ASHOKA INSTITUTE OF TECHNOLOGY AND MANGEMENT

RAJNANDGAON(C.G.)

LABORATORY MANUAL

ADVANCED ENVIRONMENTAL ENGINEERING

LAB

B. Tech-7TH SEM

(CIVIL ENGINEERING)

Subject Code: D020722 (020)

DEPARTMENT OF CIVIL ENGINEERING

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 INSTITUE VISION AND MISSION

Vision:
To excel in imparting quality technical education with ethical values.

Mission:

1. Provide state of the art infrastructure for holistic education and eco-friendly sustainable
research.
2. Create and motivate inclusivity for the benefit of society.
3. Collaborate with national and international organization for education and research
alignment.

DEPARTMENT VISION AND MISSION

Vision:
To be a school of eminence in knowledge sharing, research and in the field of Civil
Engineering.

Mission:

1. Provide quality technical education & research through appropriate pedagogy & state of
the art infrastructure.
2. Collaborate with industry and society for research, consultancy.
3. Nurture learner with soft skill through relevant training.

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 PROGRAM OUTCOMES (POs)
Engineering graduates will be able to:

1. Engineering knowledge: Apply the knowledge of mathematics, science, engineering

fundamentals, and an engineering specialization to the solution of complex engineering
problems.
2. Problem analysis: Identify, formulate, review research literature, and analyze complex
engineering problems reaching substantiated conclusions using first principles of mathematics,
natural sciences, and engineering sciences.
3. Design/development of solutions: Design solutions for complex engineering problems and
design system components or processes that meet the specified needs with appropriate
consideration for the public health and safety, and the cultural, societal, and environmental
considerations.
4. Conduct investigations of complex problems: Use research-based knowledge and research
methods including design of experiments, analysis and interpretation of data, and synthesis of
the information to provide valid conclusions.
5. Modern tool usage: Create, select, and apply appropriate techniques, resources, and modern
engineering and IT tools including prediction and modelling to complex engineering activities
with an understanding of the limitations.
6. The engineer and society: Apply reasoning informed by the contextual knowledge to assess
societal, health, safety, legal and cultural issues and the consequent responsibilities relevant to
the professional engineering practice.
7. Environment and sustainability: Understand the impact of the professional engineering
solutions in societal and environmental contexts, and demonstrate the knowledge of, and need
for sustainable development.
8. Ethics: Apply ethical principles and commit to professional ethics and responsibilities and
norms of the engineering practice.
9. Individual and team work: Function effectively as an individual, and as a member or leader
in diverse teams, and in multidisciplinary settings.
10. Communication: Communicate effectively on complex engineering activities with the
engineering community and with society at large, such as, being able to comprehend and write
effective reports and design documentation, make effective presentations, and give and receive
clear instructions.
11. Project management and finance: Demonstrate knowledge and understanding of the
engineering and management principles and apply these to one‘s own work, as a member and
leader in a team, to manage projects and in multidisciplinary environments.
12. Life-long learning: Recognize the need for, and have the preparation and ability to engage in
independent and life-long learning in the broadest context of technological change.

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 PROGRAM SPECIFIC OUTCOMES (PSOs)
PSO 1: Graduates will be able to qualify competitive examinations.

PROGRAMME EDUCATIONAL OBJECTIVES (PEOs)

The Programmed Educational Objectives of Department of Civil Engineering are given below:

PEO1: The graduate will have professional and technical career in inter disciplinary domains.
PEO2: Graduates will have effective communication, leadership, team building, problem solving,
decision making and creative skills.
PEO3: The graduate will practice ethical responsibilities towards their peers, employer and
society.

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 After the completion of this course students will be able to...

Course Code CO Statement Knowledge

Level

D020722(020).1 Examine different water quality parameters of sewage water 4

and Industrial waste water in the laboratory.
D020722(020).2 Relate significance of water quality parameter with society 3
sustainability.
D020722(020).3 Study and Determine various Air quality parameters of air 3
sampler

Course Outcomes Mapped with Program Outcomes & Program Specific Outcome:

PO1 PO2 PO3 PO4 PO5 PO6 PO7 PO8 PO9 PO10 PO11 PO12 PSO1

D020722(020).1 3 3 2 1 2 2 3 2 1 1 1 1 2

D020722(020).2 3 2 2 1 2 3 3 2 1 1 1 1 1

D020722(020).3 3 2 2 1 2 2 3 2 1 1 1 1 1

D020722(020) 3.00 2.33 2.00 1.00 2.00 2.00 3.00 2.00 1.00 1.00 1.00 1.00 1.33

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 INDEX

Date of Date of Teacher’s

S.No. Name of Experiment Grade Re-marks
Exp. submission sign
1. Determination of Fluoride content in Sewage /
Industrial wastewater.
2. Determination of Nitrates in Sewage /
Industrial wastewater.
3. Determination of Phosphates in Sewage /
Industrial wastewater.
4. Determination of Iron in Sewage / Industrial
wastewater.
5. Microbiological Examination of Sewage /
Industrial wastewater.
6. Study of Determination of MPN.

7. .Study and Report Making on Diary W/W

8. Study and Report Making on Textile Industry

W/W.
9. .Study and Report Making on Sugar Industry
W/W.

10. .Study of determination of particulates in air.

11. Study of Collection of particulate matter using

Air sampler
12. Study of air quality (SPM, Temperature).

13. Study of air samples for metals (using AA

spectrometer).

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 EXPERIMENT NO.-01

Aim:

Determination of Fluoride content in Sewage / Industrial wastewater.

Significance:

Fluoride levels are monitored in drinking water supplies to achieve the required safety. Absence
of fluoride and excessive quantities in water, both create problems. .Fluoride ion in traces in
drinking water helps in growth and development of healthy, resistant teethes and bones. It has been
scientifically established that 0.8-1.0mg/l of fluoride is essential in potable water. Consumption of
drinking water with an elevated level of fluoride leads to a chronic disease that manifests as dental
and skeletal fluorosis. WHO has established guideline value of 1.5 mgl-1 in drinking water based
on the health hazards estimates. Bureau of Indian Standards is 1.0mgl-1 as permissible and 1.5
mgl-1 as the maximum permissible limit. Prevention of fluorosis requires the screening of drinking
water. Moreover, knowledge of fluoride level in potable water is important for health-care
personnel and policymakers.

Theory:

Fluorides are analysed by a method that involves the bleaching of a preformed colour by fluoride
ions. The preformed colour is result of reaction of Zirconyl chloride octahydrate and SPADNS
dye. The colour produced is referred to as lake and the intensity of colour is reduced if Zirconium
present is reduced. Fluoride ions present in the sample reacts with the zirconium 48 dye to form
stable complex ZrF6 - . The dye becomes progressively lighter as fluoride concentration increases.
The bleaching action is the function of the fluoride ion concentration and is directly proportional
to it. Thus, Beer‘s law is satisfied and in and inverse manner.

Apparatus:

Spectrophotometer

Reagents:

Standard

fluoride solution 1ml=10µgF

Zirconyl- alizarin reagent

Mixed acid solution

Procedure:

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1. Prepare a series of standard by diluting various volume of standard fluoride solution to 100ml .
Prepare a range between 0 and 1.4 mg/l

2. To 50 ml of each standard add 10ml mixed acid Zirconyl SPADNS reagent

3. Set the spectrophotometer to a wavelength of 570nm. Adjust the spectrophotometer to zero

absorbance with reference solution i.e. distilled water with reagent.

4. Plot the concentration along x-axis and absorbance along y-axis to obtain a calibration curve. 5.
Repaet the process for the given water sample. 6. By referring the calibration curve, the
concentration for the observed absorbance is read out.

Observations:

Table 1: Observations for Calibration

S.No. Stock Fluoride Fluoride Absorbance

solution in ml

Table 2:

S.No. Sample Absorbance Fluoride in µg Fluoride in mg

from graph

Calculations:

F in mg/l = A x B/V x C

Where, A = µg F determined

B= sample diluted to this volume

C = portion taken for colour development

V = Volume of the sample

Results:

The fluoride content in the given water samples are ----

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 EXPERIMENT NO.-02
Aim:

Determination of Nitrates in Sewage / Industrial wastewater.

Apparatus:

UV Spectrophotometer, Sample Tubes, Spoon, 0.15 g, Pipets, 1.0 mL, Funnels.

Reagents:

Digestion Reagent Powder Deionized Water, Total Nitrogen Reagent A Powder, Total Nitrogen
Reagent B Tablets.

Theory:

Nitrogen is essential for plant growth, but the presence of excessive amounts in water supplies
presents a major pollution problem. Nitrogen compounds may enter water as nitrates or be
converted to nitrates from agricultural fertilizers, sewage, industrial and packing house wastes,
drainage from livestock feeding areas, farm manures and legumes. Nitrates in large amounts can
cause ―blue babies‖ (methemoglobinemia) in infants less than six months of age. Nitrate
concentration is an important factor to be considered in livestock products, where, in addition to
causing methemoglobinemia, it is responsible for many other problems. Nitrates in conjunction
with phosphate stimulate the growth of algae with all of the related difficulties associated with
excessive algae growth. Drinking Water Standards state that 10 ppm nitrate nitrogen should not be
exceeded. To the sanitary and industrial engineer, concentrations of less than 1 ppm are acceptable.

