunneloverit.Carefullytran
sferthecontentstothe1000mLstandardflaskandmakeupto1000mLmarkusingdistill
ed water.
PROCEDURE
1. Take threeCODvials with stopper(twofor thesample and one for theblank)
2. Add 2.5 mLof thesampleto eachof thetwo CODvials and the remaining
CODvial is forblank; to this CODvial adddistilledwater.
3. Add1.5mLofpotassiumdichromatereagent-
digestionsolutiontoeachofthethreeCODvials.
4. Add 3.5 mLofsulphuricacidreagent-catalyst solution in the samemanner.
CAUTION: CODvialsarehot now.
5. Cap tubes tightly. Switchon the COD Digesterand fixthe
temperatureat150º C andset thetime at 2 hours.
6. Place the CODvials into a block digester at 150°C andheat for two hours.
7. Thedigesterautomaticallyswitchesoff.Thenremovethevialsandallowittocooltother
oom temperature.
8. Meanwhile,get readywith the burette for the titration.
9. Filltheburettewiththeferrousammoniumsulphatesolution,adjusttozeroandfixthebu
rette to thestand.
10. Transfer thecontents of theblank vial to conical flask.
11. Add fewdropsofferroinindicator. Thesolution becomes bluish green incolour.
12. Titrate it with the ferrousammoniumsulphatetaken in the burette.

13. End point of thetitration is the appearance of thereddish browncolour.

Environmentalsignificance and applicationofCOD:

1. CODtest is used extensivelyin theanalysis of industrial wastes.
2. Itisparticularlyvaluableinsurveysystemtodetermineandcontrollos
sesin sewersystem.
3. It is useful to access the strengthofwastewhich contains
toxins andbiologicalresultant andorganicsubstance.
4. Theratio ofBOD to COD is useful toAccess
theamenabilityofwasteforbiologicaltreatment.
5. Theratio ofBOD to COD is greaterthan or equalto 0.8
indicatesthatthe waste waterarehighlyamenable
tobiologicaltreatment.

Further studies:

Hydrogenperoxide(H2O2) is one of the effective methods to reduce the

BOD or COD level in wastewater.

Result

TheCODof the given sampleis-----------------------

Calculation:
S.No. Samples Nitrateconc.(ppm)
1.

2.
 Aim:No:
Exp DETERMINATION OFNITRATE IN THE GIVEN
Date
To WASTEWATERSAMPLE
determine the Nitratein the given watersample.

Principle:
Nitratesreactwithphenoldisulphonicacidandproduceanitratederivative,whichinalkal
inesolutiondevelopsyellowcolourduetorearrangementofitsstructure.Thecolourproduced is
directly proportional to the concentration of nitratespresent inthe sample.

Apparatusrequired:
1. Ion meter
2. Nitrateelectrode
3. ISABbuffer solution
4. stock nitrate solution

ReagentsPreparation:
1. Stocknitratesolution:721.8mg(0.722g)ofARpotassiumnitrateisdissolvedindistille
d waterand made up to 100ml forstock solution.
2. Standardnitratesolution:Standardnitratesolutionispreparedbyevaporating50mloft
hestocksolutiontodrynessinthewaterbath.Theobtainedresidueisdissolvedin2mlofph
enoldisulfonicacidanddilutedto500ml,togive1ml=10
g.Thesolutionofvariousstrengthsrangingfrom0.0(blank)to1.0mg/Lattheintervals of
0.2 mg/Lis preparedbydilutingstocksolution with distilledwater.

Procedure
1. Switch on theion meter and fixthe nitrateelectrode with the instrument
2. Calibrate the instrument with10 ppm or 100 ppm based on the sampleconcentration
3. Take 5ml of nitratecontainingsample andadd 3%ofISAB buffer solutionto
supressthe concentration ofother ions exceptnitrate ions
4. Place the nitrateelectrode in thesample with theprobe andrecord
thecorrespondingreading

Environmentalsignificance
1. Nitratereactions [NO3-]in freshwatercan causeoxygen depletion. Thus,aquatic
organismsdependingonthesupplyofoxygeninthestreamwilldie.Themajorroutesofentr
yofnitrogenintobodiesofwateraremunicipalandindustrialwastewater,septictanks,feedl
otdischarges,animalwastes(includingbirdsandfish)anddischargesfromcarexhausts.Ba
cteriainwaterquicklyconvertnitrites[NO2-]to nitrates [NO3-].
 2. Eutrophicationisoneofthemostproblematicwaterpollution,causedbythehighlevelofnutrie
ntsinwater,mainlyphosphateandnitrate,whichisduetothefertilizersrunofffromtheagricult
uralareas,aswellastheuntreateddisposalofdomesticandindustrial wastewater into the
environments.

