Env Manual Part 2

Jawahar Education Society's,
INSTITUTE OF TECHNOLOGY, MANAGEMENT &

RESEARCH, NASHIK
DEPARTMENT OF CIVIL ENGINEERING
ENVIRONMENTAL ENGINEERING - II (401 001)
Class: B.E (Civil) Academic Year: 2017-18
INDEX
Sr. Page
Name of Experiment Date Remark Sign
No No.
01. Determination of Solids
02. Determination of Sludge Volume Index
03. Determination of Dissolved Oxygen
Determination of Biochemical Oxygen

04.
Demand
Determination of Chemical Oxygen
05.
Demand
06. Determination of Conductivity
07. Determination of Nitrites
08. Determination of Phosphates
09. Visit Report
Computer Aided Design of Sewage

10.
Treatment Plant
(Prof. M. J. Kakani) (Prof. H. A. Shahane) (Dr. M. V. Bhatkar)

Subject Incharge H. O. D (CE) Principal
JESITMR, NASHIK
Experiment No: 01
SOLIDS
Date of Performance: Date of Submission:
Introduction:
Solids in waste water indicate the concentrations of organic and inorganic
constituents. The organic fraction defines the pollutional load of waste water and the
inorganic component determines its suitability for irrigation or fish culture.
Various forms of Solids are:
Total Solids (a)
Total
Total Dissolved
Suspended Solids (e)
Solids (b)
Non-Settleable Settleable Volatile Solids Fixed Solids

Suspended Suspended (Organic) (Inorganic)
Solids (d) Solids (c) Dissolved (h) Dissolved (h)
Volatile Solids Fixed Solids

Volatile Solids Fixed Solids
(Organic) (Inorganic)
(Organic) (Inorganic)
Non-Settleable Non-Settleable
Settleable (g) Settleable (j)
(f) (i)
Briefly solids can be classified as:
Total Solids (a)
Total Suspended Solids (b) Total Dissolved Solids (e)
Volatile Suspended Solids (f+g) Volatile Dissolved Solids (h)
Fixed Suspended Solids (i+j) Fixed Dissolved Solids (k)
Environmental Engineering - II 1
JESITMR, NASHIK
When any organic and inorganic components are required.
Total Solids (a)
Total Volatile Solids Total Fixed Solids

(f+g+h) (i+j+k)
Importance of solids determination:

1. TS determination (a) classifies waste water as weak (around 350 mg/l), moderately
by (around 700 mg/l) and strong (around 1200
mg/l) _waters.
2. Settleable SS determination (c) indicates the efficiency of primary sedimentation.
Based on this, whether primary sedimentation is required or not and if required,
detention time to be adopted for PST designs are decided.
3. Volatile solids (settleable) (g) indicate the fraction of organic loading of digesters,
contributed by primary sludge from PST.
4. Non-settleable suspended solids (d) and non-settleable volatile solids (f) indicate the
pollutional load to be removed by secondary treatment.
5. Total dissolved solids (inorganic) (k) indicate the suitability of waste water for
irrigation and fish culture.
6. Total volatile solids (f+g+h) determination in sludge‟s is used for designing organic
loading of anaerobic digesters and also their efficiency of VS reduction.
Standards Recommended:
Maximum Permissible
Sr. No. Description
Limit
Sewage effluents discharged into B.I.S.4764
1. TSS , 30 mg/l
inland surface waters
Industrial effluents discharged into B.I.S.2490
2. TSS , 100 mg/l
inland surface waters
Industrial effluents falling into marine B.I.S.7968
3. TSS , 100 mg/l
coastal areas
Inland surface waters to be used on B.I.S.2296
4. TSS , 2100 mg/l (Inorganic)
land for irrigation
JESITMR, NASHIK
Determination of solids:
Principle:
Solids are determined by gravimetric analysis.
Filtering a known volume of the sample, evaporating the filtrate to dryness and
weighing the residue determine total solids volatilizing away all the organic matter in a
known volume of the sample and weighing the residue. Fixed solids are determined by
volatilizing away all the organic matter in a known volume of the sample and weighing
the residue.
Settle able solids are determined by allowing coarse suspended solids, with sp.gr
>1, to settle under still conditions over a specific over a specific period of time. The
settled sludge is evaporated to dryness and residue weighed to determine the efficiency of
sedimentation.
Discussion:
o
During total solid & total dissolved solids determine a temperature of 103 C to
o
105 C is adopted for evaporating solids to dryness, as at this temperature only water
contents is lost buy no degradation & loss in weight of solids occur. Heating solids to
o o
550 C to 600 C during volatile solids determination result in total degradation && loss of
all the organic content, the organic fraction remains as residue.
In the Imhoff cone experiment,
mg
Settled sediments ∗100
l
Efficiency of suspended solids removal =
𝑇.𝑆.𝑆 𝑚𝑔 /𝑙
If efficiency is less than 40% PST need not be provided.

If efficiency is less than 40% & 60%, it is desirable to provide PST.
If efficiency is more than 60%PST must be provided.
The plot of setting time against settled volume indicates the detention time to be adopted
for design of PST for a particular waste.
Graph-1 indicates sedimentation increase with time continuously but a maximum

detention time of two hour may be provided for PST, beyond which purification of settled
organic solids cause problems before disposal.
JESITMR, NASHIK
Graph-2 suggest, that a detention time of 1.5 hours may be adopted for primary
sedimentation; beyond Which PST size will be undesirable and uneconomical as there
will be no further sedimentation.
8
7
6
5
Settled Sludge ml/l→
4
Graph1
3 Graph2
2 Graph3
1
0
0.5 1 1.5 2
Time, h→
Graph-3 suggests that detention of 1hour will be ad dictated for primary segmentation.
Apparatus and Equipment:
Crucible, 100 ml measuring cylinder, filter paper (Whatman No 40) and funnels stand
imhoff cone. Hot air oven, muffel furnace and analytical balance.
Procedure of Test:-
a) Total solids:-
1) Weight a clean & empty crucible (A) W1 mg,
2) Take a measured volume of a waste water sample in (A)-25ml if the waste
water sample appears strong , 50ml if it appears moderately strong & 100 ml if it
o
appears weak & evaporates.To dryness in a hot air oven at 103 C -1050 C.
3) Cool the crucible to room temperature & weight W2 mg.
W2 − 𝑊1 𝑚𝑔 ∗ 1000(𝑚𝑙/𝑙)
TS (mg/l) =
volume of sample taken(ml)
b) Total dissolved solids:-
1) Weight a clean & empty crucible (B) W 3 mg
2) Take known volume of the sample, filter it through whatmen filter paper no.
40 & collect the filtrate in (B).
3) Evaporate the filtrate in (B) to dryness in a hot air oven at 103 0C
Cool the crucible to room temperature & weight W4
JESITMR, NASHIK
W4 − 𝑊3 𝑚𝑔 ∗ 1000(𝑚𝑙/𝑙) original
TDS (mg/l) =
c) Total suspended solids, mg/l = (TS -TDS)mg/l
d) Total volatile solids & total fixed solids:-

1) Keep crucible (A) containing total solids residue in a muffle furnace
maintained between 550o C& 600 0C for half an hour. Inspect the dry ash in
(A) if black specks are seen , continue heating until the ash is totally gray or
whitish-gray.
2) Cool the crucible to room temperature & weight W5 mg
TVS (mg/l) =
TFS (mg/l) =
e) Total Dissolved Solids (inorganic)
1) Keep crucible (B) containing dissolved solids residue in a muffle furnace maintained
between 550o C& 600 0C and volatize all the organic content.
2)Cool the crucible to room temperature & weight W6 mg
TDS (mg/l) =
f) Settleable and non settle able solids:-

1) Take one litre of well mixed raw waste water in an imhoff cone & note the time
2) Record ml of settled solids at interval of 30 mins (15 min if settlement is fast)
3) At the end of two hours ,syphon out the supernatant (of waste) without disturbing
settled sludge.
4) Weigh a clean & empty crucible (c)…………………..W7 mg.
5) Flush out the settled sludge in the imhoff cone completely ,using distilled water&
collect it in crucible (c)
JESITMR, NASHIK
6) Keep the crucible (c) with the sludge contests in a hot air oven maintained between
103c-105c evaporates to dryness.
7) Cool the crucible to room temp.& weigh ……………….W8 mg.
Settled solids =(W8-W7) mg/l.
settled solids(mg./l)
Efficiency of sedimentation = ∗ 100
TSS(mg/l)
Observation Table:
Settleable
Sample Description of TS TDS TSS TVS TFS TDS
Solids Remark
no sample mg/l mg/l mg/l mg/l Mg/l inorganic
Mg/l
Result & Conclusion:
JESITMR, NASHIK
Lab Quiz:
1. What is the significance of solids determination of wastewater ?
2. Give the classification of solids?
3. What is permissible limit of total solids and dissolved solids (inorganic)?
4. How the solids values are used in deciding treatment units?
5. What are the volatile solids and fixed solids and what is significance of these in wastewater?
6. At what temperature volatile solids are determined?
JESITMR, NASHIK
JESITMR, NASHIK
Experiment No.: 02
SLUDGE VOLUME INDEX (SVI)
Date of performance: Date of submission:
Introduction:
Sludge volume is an important parameter used for monitoring efficient operation
of aeration systems. SVI is the volume in ml, occupied by 1 gm of mixed liquor sample
for SVI test is drawn from outlet of an aeration tank of an activated sludge process-
conventional or modified.
Importance of SVI Determination:

1) SVI is used for determining the quantity of sludge produced in an aeration unit and
hence its efficiency.
2) It is used for determining the recirculation ratio necessary for maintain a specified
MLSS concentration in the aerator.
3) It is also used for estimating suspended solids concentration in recirculated sludge.
Discussion:
An Imhoff cone is used for determination of SVI. This represents, effectively the
principle and working of a secondary settling tank in an aerobic biological system. (In the
absence of an Imhoff cone, a 1000 ml graduated cylinder may be used particularly for
field test). The volume of sludge (ml), settled in 30 min/gm of MLSS varies from 25 to
200 depending on the quantity of sludge produced. As the purpose of biological aeration
is to convert non-settle able organic suspended solids into settable cell mass, low SVI
values indicate high quality of sludge produced and high efficiency BOD removal. sludge
produced in an aeration system is considered excellent; if it settles easily, occupies
minimum volume it is granular and highly mineralized it dewaters dries easily without
odour nuisance. Sludge to be wasted from extended aeration systems, with SVI in the rain
drop 25-50 ml/gm, can be discharge to sludge drying beds directly, without the need of
stabilisation anaerobic digestors.Slude from aerator of a conventional or standard rate
ASP, with SVI around 100ml/gm, is good in quantity but inferior to sludge produced by
an extended aeration process. It has pollutional load and requires stabilisation in a
JESITMR, NASHIK
digester before drying. Sludge from the aerator of a high rate process with SVI in the
range of 150-200ml/gm is poor in quality, odours high in volume strictly and highly
pollutional. It is unfit for disposal without proper digestion.
Associated operational parameter for Biological Aeration process