Principle:

All forms of nitrogen are converted to nitrate by an alkaline persulfate digestion. Interference from
halogen oxides is eliminated by the addition of sodium metabisulfite. Nitrate in acid reacts with
chromotropic acid to form a yellow color in proportion to the amount of nitrate in the t reated
sample.

Procedure:

Use universal sample holder

1. Preheat COD reactor to 100 ±2°C. Follow safety precautions.

2. Remove caps from two *Total Nitrogen Hydroxide Reagent Tubes (4040).

3. Use a 0.15 g spoon (0727) and a funnel (0459) to add one level measure of *Digestion Reagent
Powder (4036) to each tube. Tap funnel to dispense Powder completely

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4. Use a 1.0 mL pipet (0354) to add 2.0 mL of Deionized Water (5115PS), or organic-free water,
to one tube. This is the blank.

5. Use another 1.0 mL pipet (0354) to add 2.0 mL of sample to the other tube. This is the sample.

6. Cap both tubes and shake vigorously for 30 seconds.

7. Place the tubes in the COD reactor for 30 minutes.

8. After exactly 30 minutes, turn the reactor off. Carefully remove the tubes from the reactor and
allow them to cool to room temperature.

9. At the end of the cooling period, press ON button until spectrophotometer turns on.

10. Scroll to and select PROGRAMMED TESTS from the menu.

11. Scroll to and select ALL TESTS (or another sequence containing 62 Nitrogen T) from
PROGRAMMED TESTS menu.

12. Scroll to and select 62 Nitrogen T from the menu.

13. Carefully remove caps from the digested tubes.

14. Use a 0.15 g spoon (0727) and a funnel (0459) to add one level measure of *Total Nitrogen
Reagent A Powder (4041). Tap funnel to dispense powder completely. Cap the tubes and shake
for 15 seconds.

15. Wait 3 minutes.

16. Remove the caps from the tubes. Add one *Total Nitrogen Reagent B Tablet (4042A) to each
tube. Cap the tubes and shake for 45 seconds or until the tablet disintegrates.

17. Wait 2 minutes.

18. Remove the caps from the reacted tubes. Carefully remove the caps from two *Total Nitrogen
Acid Reagent Tubes (4043). CAUTION: Tubes contain a strong acid.

19. Use another 1.0 mL pipet (0354) to add 2 mL of digested treated blank to one Total Nitrogen
Acid Reagent Tube. This is the blank.

20. Use another 1.0 mL pipet (0354) to add 2 mL of digested treated sample to the other Total
Nitrogen Acid Reagent Tube. This is the sample.

21. Cap the tubes and invert 10 times to mix. CAUTION: The tubes will be hot. NOTE: Invert
slowly and completely for accurate results. Hold tubes with caps up. Invert the tube and wait for

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the air bubble to flow to the bottom of the tube. Turn the tube upright and wait for the air bubble
to return to the top of the tube. This is one inversion.

22. Wait 5 minutes.

23. Wipe the tubes with a damp towel to remove fingerprints and smudges. Wipe with a dry towel.

24. Insert the blank tube into the chamber. Select SCAN BLANK. Remove the Blank tube from
the spectrophotometer.

25. Insert the sample tube into the chamber. Select SCAN SAMPLE. Record the result as Total
Nitrogen in mg/L N.

26. Press OFF button to turn the spectrophotometer off or press EXIT button to exit to a previous
menu or make another menu selection.

NOTE: For greater accuracy, use laboratory grade pipets. To order reagent refills, order code R-
4026.

Result:

The quantity of Total Nitrogen present in the given sample is mg/L N

11
 EXPERIMENT NO.-03
Aim:
Determination of Phosphates in Sewage / Industrial wastewater.
Apparatus:
UV Spectrophotometer, Sample Tubes.
Reagents:
Digestion Reagent Powder, Total Phosphorus LR Hydroxide Reagent, Phosphate Acid Reagent,
Phosphate Reducing Reagent.
Theory:
Phosphorus in natural waters and wastewaters occurs almost exclusively in the form of
orthophosphates, condensed phosphates (pyro-, meta- and other polyphosphates) and organically
bound phosphates. Phosphates may be added in small amounts to water supplies during treatment.
Larger amounts are introduced to water used for cleaning or laundering as components of
commercial cleaning preparations. Phosphates are used to treat boiler water and are components
of agricultural and residential fertilizers. Phosphorus is an important nutrient for aquatic plants.
The amount found in natural water is generally not more than 0.1 mg/L unless the water has
become polluted from wastewater sources or excessive drainage from agricultural areas.
Principle:
Pretreatment of the sample with heat and acid provides conditions for the hydrolysis of condensed
inorganic phosphates. Heat, acid and persulfate convert the organic phosphates to orthophosphate
during the digestion. Ammonium molybdate and antimony potassium tartrate react in a filtered
acid medium with dilute solutions of phosphate to form an antimonyphosphomolybdate complex.
This complex is reduced to an intense blue colored complex by ascorbic acid. The color is
proportional to the amount of phosphate present.
Procedure:
Use universal sample holder
1. Preheat COD reactor to 150 ±2°C. Follow safety precautions.
2. Remove cap from a *Total Phosphorus Acid Reagent Tube (4035). Use a 1.0 mL pipet (0354)
to add 5.0 mL of sample.
3. Use the 0.15 g spoon (0727) and a funnel (0459) to add one level measure of *Digestion Reagent
Powder (4036). Tap funnel to dispense powder completely. Cap tube tightly and shake until
powder dissolves completely.
4. Place the tube in the COD reactor for 30 minutes
5. At the end of the heating period, turn the reactor off. Carefully remove the tube from the reactor
and allow it to cool to room temperature.
6. At the end of the cooling period, press ON button until spectrophotometer turns on. 7. Scroll to
and select PROGRAMMED TESTS from menu.
8. Scroll to and select ALL TESTS (or another sequence containing 82 Phosphorus T LR from
PROGRAMMED TESTS menu.

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9. Scroll to and select 82 Phosphorus T LR from the menu.
10. Carefully remove the caps from the digested tube. Use another 1 mL pipet (0354) to add 1.0
mL of *Total Phosphorus LR Hydroxide Reagent (4038) to the tube. Cap and invert to mix.
11. Wipe the vial with a damp towel to remove fingerprints and smudges. Wipe with a dry towel.
12. Insert the tube into the chamber. Select SCAN BLANK. Remove the tube from the
spectrophotometer.
13. Use another 1 mL pipet (0354) to add *1.0 mL of Phosphate Acid Reagent (V-6282). Cap and
invert tube to mix.
14. Use the 0.1g spoon (0699) and a funnel (0459) to add one level spoon of Phosphate Reducing
Reagent (V-6283). Tap funnel to dispense powder completely. Cap tube and shake until powder
dissolves.
15. Wait 5 minutes.
16. Wipe the tubes with a damp towel to remove fingerprints and smudges. Wipe with a dry towel.
17. Insert the tube into the chamber. Select SCAN SAMPLE. Record the result as Total
Phosphorus in mg/L PO4.
18. Press OFF button to turn the spectrophotometer off or press EXIT button to exit to a previous
menu or make another menu selection.
NOTE: For greater accuracy, use laboratory grade pipets.
Result:
The quantity of Total Phosphorus present in the given sample is mg/L PO4

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 EXPERIMENT NO.-04
Aim:
Determination of Iron in Sewage / Industrial wastewater.
Apparatus:
UV Spectrophotometer, Sample Tubes.

Reagents:
Acid Phenanthroline Indicator, Iron Reducing Reagent.

Theory:
Iron is usually present in natural water and is not objectionable, if concentration is less than
0.3 ppm. It may be in true solution in colloidal state that may be peptized by organic matter,
in the inorganic and organic iron complexes, or in relatively coarse suspended particles. It
may be ferrous or ferric, suspended or filterable. Iron exists in soils and minerals mainly as
insoluble ferric oxide and iron sulphide (pyrite). It occurs in some areas, also as ferrous
carbonate (siderite), which is very slightly soluble.

Principle:
The phenanthroline method is the preferred standard procedure for the measurement of iron
in water except when phosphate or heavy metal interferences are present. The method
depends upon the fact that 1, 10-phenanthroline combine with Fe++ to form an orange-red
complex. Its colour conforms to Beer‘s law and is readily measured by visual or photometric
comparison. Small concentration of iron can be most satisfactorily determined by
colorimetric analysis. It is also based on Beer‘s law. By measuring the intensities of
transmitted and incident light through a coloured solution and knowing its optical density or
transmission, we can prepare a calibration curve and subsequent concentration can be read.
Procedure:
Use universal sample holder.
1. Press and hold ON button until spectrophotometer turns on.
2. Scroll to and select PROGRAMMED TESTS.
3. Scroll to and select ALL TESTS (or another sequence containing53 Iron Phen) from
TESTING MENU.
4. Scroll to and select 53 Iron Phen from menu.
5. Rinse a clean tube (0290) with sample water. Fill to the 10 mL mark withsample.
6. Insert tube into chamber, close lid and select SCAN BLANK.
7. Remove the tube from Spectro. Remove the cap and add 6 drops of *AcidPhenanthroline
Indicator (2776). Cap and invert the tube 4 times to mix reagents. Wait five minutes for
maximum color development.