Further studies:
Reverseosmosis is oneof theefficient methods to removenitrate
Thehighconcentrationofnitrate in water is indicative of pollution.

Result

Theamount of Nitrate present in the given sampleis------------.

Calculation:

Absorbance of sampleXConc. of Std X1000Phosphates

= --------------------------------------------------

(asmg/L) Absorbance of Std.XSample taken

Exp No: DETERMINATION OFPHOSPHATE IN THEGIVEN
WASTEWATERSAMPLE
Date
Ai
m To determine theamount of phosphatepresent in the givenwastewatersample.

Principle
InacidicconditionsorthophosphatereactswithammoniummolybdateformingM
olybdophosphoricacid,reducedfurthertomolybdenumbluebystannouschloride.Theint
ensityofthebluecolourisdirectlyproportionaltotheconcentrationofphosphate.Theabsor
bance is noted at 690nm usingspectrophotometer.

Apparatusrequired:
1. Spectrophotometer
2. LabGlassware
3. Hot Plate
4. Nessler'sTube.

Reagents:

Ammonium molybdatereagent:
25gammoniummolybdateisdissolvedin175mldistilledwater.280mlconcentrat
edsulphuricacidisaddedto400mldistilledwaterandcooled.Molybdatesolutionisaddeda
ndthe mixturediluted to 1000ml.
Stannous chloride reagent:
2.5gfreshstannouschlorideisdissolvedin100mlglycerol,heatedonwaterbathan
dstirred with the glass rodto fasten dissolution.
Standardphosphate solution:
219.5mgofdriedARpotassiumhydrogenphosphateisdissolvedindistilledwater
andmadeupto1000ml,where1ml=50.0g.ofphosphate.10mlofthestocksolutionismad
eupto1000mltogive1ml=0.05mg.Standardsofstrengthrangingfrom0(blank)to0.05mg/
Latintervals of0.01mgis preparedbydilutingthe stockwith distilledwater.

Procedure:
1. To50mlofthefilteredsample,4mlofammoniummolybdatereagentandabout4-
5drops of stannous chloride reagent is added.
2. Afterabout10 min but before12 min, the colourdeveloped
ismeasuredphotometricallyat 690nm andcalibration curveisprepared.
3. A reagentblank is always run with sametreatment with distilledwateras sample.
4. Thevalueofphosphateisobtainedbycomparingabsorbanceofsamplewiththesta
ndardcurve andexpressedasmg/L.
Environmental Significanceand application

1. Presenceofphosphatesinwaterandwastewateranalysishasagreatsignificance.Phosphatein
smallconcentrationare
usedinwatersuppliestoreducescaleformation,toincreasecarryingcapacityofmains,toavoi
dcorrosioninwatermains,toremoveironandmanganeseinmicroquantitiesandincoagulatio
nespeciallyinacidconditions.
2. Thepresenceofphosphatein largequantities in freshwatersindicates
pollutionthroughsewageandindustrialwastes.Itpromotesgrowthofnuisancecausingmicro
-
organisms.Thoughphosphatepossesesproblemsinsurfacewaters,itspresenceisnecessaryf
orbiologicaldegradationofwastewaters.Phosphorusisanessentialnutrientforthegrowthofo
rganismsandhelpsfortheprimaryproductivityofabodyof water.

Further studies:
Electro-coagulation is oneof themethods to remove phosphate from wastewater

Result

Theamount of Phosphate present in thegiven sampleis------------.

TABLE

BuretteReadi Volumeof
VolumeofSamp SodiumThiosulph DissolvedOxygen
S.N Tempera ng(mL)
le(mL) ate(mL) (mg/L)
o. ture
(ºC) Initial Final

1
.
2
.
3
.

BuretteSolution:SodiumThiosulphatePipete
Solution:Sample
Volume of Sodium Thiosulphate V1= ml
Normality of Sodium Thiosulphate N1= N
Volume of sample V2 = ml
Indicator:Starch

Initial D.O.

Final D.O.

BOD Calculation

BOD5(mg/L)=[(InitialDO–FinalDO)xdilutionfactor]
Where
Dilution factor =
Exp No: DETERMINATIONOFBIO-
Aim
Date CHEMICALOXYGENDEMAND(B.O.D
TEST)
To determine theBOD inthe givenwastewatersample.