Average BOD
SVI MLSS F/M Aeration Quantity
Process Sludge removal
ml/g mg/l 1/d Time,Hr Of sludge
,d Effi. %
150- 500- 0.5 -
High Rate 3-4 5 60-75 Poor
200 1000 1.0
Good, as
50- indicated by
2000- 0.2 -
(100)- Conventional 6-10 10 80-90 the medium
3000 0.5
150 value 100
ml/g
Extended 4000- 0.05 -
25-50 24-36 25 90-98 Excellent
aeration 6000 0.2
Sludge Bulking:
If SVI is more than 200ml/gm sludge produced in a biological aeration system is
said to be bulked. Bulked sludge indicates failure of the process.Slude bulking is a major
operational problem; which increases effluent BOD and decreases process efficiency.
Causes of sludge bulking:

a) Poor characteristics of influent waste water
1) Frequent variation in quantity and quality of influent.
2) Low pH (Filamentous organisms such as Beggiatoa & Sphaerotilus grow below pH
5.These multicellular organisms get water-entrained and remain suspended without

settling down in S.S.T)
3) Low temperature resulting in decreasing bacterial activity.
4) Staleness or septicity of influent.
5) Low nutrient (The common BOD: N: P weight ratio required for biological treatment is
100 : 5 : 1).
JESITMR, NASHIK
6) High carbohydrates contribute to sludge bulking.
b) Poor plant design and operation.

1) Sufficient aeration.
2) Insufficient mixing of recirculated sludge with influent waste water.
3) Organic over loading (high F/M).
4) In sufficient hydraulic retention tank or aeration tank.
5) In sufficient sludge retention time.
6) Improper recirculation of sludge resulting in fluctuating MLSS in the aerator.
7) Retention of sludge in SST for too long promoting an aerobic condition contributed to
sludge bulking.
c) Emergency control measures

1) Controlled chlorination of bulk sludge to kill multicellular organism only.
2) Reaeration of return sludge on recycle line
d) Long term control measures:-

1) Modification and improvement of influent characteristics.
2) Modification and improvement of plant design and operational parameters.
Recirculation ratio and Concentration of return sludge:-

Sludge Volume Index is related to volume and concentration of return sludge.
.
JESITMR, NASHIK
Qr/ (Q+Qr) =V/1000, RCR=Qr / Q=V / (1000-V)

Where, V = volume of settled sludge per litre, ml
Q = average waste water flow m3/day
Qr = recirculated sludge.m3/day.
(Suspended solid concentration = [1000(ml/lit) ×1000(mg/gm)] / SVI ml/gm

In recirculated sludge.mg/l. )
= (106/SVI) mg/l
Determination of SVI:
Principle:
SVI determination is based on estimating the volume of sludge settled in 30
minutes per gram of MLSS.
Apparatus
Imhoff Cone, (or 1000 ml measuring jar),50ml measuring cylinder,
Crusibles,250ml beakers, Whatman filter paper no 40, Hot ait oven.
Procedure:
A)
1) Take exactly 1 lit of mix liquor sample from an aerobic tank and allow it to settle in an
Imhoff cone.
2) Record volume of settled sludge (Vml/lit) at the end of 30 min.
B)
1) Weigh a clean and empty crucible (P) W1 (mg).
2) Stir up the Imhoff cone contents well, collect 50ml of mix liquor in (P) (25ml, if a high
value of MLSS is expected)and evaporate to dryness in a hot ait oven.
3) Cool the crucible (P) to room temperature and weigh with solids residue W2
(mg)
4) Weigh a clean and empty crucible (Q) W3(mg). Stir up the Imhoff cone
contents again collect 50ml (or 25ml)of mixed liquor and filter through the corrugated
Whatman no.40 filter paper and collect the filtrate in crucible(Q) and evaporate to
dryness.
5) Cool the crucible (Q) with dissolved solids residue and weigh W4 (mg).
JESITMR, NASHIK
Calculations:
Mixed Liquor Total Solids (MLTS), mg/l = [(W2-W1) (mg) ×1000(ml/l)] (ml)
Sample taken
Mixed Liquor Dissolved Solids (MLDS), mg/l = [(W4-W3) (mg) ×1000ml/l]

Original sample taken (ml)
Mixed Liquor Suspended Solids (MLSS) = MLTS – MLDS
SVI, ml/g = [V (ml/l) ×1000(mg/g)] / MLSS (mg/g)
Observation Table:
Volume of
Description MLSS
Sample No settled SVI ml/g Remarks
of Sample mg/l
Sludge,ml/l
(Note:- SVI value has practical significance if the corresponding MLSS value is not
satisfactory).
Result and Conclusion:
JESITMR, NASHIK
Lab Quiz
1) Define SVI ?
2) What is the location for sample collection for SVI test ?
3) What is purpose of SVI determination ?
4) How the recirculation ratio is decided from SVI values ?
5) Give the classification of sludge with reference to SVI values ?
6) What are MLSS and MLVSS ?
7) What is mean by poor quality sludge ?
JESITMR, NASHIK
JESITMR, NASHIK
JESITMR, NASHIK
Experiment No.: 03
DISSOLVED OXYGEN (DO)
Introduction:
Atmospheric oxygen is not readily soluble in water, Its solubility is directly
proportional to its partial pressure. (For example, at a specific temperature such as 20°C,
with Henrys law constant being 43.8 mg/ l x atmosphere and partial pressure of oxygen
being 0.2094 atmosphere at 1 atmosphere of air,
DO saturation value = 43.8 (mg / l x atm). X 0.2094 (atm) = 9.17 mg / l)
DO Saturation decreases with the rise in temperature, decreases with rise in salt
concentration, decreases with the rise in altitude and decreases with the rise in organic
concentration.
Variation of DO with temperature
(Clean water at zero altitude or 1 atmospheric pressure)
Temperature
0 5 10 15 20 25 30 35 40 45 50
ºC
DO Saturation
14.62 12.80 11.33 10.15 9.17 8.38 7.63 7.0 6.6 6.1 5.6
mg/l
Temp Chloride Concentration in Water at 1 atm.

°C 0 mg/l 1000 mg/l 5000 mg/l 10000 mg/l 20000 mg/l
DO Saturation Value, mg/l
0 14.62 14.46 13.80 12.97 11.32
10 11.33 11.21 10.74 10.73 8.98
20 9.17 9.08 8.73 8.30 7.86
30 7.63 7.56 7.26 6.86 6.49
JESITMR, NASHIK
Variation of DO with salt Concentration:

Higher altitudes with lowered atmospheric pressures have a profound effect on
the solubility of oxygen in water. The altitude h (m) of any place being known the
corresponding atmospheric pressure (p mm of mercury ) can be obtained from the
equation.
h= (0.0109803)p² - (26.88852 ) p + (14119.57)
DO saturation value, at a particular atmospheric pressure p mm of mercury, = DO
saturation at 760 mm of mercury x (P-Pₒ) / (760-Pₒ),
Where Pₒ is the vapour pressure at a specific temperature.
Variation of DO with Altitude (Clean water )

Alt- Alt- Alt-
Alt-0m Alt-500m
Temp ºC P0 mm 1000m 2000m 3000m
P=760mm P=716mm P=763mm P=596mm P=527mm
DO Saturation Value mg/l
0 5 14.62 13.77 12.94 11.44 10.11
5 7 12.80 12.05 11.32 10.01 8.72
10 9 11.33 10.67 10.02 8.86 7.82
15 13 10.15 9.55 8.97 7.92 6.98
20 18 9.17 8.63 8.10 7.14 6.29
25 24 8.38 7.88 7.48 6.46 5.73
30 32 7.63 7.17 6.72 5.91 5.19
Note: DO determined, at a particular place (Known altitude ) and at a specific

temperature should not exceed its corresponding saturation value (unless condition super
saturation exist. )
Decrease of DO with increase in organic concentration indicates pollutional load
of receiving water bodies. This is a great significance to sanitary engineers.
Higher temperature, higher salt concentration, higher altitude and higher organic
content have a compounding effect in drastically decreasing the solubility of oxygen in
water. However these parameters rarely combine to produce the worst effect in nature.
JESITMR, NASHIK
Importance of DO Determination:
1) DO determination at various points along the river course are carried out to define the
pollutional status of the river. DO level of more than 3mg/ lit. Normal flowing river
water.
2) DO measurements are important for maintaining aerobic conditions in aerobic
biological treatment uints.
3) Determination of DO is the basis of the BOD test.
4) DO value are used to control the corrosion of iron and steel distribution system and
steam boilers.
DO Fixation:
Many times, particularly while determining DO of river water samples, it is not
convenient to carry out the entire determination of the field. As DO values changes with
time during transit (from the sampling site to the laboratory) because of variation in
temperature and biological reactions, it is necessary to fix the DO in the samples at the
site at the time and the temperature of collection. DO fixation is done by adding 2ml of
Manganous sulphate and 2ml of alkali iodide azide. For best results the samples may be
stored below 10° C during transit and titrated within 6 hours of fixation.
DO Determination:
Principle:
For estimation of DO content in a sample, iodine added to sample is oxidized
under acidic conditions to free iodine. The amount of free iodine liberated is equivalent to
the amount of DO originally present in the sample ( the liberated iodine is estimated by
titrating against standardized sodium thiosulphate using starch as indicator).
The amount of free iodine estimated is a measure of DO in the sample.
Apparatus:
Burette, pipettes, 5 ml and 250 ml measuring cylinders, 300 ml of BOD bottles, conical
flask and thermometers.
Chemicals:
Manganous Sulphate, Alkali Iodide Azide, Conc. Sulphuric acid, Starch.
JESITMR, NASHIK
Procedure of Test:
1) Take a 250 ml reagent bottle (or 300 ml BOD bottle) and fill it up completely with the
sample.Tap the bottle all round to release entrapped air bubble.Record the temperature.
Stopper the bottle.
2) Remove the stopper and add 2ml of MnSO4 using the pipette dipping the open end of
the pipette below the liquid surface.
3) Add 2 ml alkali iodide azide using a pipette, dipping the open end of the pipette below
the liquid level.
a) If DO is absent stable white precipitate of manganous hydroxide is formed.
MnSO4 + 2 KOH → Mn(OH)2 + K2SO4↓
White ppt.
The experiment may be stopped at this stage.
b) If DO is present, manganous ions are oxidized to manganic ions and brown
precipitate of manganic basic oxide is formed.
Mn(OH)2 + ½ O2 → MnO(OH)2↓
Brown ppt.
Stopper the bottle and mix by inverting the bottle several times.
4) Remove the stopper add 2ml of concentrated sulphuric acid (36N) (a measuring
cylinders may be used for adding the acid ) Stopper the bottle and mix by inverting
bottle several time until the brown precipitate completely dissolves to yield a uniformly
yellow coloured free iodine solution. Under acidic conditions; manganic basic oxidizes
iodide to free iodine.
MnO(OH)2 + 2H2SO4 + 2KI → MnSO4 + K2SO4 + 3H2O + I2
5) Take 203 ml of iodine solution in a conical flask. (The extra 3ml is the correction for 4
ml of reagent added for DO fixation ) Titrate against standardized sodium thiousulphate
using 1 to 2 ml of starch as an indicator.This is an oxidation reduction reaction. Free
iodine, an oxidizing agent, is reduced to iodide and sodium thiousulphate a reducing
agent is oxidized to sodium tetra thionate.
I2 + 2Na2S4O6 + 2NaI
6) Stop the titration at the end point, when the solution in the flask turns blue to colorless.
Record the amount of titrant used (x ml) upto first disappearance of blue colour.
(Note: After some time absorption of atmospheric oxygen liberates more free iodine.
Which reacts with starch to give a blue colour again. Further use of titrant to reduce this
blue colour will give an erroneously high DO value ).
JESITMR, NASHIK
Action of Starch as an Indicator:

Starch is an absorption type of indicator. During titration of iodine with sodium
thiosulphate, addition of starch results in the formation of a weak blue complex due to
absorption of iodine on colloidal starch particles. As iodine is extracted and reduced the
intensity of blue colour gradually decreases. When all the free iodine is reduced to iodide,
the blue colour totally disappears. This indicates the end point of titration.
7) Calculate DO in the sample in mg/l.
Observation table:
Serial No. of Description of Temperature DO
Remarks
Sample Sample of Sample Mg/l
Calculations:
DO, mg/l = [ml of titrant used x normality of titrant x equivalent weight of oxygen]
ml of sample taken
= X (ml) x N (mg/ml) x 8 x 1000 ml/l

200 (ml)
(Note: Generally 0.025 N titrant is used against 200 ml of the sample, so that DO values
in mg/l are numerically equal to ml titrant used, as 0.025x 8 x 1000/ 200 = 1).
Sample 1: DO, mg/l =

Tap water

Hot Water
JESITMR, NASHIK

River or lake water

Wastewater
Standardization of Na2S2O3:
Necessity:
For preparing a standard solution of sodium thiosulphate, equivalent weight is obtained
from formula Na2S2O3.5H2O. As water of hydration is lost under varying condition of
temperature and humidity, the normality of sodium thiosulphate will not be exactly as
calculated from its formula.
Further, dilute Na2S2O3 on standing undergoes aerobic oxidation and also degradation
by absorption of atmospheric CO2. Therefore for best results, it is necessary to
standardize a dilute titrant against a primary standard (such as K2Cr2O7) on the day of
titration.
Method of standardization using standard K2Cr2O7:

1) Place about 2g of KI in a conical flask.
2) Add 100ml of distilled water (to suppress sublimation of iodine)
3) Add 10 ml of diluted sulphuric acid (prepared by taking 9 ml distilled water 1) and 1
ml of conc. H2SO4 to it)
4) Add 10 ml of 0.025N K2Cr2O7
5) Add 100ml of distilled water (to prevent masking of starch end point by 1) greenish
trivalent chromium ions)
6KI + 7H2SO4 + K2Cr2O7 → Cr2(SO4)3 + 3I2 + 4K2SO4 + 7H2O
6) This is a slow reaction. Wait for 5 minutes to allow al the dichromate added to react
completely to release an equivalent amount of free iodine.
7) Titrate against the given Na2S2O3, using starch as indicator (1 to 2 ml ). Record the
volume of titrant used (V ml ) upto the point when blue colour in the flask just
disappears.
JESITMR, NASHIK
Then Na2S2O3 K2Cr2O7
NxV = NI x VI
Normality of titrant = N = NI x VI = 0.025 x 10
V V
This value of N should be used for determination of DO
Importance of Azide in alkali-iodine-Azide (Winkler’s azide modification):

Azide used to suppress nitrite ion interference samples of biologically treated
sewage effluents, stagnant river water samples and incubated BOD samples generally
contain nitrites. During DO determination, when H2SO4 is added, nitrites convert iodine,
to free iodine (I°2)
2NaNO2+2NaI+2H2SO4 → N2O2+I2+2H2O+2Na2SO4
The reduced N2O2 is oxidized by atmospheric oxygen to nitrite again, with some
of the first- reaction products entering the second reaction to maintain equilibrium.
N2O2 + ½O2 + H2O + 2Na2SO4 → 2NaNO2 + H2SO4

Thus the interfering nitrite is recycled, which liberates some more free I°2 and
blue colour with starch. This is erroneously interpreted as due to the presence of high DO
in the sample (even when there is none sometimes)
Interference due to Fe²+, aldehydes, ketones (and even NO2ˉ ) can be removed by
oxidizing the reducing agents by excess of acidified KMnO4. Excess KMnO4 is reduced
by potassium oxalate before DO determination.
Significance of DO in tap water:

When residual chlorine is present in tap water, chloride concentration being
generally low, DO fluctuates with temperature and atmospheric pressure. However it has
no sanitary significance.
When residual chlorine is absent in tap water, a low DO in the sample particularly
below 4mg/l suggests that water quality is suspects and aeration and disinfections are
necessary.
JESITMR, NASHIK
Result and Conclusion:
JESITMR, NASHIK
Lab Quiz:
1). What is the effect of temperature, salt‟s concentration, biological activity, altitude on
DO present in water?
2). What is maximum DO present in unpolluted water?
03). What are the different methods of DO determination?
04). What is concentration of DO in fresh sewage and effluent?
05). Explain the action of starch in DO determination?
06). What is the minimum DO requirement for survival of an aquatic life?
07). What is the effect of DO on distribution system?
08). What is colour of precipitate in DO determination while DO is present / absent?
09). What is the significance of 0.025N sodium thi-sulphate?
10). Explain the reaction of reagents added in DO determination?
JESITMR, NASHIK
JESITMR, NASHIK
JESITMR, NASHIK
Experiment No.: 04
BIOCHEMICAL OXYGEN DEMAND (BOD)
Introduction:
BOD is defined as amount of dissolved oxygen utilized by heterotrophic aerobic
microorganisms, while oxidizing decomposable organic matter, present in wastewater.
DO and „BOD‟ are dynamically inter-related. They are two different parameters
graduated in opposite direction of same measuring device (used for evaluating pollution
strength of water bodies) with a very delicate measure of overlap in between. It is within
this overlap stretch, that the forces of purification process in natural water bodies are
operative. Whereas high „DO‟ in natural water body (promoting existence and growth of
fish and such other aquatic life) is an indication of purity of water, low „DO‟ is an
indication of pollution. However when 'DO' becomes zero, pollution strength becomes
indeterminate. Stale domestic sewage having a „BOD‟ of 230 mg/l, dairy wastewater with
a „BOD‟ of 2000 mg/l, distillery effluent with high a „BOD‟ as 30000 mg/l all have zero
„DO‟. Therefore when pollution load is high, determination of „BOD‟ rather than „DO‟,
assume significance. BOD exertion varies with time, temp and organic matter. Therefore
time (day) and temp (°C) are maintained constant, so that „BOD‟ specifically measures
the biodegradable conc. of organic matter in wastewater.
During „BOD‟ reaction, primary the carbonaceous component of organic matter is
degraded by soil bacteria and protozoa into CO2, H2O, NH3, and bacterial and protozoan
cells over a period of 1st 8 days. By this time nitrifying bacteria develops into large
enough number to start oxidizing NH3 into nitrites and nitrates. These cause interference
in the estimation of carbonaceous „BOD‟ beyond 7 or 8 days. Hence it is customary to
determination of 5 days „BOD‟, which is a fair measure of the pollution strength of
wastewater. During the „BOD‟ test, to eliminate variation in biological activity because of
variation in temperature, the temperature throughout the test is maintained constant at
20°C. Selection of 20°C is based on the consideration that it is the medium temperature
value of natural water bodies and also, at that temperature, multiplication of soil bacteria
that stabilize carbonaceous matter is satisfactory, whereas growth of nitrifying is inhibited
during the period of test. Thus determination of 5 days BOD at 20°C is conventionally the
JESITMR, NASHIK
standard practice. Unless mentioned otherwise, simply „BOD‟ means 5 days „BOD‟ at
20°C.
Expected ‘BOD’ exertion or satisfaction as % of ultimate (BOD) in relation to time
(days), at 20°C for domestic sewage
Incubation time, BOD exerted as % Incubation time, BOD exerted as %
days of BODL days of BODL
1 21 8 84
2 37 9 90
3 55 10 94
4 60 11 96
5 68 12 97
6 75 13 98
7 80 14 99
Importance of BOD tests:

1) BOD tests are used for determining the pollution strength of organic waste,
domestic or industrial.
2) They used for designing suitable treatment methods, organic loading of treatment
plants and also for evaluating efficiencies of unit operation and treatment systems.
3) They are used for determining suitability of treated efficiencies for disposal with
reference to recommended standards.
4) BOD tests are also used in carrying out stream sanitation studies and for enforcing
water pollution control measures.
Standard recommended:
Sr. Description Maximum Remarks
No. permissible
BOD at 20°C
1 Inland surface waters for use as water for public 3 mg/l I.S. 2296
water supply and for bathing
2 Domestic sewage effluents discharge in to inland 20 mg/l I.S. 4764
surface waters
3 Industrial effluents discharged in to inland surface 30 mg/l I.S. 2490
waters
JESITMR, NASHIK
4 Treated effluents to be discharged on land 200 mg/l I.S. 2490