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8. After five minutes, mix, insert tube into chamber, close lid and select SCANSAMPLE.
Record result as ppm Ferrous Iron.
9. Remove tube from Spectro. Use the 0.1g spoon (0699) to add one measureof *Iron
Reducing Reagent (2777). Cap and invert 15-20 times to mix, wait 5minutes for maximum
color development.
10. After 5 minutes, mix insert tube into Spectro. Close lid and select SCANSAMPLE.
Record result as ppm Total Iron.
11. Press OFF button to turn spectrophotometer off or press EXIT button to exit toa previous
menu or make another menu selection.
12. Total Iron (ppm) - Ferrous Iron (ppm) = Ferric Iron (ppm)

NOTE: For best possible results, a reagent blank should be determined to account for any
contribution to the test result by the reagent system. To determine thereagent blank, follow
the above test procedure to scan distilled or deionizedwater blank. Then follow the above
procedure to perform the test on a distilled ordeionized water sample. This test result is the
reagent blank. Subtract the reagentblank from all subsequent test results of unknown
samples. It is necessary todetermine the reagent blank only when a new lot number of
reagents is obtained.

Result:
1. The quantity of ferrous iron present in the given sample is ppm.
2. The quantity of Total Iron present in the given sample is ppm.
3. The quantity of Ferric Iron present in the given sample is ppm.

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 EXPERIMENT NO.-05
AIM:

Microbiological Examination of Sewage / Industrial wastewater.

THEORY:

Wastewater treatment is a complicated and costly process. This is in large part due to the enormous
amount of wastewater produced globally every day. As modern wastewater treatment plants need
to reduce pollutants to an ever lower level and do so at a lower cost, many have started to look for
alternatives to the commonly used treatment processes. Photobioreactors are bioreactors
specifically designed to grow photosynthetic organisms like algae. While their main use has been
biomass production, they are also being investigated for use in wastewater treatment, due to the
ability of microalgae to take up nutrients from water. Compared to photobioreactors growing a
single species of algae, algal systems for wastewater treatment contain a consortia of different
microbes as wastewater itself contains a large variety of different microorganisms In monoculture
cultivation this would be considered contamination, however it can be beneficial for wastewater
treatment as the microbial processes are more robust in terms of the metabolic pathways in the
system. Muñoz and Guieysse have also pointed out that mixed consortium photobioreactors have
a higher capacity for producing biomass than pure cultures, which could be useful for production
of biodiesel or biogas to offset the energy requirements of the process. Because biotechnological
systems rely on microbial communities to achieve their goals, there is a growing need to
understand the interactions between algal and bacterial communities to enhance the available
technologies and to create new ones .In the past few years several studies have provided valuable
insights into the communities in multi-species photobioreactors using molecular methods For
example the microbiome of a municipal wastewater treating photobioreactor prototype, revealing
the key species present. Similarlyanalysed the metagenome of algae associated biofilms and
described some of the bacterial-algal interactions found.

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Fig.1 Experimental wastewater treating photobioreactor system combining microalgae with the
activated sludge process in Västerås wastewater treatment plant, Sweden.

METHODOLOGY:

Wastewater and lake water origin and properties The plant is designed to treat sewage from 118
000 population equivalents. The inflowing raw wastewater is screened, pre-precipitated with iron
sulphate and biologically treated with activated sludge process. Glycol is added to the water to
support predenitrification. Samples were taken from the top layer in the centre of the mixed basin
after some of the original phosphorous was removed.
Lake water, used to add algae to the photobioreactor system, was sampled from a yacht harbour
near the WWTP from the upper layer (0.5 m) of Lake Mälaren, the third largest lake in Sweden
(Kvarnäs, 2001). Sampling was done following the SS/ISO 5667-3:2004 standard with sterilised
equipment and samples were immediately transported to a refrigerator at 4°C.

EXPERIMENTAL SETUP:
To test the ability of algae grow in wastewater an initial proof of concept experiment was set up
with 250 mL flasks. Lake- and wastewater ratios of 30/70, 50/50 and 70/30 were tested and
compared to pure lake- and wastewater samples (Fig. 5a). The flasks were shaken manually every
24 hours and algal growth was measured. The 70/30 Wastewater/lake water mixture showed the
most growth, and thus this mixture was used in subsequent experiments. To further test the effect
of lake water inoculation, reactors with a volume of 1 L were used (Fig. 5b). Four separate reactors
were set up in modified fermenters consisting of glass cylinders with stainless steel tops and
bottoms.
The reactors were set up with four different conditions:
1. A tap water reactor (TWR) containing 30% tap water and 70% Wastewater,
2. A lake water reactor (LWR) containing 30% lake water and 70% Wastewater and
3. A wastewater reactor (WWR) containing 100% wastewater.
As a control a sterilized wastewater reactor (SWR) was set up to test for contamination.
The experiments were conducted on three separate occasions with similar conditions to test
whether the season when lake water was sampled had an effect on algal growth in the
photobioreactor – one in August, one in November and one in December (Paper I). A similar setup

17
was also used to study the effect of nitrification inhibition on the growth of microalgae (Paper II).
The experimental plan was however modified such that all 4 reactors contained 30% lake water
pre-grown for 1 week at 23°C and 70% wastewater. The algae were grown in the lake water before
the experiment to increase the amount of algae in the water prior to mixing wastewater. Two of
the reactors had only WW and LW for normal operation while the other two had 0.05 g of
allylthiourea (ATU) added to inhibit nitrification.

Algal community composition and growth dynamics

In the proof of concept experiments conducted in 250 ml flasks to study algal inoculation of
wastewater with lake water, optical density (OD) at 630 nm was used as an indicator of algal
growth. Due to the complex nature of the wastewater samples this proved to be a poor indicator of
true algae growth. As a result subsequent experiments used chlorophyll a concentration
measurements to get a better indication of algal growth.The algae present in the reactors were
visually examined using an Alphaphot-2 YS2 at 150x magnification.

Figure 5. 250 ml flasks used in the proof of concept experiments (a), 1L photobioreactors used in the
experiments studying the effect of lake water inoculation and nitrification inhibition on algal growth
(b) and 20L photobioreactors designed and built to study the bacterial and algal community and
functional genes in lake water inoculated and uninoculated reactors(c).

RESULT AND DISCUSSION:

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 EXPERIMENT NO.-06
Aim:

Study of Determination of MPN.

Methodology:

Bacteriological Analysis - Multiple Tube Fermentation Technique.

Apparatus:

Autoclave, BOD incubator, Durham‘s tubes, Borosilglasswares etc.

Reagents:

Mackonkey broth solution

Theory:

The Most Probable Number (MPN) technique is an important technique in estimating microbial
populations in soils, waters, and agricultural products. The methodology for the MPN technique
is dilution and incubation of replicated cultures across several serial dilution steps. MPN is the
number, which indicates the bacteria density, which is most likely to be present in water. The MPN
is based on the application of laws of statics to the results of test and is, therefore more accurate
than Coliform Index (CI) method.

The MPN index of coliform micro-organism for potable water shall be less than 1 in 100 ml of
water sample as per BIS: 10500-1991. There are many advantages of using the MPN technique.
MPN methodology results in more uniform recovery of a microbial population. Furthermore, the
detection of organisms through process-related attributes often results in the recovery of mixed
populations with similar functional roles in soils. For a more detailed study, the mixed populations
can be separated into individual colonies. Another advantage of MPN techniques is that, unlike
direct quantitative procedures, it measures only live and active organisms. Microscopic techniques
sometimes confuse live and dead cells. Despite the numerous advantages of using MPN
methodology there are a few disadvantages to the method.

MPN procedures tend to require more labor and materials than microscopic procedures. Also,
MPN estimates often have a lower order of precision than do well-replicated direct counts. There
are two techniques to find most probable number of confirmed microorganisms in a water sample.
They are

(a) multiple tube fermentation technique and

(b) membrane filter technique.

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Multiple tube fermentation technique is more useful than membrane filter technique because of its
applicability to almost all kinds of waters.

Procedure:

1) Wash thoroughly and sterilize all the glasswares before use.

2) Prepare the Broth solution of both double strength (DS) & single strength (SS) as per the
specifications
3) Arrange the series of 10.0, 1.0 & 0.1 ml combination. (05 test tubes for each combination).
4) Place 10 ml broth (DS) solution in each of first 05 test tubes, 10 ml (SS) solution in remaining
10 test tubes.
5) Drop Durham‘s tube (inverted) in each test tube and plug the test tube with cotton.
6) Again sterilize the solution and other glasswares.
7) Add 10 ml representative sample in each of the first 05 (DS) tubes, 1.0 ml sample in second 5
(SS) tubes and 0.1 ml sample in remaining 5 (SS) tubes and plug the test tube with cotton.
8) Incubate the tubes for initial 24 hours for preliminary observation of +ve tubes and another 24
20C.hours for confirmative observation at about 35
9) Note down the +ve test tubes from each combination and refer the MPN table for the final value.
10) If the combination is not matching with the table, use the following formula,

Calculation:

Result:

1. Total Coliform MPN/100ml

20
 EXPERIMENT NO.-07
Aim:

Study and Report Making on Diary W/W.