ApparatusRequiredBO
D incubatorBOD
bottle (300ml)

Principle
Ifsufficientoxygenisavailableinwastewater,theusefulaerobicbacteriawillflourishandcause
theaerobic biologicaldecompositionof
wastewaterwhichwillcontinueuntiloxidationiscompleted.Thedissolvedoxygeninthesampl
eisthen"fixed"
byaddingaseriesofreagentsthatformanacidcompoundthatisthentitratedwithaneutralizingc
ompoundthatresultsinacolorchange.
Thepointofcolorchangeiscalledthe"endpoint,"whichcoincideswiththedissolvedoxygenco
ncentrationinthesample.Theamount of oxygenconsumed in this process is the BOD.

ChemicalsRequired:
1. Sodium Hydroxide
2. ManganousSulphate
3. Potassium iodide
4. Sodium Thiosuiphate
5. Conc.H2SO4
6. Starch

ReagentPreparation:
1. ManganousSulphate:

12 gof ManganousSulphateis dissolved in 25mlofdistilledwater. 2.

Alkaline—Iodide Solution

9 gof Sodium Hydroxide and 2.5 gofPotassium iodide aredissolved in

25mlofdistilled water.
3. SodiumthiosulphateSolution (0.025 N)

6.2gof Sodium thiosulphateis dissolved in 1 litreof water.

4. Starch Solution
Take 1gm of starch.Preparepastewith distilledwater. Make100 ml with waterandboil
bystirringandcoolit.
 Procedure-I
1. Distilledwaterisaeratedfor4hourstoattainsaturatedDissolvedOxygen(DO)level.Indistilledwater1
mlofeachnutrients(Phosphate
buffer,MagnesiumSulphate,CalciumChlorideandFerricChloride)and1mlofpreacclimatizedseedp
er1litreofdistilled wateris added.

2. TwoBODbottlesaretaken.Thewastewatersample1mlistakenintheBODbottlesandtheaeratedwateri
sfilled.DOtestisconductedfortheoneBODbottlesamplebythe followingsteps and initial DOis
noted

3. 1mlofManganeseSulphatesolutionisadded,followedby1mlofAlkali–Iodide–
Azidereagent. Then thebottle is mixed twiceandallowed to precipitate settle.

4. 1mlofSulphuricAcidisaddedandmixedtwice.200mlofsampleistakenandtitratedagainst Sodium
thioSulphatesolution withstarchindicator.

5. Disappearanceofbluecolouristakenasendpoint.VolumeofSodiumthioSulphateconsumed is noted.

6. Anotherbottleisplacedinincubatorat20⁰C.After5daysDOtestisconductedandfinal DO is noted.

Environmentalsignificance and application:

1. Thehealth orcleanlinessofalakeorstreamgetsaffected
2. TheamountofdecompositionoccurringinthelakeorstreamgetsincreasedwhenBOD is increased
leads toodour problem.
3. TheratioofBODtoCODisusefultoAccesstheamenabilityofwasteforbiologicaltreatment.
4. TheratioofBODtoCODisgreaterthanorequalto0.8indicatesthatthewastewaterarehighlyamenable
to biologicaltreatment.

Further studies:

Hydrogenperoxide(H2O2) is oneof theeffectivemethods to reduce theBODor COD level inwastewater.

Result
o
BOD5ofgivensampleat 20 C=
inmg/l
Exp No: DETERMINATION OF POTASSIUMIN THE GIVEN
Date WASTEWATERSAMPLE
Ai
m To determine theamount of potassiumpresent in the givenwastewatersample.

Principle:
Traceamountofpotassiumcanbedeterminedbydirectreadingofflamephotometer
ataspecificwavelengthof766.5nmbysprayingthesampleintotheflame.Thedesiredspectr
allinesarethenisolatedbytheuseofinterferencefiltersorsuitableslitarrangements.Theint
ensityof light is measuredbythe phototube.
WorkingprincipleofFlamephotometer:Theemissionofcharacteristicradiationsb
yalkaliandalkalineearthmetalsandthecorrelationoftheemissionintensitywiththeconcen
trationoftheelementformthebasisofflamephotometry.Theprincipleoftheflamephotome
terdependsonthe"EmissionSpectroscopy"inwhichtheelectronsofthemetalsafterabsorbi
ngenergygetexcitedfromgroundstatetohigherenergylevelandreturnbacktothegroundst
atewithemissionoflight.Thesampleundertestisintroducedintoflameinsolutionbymeans
ofatomizer.Theradiationfromtheflameentersadispersingdeviceandisolatesit(radiation)
fromtheflametothedesiredregionofthespectrum.Thephototubemeasurestheintensityofi
solatedradiation,whichisproportionaltotheconcentrationoftheelementpresent in the
sample.