5 Industrial effluence falling in to marine coastal 100 mg/l I.S. 7968
areas
Determination of BOD:
Principle of test and discussion:

Principle:
A known volume of a sample of waste water, diluted using specially prepared
distilled water, is incubated at 20°C for 5 days. DO depletion in test bottles is a measure
of fair amount of biodegradable organic matter present in the sample. To avoid getting
zero 5-days „DO‟, a dilution technique is adopted.
Discussion:
DO depletion is the difference between immediate „DO‟ of the diluted sample and
5-days „DO‟ of diluted and incubated sample. Immediate „DO‟ should be determined
within 15 minutes of dilution of sample, to minimum the effect of the time & temperature
gradient on biological activity. Immediate „DO‟ should be quite high near the saturation
value. A value of around 7 mg/l however is considered satisfactory. 5 days DO of diluted
and incubated sample should be at least 2 mg/l and also „DO‟ depletion should not be less
than 2 mg/l. So, empirically, the maximum & minimum limits of „DO‟ depletion are ‘(7-
2) = 5 mg/l’ and ‘(7-5) = 2 mg/l’
Dilution techniques:
This is based on the expected „BOD‟ value of the test sample considering the
equation „BOD5‟ (at 20°C) = (immediate ‘DO’ of diluted sample – 5 day ‘DO’ of diluted
and incubated sample) × dilution factor
This may be = (7 mg/l – 5 mg/l) DF ---------- (min)
or = (7 mg/l – 2 mg/l) DF ---------- (max)
This dilution factor should be chosen that the expected „BOD‟ of sample lies
within the ranges of minimum and maximum „BOD‟ values obtainable. Example: If
expected „BOD‟ is 20 mg/l, DF may be 5.So that (7-5) × 5 = 10 mg/l (min obtainable)
and (7-2) × 5 = 25 mg/l (max obtainable).When dilution is 1 to 5, one volume is diluted to
5 volumes i.e. 1 + 4 = 5
JESITMR, NASHIK
When expected „BOD‟ of sample is fairly known, at least two consecutive

dilutions are adopted for each sample, to provide an expanded range of measurable BOD.
Experience, history of sample and visual observation of colour and suspended solids
concentration enable the expected BOD5 to be estimated fairly sensible. If the expected
„BOD‟ is about 100 mg/l, adopt dilution of 1 to 20 & 1 to 40, so that the measurable
range of „BOD‟ extends from 40 mg/l to 200 mg/l with an overlap in between. Within this
range the actual „BOD‟ of sample is determinable.
If the strength of sample is not known but the „BOD‟ of sample is broadly except
to be within a range guided by the description of sample, then three consecutive dilutions
are adopted one below & one above the expected range to allow for error in judgment.
For example, if BOD of sample is expected to be between 200 & 500 mg/l, then three
consecutive dilutions 1 to 50, 1 to 100 & 1 to 200 are recommended giving a range of
measurement „BOD‟ from 100 mg/l to 1000 mg/l. The actual „BOD‟ of sample will be
determinable within this range (keeping several dilutions at the same time is important, as
the BOD5 test cannot be repeated after five days, unless the original sample is specially
preserved). The „BOD‟ test is considered a failure for any particular dilution, if the 5 day
„DO‟ is equal to or nearly equal to, immediate „DO‟ i.e. dilution has been too much or if
the 5 day „DO‟ is equal to zero or less than 0.5 mg/l, i.e. dilution has been too less. If two
dilution of sample give satisfactory result & the variation in test result is less than 5%,
then the average value represents the „BOD‟ value. If the variation in test results is more
than 5%, then only dilution, which gives greater „DO‟ depletion, is considered more
significant and is recorded for use. Direct „BOD‟ determination of sample is possible only
when the expected „BOD‟ is very low & no dilution is required i.e. DF = 1, ideally the
range of BOD5 at 20°C determinable without dilution is 2 to 7.17 mg/l.
Seeding:
Seeding is inoculating organic matter with live microorganisms that can initiate
biodegradation of organic matter under favourable conditions. Samples of domestic
sewage & industrial effluents mixed with sanitary sewage, in the pH range of 6 to 8.5,
themselves contain enough living microorganisms and do not requires seeding.
Samples of industrial organic wastes; such as sugar factory waste, paper and pulp
mill waste, textile waste, distillery waste etc require seeding particularly when their pH
correction and seeding at time of test. The seed may be bacteria from organically rich soul
JESITMR, NASHIK
or the supernatant of aerated domestic sewage or an extract from the aerator mixed liquor
of a successfully working ASP.
Apparatus and equipment:

Burette, pipette, 5 ml and 1000ml measuring cylinders, 300 ml „BOD‟ bottles, pH
meter, compressor (or magnetic stirrer or fish tank aerator), „BOD‟ incubator.
Chemicals:
A) All the chemicals used for DO determination
B)
a) Phosphate buffer [KH2PO4 (21.75 g) + Na2HPO4. 7H2O (33.4 g) + NH4Cl (1.7
g)] per litre
i) Maintain optimum pH (around 7.0) thought the test necessary for bacterial
growth and metabolism.
ii) Provides essential nutrients N and P, necessary for bacterial growth.
iii) K and Na provide osmotic pressure, necessary for bacterial ingestion of
food and nutrients. They are also trace nutrients.
b) Magnesium chloride [MgCl2 (27.5 g per litre)]
c) Calcium chloride [CaCl2 (27.5 g per litre)]
d) Ferric chloride [FeCl2. 6H2O (22.5g per litre)]
C) 1N, NaOH and H2SO4 used for neutralizing waste water samples, if their pH is
outside the range of 6 to 8.5
Procedure of test:
A) When seeding is not required:
1) Dilution water- Prepare dilution water by taking distilled water in a bottle about
one litre per sample and aerate it using a compressor or a magnetic stirrer or a fish
tank aerator for at least half an hour. (The duration of aeration is governed by the
requirement; immediate „DO‟ should be quite high- at least 7 mg/l). Keep the
bottle, loosely plugged with cotton, in „BOD‟ incubator for at least 10 hours. (This
will hold „DO‟ in dilution water in equilibrium with the air in the incubator at
20°C- the temperature of test).
2) Take 1 litre of aerated distilled water per dilution and add each of nutrients
phosphate buffer, MgSO4, CaCl2 and FeCl2, 1 ml per litre of dilution water.
JESITMR, NASHIK
3) Mix properly and fill two „BOD‟ bottles with dilution water prepared above as
blank one bottle for immediate „DO‟ and for 5 day „DO‟.
4) Shake the sample well and add a calculated quantity in a measuring jar as per the
dilution adopted. Fill up the jar with dilution water to make up 1000 ml
5) Mix the jar content vertically without aerating. For this a long glass tube (such as
an old 50 ml burette open at both ends without the regulating cock) may be used.
6) Fill up three „BOD‟ bottles A, B & C with the diluted sample. Tap the bottles to
release all entrapped air bubbles. Stopper the bottles.
7) Keep the bottle B & C in the incubator maintain at 20°C.
8) Find out immediate „DO‟ of bottle A. (This should be done within 15 minutes of
diluting the sample- to minimize errors due to the effects of temperature gradients).
Also determine initial „DO‟ of one of the blank bottle.
9) After 5 days, determine „DO‟ of incubated sample in bottles B & C and remaining
blank bottle.
10) Calculate „BOD‟ of sample
Observation table:
Sample Description Dilution Bottle DO0 DO5 BOD at Remark
No. of the Adopted No. 20°C
sample
1
Calculations:
BOD at 20°C = [(D1 - D2) - (B1 - B2)] × DF
Where,
D1 & D2 = 0 day & 5 day DO of sample
B1 & B2 = 0 day & 5 day DO of blank solution
JESITMR, NASHIK
Sample No. 1: Dilution-1, BOD =

Dilution-2, BOD =
Dilution-2, BOD =
B) When seeding is required:

1) Seeded dilution water: To prepare seeded dilution water, first ensure by a
microscopic study that the seed material contain a large population of live bacteria
protozoa. Add 1.5 ml of seed and 1.5 ml each of phosphate buffer, MgSO4, CaCl2
& FeCl3 to 1.5 L of distilled water. Aerate the dilution water for an hour &
incubate at 20°C for at least 10 hours.
2) Take 300 ml – 400 ml of seeded dilution water in 1000 ml jar.
3) Check and correct the pH of sample to 7.0, if it is outside the range of 8.5. Shake
well add a calculated quantity of the sample to the jar as per dilution adopted. Fill
up the jar to the 1000 ml mark with seeded dilution water.
4) Mix vertically
5) Fill up 3 BOD bottles P, Q & R. Remove all air bubbles. Stopper and keep all the
three bottles in the incubator.
6) Fill up a fourth bottle S with seeded dilution water. Remove air bubbles and
stopper the bottle. This is known as the seed blank (It is aerated distilled water,
which contains only the seed and nutrients and no sample).
7) Now keep the blank seed S also in the incubator.
8) After 5 days of incubation, determine DO in the bottle P, Q, R & S.
9) Calculated the BOD of seeded sample.
Calculations:-
BOD at 20°C = (Immediate DO of diluted sample- 5 day DO of diluted &
incubated sample) × DF
Dilution-2, BOD =
Dilution-2, BOD =
JESITMR, NASHIK
Observation table:
Sample Description Dilution Bottle DO5 of DO5 of BOD Remark
No. of the sample Adopted No. seeded incubated at
blank sample 20°C
1
Alternative method of seed correction:

When the dilution water is seeded, set up a separate series of seeded series of seed
dilution for incubation and select the dilution that yield 2 to 5 oxygen depletion, in 5 days,
these depletions to calculate the correction due to small amount of seed in the dilution
water. When the expected 'BOD' value is high and a variation up to 10% is not
significant, the effort involved in evaluating the amount of „BOD‟ in seed dilutions is
superfluous.
Result and Conclusions:
JESITMR, NASHIK
JESITMR, NASHIK
LAB QUIZ
1) Define BOD?
2) What is significance of BOD determination?
3) Explain the reason for determining BOD for 5 days at 20°C and 3 days at 27°C?
4) What are the limitations of BOD test?
5) What precautions should be taken in BOD experiment?
6) What is mean by seeding? Explain the necessity of seeding for particular waste water?
7) What is necessity of diluting the given sample? How the dilution ratio is decided?
8) Give reason for getting white precipitation after adding reagents in BOD bottles after
5 days?
9) What is use of BOD value?
10) Give the approximate BOD values for different waste water?
11) What should be the BOD in treated effluent?
JESITMR, NASHIK
JESITMR, NASHIK
Experiment No.: 05
CHEMICAL OXYGEN DEMAND (COD)
Introduction:
COD is a measure of the total quantity of oxygen required for oxidation of nearly
all organic compounds in waste waters, by the action of a strong oxidizing
agents.K2Cr2O7 is used as the chemical oxidizing agent, as it can oxidize a large variety
of organic substances into CO2 and H2O. Aromatic hydrocarbons and pyridine exceptions-
they remain unoxidized.
Chemically oxidized matter (estimated by COD test)
Inorganic oxidizable matter Organic matter