Theory:

Due to highly biodegradable nature of dairy wastewater its treatment requires urgent
attention but as such treatment is not a big issue. Biological treatment technologies can
readily treat the dairy wastewater. The final effluent can be readily used for irrigation and
sludge itself becomes a good fertilizer. If waste is disposed in water bodies or ground BOD
becomes the major concern. It may lead to anaerobic conditions and related problems. The
BOD is in a range of 1000 to 2000 mg/L (1) obviously, Biologic threatening is required for
it. The Biological treatment may be Activated sludge process, Trickling filter, aerated
lagoon or oxidation pond. However anaerobic process is also found to be successful. Dairy
waste water is an area, already quite exposed.
Pretreatments
Equalization
Neutralization
Separation / Clarification
Secondary Treatments Biological
Methods Activated
sludge process Aerobic
process
Oxidation ditch / trickling filters
Rotating biological discs
Anaerobic digestion
Procedure:

The industry collects the milk and pasturieses it first. The various processes held in
The dairy are discussed below:
1. Pasteurization
2. Powderisation
3. Butter making
4. Ghee making
5. Cheese making
6. Preparation of whole milk and skimmed milk.

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Observation:

Sr.no. Characteristics Unit Value

1. BOD5 @ 20 0C mg/1
2. COD mg/1
3. pH --
4. Total solid mg/1
5. Total dissolved solid mg/1
6. Total suspended solid mg/1
7. Total fixed solid mg/1
8. Total volatile solid mg/1
9. Dissolved fixed solid mg/1
10. Alkalinity mg/1
Table 1: Characteristics of composites waste water

Sr.no. Characteristics Unit Value

1. BOD5 @ 20 0C mg/1
2. COD mg/1
3. pH --
4. Total solid mg/1
5. Total dissolved solid mg/1
6. Total suspended solid mg/1
7. Total fixed solid mg/1
8. Total volatile solid mg/1
9. Dissolved fixed solid mg/1
10. Alkalinity mg/1
Table2: Characteristics of treated effluent

22
Conclusion:

REFERENCES
[1] .Banes D. Forster, Hrudey S.E. Survey Industrial WasteWater Treatment, Vol. 1 : Food & Allied
Industries.
[2]. Course manual Industrial waste treatment proposed byNEERI and CPHEEO, 1975.
[3]. I.E. 2490-1982 Indian Standards for Industrial andSewage Effluent Discharge.
[4]. LS. 8682-1983 Indian Standards for Dairy Wastewater.

23
 EXPERIMENT NO.-08
AIM:

Study and Report Making on Textile Industry W/W

INTRODUCTION:

The word textile comes from the Latin word ‗texere‘ which means to weave. Textiles can be woven
by both hand and machines. The textile industries are classified on the basis of the types of textile
fiber they use. The raw materials for textiles are natural and synthetic fibres. The textile raw
materials can be classified into three main categories: cellulose fibres (cotton, rayon, linen etc),
protein fibres (wool, silk etc) and synthetic fibres (polyester, nylon, acrylic etc). Cellulose fibers
are obtained from plant sources such as cotton, rayon, linen, ramie, hemp and lyocell Protein fibers
are obtained from animals and include wool, angora, mohair, cashmere and silk. Artificially
synthesized fibres include polyester, nylon, spandex, acetate, acrylic, ingeo and polypropylene.
However, the most of the textiles are produced from cotton liners, petrochemicals and wood pulp.

MATERIALS AND METHODS:

Characterization and Composition of textile wastewater

The different manufacturing steps in Textile industry, such as desizing, mercerization, bleaching,
neutralization, dyeing, printing and finishing have been discharging the following Colour.

A major contribution to colour in textile wastewater is usually the dyeing and the washing
operation after dyeing which as much as 50% of the dye might be released into the effluents
.Textile dyes are mainly cationic, anionic and non-ionic dyes.

TDS and TSS

Total dissolved solids (TDS) is a measure of the combined content of all inorganic and organic,
substances contained in a liquid in molecular, ionized or micro-granular (colloidal sol) suspended
form. TDS is used as an indication of aesthetic characteristics of drinking water and as an aggregate
indicator of the presence of a broad array of chemical contaminants. TSS is solid materials,
including organic and inorganic, that are suspended in the water. TDS are difficult to be treated
with conventional treatment systems. Disposal of high TDS bearing effluents can lead to increase
in TDS of ground water and surface water. TSS in effluent may also be harmful to vegetation and
restrict its use for agricultural purpose.

Toxic Metals
Waste water of textiles is not free from metal contents. There are mainly two sources of metals.
Firstly, the metals may come as impurity with the chemicals used during processing such as caustic
soda, sodium carbonate and salts. Secondly, the source of metal could be dye stuffs like metallised
mordent dyes.
The metal complex dyes are mostly based on chromium. A number of metals including cadmium,
chromium, copper, iron, lead, mercury, nickel and zinc. Many metals, which are usually only

24
available naturally in trace quantities in the environment, can be toxic to humans, plants, fish and
other aquatic life. Sulphur and Sulphide Textile dyeing uses large quantities of sodium sulphate
and some other sulphur containing chemicals. Textile wastewaters will therefore contain various
sulphur compounds and once in the environment sulphate is easily converted to sulphide when
oxygen has been removed by the BOD of the effluents

Oil and Grease

This includes all oils, fats and waxes, such as kerosene and lubricating oils. Oil and grease causes
unpleasant films on open water bodies and negatively affect aquatic life. They can also interfere
with biological treatment processes and cause maintenance problems as they coat the surfaces of
components of ETPs.

Residual Chlorine
The use of chlorine compounds in textile processing, residual chlorine is found in the waste stream.
The waste water (if disposed without treatment) depletes dissolved oxygen in the receiving water
body and as such aquatic life gets affected. Residual chlorine may also react with other compounds
in the waste water stream to form toxic substances.

pH
pH is a measure of the concentration of hydrogen ions in the wastewater and gives an indication
of how acid or alkaline the wastewater is. This parameter is important because aquatic life such as
most fish can only survive in a narrow pH range between roughly pH 6-9.

BOD and COD

Biochemical oxygen demand ( BOD) is defined as the amount of dissolved oxygen needed by
aerobic biological organisms in a body of water to break down organic material present in a given
water sample at certain temperature (20oC) over a specific time period (5-day). BOD can be used
as a gauge of the effectiveness of wastewater treatment plants. COD is a measure of the oxygen
equivalent of the organic material chemically oxidised in the reaction and is determined by adding
dichromate in an acid solution of the wastewater.

Textile effluent treatment processes

Many pollutant removal technological processes have been developed in the past decades to treat
the textile wastewater. The treatment processes is being chosen on the basis of composition,
characteristics and concentration of material present in the effluents. These processes are pre-
treatment or preliminary, primary or physicochemical, secondary, tertiary treatment or combined
treatment processes depending on type, sequence and method of removal of the harmful and
unacceptable constituents. Most commonly used processes are being discussed below:

Pre-treatment processes or preliminary treatment prior to textile dyeing, the fabric must be clean
& clear of all impurities. It should be free from dust particles and colouring materials. In order to

25
obtain a white pure fabric, the fabric undergoes a series of cleaning steps covered in Pre-treatment.
The process of fabric treatment prior to dyeing or printing in order to achieve a clean fabric is
known as pre-treatment. The basic aim of the pre-treatment is to prepare the fabric for dyeing and
printing which gives the best result in respect to economy and quality. It is assumed that 70%
dyeing & printing faults are coming from the pre-treatment. Natural fibers and synthetic fibers
contain primary impurities that are contained naturally, and secondary impurities that are added
during spinning, knitting and weaving processes.

The most conventional treatment processes in textile wastewater treatment is the removal of
suspended solids, excessive quantities of oil and grease and gritty materials. The coarse
suspended materials such as yarns, lint, pieces of fabrics, fibres and rags is being removed
from the effluent by using bar and fine screens. The screened effluent then undergoes settling
for the removal of the suspended particles. The floating particles are removed by mechanical
scraping systems. Neutralization is done to reduce the acidic contents of the effluents.
Sulphuric acid and boiler flue gas are the most commonly used chemicals to alter the pH. A
pH value of 5-9 is considered ideal for the treatment process. The common primary
treatment processes are shown as follows.

Equalization

Effluent treatment plants are usually designed to treat wastewater that has a more or less
constant flow and a quality that only fluctuates within a narrow margin. The equalization
tank overcomes this by collecting and storing the waste, allowing it to mix and become a
regular quality before it pumped to the treatment units at a constant rate.

Floatation

The floatation produces a large number of micro- bubbles in order to form the three-
phase substances of water, gas, and solid. Dissolved air under pressure may be added to
cause the formation of tiny bubbles which will attach to particles. Under the effect of
interfacial tension, buoyancy of bubble rising, hydrostatic pressure and variety of other
forces, the microbubble adheres to the tiny fibres. Due to its low density, the mixtures
float to the surface so that the oil particles are separated from the water. So, this method
can effectively remove the fibers in wastewater.