Apparatusrequired:
1. Flame Photometer,
2. LabGlassware
3. WhattmanFilterPaper.

Reagentsrequired

1. Deionised distilledwater.
2. Stockpotassiumsolution: 1.907g ofdriedPotassium chloride,is dissolved
in1000ml of distilledwater, to give 1ml = 1mgof potassium
3. WorkingPotassiumsolution:Workingstandardsofsuitablestrengthsareprepare
dfrom thestock solution.

Procedure:

1. Thefilteroftheflamephotometerissetat766.5nm(markedforPotassium,K)thefla
me is adjusted forbluecolour.
2. Thescale is set to zero and maximum usingthe highest standard value.
 3. Astandardcurveofdifferentconcentrationispreparedbyfeedingthestandardsolutions.
Thesampleis filteredthroughthefilterpaperandfedintotheflamephotometer.
4. Theconcentration is found from the standardcurveor as direct reading

Environmental Significanceand application:

1. Potassiumpermanganateisusedinwatertreatment,concentrationsofaddedpotassiumcanbe
uptoamaximumof10mg/l,butnormallyconcentrationswouldbeless than this.
2. Toxicityresultingfromhighdosesofsaltsubstituteshavedescribedchesttightness,nauseaan
dvomiting,diarrhoea,hyperkalaemia, shortness of breath and heartfailure.

Further studies:
Reverseosmosis is oneof thebestmethods to remove higher concentration
ofpotassium in Drinkingwater

Result

Theamount of Potassiumpresent in thegiven sampleis-----------------

Exp No: DETERMINATIONOFSODIUMINTHEGIVENWASTEWATERSA
Date MPLE
Ai
m Todetermine theamount of sodium present in thegiven wastewatersample.

Apparatusrequired:
1. Flame Photometer,
2. LabGlassware
3. WhattmanFilterPaper.

Reagentsrequired:

1. Deionised water
o
2. Stocksodium solution:2.542g of Sodium chloride of dried(at140 C)
wasdissolvedin 1000ml distilledwatertogive 1ml =1mgof sodium.
3. WorkingPotassiumsolution:Workingstandards of suitablestrengths
werepreparedfrom thestock solution.

Procedure:
1. Thefilterof the flame photometeris set to 589nm (marked for Sodium, Na).
2. Byfeedingdistilledwaterthescaleissettozeroandmaximumusingthestandardofhi
ghest value.
3. Astandardcurvebetweenconcentrationandemissionispreparedbyfeedingthesta
ndard solutions.
4. Thesampleisfilteredthroughfilterpaperandfedintotheflamephotometerandthec
oncentration is foundfrom graphor bydirectreadings.

Environmentalsignificance and application:

1. Sodium salts are usedinwatertreatment,
includingsoftening,disinfection,corrosioncontrol, pH adjustment, and
coagulation.
2. Acuteeffectsofsodiummayincludenausea,vomiting,convulsions,muscu
lartwitchingandrigidity, and cerebral and pulmonaryoedema.
3. sodium mayaffect thetaste ofdrinking-water at levels above about 200 mg/litre.

Further studies:
Reverseosmosisis one of thebestmethods to remove higherconcentration
ofsodiumin drinkingwater

Result

Theamount of Sodium present in thegiven sampleis-----------------

ExpNo: DETERMINATIONOFCALCIUMINTHEGIVENWASTEWATERSA
Date MPLE
Aim:
To determine thecalcium in the given watersample.

Principle:
When EDTA (Ethylene-diamine tetra acetic acid) is added to the water
containing calcium and magnesium, it combines first with calcium. Calcium can
be determined directly with EDTA When murexide indicator is added to the
solution containing calcium, all the calcium gets complexed by the EDTA at
pH12-13. The end point is indicated from a colour change from pink to purple.
Apparatusrequired:
1. Flame Photometer.
2. LabGlassware.
3. WhattmanFilterPaper.
Reagents:
Standardcalciumsolution:
Weighaccurately6,24g0fanalyticalgradecalciumcarbonateanddissolveinminimumqu
antityof1:1HClandmakeexactlyupto250mlusingdoubledistilledwater.Thesolutionso
obtained will have 1000ppm of ca. dilute this solution to 1:9 to make stdsolution of
100 ppm

Procedure:
1. Thefilterof the flame photometeris set toca range
2. Byfeedingdistilledwaterthescaleissettozeroandmaximumusingthestandardof
highest value.
3. A standardcurve betweenconcentrationandemissionis preparedby feeding
thestandardsolutions.
4. Thesampleisfilteredthroughfilterpaperandfedintotheflamephotometerandthe
concentration is foundfrom graphor bydirectreadings.