(Cyanide, ferrous compounds, nitrates,
Chlorides, Sulphates etc.) Biodegradable Non-Biodegradable
(Cellulose,Lignin)
Nitrogenous Carbonaceous
BOD is measure of the carbonaceous component of biodegradable organic matter
in a waste, whereas COD measures nearly all the oxidizable matter in a waste. Therefore
COD for waste is greater than its BOD value. Both BOD and COD values of any waste
are important parameters, as their interrelationship decides the type of treatment to be
adopted for the waste. If COD is very much greater than BOD, then the waste is not
biodegradable. Biodegradability of the waste is indicated by the treat ability index (T.I.).
T.I.=BOD/ (COD-BOD)
T.I. less than 0.5 indicate the waste is not amenable to biological treatment
especially aerobic. Chemical treatment may be suggested. Chemical treatment may be
precipitation of pollutant, coagulation (followed by flocculation and sedimentation),
oxidation, absorption etc. T.I. between 0.5 and 1.0 indicates that biological treatment for
the waste may be considered with necessary nutrient supplementation. T.I. more than 1.0
indicates that the waste is amenable to biological treatment. All biodegradable wastes are
JESITMR, NASHIK
chemically degradable. However, for any waste providing biological treatment should be
first explored, as it is more economical.
COD/BOD ratios and treat ability indicates of some common wastes:
Waste COD/ T.I. Waste COD/ T.I.
BOD BOD
Phenol waste 1.3 3.0 Soft drink 2.1 0.9
Pharmaceuticals 1.4 2.3 Synthetic Textiles 2.2 0.8
Dairy waste 1.5 2.0 Paper & Pulp 2.4 0.7
Domestic waste 1.8 1.2 Straw board waste 3.0 0.5
Metal processing 1.9 1.1 Metal planting 4.5 0.3
Sugar mill waste 2.0 1.0 Electroplating Zero
Importance of COD Test:

1) COD value indicates practically the overall pollutional strength of a raw waste,
domestic or industrial
2) COD & BOD values of waste are used for determining its treat ability index.
3) COD test is used for quickly evaluating performance efficiency of treatment units and
correcting errors immediately, as the test can be completed in three hours as against five
days required for BOD test.
4) By knowing the general COD/BOD ratio for a waste, BOD values can be worked out
in an emergency for COD test results.
5) COD test is used for determining the suitability of the treated waste for disposal.
Limitations of COD Test:

The test adopts an artificial procedure. It cannot differentiate between biologically
degradable and biologically resistant organic matter, whereas BOD test simulates
conditions obtainable in a natural stream.
COD test does not indicate, time-wise, the rate and extent of removal of
pollutional load of wastes on nature; whereas BOD1, BOD2, BOD3 to BOD20 indicate the
natural rate of biodegradation of a particular waste.
JESITMR, NASHIK
Standards Recommended
Maximum permissible
Sr. No. Description
COD
Industrial effluents discharge into inland surface
1 250mg/l, IS 2490
waters
2 Industrial effluents falling into marine coastal area 250mg/l, IS 7968
Determination of COD:
Principle:
A known volume and normality of a potent oxidizing agent is used to oxidize all
oxidizable matters in the sample as completely as possible. Oxidation is carried out for an
o
extended period at 100 C.The residual oxidizing agents is estimated using a suitable
reducing agent. The amount of oxidizing agent consumed as a measure of the overall
pollutional load of the waste.
Discussion:
Oxidizing Agent: The oxidizing chemical used is K2Cr2O7 it is readily available in a pure
analytical grade and the standard prepared retain their normality for very long, acidified
dichromate oxidizes nearly all type of organic matters in to CO2 and water.
C6H12O6 + [4K2Cr2O7 + excess of K2Cr2O7] + 16H2SO4  6CO2 + 22H2O + 4Cr2(SO4)3

+ 4K2SO4 + [Excess of K2Cr2O7]
The color of dichromate indicating, being orange helps in reckoning the process of
residual dichromate after heating-which is essential for the success of the test.
Dichromate consumed during the test is the difference between the dichromate
concentration remaining as excess after hot digestion. The initial concentration of
dichromate is estimated by running a blank through the test, which will practically
eliminate error due to any oxidizable matter present in dilution water.
Reducing Agent:- The reducing agent, which is used as titrant is, ferrous ammonium
sulphate. The ferrous ion reduces dichromate completely and excess of Fe++gives a sharp
reddish brown end point with ferrion indicator.
JESITMR, NASHIK
6Fe(NH4)2+K2Cr2O7+K2Cr2O7+H2SO4 3Fe(SO4)3+7H2O+6(NH4)2SO4+Cr2 (SO4)3+K2SO4
COD of waste sample, mg/l

= (a-b) x [Normality of titrant] x [Equivalent wt of oxygen] x 1000 x D.F.
Volume of sample. (20ml)
Where a = ml of titrant used for blank
b = ml of titrant used for sample (direct or diluted) Volume of sample taken
is generally 20 ml (direct or diluted)
It is conventional to use 0.25 N K2Cr2O7 as each ml of dichromate is equivalent to
2 mg of oxygen and so a large range of COD is determinable. The titrant Fe(NH4)2(SO4)2
is prepared to be 0.1 N; so that, in an ideal case,25 ml will be required to reduce 10ml of
0.25 N K2Cr2O7 in the blank, allowing sufficient reaction tin\me for the complete
reduction of dichromate (Cr3+). During the estimate of dichromate consumption, for most
significant results, b should be minimum of 4 ml & (a-b) should be a minimum of 4 ml.
Dilution technique:
This is based on the excepted COD of the test sample considering the equation,
COD mg/l = (a-b) x 0.1 x (mg/ml) x 8 x 1000(ml/l) x D.F.
20 ml
COD may be = (25-21) x 0.1 x 1000 x D.F.(minimum)
20 ml
That is, COD =160 x (D.F.) (minimum) & 840 x D.F. (maximum). The dilution
factor should be so chosen, that the expected COD value of a sample lies within the range
of minimum & maximum COD values obtainable.Ex. If expected COD value is 2000
mg/l,
D.F. may be 5 & 10. There should be overlapping dilutions for each sample. The
range of COD obtainable will be form 800 mg/l to 8400 mg/l.1 to 5 dilutions is carried
out by diluting 20 ml of the (well mixed) sample to 100 ml, mixing well and extracting 20
ml of the diluted sample for the COD test, the test of the diluted is rejected.
For domestics‟ sewage & treated industrial effluents, recommended dilution
factors are land 5.For raw industrial effluents such as sugar factory waste dairy waste
paper & pulp mill waste etc. D.F. may be 5 to 20. For distillery- spent wash; D.F. may be
100 & 200 or 200 & 250.
JESITMR, NASHIK
Failure of COD test
The COD test is considered a failure when-

1. b > a
2. (a-b) < 4ml (2ml absolute minimum)-dilution is too high
3. B < 4ml (2ml absolute minimum)-dilution is too less
4. When the sample flasks show green color either immediately after addition of
acid or during or after heating but are fore titration. This happens, when the dilution is
too less and the oxidizable matter in the sample is in excess of the oxidizing agent
added. The total green color is because of the complete reduction of all the
dichromate (Cr6+) to chromate (Cr3+). Lack of residual dichromate before titration
makes dichromate consumption indeterminate.
5. The test is also a failure, when the blank also turns green after the addition of
H2SO4, indicating that the acid used is substandard.
Importance of HgSO4:
HgSO4 is used during the test to prevent the interference due to chlorides in
wastewater. Chlorides reduce dichromate (Cr6+) to chromate (Cr3+) in an acidic medium,
thus resulting in a higher COD value.
6NaCl + K2Cr2O7 + 7H2O 3Cl2 + 7H2O +3Na2SO4 + Cr2 (SO4)3 +K2SO4.
If HgSO4 is present, it combined with chlorides reduce chlorides to form poorly
ionized HgCl2 thus preventing reduction of dichromate by chlorides.
HgSO4 + 2NaCl HgCl2 + Na2SO4
HgSO4 should be added to the sample before addition of dichromate and acid. 400 mg of
HgSO4 added to 20 ml of sample suppresses interference due to 4870mg/l of chlorides
concentration n the sample, which is generally not exceeded in inland wastewater.
However if seawater infiltration is suspended, use of 1 to 20gm of Hg4SO4 may be
necessary to suppress interference due to chlorides in the range of 11000 mg/l to 23000
mg/l in the sample
Importance of Ag2SO4:Ag2SO4 is a catalyst, which enables dichromate to oxidize low
molecular weight fatty acids & straight chain aliphatic compounds.
Ferrion (Ferrous 1, 10-phenonthroline sulphate)
This a soluble organic indicator, which exists in two, different colors the change
in color with a change in oxidation-reduction potential. In the first state, when the
JESITMR, NASHIK
oxidizing agent is in excess, the color of the indicator merges with the color of
dichromate. As the titration progress, orange dichromate (Cr6+) is reduced & green
chromate (Cr3+) increases. At the end point when all the dichromate ions are completely,
addition of a very little excess of the titrant makes ferrous ions available 1-10
phenonthroline in ferrion to form a reddish-brown complex (the color & composition of
the indicator itself) in second state.
Apparatus & equipment:-
50 ml burette, 10ml pipette,100ml measuring cylinder, 250 ml beaker. Reflux
apparatus (9-coiled condensers attached to 250 ml COD flasks with ground glass necks
mounted on heating equipment).
Chemicals:-
1. 0.25 N Potassium dichromate (K2Cr2O7 (12.259) gm/lit)-oxidizable agent.
2. Conc. H2SO4 (36N) –provide low pH necessary for oxidation by
dichromate.
3. 0.1N Ferrous ammonium sulphate [(Fe (NH4)2(SO4)6H2O (39gm+36N
H2SO4 (20 ml) per liter].
4. Ferrion[1,10-phenanthrolone monohydrate (1.735gm) +FeSO47H2O
(0.695gm) per 100ml acidified].
5. Mercuric sulphate (analytical crystals).
6. Silver Sulphate (reagent powder).
Standardization of Ferrous ammonium sulphate