26
Coagulation flocculation sedimentation

Coagulation flocculation sedimentation is a physical process which involves slow mixing of

the effluent with paddles bringing the small particles together to form heavier particles that
can be settled and removed as sludge Active on suspended matter, colloidal type of very small
size, their electrical charge give repulsion and prevent their aggregation. Adding in water
electrolytic products such as aluminium sulphate, ferric sulphate, ferric chloride, giving
hydrolysable metallic ions or organic hydrolysable polymers (polyelectrolyte) can eliminate
the surface electrical charges of the colloids. This effect is named coagulation. Normally the
colloids bring negative charges so the coagulants are usually inorganic or organic cationic
coagulants (with positive charge in water). The metallic hydroxides and the organic polymers,
besides giving the coagulation, can help the particle aggregation into flocks, thereby
increasing the sedimentation. The combined action of coagulation, flocculation and settling
is named clariflocculation. Settling needs stillness and flow velocity, so these three processes
need different reactions tanks. This processes use mechanical separation among
heterogeneous matters, while the dissolved matter is not well removed (clariflocculation can
eliminate a part of it by absorption into the flocks). The dissolved matter can be better
removed by biological or by other physical chemical processes But additional chemical load
on the effluent (which normally increases salt concentration) increases the sludge production
and leads to the uncompleted dye removal.

Adsorption

The adsorption process is used to removes colour and other soluble organic pollutants from
effluent. The process also removes toxic chemicals such as pesticides, phenols, cyanides and
organic dyes that cannot be treated by conventional treatment methods. Dissolved organics
are adsorbed on surface as waste water containing these is made to pass through adsorbent.
Most commonly used adsorbent for treatment is activated carbon. It is manufactured from
carbonaceous material such as wood, coal, petroleum products etc. A char is made by burning
the material in the absence of air.

The char is then oxidized at higher temperatures to create a porous solid mass which has
large surface area per unit mass. The pores need to be large enough for soluble organic

27
compounds to diffuse in order to reach the abundant surface area.

The activated carbon once it is saturated needs replacement or regeneration.

Regeneration can be done chemically or thermally. The chemical regeneration can be
done in within the column itself either with acid or other oxidizing chemicals. This
normally effects partial recovery of activity and necessitate frequent recharging of
carbon. For thermal regeneration, the exhausted carbon is transported preferable in
water slurry to regeneration unit where it is dewatered and fed to furnace and heated in
a controlled conditions. This process volatilize and oxidize the impurities held in carbon.
The hot reactivated carbon is then quenched with water and moved back to the site. This
results in almost complete restoration of its adsorption. There are some other materials
such as activated clay, silica, flyash, etc are also known to be promising adsorbents.

Secondary Treatment

The Secondary treatment process is mainly carried out to reduce the BOD, phenol and
oil contents in the wastewater and to control its colour. This can be biologically done
with the help of microorganisms under aerobic or anaerobic conditions. Aerobic
Bacteria use organic matter as a source of energy and nutrients. They oxidize dissolved
organic matter to CO2 and water and degrade nitrogenous organic matter into ammonia.
Aerated lagoons, trickling filter and activated sludge systems are among the aerobic
system used in the secondary treatment. Anaerobic treatment is mainly used to stabilize
the generated sludge.

28
Fig. Secondary treatment Processes.

Aerated lagoons are one of the commonly used biological treatment processes. This
consists of a large holding tank lined with rubber or polythene and the effluent from the
primary treatment is aerated for about 2-6 days and the formed sludge is removed.

The BOD removal efficiency is up to 99% and the phosphorous removal is 15-25% . The
nitrification of ammonia is also found to occur in aerated lagoons. Additional TSS removal
can be achieved by the presence of algae in the lagoon (EPA, 2002). The major disadvantage
of this technique is the large amount of space it occupies and the risk of bacterial
contamination in the lagoons.

29
Trickling filters are another common method of secondary treatment that mostly operates
under aerobic conditions. The effluent for the primary treatment is trickled or sprayed over
the filter. The filter usually consists of a rectangular or circular bed of coal, gravel, Poly Vinyl
Chloride (PVC), broken stones or synthetic resins). A gelatinous film, made up of
microorganisms, is formed on the surface of the filter medium. These organisms help in the
oxidation of organic matter in the effluent to carbon dioxide and water . Trickling filters do
not require a huge space, hence making them advantageous compared to aerated lagoons.
However, their disadvantage is the high capital cost and odour emission.

Aerobic activated sludge processes are commonly used. It involves a regular aeration of
the effluent inside a tank allowing the aerobic bacteria to metabolize the soluble and
suspended organic matters. A part of the organic matter is oxidized into CO2 and the
rest are synthesized into new microbial cells (NESC, 2003). The effluent and the sludge
generated from this process are separated using sedimentation; some of the sludge is
returned to the tank as a source of microbes. A BOD removal efficiency of 90-95% can
be achieved from this process, but is time consuming (Yasui et al., 1996). Sludge‘s
formed as a result of primary and secondary treatment processes pose a major disposal
problem. They cause environmental problems when released untreated as they consist
of microbes and organic substances (Wright, 2013). Treatment of sludge is carried out
both, aerobically and anaerobically by bacteria. Aerobic treatment involves the presence
of air and aerobic bacteria which convert the sludge into carbon dioxide biomass and
water. Anaerobic treatment involves the absence of air and the presence of anaerobic
bacteria, which degrade the sludge into biomass, methane and carbon dioxide (Mittal,
2011).

Tertiary Treatment or Advance methods treatment Textile effluents may require tertiary
or advance treatment methods to remove particular contaminant or to prepare the treated
effluent for reuse. There are several technologies used in tertiary treatments includ ing
electrodialysis, reverse osmosis and ion exchange. Electrolytic precipitation of textile
effluents is the process of passing electric current through the textile effluent using
electrodes.

As a result of electro chemical reactions, the dissolved metal ions combine with finely
dispersed particles in the solution, forming heavier metal ions that precipitate and can
be removed later. One of the disadvantages is that a high contact time is required
between the cathode and the effluent.

30
 Fig. 1. A flow diagram for various steps involved in processing textile in a cotton mills.

Biochemical and physicochemical combination processes

In recent years a large number of difficult biodegradable organic matter such as PVA slurry,
surface active agents and new additives enter into the dyeing wastewater, which result in the
high concentration of the organic matter, complex and changeable composition and the
obvious reduction of the biodegradability. The CODCr removal rate of the simple aerobic
activated sludge process which was used to treat the textile dyeing wastewater has decreased
from 70% to 50%, and the effluent cannot meet the discharge standards. More seriously,
quite a number of sewage treatment facilities can‘t normally operate even stop running.
Therefore, the biochemical and physicochemical combination processes has been gradually
developed and its application is increasingly widespread

31
Fig.. Components of conventional physico-chemical treatment.

Fig. Components of conventional physico-chemical treatment.

Membrane separation process

Membrane separation process is the method that uses the membrane‘s microspores to
filter and makes use of membrane‘s selective permeability to separate certain substances
in wastewater. Currently, the membrane separation process is often used for treatment
of dyeing wastewater mainly based on membrane pressure, such as reverse osmosis,
ultrafiltration, nanofiltration and microfiltration. Membrane separation process is a new
separation technology, with high separation efficiency, low energy consumption, easy
operation, no pollution and so on. However, this technology is still not large-scale
promoted because it has the limitation of requiring special equipment, and having high

32
 investment and the membrane fouling and so on.

RESULT AND DISCUSSION:

33
 EXPERIMENT NO.-09
AIM:

Study and Report Making on Sugar Industry W/W.

MANUFACTURING PROCESS:-

These are two categories of sugar manufacturing process. (i) Carbonation process. (ii) Solicitation
process.
Most of the sugar factories in India follows double sulphitation process and produce plantation
white sugar.
The mover unit operations are
(i) Milling (ii) Clarification (iii) Evaporation (iv) Crystallization (v) Centrifugation

(i) Milling—The cane received in the factory yard is fed to the cannier by mechanical un loader
from tracks and trailers while the cane carts are manually emptied. The cane is passed through
preparatory devices like knives for cutting the stalks in to fine chips before being subjected to
crushing in a milling tandems comprising 4 to 6 there roller mills. Fine preparation with its impact
on final extraction is receiving special attention and shredder and particularly the fiberizes are
gaining popularity. The mills are of modern design, being equipped with turbine drive special
feeding devices, efficient compound inbition system etc. In the best milling practice more than
95% of the sugar in the cane goes in to the juice this percentage being called the sucrose effraction
or more simply the extraction. A fibrous residue called bagasse with a low sucrose content is
produced about 25 to 30% of cane, which contains 45 to 55% moisture. This bagasse usually goes
to the boiler as fuel and many factories use the bagasse for wallboard or paper manufacture, cattle
feeding or other commercial by product utilization.

(ii) Clarification—The dark green juice form the mills is acidic (PH-4.5) and turbid, called raw
juice or mixed juice. The clarification process, designed to remove both so luble and insoluble
impurities, universally employs lime and heat as the deriving agents. The mixed juice after being
heated to 65 to 750C is treated with phosphoric acid, sulphur dioxide and milk of lime for removal
of impurities in suspension in a continuously working apparatus. The Sulphur dioxide is generated
by combustion of sulphur, while lime is either produced in kiln from lime stone or brought as such
and stored in a separated house. The treated juice on boiling fed to continuous clarifier from which
the clear juice is decanted while the settled impurities known as mud is sent to rotary drum vacuum
filter for removed of un watered stuff called process mud is discarded or returned to the fields as
fertilizer. The clear juice goes to the evaporators without further treatment.

(iii) Evaporation -The clarified juice having much the same composition as the mixed juice,
except for the precipitated impurities, removed by the clarification process contains about 85%
coater. About 75% of this water is evaporated in vacuum Multiple effects consisting of a

34
succeeding (Generally four) of vacuum boiling cells arranges in series so that each succeeding
body has higher therefore boils at a lower temperature. The vapors from one body can thus boil
the juice in the next one by this system the steam introduced in on the first body does multiple
evaporation. The vapours from the final body goes to condenser. The syrup levees the last body
continuously with about 60% solids and 40% water.