Environmental Significance
HardwatertypicallycontainshighconcentrationsofCaandMgcations,whichi
nterferewiththeuseofthewaterformanyapplications.Theseionsdiminishtheeffective
nessofsoapsanddetergentsforcleaningoperations.Theyreducethequalityofdrinking
ofwaterandtheycontributetotheaccumulationofinsolublesaltdepositsinstoragevess
els or plumbing

Further studies
Using of ion exchangeresins, lime sodatreatment,reverse osmosis aresomeof
thewatersofteningmethods adopted to remove higher concentration ofcalcium in
water

Result
Theamount of Calciumpresent in thegiven sample is-----------------
ExpNo: DETERMINATION OFHEAVY METALS
Date -CHROMIUM,LEADANDZINC (DEMONSTRATION
ONLY)
AI
M
To determine theheavymetals ina givenwatersample.
PRINCIPLE
Asignificantpartoftheanthropogenicemissionsofheavymetalsendsup
inwastewater.Majorindustrialsourcesincludesurfacetreatmentprocesseswithele
mentssuchasCd,Pb,Mn,Cu,Zn,Cr,Hg,As,FeandNi,aswellasindustrialproductst
hat,attheendoftheirlife,aredischargedinwastes.Majorurbaninputstosewagewate
rincludehouseholdeffluents, drainagewater,businesseffluents(e.g.car washes,
dentaluses,otherenterprises,etc.),atmosphericdeposition,andtrafficrelatedemiss
ions(vehicleexhaust,brakelinings,tires,asphaltwear,gasoline/oilleakage,etc.)tra
nsportedwithstormwaterintotheseweragesystem.Formostapplicationsofheavy
metals,theapplicationsareestimatedtobethesameinnearlyallcountries,butthecon
sumptionpatternmaybedifferent.Forsomeapplicationswhichduringthelastdecad
ehasbeenphasedoutinsomecountries,theremay,however,todaybe
significantdifferences in uses
Mostcommonsourcesofheavymetalstowasteand/orwastewaterare(i)Miningandex-
traction;byminingandextractionapartoftheheavymetalswillendupintailingsand
otherwasteproducts.Asignificantpartoftheturnoverofthefourheavymetalswithm
iningwasteactually concernsthepresenceoftheheavy metalsinwastefromextracti
onofothermetalslikezinc,copperandnickel.Itshould,however,bekeptinmindthat
miningwasteis
generatedin-dependentofthesubsequentapplicationoftheheavy metal.
(ii)Primary smelting
andprocessing;aminorpartoftheheavymetalswillendupinwastefromthefurther
processingofthemetals.(iii)Usephase;asmallpartoftheheavymetalsmay
belostfromtheproductsduringusebycorrosionandwear.Effluentsfromtextile,leat
her,tannery,electroplating,galvanizing,pigmentanddyes,metallurgicalandpainti
ndustriesandothermetalprocessingandrefiningoperationsatsmallandlarge-
scalesectorcontainconsiderableamountsof toxic metalions. The toxic
metalsand
theirionsarenotonlypotentialhumanhealthhazardsbutalsotoanotherlifeforms.Toxicmet-
alions causephysicaldiscomfortandsometimes life-threateningillness including
irreversibledamagetovitalbody system .Fromtheecotoxicologicalpointofview,th
emostdangerousmetalsaremercury,lead,cadmiumandchromium(VI).Inmanyins
tances,theeffectofheavymetalsonhumanisnotwellunderstood.Metalionsintheen
vironmentbioaccumulateandarebiomagnifiedalongthefoodchain.Therefore,thei
rtoxiceffectismorepronouncedinanimalsathighertrophiclevels.Minetailingande
ffluentsfromnon-
ferrousmetalsindustryarethemajorsourcesofheavymetalsintheenvironment.Ava
rietyofinorganictechniquescanbeusedtomeasuretraceelementsinwastewaterincl
udingflameatomicabsorptionspectrometry (FAAS)andgraphitefurnace (or
electrothermal)atomicabsorptionspectrometry (GFAASor ETAAS),
inductively coupled plasma opticalemissionspectrometry(ICP-
OES)andinductively coupledplasma mass spectrometry(ICP-MS).
Dependingupon the number of elementsto be determined,
expectedconcentration range of analytes and the
number of samples to