Necessity:
Ferrous ammonium sulphate, being a reducing agent, is slowly oxidized by the
oxygen dissolved from air-from the moment the titrant is prepared. The strength of the
titrant gradually drops on standing and exposure. Therefore standardization is required
every time the titrant is used.
Procedure:
1) Pipette out 0.25 N K2Cr2O7 accurately in to a 100 ml volumetric flask and dilute to
100 ml (using distilled water).
2) Add 30 ml of conc.
3) Cool to room temperature (this is very important).
4) Add 2 to 3 drops of ferrion indicator.
JESITMR, NASHIK
5) Titrate against the given ferrous ammonium sulphate. Record the amount of titrant
(Xml) used up to the end point, when the contents change from dark-green to
stable reddish brown colour.
Fe (NH4)2(SO4) = K2Cr2O7
N x X (ml) = 0.025 x 100ml
Normality of titrant N = 0.025 x 100ml / X
Procedure of COD test:
A } 1) Take three COD flasks P, Q, &R place about 400 mg of H2SO4 in each flask.
2) Add 20ml of distilled Water to flask P (blank) & 20ml of sample direct or diluted to
flasks Q & R (adopt two different dilutions for each sample).
3) Add 10ml of 0.25N K2Cr2O7accurately, using a pipette, to each flask.
4) Add 30ml conc. H2SO4 (36N) to each flask.
5) Add about 200 mg of Ag2SO4 to each flask.
6) Add 3 to 4 glass beads or rounded quartz pebbles (to minimize bumping of acid
mixture during boiling).
B}1) Attach all three flasks to reflux condensers. Heat and digest for two hours.
2) Cool the flasks .Add 20ml of distilled water down each condenser attached to P, Q, &
R (to wash down condensed organics sticking to coiled surfaces).
3) Detach the flasks and add 70ml of distilled water to each.
4) Cool the flasks to room temperature. If the flask content are at
C}1) Titrate all the three flasks against standardized ferrous ammonium sulphate using 2
to 3 drops of ferroin indicator.
2) Record titrant used (a) ml for blank flask P & (b) ml for sample flask Q, (c) ml for
sample flask R
Observation Table
Sample Sample Dilution ml of titrant used COD Remarks
No. Description For For mg/l
blank sample
1 1 to
1 to
2 1 to
1 to
JESITMR, NASHIK
Calculations:
Sample No.1, Dilution-1: COD, = (a-b) ml x N (mg/ml) x 8 x 1000(ml/l) x D.F.
(1 to ) mg/l 20ml
Dilution-2: COD, = (a-c) ml x N (mg/ml) x 8 x1000(mg/l) x D.F.
(1 to ) mg/l 20ml
Note:-1) If both dilutions give satisfactory results, variation being within 10% record
the average COD value.
2) If the variation in results is more than 10% choose the results for which
(a - b) or (a - c) is greater
Result & Conclusions:
JESITMR, NASHIK
Lab Quiz:
1) Define COD?
2) What is the role of HgSO4 in the reaction?
3) What is the structure of ferroin?
4) What is septic and stale sewage?
5) Differentiate between BOD and COD.
6) Why do the BOD analysis aand COD analysis give different results for the same
sample?
JESITMR, NASHIK
JESITMR, NASHIK
Experiment No.: 06
CONDUCTIVITY
Introduction:
Irrigation water, which may be river water, lake water, well water or treated waste
water, is evaluated by its total salt concentration. Excessive salts in water reduce the
osmotic activity of plants and diminish the absorption of nutrients from soil, affecting
crop growth and crop yield. As salt solution conduct electricity, the concentration of salt
in irrigation water is evaluated by determining in electrical conductivity.
Electrical conductivity is the reciprocal of electrical resistivity, which is the
resistance in omhs of a conductor (metallic or electrical), 1 cm2 in cross-section and 1cm
in length. Therefore conductivity of electrical conductance of a liquid is the reciprocal of
resistance offered by 1 cm3 of the liquid at a specified temperature. It is expressed in
mhos/cm, milliohms/cm or microhms/cm.
Discussion:
Low salinitly ( EC < 3000 micromhos/cm ) in irrigation water is generally caused by
Ca++, Mg++ and HCO3- ions.
High salinity ( EC 3000 – 10000 micromhos/cm) is caused by combination of Ca++,
Mg++, Na+ and rarely K+ cations with HCO3- , SO4- and Cl- ions.
Very high salinity ( EC >10000 micromhos/cm) is caused by Na+ and Cl- ions. (
Bicarbonate ions in combination with the cations can push the PH upto 8.3 but when
carbonate ions are present, PH may go above the 9 making water unsuitable for irrigation )
Electrical conductivity proportional to the ionizable fraction of dissolved solid
concentration. Therefore measurement of conductivity may be used to obtain a quick
major of dissolved salts in water.
For water width PH 5 to 9 and temperature 100C and 40oC, an empirical expression is
Total dissolved solids (inorganic) = K x (1.02)T-25 x conductivity
(mg/lt) (miromhos/cm)
K is factor depending upon the electrolytic character of water.
JESITMR, NASHIK
K=0.7, if the dissolved solid in irrigation water contains 83% (generally maximum) salts
which conduct current.
K=0.58, if only the electrolytic component of irrigant is required. Salinity problem related
to water quality occurs; if the total quantity of salt in irrigation water is high enough to
accumulated in the soil plant root zone. Salt built up at the root zone is governed by
leaching action of soil, which is influence by the drainage characteristics of soil. Light
textured soils, having clay contained of less than 10% have excellent internal and surface
drainage. EC of irrigation water from 6000-8000 micromhs/cm may be consider safe for
semi tolerant crops, because of effective leaching action. Medium textured soils, having a
clay content of 10-20%,have good drainage, permitting application irrigation water with
EC ranging from 2000 - 4000 micromhos/cm.
Deep black soil, having a clay content of more than 30% poor drainage characteristics,
restricting EC of irrigation water to a safe maximum limit of 2000 micromhos/cm.
Salt tolerance levels of some crops, as determined by maximum EC values, Beyond

which normal crop-yield stars dropping
Crop variety EC of saturated soil EC of irrigation water,
extracted, (micromhos/cm)
(micromhos/cm)
Field Crops
1) Corn 1,700 1,100
2) Wheat 6,000 4,000
3) Cotton 7,700 5,100
Forage crops
Different types of grasses 1500 to 7500 1000 to 5000
Vegetable Crops
1) Beans & carrot 1000 700
2) Lettuce 1300 900
3) Potato & sweet 1600 1100
potato
Fruit Crops
1) Apple, orange, grapes 1700 1000
& lemon
2) Pomegranate 2700 1800
3) Date palm 4000 2700
JESITMR, NASHIK
Although many crops have high salt to tolerance levels, it is imperative to supply
irrigation water with a low salt concentration , to allow for possible build-up of salinity at
the plant root zone in the soil specially in arid regions.
Classification of EC of irrigation water in relation to its application

EC at 25˚ C,
Salinity Application
Micromhos/cm
<250 Low Suitable for all crops-field crops, forage crops(grasses),

vegetable crops and fruit crops- on all soils.
Suitable for field crops, forage crops, fruit crops, & vegetable
250 to 750 Mediam
crops on soil with moderate drainage.
Suitable for some salt tolerant field crops,(cotton,wheat), some
750 to 2250 High varieties of grasses & of fruit crops(pomegranate, date palm )
on soil with good drainage.
Suitable for a very few salt tolerant field crops,(cotton, wheat),
Very
2250 to 3000 & a few varieties of grasses only on soils with excellent
high
drainage.
In addition to affecting plant growth, salinity in water also affects fish culture. Salinity
reduces solubility of oxygen and results in diminished intake of oxygen through the grills
of fish.
Standards Recommendations
1) Tolerance limits for inland surface waters for irrigaton-
a) Electrical conductance at 25˚C max. 3000 micromhos/cm (IS 2296)
b) TDS (inorganic), max. 2100 mg/l (IS 2296)
2) Tolerance limits for inland surface waters for fish culture-
Electrical conductance at 25˚C, max. 1000 micromhos/cm (IS 2296)
Determination of conductivity:-
Principle:-
Determination of conductivity is based on measuring the resistance of a column of
solution of area A (cm2) & length one cm.
JESITMR, NASHIK
Equipment & glassware:

Conductivity meter and measuring cylinder.
Chemicals:
0.01N potassium chloride (where conductivity is 1410 micromhos/cm)
Procedure:
1) Connect the electrodes with instrument. Submerge the electrodes in distilled water.
Switch on the power knob, 5 min. before starting the experiment.
2) Prepare standard solution (KCL) of strength 0.1N, 0.01N, 0.001N. use proper
solution depending on the expected conductivity of the sample.
3) When instrument is on & electrode submerged in distilled water, it will show the
display as “Put standard”.
4) Immerse the electrode in “standard solution” Press the Knob CAL. It will show
“System busy” after few seconds, it will display all constant. If required a press
knob „COND‟ to know conductivity of a standard solution. Conductivity will be
measure in MS or US and the working temperature will be also displayed.
Conductivity value obtained above is at working temperature. The instrument can
also be set to give conductivity reading at standard temperature of 25˚C by
applying “TEMPCORR”.
5) Immerse the electrode in sample and press COND records the conductivity and
working temperature of a sample.
6) Estimate the dissolved solids in sample.
Observations:
Sample Temperature Conductivity Total dissolved
Micromhos/cm solids mg/l
JESITMR, NASHIK
Calculations:
Dissolved solid Concentration =
Results and Conclusion:
JESITMR, NASHIK
Lab Quiz
1. Define conductivity?
2. What is purpose of conductivity determination for treated effluents?
3. How it is decided whether the treated effluent can be used for irrigation purpose or not?
4. What are the recommended standards of conductivity for treated effluent may be used for
irrigation purpose?
5. What is the relation between conductivity and TDS content?
6. What is the effect of temperature on electrical conductivity?
7. What are the unit of electrical conductivity?
JESITMR, NASHIK
JESITMR, NASHIK
Experiment No.: 07
DETETMINATION OF NITRITES IN WASTEWATER
Introduction:
Various forms of nitrogen in sewage/wastewater are derived from nitrogenous
organic matter. The nitrogenous organic matter is biodegraded as per the nitrogen cycle.
Thus nitrogen occurs in various form sewage or wastewater such as ammonia

nitrogen, nitrogen (nitrites) & total nitrogen, which is sum of ammonium, and organic
nitrogen.
Organic nitrogen is present in fresh sewage sample. It is ammonified by biological
activity to ammonia(NH3). Ammonia is further converted to nitrites(NO2) and
nitrate(NO3) by nitrifying bacteria. Nitrate nitrogen and nitrite nitrogen may be present in
fresh sewage sample if it exists in water supply or ground water,which has in-filtered the
sewerage system.it will disappear rapidly as sewage becomes state and it‟s seldom found
in the influent to sewage treatment plants. It is often found in the effluents from
secondary treatment and the quantity is an indication of the completeness of oxidation by
the particular process.
JESITMR, NASHIK
Determination of nitrite (nitrogen) in wastewater by spectrophotometer:

Interference:
This method is interfered with by relatively large amount , upto 1000 times, of the
alkaline earths, zinc, nickel, arsenate, benzoate, borate, bromide, chloride, fluoride,
iodate, molybdate, phosphate, sulphate, and thiocyanate. Numerous heavy metals such as
gold, lead, bismuth, iron, or mercury interfere by precipitations and others because of
coloured salt. Aliphatic amines react with nitrites to liberate the gaseous nitrogen.
Ammonia does not interfere in the small concentrations usually encountered. Strong
reducing or oxidizing agents should be absent.
Preservation of samples:
Determination of nitrites content must be made on fresh samples because
conversion of Nitrite into either nitrate or ammonia by biological action proceed
unintrruptely, unless the sample is temporarily preserved with 1500 mg/lit withH2SO4 as
given below. The nitrogen balance may be preserved for 24 hours by adding sufficient
H2SO4 to produce 1500mg/lit acidity in sample, equivalent to PH 2 to 3.this treatment
will lower the suspended matter and settleable matter and it will not preserve the nitrogen
balance longer than 24 hour.
Apparatus:
Spectrophotometer, for use at 520 mu providing a light path of 1 cm or longer.
Reagents:
1. Sulfanilic acid solution-dissolve 0.60 gram sulfanilic acid in 70 ml hot distilled
water, add 20 ml conc.HCL, dilute to 100 ml with water mix thoroughly.
2. napthylamine-dissolve 0.60 g napthylamine hydrochloride and 1 ml conc. HCL
in distilled water and dilute to 100ml.
3. sodium acciate solution(2M)-16.40g NaC2H3O2 in distilled water and make up to
100 ml. filter if the solution is not clear.
4. stock sodium nitrite solution- dissolve 0.4926g NaNO2 in 1000 ml nitrite free
distilled water.
5. Diluten100 ml stock solution to 1000 ml, then dilute 50 ml of this solution to 1000
ml with sterilized nitrite free distilled water, add 1 ml chloroform and preserve in
sterilized bottle,
6. 1ml=0.0005mg N or 0.001642mg NO2
7. manganous sulphate solution-dissolve 480 g MnSO4. 4H2O or 364g MnSO4.
H2O in distilled water, filter and dilute to 1 liter.
JESITMR, NASHIK
8. potassium permagnate solution- dissolved 0.4 g KMnO4. 4H2O in 1 liter of

distilled water.
9. zinc sulphate solution- dissolve 100g ZnSO4. 7H2O in 1 liter of distilled water.
10. ammonium oxalate solution- dissolve 0.90g (NH4)2C2O4H2O in 1 liter distilled
water.
11. nitrite free water- add 1 ml conc. H2SO4 and 0.2 ml MnSO4 solution to 1 liter
distilled water and make pink with 1 to 3 ml KMnO4 solution. After 15 minutes
decolorize with (NH4)2C2O4 solution.
Procedure:
1. Treatment of sample :- Add 1ml zinc Sulphate solution to 100ml of sample.
Mix thoroughly , add 0.4 to 0.5 ml NaOH solution to obtain a pH of 10.5 ;
again mix& clarify by centrifuging or filtering through filter, discarding the
first 25 ml of filtrate
2. Place 10 ml clarified sample in a 50 ml volumetric flask & dilute to 25ml. If
the sample is acidic or alkaline, neutralize to pH 6.5- 7.5 with a few drops of
dilute HCl or NaOH.
3. Measure 1ml sulfanilic acid solution in to the diluted sample, mix and allow to
stand atleast 3 min and not more than 10 min for diazotization. The pH of this
solution should be about 1.4.
4. Add 1ml napthylamine hydrochloride solution & 1ml sodium acetate solution.
This should buffer the system to a pH of 2.5. Dilute to 50 ml and mix well.
5. After 10 min and before 30 min , measure the intensity of radish purple colour
in a spectrophotometer of wavelength of 520 m u.
6. Transmittance reading should be made against a reagent blanks and parallel
checks should be run frequently of against known nitrite standard preferably in
nitrogen range of the sample.
Preparation of calibration curve:

a. Prepare standard solution by diluting standard nitrite solution 0.2 ml, 0.4 ml 1
ml, 1.5 ml, 1.8 ml, 2 ml, 2.5 ml and 4 ml to 50 ml with distilled water.
b. Repeat steps 3 to 6 of above part.
c. Prepare blank solution with 50 ml -distilled water and treat in the same way as
standard solution.
JESITMR, NASHIK
d. Set absorbance zero with blank and record the absorbance of standard
solution.
e. Plot graph of absorbance against NO2 concentration.
f. Estimate NO2 concentration of sample for calibration.
Observation table:
Volume of Total volume Concentration Concentration Absorbance

std. solution of Nitrites of Nitrogen
Nitrite
Calculations:
JESITMR, NASHIK
JESITMR, NASHIK
Lab Quiz:
1) What are the different forms of nitrogen present in wastewater?
2) What are the sources of nitrogen in wastewater?
3) What are the different methods of nitrite determination?
4) Why nitrites should be removed from waste water?
5) What are the different treatment methods for removal of nitrites?
6) What does the presence of nitrites indicate in waste water?
JESITMR, NASHIK
JESITMR, NASHIK
Experiment No.: 08
DETERMINATION OF PHOSPHATES IN WASTEWATER
Introduction:
Phosphates occur solely in waste water as Orthophosphates, Condensed or acid
hydrolysed phosphates (Pyro, meta and ortho polyphosphates) and Organically bound
Phosphate. Phosphate ion concentration in three selected areas of Coastal Guyana in the
county of Berbice, Demerara and Essequibo was determined using Stannous Chloride-
Molybdate Calorimetric, Spectrophotometric method. The first step involves the
conversion of condensed and Organically bound phosphate ion to soluble Orthophosphate
by acid oxidation using H2SO4 and HNO3 and the second stage involves the
spectrophotometric determination of phosphorus in the soluble Orthophosphate at 660
NM by the molybdenum (Mo) blue method using stannous (II) chloride as the reducing
agent. The applicable range of this method is 0.01 to 6 P/L. The UK Standard and the
Caricom (1981 draft) for Phosphorus in potable water is 2.2 mg/L. The European Union
(EU) maximum admissible concentration (MAC) of Phosphorus in Potable water is 5
mg/L.The world Resources Institution has identified 375 hyponix coastal zones of which
Guyana is not included. It seems that the selected Guyana water is not polluted with
Phosphate anion but Guyana‟s water must continued to be monitored as Industrilisation
and development increased.
This method is applicable to the analysis of drinking water, surface waters,
domestic and industrial waters. It can be modified to compensate for turbidity, colour,
salinity and dissolved organic compounds in the sample.Phosphate is a salt of phosphoric
acid, H3PO4 with empirical formula PO4 -. It consists of one central phosphorus atom
surrounded by four oxygen atoms in a tetrahedral arrangements. The phosphate anion is a
hypervalent molecule and incorporates phosphorus.
JESITMR, NASHIK
The Phosphate ion carries a negative three formal charge and is the conjugate
base of the hydrogen phosphate anion, HPO42-, which is the conjugate base of
H2PO4-, the dihydrogen phosphate ion, is the conjugate base of H3PO4, phosphoric
acid. These equilibrium reactions are shown below:
H3PO4 ↔ H+ + H2PO4- - - - - - (1)

H2PO4- ↔ H+ + HPO42- - - - - -- (2)
HPO42- ↔ H+ + PO 43 - - - - - - (3)
In dilute aqueous solution, phosphate exists in four forms. In strongly basic
medium, the phosphate ion (PO4- predominates, whereas in weakly basic conditions, the
hydrogen phosphate ion (HPO4- prevails. In weakly acidic conditions, the dihydrogen
phosphate ion (H3PO4-) is most common. In strongly acidic conditions, aqueous
phosphoric acid , H3PO4 is the main form. Organophosphate is an ester
Phosphate can also form polymeric ion such as diphosphate (pyrophosphate,
P2O7- triphosphate, P3O10- etc. Metaphosphate ions which are long linear polymers have
an empirical formula of PO3- and are found in many compounds.
JESITMR, NASHIK
Biologically, Phosphates are found in the form of Adenosine Phosphates (AMP,

ADP and ATP) and in DNA and RNA. Hydrolysis of these results in the release of
phosphates. Phosphates are useful as buffering agents in the Biological system. Phosphate
salts are used to prepare buffer solutions at cell pHs. These include Na2HPO4, NaH2PO4
and the corresponding potassium salts. Phosphates form the structural material of bone
and teeth. These structures are made up of calcium phosphate in the form of
hydroxyapatite. Phosphates anion occurs in natural and wastewaters as Orthophosphates,
Condensed or acid hydrolysed phosphates (Pyro-, meta-, and other polyphosphates), and
organically bound phosphates. They occur in solution, in particles or detritus, or in the
bodies of aquatic organisms. These forms of phosphate arise from a variety of sources.
Phosphates may also occur in bottom sediments and in biological sludge.
Orthophosphate, condensed phosphate and organically bound phosphate are referred to as
the total phosphorus content.
On the positive side, phosphorus in phosphates is essential to the growth of plants,
animal and microorganisms. It is an essential part of the process of photosynthesis and
can be the nutrient that limits the primary productivity of a body of water. In instances,
where phosphate is a growth-limiting nutrient, the discharge of raw or treated wastewater,
agricultural drainage, or certain industrial wastes to that water may stimulate the growth
of photosynthetic aquatic micro and macro-organisms in nuisance quantities. Phosphorus
is involved in the formation of all oils, sugars, starches etc. It helps with the
transformation of solar energy into chemical energy, proper plant maturation,
withstanding stress and it also encourages blooming and root growth The discharge of
wastewater containing phosphates may also cause algae growth in quantities sufficient to
cause taste and odor problems in drinking water supplies. Dead and decaying algae can
cause oxygen depletion problems which in turn can kill fish and other aquatic organisms
in streams via a process called Eutrophication. Both the excess of nitrates and phosphates
contribute to the high levels of Eutrophication in water ways . For this reason, phosphates
removal is an essential role of wastewater treatment plants and testing for phosphorus in
the plant effluent is critical to water quality.
Small amounts of Orthophosphate or certain condensed phosphates are added to
some water supplies during treatment. Larger quantities of the same compounds may be
added when the water is used for laundering or other cleaning, because these materials are
major constituents of many commercial cleaning preparations.
JESITMR, NASHIK
Phosphates are used extensively in the treatment of boiler waters.