(iv) Crystallization—The syrup is again treated with sulphur dioxide before being sent to the pan
station for crystallization of sugar. Crystallization takes place in single effect vaccum pan, where
the syrup is evaporated until saturated with sugar. At this point ―Seed grain‖ is added to serve as a
nucleus for the sugar crystals and more syrup is added as water evaporates. The growth of crystals
continue until the pan is full given is skilled sugar boiler (or adequate instrumentation) the original
crystals can be growing without the formation of additional crystals, so that when the pan is just
full, the crystals, are all of desired size and the crystals and syrup or a dense mass known as
―masticate‖. The ―strike‖ is then discharged through a foot valve in to a crystallizer.

(v) Centrifugation— The masticate from crystallizer is drawn into revolving machines called
centrifuges. The cylindrical ―basket‖ suspend on a ―spindle‖ was perforated sides lined with wire
cloth, inside of which are metal, steels containing 400 to 600 perforations per square inch. The
basket revolves at speed from 1000 to 1800 spm. The perforated lining retain the sugar crystals,
which may be washed with water, if desired. The mother Liquor ―molasses‖ passes through the
lining because of the centrifugal force exerted and after the sugar is ―purged‖ if is cut down leaving
the centrifuge ready for another charge of masticated. Modern installations are executive of, the
high speed type with automation control for the whole cycle. Low grades may be purged by
continues centrifuges. The mother liquor separated from commercial sugar is again sent to pan for
boiling and re crystallization. Three stage of recrystallization are adopted to ensure maximum
recovery of sugar in crystal form. The final mother liquor to as final molasses is sent out the factory
as waste being unsuitable for recovery of sugar under commercial conditions from economical
point of view. Final molasses used as a base for cattle feed in the manufacture of industrial alcohol,
in yeast production etc.

WATER BALANCE:

Sources
(1) Water comes from outside such as river, canals, well, dam bore well etc.
(2) Water comes along with sugarcane.
Use—The water utilized in the sugar industry can be classified in to two categories.
(1) External Water (Cold Water)—The external water does not generally come in contact with the
sugar does not generally come in contact with the sugar manufacturing process directly. The
external water such as cooling water used for condensing and cooling power turbines, mill
turbines, mill bearings, crystallizes sulfur burners, air compressors, vacuum pumps, hot liquor
pumps etc. and water used for floor washing, vessel washing and domestic use.

35
(2) Internal Water—The internal water such us the water from the cane itself imbibition water,
clarification water, boiling water and purging water which is directly involved in the sugar
manufacturing process. Clean cane containing about 70% water, wherefore the water coming from
the cane itself is a primary source for sugar manufacturing process. The water from cane itself in
the form of condensate is more than sufficient for the internal process of sugar manufacturing such
as condensate water used for imbibition, boiler, filter, cake washing, milk of lime preparation
movement water at pans, molasses, dilutions, centrifugal, melting etc.

SOURCES OF EFFLUENTS:

The waste water generated from different sub streams can be classified as follows—
(1) Mill House—The effluent consists of water used for cleaning the mill house floor which is
liable to be converted by spills and pleased sugar juice (This clearing up operation will prevent
growth of bacteria on the juice-covered floor).Water used for cooling of mills also forms part of
the waste water from this source. Basically this water contains organic matter like sucrose,
bagacillo, oil and grease from the bearings fitted in to the mills.
(2) Waste Water from Boiling House—The waste water from boiling house results from leakages
through pumps, pipelines and the washings of various section such as evaporators, juice heaters,
clarification, pans crystal is action, and centrifugation etc. The cooling water from various pumps
also forms part of water.
(3) Waste Water from Boiler Blow-down— The water used in boiler contains suspended solids
dissolved solids like calcium salts, magnesium salts, sodium salts, fatty salts etc. These salts get
concentrated after generation stream from the original water volume. These solids have to be
expelled time to time to save the boiler being covered up by scales.
(4) Excess Condensate—The excess condensate does not normally contain any pollutant and is
used as boiler feed water and the washing operations. Sometimes it gets contaminated with juice
due to entertainment of carry over of solids with the vapours being condensed in that case if goes
in to the waste water drain. The treatment requirement in this case is almost negligible and can
replace fresh water or let out directly as irrigation water after cooling it to ambient temperature.
(5) Condenser cooling water—Condenser cooling water is recirculated again unless it gets
contaminated with juice, which is possible due to defective entrainment separators, faulty
operation beyond the design rate of evaporation etc. if gets contaminated, the water should go into
the drain invisibly. This volume of water is also increased by additional condensing of vapour of
trained from the boiling juice the pan.
(6) Soda and Acid Wastes— The heat exchangers and evaporator are cleaned with caustic soda
and hydrochloric acid in order to remove the formation of the deposits of scales on the surface of
the tubing. In India, most of the sugar factories let this valuable chemical go into drains. The soda
and acid wash contribute considerable amounts of organic and inorganic pollutions and may cause
shock loads to waste water treatment once in a fortnight or so.

36
VOLUME OF EFFLUENT:
Volume of effluent use from mill to mill depending on the crushing capacity of mill and reliability
and management of water conductor of plant machinery etc.
Characteristics of Effluents
The characteristics of individual and combined effluents very from mill to mill and from time to
time. All the individual effluents excluding spray pond overflow are acidic and coloured posters
disagreeable older, high BOD and suspended solid. The oil and grease content is also high. The
characteristics of effluents of a typical sugar mill

EFFECTS OF EFFLUENTS:

37
 EXPERIMENT NO.-10
AIM:

Study of determination of particulates in air.

INSTRUMENTS

a. High volume sampler (HVS)

b. Whatman filter paper

c. Impingers

PRINCIPLE

PM10 and TSPM are measured by passing air at flow rate of about 1 lpm through high efficiency
cyclone which retains the dust particles greater than 10 micron size and allow only fines (less than
10 micron particles) to reach the glass microfibre filter where these particles are retained. The
instrument provides instantaneous flow rate and the period of operation (on- time) for calculation
of air volume passed through the filter. Amount of particulates collected is determined by
measuring the change in weight of the cyclone cup and filter paper.

REAGENTS FOR GASEOUS POLLUTANTS

a. 0.1 N Sodium tetra-chloratemercurate (SO2)

b. Sodium hydroxide and sodium arsanite (NO2)

PROCEDURE

i. For particulates

a. Perform leak check of the instrument before starting the sample.

b. Filter paper need to be inspected for pin holes.

c. Filter conditioning need to be done at 20-25oC temperature and less than 50% Relative

Humidity.

d. Never fold filter completely.

e. Do not touch filters by dirty hands always use disposable hand gloves.

f. Under take regular cleaning of key components of the machine.

g. Ensure stable power supply to the machine. Do not leave loose contact of supply wire to

38
the machine.

h. Always fill up distilled water in manometer assembly.

i. Do not switch on and off machine using Timer Switch.

j. Clean impinge and rotameter regularly and also clean manifold once in two months.

k. Do not take flow reading immediately after switching on the machine. Give 5 minute for

flow stabilization and for heat up the blower components.

l. Always attach a new weighed cyclone cup with every filter change.

m. Do not switch on machine without filter paper.

n. If machine is not expected to be operated within 48 hrs drain out the manometer water and store
machine with water in the manometer tank.

o. Do not run machine during rain in open atmosphere.

ii. For gaseous

The increasing general awareness of atmospheric pollution and its hazards to the health and well-
being of industrial workers, educational buildings, offices etc., is bound to result in greater stress
on accurate, reliable and frequent assessment of work place pollution and worker-exposure. Use
additionally impinge tray with HVS sampler simultaneously sample gaseous pollutants.

CALCULATION FOR PARTICULATES

a. Initial Manometer Reading =

b. Final Manometer Reading =

c. Initial Filter Paper Weight =

d. Final Filter Paper Weight =

e. Initial Cyclone Cup Weight =

f. Final Cyclone Cup Weight =

g. Total Suspended Particulate Matter Concentration =

REFERENCES

a. CPCB (2011), Guidelines for the Measurement of Ambient Air Pollutants, Volume-1, Delhi.

39
b. IS 5182 Part 2 Method of measurement of air pollution: Sulphur dioxide.

c. IS 5182 (Part 6)-2006: Indian standards, Method of measurement of air pollution: Nitrogen
dioxide.

d. IS 5182 (Part 14)-2000 (reaffirmed 2005): Indian standards, Method of measurement of air
pollution: Guidelines for planning the sampling for atmosphere.

e. Rao, M.N., and Rao, H.V.N., Air pollution. Tata McGraw-Hill Publishing Co. Ltd., New Delhi
1989.

40
 EXPERIMENT NO.-11
AIM:

Study of Collection of particulate matter using Air sampler

INSTRUMENT

Environmental dust monitor with weather house (automatic sampler) for PM10, PM2.5 and
PM1.0.