berun,themostsuitabletechniqueforbusinessrequirementscanbechosen.Severali
ndustrialwastewaterstreamsmaycontainheavymetalssuchasSb,Cr,Cu,Pb,Zn,Co
,Ni,etc.Thetoxicmetals,existinginhighoreveninlowconcentrations,mustbeeffect
ively
treated/removedfromthewastewaters.Amongthevarioustreatmentmethodsappliedtoremovehe
avyortracemetals,chemicalprecipitationprocesshasbeenthemostcommontechnology.

3. DeterminationTechniquesofHeavy Metals in WasteWater Samples

Inordertodeterminetheheavytracemetals,therearemanyinorganictechniquessuchasFAAS,
ETAAS,ICP-OES,ICP-MSaswellasanodicstripping
andrecentlylaserinducedbreakdownspectroscopy(LIBS).Eachtechniquehasitsownadvantage
sanddisadvantageswhichwill be discussed in this chapter.
Actuallyallthestepsofananalysis,namely(i)representativesampling,
(ii)topreventanalytelosse.g.itssorptiononvesselwall,
(iii)contaminationfromtheenvironment,wares,chemicalsaddedtothesample,
(iv)transferthesampletothelab,(v)treatmentofsampleprior to
analysis(leaching,extraction,preconcentration/separationoftheanalytes,
(vi)chooseofthemethodconsideringitslimitations,(vii)calibrationofthevessels,instrumentetc,
(viii)preparationofsample,allsolutions,standardscorrectlyandappropriately,
(ix)totesttheaccuracyofthemethodusingCertifiedReferenceMaterials(CRM),
(x)evaluationofresultsstatisticallyandreportingarealltheringsofachain.Eachstepisimportantand
potentialsourceoferrorifnotappliedconveniently.Theweakestringofthechainlimitsthe
accuracyandquality of the results.Ifitis broken,the analysiscollapses.Therefore,allthe stepsof
ananalysisshould be performedwithcaution.
Aproblemorerroreveninoneofthosestepscausestheresulttobewrong.Asinallanalyses,samplep
reparationstepisthemostimportantonewhichshouldbecompletedquickly,easyandsafely.Waste
watersamplesmaycontainparticulatesororganicmaterialswhichmayrequirepretreatmentbefor
espectrometricanalysis.Inordertoanalyzetotalmetalcontentofasample,concentrationofmetalsi
norganicallyandorganicallybound, dissolvedorparticulatedmaterialsshouldbefound.

PROCEDURE
AtomicAbsorptionSpectrometry(AAS)isananalyticalmethodforquantificationofover70d
ifferentelementsinsolutionordirectlyinsolidsamples.Proceduredependsonatomization
ofelements
bydifferentatomizationtechniqueslikeflame(FAAS),electrothermal(ETAAS),hydrideorcoldv
apour.Eachatomizationtechniquehasitsadvantagesandlimitations or drawbacks.
TwotypesofflameareusedinFAAS:(i)air/acetyleneflame,(ii)nitrousoxide/acetyleneflam
e.Flametypedependsonthermalstabilityoftheanalyteanditspossiblecompoundsformedwithflam
econcomitants.Temperatureformedinairacetyleneflameisaround2300°Cwhereasacetylene-
nitrousoxide(dinitrogen oxide)flameisaround3000°C.
Generallywithair/acetyleneflameantimony,bismuth,cadmium,calcium,cesium,chromium,co
balt,copper,gold,itidium,iron,lead,lithium,magnesium,manganese,nickel,palladium,pl-
atinium,potassium,rhodium,ruthenium,silver,sodium,strontium,thallium,tinandzinccanbedet
ermined.

On the otherhand
forrefractoryelementssuchasaluminium,barium,molybdenum,osmium,rhenium,silicon,thor
ium,titaniumandvanadium,nitrousoxide/acetyleneflame
shouldbeused.Butsomeelementslikevanadium,zirconium,molibdeniumandboron
haslowersensitivityinthe determinationbyFAASbecause thetemperature isinsufficient to
breakdowncompoundsoftheseelements.
AAS-INSRUMENTATION

RESULT:
TheConcentrationof HeavymetalslikeChromium,LeadandZincwerestudiedbythemeans of
demonstration