Orthophosphates applied to agricultural or residential cultivated land as fertilizers are
carried into surface waters with storm runoff and to a lesser extent with melting snow.
Organic phosphates are formed primarily by biological processes. They are contributed to
sewage by body wastes and food residues, and also may be formed from Orthophosphates
in biological treatment processes or by receiving water biota.
Phosphates also occur in bottom sediments and in biological sludge, both as precipitated
inorganic forms and incorporated into organic compounds. The excess of phosphorous in
water is largely due to fertilizer run off from the application of fertilizers to crops. They
are very beneficial to plant growth, however they can also introduce some of the more
toxic substances present in livestock excretions, such as pharmaceuticals or bacteria.
Phosphates enter waterway from human and animal waste, phosphorous rich
bedrocks, laundry, cleaning industrial effluents, and fertilizer runoff. Providing sufficient
quantities
Determination of Phosphates in wastewater by spectrophotometer:

Interference:
This method is interfered with by relatively large amount , upto 1000 times, of the
alkaline earths, zinc, nickel, arsenate, benzoate, borate, bromide, chloride, fluoride,
iodate, molybdate, phosphate, sulphate, and thiocyanate. Numerous heavy metals such as
gold, lead, bismuth, iron, or mercury interfere by precipitations and others because of
coloured salt. Aliphatic amines react with nitrites to liberate the gaseous nitrogen.
Ammonia does not interfere in the small concentrations usually encountered. Strong
reducing or oxidizing agents should be absent.
Preservation of samples:
Determination of Phosphates content must be made on fresh samples because
conversion of Nitrite into either nitrate or ammonia by biological action proceed
unintrruptely, unless the sample is temporarily preserved with 1500 mg/lit withH2SO4 as
given below. The nitrogen balance may be preserved for 24 hours by adding sufficient
H2SO4 to produce 1500mg/lit acidity in sample, equivalent to PH 2 to 3.this treatment
will lower the suspended matter and settleable matter and it will not preserve the nitrogen
balance longer than 24 hour.
Apparatus:
Spectrophotometer, for use at 885 mu providing a light path of 1 cm or longer.
JESITMR, NASHIK
Reagents:
1. Sulfanilic acid solution-dissolve 0.60 gram sulfanilic acid in 70 ml hot distilled
water, add 20 ml conc.HCL, dilute to 100 ml with water mix thoroughly.
2. napthylamine-dissolve 0.60 g napthylamine hydrochloride and 1 ml conc. HCL
in distilled water and dilute to 100ml.
3. sodium acciate solution(2M)-16.40g NaC2H3O2 in distilled water and make up to
100 ml. filter if the solution is not clear.
4. stock sodium nitrite solution- dissolve 0.4926g NaNO2 in 1000 ml nitrite free
distilled water.
5. Diluten100 ml stock solution to 1000 ml, then dilute 50 ml of this solution to 1000
ml with sterilized nitrite free distilled water, add 1 ml chloroform and preserve in
sterilized bottle,
6. 1ml=0.0005mg N or 0.001642mg NO2
7. manganous sulphate solution-dissolve 480 g MnSO4. 4H2O or 364g MnSO4.
H2O in distilled water, filter and dilute to 1 liter.
8. potassium permagnate solution- dissolved 0.4 g KMnO4. 4H2O in 1 liter of
distilled water.
9. zinc sulphate solution- dissolve 100g ZnSO4. 7H2O in 1 liter of distilled water.
10. ammonium oxalate solution- dissolve 0.90g (NH4)2C2O4H2O in 1 liter distilled
water.
11. nitrite free water- add 1 ml conc. H2SO4 and 0.2 ml MnSO4 solution to 1 liter
distilled water and make pink with 1 to 3 ml KMnO4 solution. After 15 minutes
decolorize with (NH4)2C2O4 solution.
Procedure:
1. Treatment of sample :- Add 1ml zinc Sulphate solution to 100ml of sample. Mix
thoroughly , add 0.4 to 0.5 ml NaOH solution to obtain a pH of 10.5 ; again mix&
clarify by centrifuging or filtering through filter, discarding the first 25 ml of
filtrate
2. Place 10 ml clarified sample in a 50 ml volumetric flask & dilute to 25ml. If the
sample is acidic or alkaline, neutralize to pH 6.5- 7.5 with a few drops of dilute
HCl
3. Measure 1ml sulfanilic acid solution in to the diluted sample, mix and allow to
stand at least 3 min and not more than 10 min for diazotization. The pH of this
solution should be about 1.4.
JESITMR, NASHIK
4. Add 1ml napthylamine hydrochloride solution & 1ml sodium acetate solution.
This should buffer the system to a pH of 2.5. Dilute to 50 ml and mix well.
5. After 10 min and before 30 min , measure the intensity of radish purple colour in
a spectrophotometer of wavelength of 885 m u.
6. Transmittance reading should be made against a reagent blanks and parallel
checks should be run frequently of against known nitrite standard preferably in
nitrogen range of the sample.
Preparation of calibration curve:
a. Prepare standard solution by diluting standard Phosphates solution 0.2 ml, 0.4 ml
1 ml, 1.5 ml, 1.8 ml, 2 ml, 2.5 ml and 4 ml to 50 ml with distilled water.
b. Repeat steps 3 to 6 of above part.
c. Prepare blank solution with 50 ml -distilled water and treat in the same way as
standard solution.
d. Set absorbance zero with blank and record the absorbance of standard solution.
e. Plot graph of absorbance against Phosphates concentration.
f. Estimate Phosphates concentration of sample for caliberation.
Observation table:
Volume of Total Concentration Concentration

Absorbance
std. solution volume of Phosphates of Phosphates
JESITMR, NASHIK
JESITMR, NASHIK
Lab Quiz:
1) What are the three basic forms of phosphorus found in wastewaters?
2) What is the significance of excess phosphates in water?
3) What is Eutrophication?
4) What are the different methods of phosphate analysis in water?
5) State the components of instruments for optical spectrophotometry.
6) What are the sources and health effects of Phosphates?
JESITMR, NASHIK
JESITMR, NASHIK
Experiment No.: 09
VISIT TO DOMESTIC/ INDUSTRIAL WASTEWATER
TREATMENT PLANT
Date of Visit: Date of submission:
JESITMR, NASHIK
JESITMR, NASHIK
JESITMR, NASHIK
JESITMR, NASHIK
Experiment No.: 10
COMPUTER AIDED DESIGN OF SEWAGE TREATMENT
PLANT (STP)
Date of Performance Date of submission:
JESITMR, NASHIK
JESITMR, NASHIK

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Jawahar Education Society's,

INSTITUTE OF TECHNOLOGY, MANAGEMENT &

DEPARTMENT OF CIVIL ENGINEERING

ENVIRONMENTAL ENGINEERING - II (401 001)

Class: B.E (Civil) Academic Year: 2017-18

01. Determination of Solids

02. Determination of Sludge Volume Index

03. Determination of Dissolved Oxygen

Determination of Biochemical Oxygen

06. Determination of Conductivity

07. Determination of Nitrites

08. Determination of Phosphates

09. Visit Report

Computer Aided Design of Sewage

(Prof. M. J. Kakani) (Prof. H. A. Shahane) (Dr. M. V. Bhatkar)

Date of Performance: Date of Submission:

Total Solids (a)

Non-Settleable Settleable Volatile Solids Fixed Solids

Volatile Solids Fixed Solids

Briefly solids can be classified as:

Total Solids (a)

Total Suspended Solids (b) Total Dissolved Solids (e)

Volatile Suspended Solids (f+g) Volatile Dissolved Solids (h)

Fixed Suspended Solids (i+j) Fixed Dissolved Solids (k)

When any organic and inorganic components are required.

Total Solids (a)

Total Volatile Solids Total Fixed Solids

Importance of solids determination:

If efficiency is less than 40% PST need not be provided.

Graph-1 indicates sedimentation increase with time continuously but a maximum

d) Total volatile solids & total fixed solids:-

f) Settleable and non settle able solids:-

Result & Conclusion:

Date of performance: Date of submission:

Importance of SVI Determination:

Associated operational parameter for Biological Aeration process

Causes of sludge bulking:

5.These multicellular organisms get water-entrained and remain suspended without

6) High carbohydrates contribute to sludge bulking.

b) Poor plant design and operation.

c) Emergency control measures

d) Long term control measures:-

Recirculation ratio and Concentration of return sludge:-

Qr/ (Q+Qr) =V/1000, RCR=Qr / Q=V / (1000-V)

(Suspended solid concentration = [1000(ml/lit) ×1000(mg/gm)] / SVI ml/gm

Mixed Liquor Dissolved Solids (MLDS), mg/l = [(W4-W3) (mg) ×1000ml/l]

Mixed Liquor Suspended Solids (MLSS) = MLTS – MLDS

SVI, ml/g = [V (ml/l) ×1000(mg/g)] / MLSS (mg/g)

Result and Conclusion:

Date of performance: Date of submission:

Temp Chloride Concentration in Water at 1 atm.

Variation of DO with salt Concentration:

Variation of DO with Altitude (Clean water )

Note: DO determined, at a particular place (Known altitude ) and at a specific

Action of Starch as an Indicator:

= X (ml) x N (mg/ml) x 8 x 1000 ml/l

Sample 1: DO, mg/l =

Sample 2: DO, mg/l =

Sample 3: DO, mg/l =

Sample 4: DO, mg/l =

Method of standardization using standard K2Cr2O7:

Then Na2S2O3 K2Cr2O7

Importance of Azide in alkali-iodine-Azide (Winkler’s azide modification):

N2O2 + ½O2 + H2O + 2Na2SO4 → 2NaNO2 + H2SO4