WORKING PRINCIPLE

The dust particles are measured by the physical principle of orthogonal light scattering. Here
particles are illuminated by a laser light in an angle of 90 degree. All units of environmental dust
monitor use light-scattering technology for single-particle counts. The scattered signal from the
particle passing through the laser beam is collected at approximately 90° by a mirror and
transferred to a recipient-diode. The signal of the diode is feed, after a corresponding
reinforcement, to a multi-channel size classifier. This pulse height analyzer then classifies the
signal high of each channel. These counts of each channel are converted each minute in a mass
distribution from which the different PM values derive. Measurement principle

SAMPLING LOCATION GUIDELINES

Sampling location should be located depending upon the objective of measurement campaign and
be kept at an altitude depending upon the type of study region (roadways, industrial area, disposal
sites, residential area, etc). Generally it is kept at a height of about 3m to 10m from the ground
level and sufficiently away from the disturbance of direct obstacles from the source under
consideration.

SAMPLING FREQUENCY GUIDELINES

Sampling is carried out for various purposes. The regular monitoring campaign of national ambient
air quality includes measurement of particulate matter typically for 24 hours at least twice a week
making about 104 samples a year.

STEPS FOR SAMPLING

a. Prepare a sampling assembly.

41
b. Set the time constant depending upon the required averaging period.

c. Instrument can be switch on and it will display concentration values in μg/m3

d. Simultaneously instrument will start recording the concentration values in the memory card.

REFERENCES

a. CPCB (2011), Guidelines for the Measurement of Ambient Air Pollutants, Volume-1, Delhi.

b. IS 5182 (part 23), 2006, Indian standards – Methods for measurement of air pollution, Part-23
– Respirable suspended particulate matter (PM10), cyclonic technique.

c. GRIMM, environmental dust monitor (model 1.107) manual.

d. IS 5182 (Part 14)-2000 (reaffirmed 2005) : Indian standards, Method of measurement of air
pollution: Guidelines for planning the sampling for atmosphere.

e. Rao, M.N., and Rao, H.V.N., Air pollution. Tata McGraw-Hill Publishing Co. Ltd., New Delhi
1989.

42
 EXPERIMENT NO.-12
AIM:

Study of air quality (SPM, Temperature).

APPARATUS:

Indoor air quality monitor (automatic sampler) for carbon monoxide (CO), carbon dioxide

(CO2), temperature and humidity.

INDOOR AIR QUALITY MONITOR:

With 90% of our time spent indoors, determining the quality of the air we breathe indoors is essential
for good health and productivity. The IAQ monitor key indoor air quality indicators including CO2,
humidity, temperature and CO. Should these measurements fall outside recognized guidelines; further
tests can be made to suggest an appropriate course of action. For example, ventilation studies show
that as room temperatures rise above 75°F(24°C) the ability of occupants to concentrate can drop by
up to 50% and high levels of carbon dioxide will indicate poor ventilation that results in drowsiness
and perceived stuffiness. Both situations are very common and seriously affect productivity. Over-
ventilation wastes energy and results in increased building running costs. The Surveyor range has been
designed with the user in mind. Minimal training is required to use the instruments as the intuitive
menu system and display provide step-by-step guides for each operation that are updated when smart
probes are plugged in.

STEPS FOR SAMPLING:

a. Prepare a sampling assembly.

b. Set the time constant depending upon the required averaging period.

c. Instrument can be switch on and it will display concentration.

d. Simultaneously instrument will start recording the concentration values in the memory card.

e. Using data transfer cable (ie. RS232 cable) can download data from instrument to personal
computers.

REFERENCES

a. AQ-5000, indoor air quality monitor manual, QUEST technology, USA.

43
 EXPERIMENT NO.-13
AIM:

Study of air samples for metals (using AA spectrometer).

APPARATUS:

Glassware
[Note: All glassware should be Class A borosilicate glass and should be cleaned with laboratory
detergent, rinsed, soaked for 4 hr in a 20% (w/w) HNO3, and rinsed several times with distilled
water.]

 Beakers. Borosilicate glass, including 30 mL, 125 mL, 150 mL Phillips or Griffin.
 Volumetric flasks. 10 mL, 100 mL, 1 L.
 Pipettes. Volumetric, including 1, 2, 4, 8, 15, 30, 50 mL.
 Additional glassware. As required depending on dilution required to obtain
concentrations above the detection limit, in the response range.

SUMMARY OF METHOD :

1 Collection of Sample
 Particulate matter from ambient air may be collected on glass fiber filters using a high-
volume sampler. The high-volume sampler must be capable of sampling at an
average flow rate of 1.70 m3/min (60 ft3/min).Constant air flow is maintained by
a mass flow controller over a 24-hr period.
 Air is drawn into a covered housing and through a filter by means of a high-flow rate
blower at a flow rate [1.13 to 1.70 m3/min. (40 to 60 ft3/min)] that allows suspended
particles having diameters <100 µm (Stokesequivalent diameter) to pass to the filter
surface. Particles 100-0.1 µm diameter are ordinarily collected on glass fiber filters.
The mass concentration (µg/m3 ) of suspended particulates in the ambient air is
computed by measuring the mass of collected particulates and the volume of air
sampled. After the mass is measured, thefilter is ready for extraction to determine
metal concentration.

2 Sample Extraction
 Samples collected on glass fiber filters may be extracted by either hot acid procedure
or by microwaveextraction (see Method IO-3.1).
 The preferred method of extraction is by microwave extraction. In operation, a 1"
x 8" strip is cut from the 8" x 10" filter as described in the Federal Reference Method
for Lead. The metals are extracted from the filter strip by a hydrochloric/nitric acid
solution using a laboratory microwave digestion system. After cooling, the
digestate is mixed and filtered with Acrodisc syringe filters to remove any insoluble
material.

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 3 Sample Analysis

 The trace element concentrations in each sample are determined by atomic absorption
spectrometry. This technique operates by measuring energy changes in the atomic
state of the analyte. The sample is vaporized and dissociates into its elements in the
gaseous state. The element being measured is aspirated into a flame or injected into
a graphite furnace and atomized. The atoms in the unionized or "ground" state absorb
energy, become excited, and advance to a higher energy level.
 A light beam containing the corresponding wavelength of the energy required to raise
the atoms of theanalyte from the ground state to the excited state is directed through
the flame or furnace. This wavelength is observed by a monochromator and a detector
that measures the amount of light absorbed by the element, hencethe number of atoms
in the ground state in the flame or furnace. A hollow cathode or electrode less
dischargelamp for the element being determined provides a source of that metal's
particular absorption wavelength.
 The data output from the spectrometer can be recorded on a strip chart recorder
or processed by computer. Determination of metal concentrations is performed from
prepared calibration curves or read directly from the instrument.

ANALYSIS EQUIPMENT:

 Atomic Absorption Spectrometer. Equipped with air/acetylene and nitrous

oxide/acetylene burner heads or graphite furnace.
 Hollow cathode or electrode less discharge lamp. For each element to be
determined.
 Acetylene gas and regulator. Cylinder of acetylene equipped with two gauge, two
stage pressurereducing regulator with hose connections.
 Nitrous oxide gas and regulator. Cylinder of nitrous oxide equipped with 2 two
gauge, two-stagepressure reducing regulator with hose connections.
 Heating tape and rheostat. May be required to heat second stage of nitrous oxide
gas cylinderregulator and hose to prevent freeze-up of line.
 Air supply. Clean, dry compressed air with a two-stage regulator.
 Parafilm M sealing film. A pliable, self-sealing, moisture-proof, thermoplastic
sheet material,substantially colorless is recommended for use in sealing the acidified
sample beakers. Commercially available Parafilm M satisfies this requirement.
Reagents:
Nitric Acid (HNO3) Concentrated. ACS reagent grade HNO3 and commercially
available redistilledHNO3 which have sufficiently low metal concentrations.
Hydrochloric Acid (HCl) Concentrated. ACS reagent grade.
Water. ASTM Type I (ASTM D193) or equivalent. The same source or batch of
distilled, deionizedwater must be used for all purposes in the analysis.

45
ANALYSIS:

Receiving of Sample From Extraction Laboratory

 The sample should be received by the atomic absorption spectroscopist in a centrifuge

tube from the extraction procedure outlined in Method IO-3.1.

[Note: The entire extract volume of filter digestate was not received from
extraction laboratory. The totalvolume should have been 20 mL ± 0.5 mL, but
only 10 mL may have been sent for analysis.]

 The solution may be analyzed directly for any elements of very low concentration
in the sample.Aliquots of this solution may be then diluted to an appropriate volume
for the other elements of interest present at higher concentrations.
 Filter blanks must be subject to the entire extraction and analytical procedure and
processed asdescribed.
 Some relatively rare chemical forms of some of the elements listed in Table 2 may
not be dissolved by the procedures stated in this method. If such chemical forms are
suspected, results of their procedure shouldbe compared to results of a non-destructive
technique, which does not require sample dissolution, such as X-ray fluorescence.
 Because of the differences between makes and models of atomic absorption
spectrometers, formulating detailed instructions applicable to every instrument is
difficult. Consequently, the user should follow manufacturer's operating
instructions.
1. Flame Procedure

 Set the atomic absorption spectrometer for the standard conditions as follows:
choose the correcthollow cathode lamp or electrode less discharge lamp, install,
and align in the instrument; position the monochromator at the value recommended
by the manufacturer; select the proper monochromator slit width; set the light source
current according to the manufacturer's recommendation; light the flame and
regulate theflow of fuel and oxidant; adjust the burner for maximum absorption
and stability; and balance the meter.
 If using a chart recorder, set the chart speed at 8-15 cm/min and turn on the power,
servo, and chart drive switches. Adjust the chart pen to the 5% division line. Also
adjust instrument span using highest calibration standard. While aspirating the
standard sample, span instrument to desired response.
 Run a series of standards of the metal of interest and construct a calibration curve as
in Section 11.3. Set the curve corrector of a direct reading instrument to read the
proper concentration.
 To evaluate the contribution to the absorbance from the filters and reagents used,
blank samplesmust be analyzed. Usually blanks will be provided with each set of
samples (see Section 9.2). Subject the blank to the entire analysis procedure. The

46
 absorbance obtained from the aspiration of the blank solution issubtracted from
the sample absorbance.
 The sample can be analyzed from the centrifuge tube or an appropriate amount of
sample decanted into a sample analysis tube. At least the minimum sample volume
required by the instrument should be available for each aspiration.
 Aspirate samples, standards, and blank into the flame and record the absorbance.
Aspirate distilled water after each sample or standard. If using a recorder, wait for
response to stabilize before recording absorbance.
 To the extent possible, all determinations should be based on replicate analyses.
 Determine the average absorbance value for each known concentration and correct
all absorbance values by subtracting the blank absorbance value. Determine the metal
concentration in Fg metal/mL from the calibration curve as by direct reading from
the instrument.
Dilute samples that exceed the calibration range by taking an aliquot of the sample and
diluting the sample to a known volume with a solution of the same acid
concentration and ionization and chemical suppressants as the calibration
standards and reanalyzed.
Check for drift of the zero point resulting from possible nebulizer clogging,
especially whendealing with samples of low absorbance.
Aspirate a mid-range standard with sufficient frequency (once every 10 samples,
after every 5 full MSAs or every 2 hr) to verify the continuing accuracy of the
calibration curve.
2. Furnace Procedure
 In graphite furnace atomic absorption, only a few microliters of the sample are placed
in the furnace. Within seconds or fractions of a second, the sample is atomized.
Graphite furnace analysis is more sensitivefor trace element determination than the
flame detection limit because it requires a smaller sample volume. Asa general rule,
samples that can be analyzed by flame or furnace may be more conveniently run with
flame since flame atomic absorption is faster, simpler, and has fewer interference
problems.
 When some samples are atomized, they may absorb or scatter light causing sample
absorbance to be greater than it should be, necessitating background correction. If
some sample remains unburned, memory effects can occur. Blank burns should be
run, and the graphite furnace should be cleaned by running at full power at
intervals during determination series.
 Inject a measured µL aliquot of sample into the furnace and atomize. If the
concentration found is greater than the highest standard, the sample should be diluted
in the same acid matrix and reanalyzed. Multiple injections can improve accuracy
and help detect furnace pipetting errors.
 Run a mid level check standard and a blank standard after every 10 sample
injections, after 5 full MSAs, or at 2-hr intervals. Standards are run in part to
monitor the life and performance of the graphite tube.Lack of reproducibility or
significant change in the signal for the standard indicates that the tube should be
replaced. Tube life depends on sample matrix and atomization temperature. A

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 conservative estimate of tube life is about 50 firings. A pyrolytic coating will
extend that estimated life by a factor of three.
 To determine the metal concentration by direct aspiration and furnace, read the metal
value in µg/L from the calibration curve or directly from the read-out of the
instrument.
 If sample dilution was required, calculate the final concentration using the

following formula:µg/L metal in sample = A x (C + B) / C

2.2 where:
 A = µg/L of metal in diluted aliquot from
calibration curve.B = Acid blank matrix
used for dilution, mL.
 C = Sample aliquot, mL.
3. Method of Standard Procedure:

 If chemical interferences are suspected, the method of standard additions may be used
to evaluate them; and if deemed desirable, the method may be used to make an
accurate determination of metal concentration in the presence of an interference.
 Take three identical portions from a sample. Dilute the first portion to a known
volume with the solvent used in the standard solutions. Add known but different
amounts of the metal of interest to the second and third portions. The additions and
dilutions should be kept as small as possible by using micro liter pipets.
 Aspirate each portion and measure the absorbance. Plot the absorbance values (Y-
axis) against metalconcentration (X-axis). Consider the first portion concentration
to be 0 and that of the others as the knownamount added to each. Draw the curve
through these points; it should be a straight line. The metal concentration in the
unknown is measured as the distance from the origin along the X-axis in the
negativedirection using the same concentration scale factor.
 Compare the values obtained for the same samples by direct comparison to the
calibration curve.If the values are the same, no chemical interferences are present,
and subsequent analyses can be made by direct comparison to the standard
working curve.
 If the slope of the spiked sample curve is not parallel to the original calibration curve,
an interferencemay be present. Standard additions may allow metal concentration
to be determined in the presence of interference by using the standard addition
curve as the calibration. This method can give incorrect values ifthe interferant
does not associate with the additions to the same extent as in the original analyte.

CALCULATIONS:

Determination of background concentration of metals in filter:

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 1.1 Use glass fiber filters to collect particulate matter with the high volume sampler.
High quality filters with reproducible properties must be used in sampling for
metals in ambient air. Analyze 5% of the total numberof filters for the presence
of specific metals, prior to sample collection, to verify reproducibility and low
background metal concentrations.
1.2 Cut one 1" x 8" strip from each filter. Extract and analyze all strips separately,
according to the directions given as delineated in Inorganic Compendium Method
IO-3.1.

1.3 Calculate the total metal in each filter as:

Fb = µg metal/mL x (20 mL/strip) x (9)

where:
Fb = Amount of metal per 72 square inches of filter, µg.

µg metal/mL = metal concentration

determined from Section 11.2.20 mL/strip =
total sample volume from extraction
procedure.
9 = 464.52 cm2/51.61 cm2.

1.4 Calculate the mean, Fm, of the values and the relative standard deviation (standard
deviation/mean x 100). If the relative standard deviation is high enough so that, in
the analyst's opinion, subtraction of Fm may resultin a significant error in the µg
metal/m3, the batch should be rejected.

1.5 For acceptable metal/batches, use the value of F m to correct all

metal/analyses of particulate matter collected using that batch of filters. If the
analyses are below the method detection limit (MDL) from Table 1, no correction is
necessary.

a. Sample Air Volume

At standard temperature and pressure (stp) [25EC and 760 mm Hg] for sample air
volume rotameter, use the following equation:

Vstd = [(Qi + Qf) / 2] t

where:
Vstd = air volume sampled, m3.
Qi = initial air flow
rate, m3/min at stp.Qf

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 = final air flow rate,
m3/min at stp.
t = sampling period (elapsed time), min.

For samplers equipped with flow recorders:

V = (Q) (t)

where:
Q = average sampling rate, m3/min at stp.

Metal Concentration
1 Estimation of Metal of Interest Concentration of the Blank Filter. For testing
large batches of filters (>500 filters), select at random 20 to 30 filters from a given
batch. For small batches (<500 filters) alesser number of filters may be taken. Cut
a 2.5 x 20.3 cm (1" x 8") strip from each filter. Analyze all stripsseparately.
2 Calculate total metal of interest in each filter as:

Fbi = (µg metal/mL) x (final extraction volume [i.e., 20 mL]/strip) x (9)

Where:
Fbi = amount of metal per 465 square cm (72 square
in.) of blank filter, µg.µg metal/mL = metal concentration
determined from Section 11.2.
Final extract volume (mL)/strip = total sample extraction volume from extraction procedure
(i.e., 20 mL).
9 = 464.52 cm2/51.61 cm2.

3 Calculate the mean, Fm, and the relative standard deviation (100 x

standard deviation/mean). Fm = E Fbi

/n

Where:
Fm = average amount of metal per
72 in.2 of filter, µgFbi = amount
of metal per 72 in.2 for each filter,
µg
n = number of blank filters analyzed.

4 The standard deviation (SD) of the analyses for the blank filters is given by

50
 equation

SD = [E (Fbi - Fm)2 / n - 1]½

The relative standard deviation (RSD) is given by the following equation:

RSD = (100) (SD) / Fm

If the relative standard deviation is high enough so that in the analyst's opinion
subtraction of Fm the mean mayresult in a significant error in the µg metal/m3, the
batch should be rejected. For acceptable batches, use thevalue of Fm to correct all
analyses (see Section 12.2.3) collected using that batch of filters. If Fm is below the
lower detectable limit (LDL), no correction is necessary.
5 Calculation of Metal of Interest Concentration of the Exposed Filter.
Metal concentration in the air sample can be calculated from data tabulated on data
record form as follows:

C = [(µg metal/mL x (final extraction volume [i.e., 20 mL]/strip)(9) - F m]/ Vstd

Where:
C = concentration, µg metal/std. m3.
µg metal/mL = metal concentration determined from Section 10.
Final extract volume (mL)/strip = total sample extraction volume from extraction
procedure (i.e., 20 mL),
9=
_____[_U__s_e_a__b_l_e__f_i_l_te__r__a_r_e_a_,__2_ 0_ __c_m
___x___2_3__c__m___(_8_"__x
___9_"_)_]________________
[Exposed area of one strip, 2.5 cm x 20 cm (1" x 8")]
Fm = average concentration of
blank filters, Fg. Vstd = air
volume pulled through filter,
std. m3.

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END OF LAB MANUAL
52