Experiment- 1

Aim- Measurement of Noise level

Procedure

Note: Make the measurements suggested below using A weighting and then C weighting. Record
all the data indicated by the Table headings below, including Source of Sound, Estimated
Distance from Meters, dB (A weighting), dB (C weighting), and your subjective judgments of
the loudness of the sounds (such as “very quiet”, “medium”, “loud”, “very loud”, etc.). Please
cover your ears for all sounds which could be potentially damaging.

Report: 1) Measure and record the sound pressure level (SPL) produced by the background
noise in the lab, along with the other data requested in the Table.

2) Measure and record the SPL produced when your lab partner screams at you as loudly as he or
she can. Try two or three difference distances from the sound level meter, e.g., 5 ft., 10 ft. and 15
ft. Note to the screamer: Do not scream so loudly that you damage your vocal folds! Note to the
listener: Cover your ears!

3) Measure and record the SPL produced when your lab partner speaks to you in a normal
fashion.

4) Measure and record the SPL produced by singing or playing various musical instruments (if
they are available) for two or three different distances from the sound level meter.

5) Have your partner try to sing (or play a musical instrument) a few notes in a scale (within an
octave) at what he or she considers to be the same loudness and record the actual sound levels
produced when this is attempted. (a) How large a variation typically occurs in the SPL from one
note to the next?

6) If anyone has a car parked nearby, it would be interesting to measure the SPL produced by
honking the horn, first when the sound level meter is relatively close to the horn, and then when
the meter is several feet away from the car.
7) Whistle as loudly as you can and measure the SPL (cover your ears).

8) Record the SPL in a place which you consider to be very quiet (possibly a room next door
where no one is present).

9) Turn up the volume of a stereo sound system (one will be set up in the lab) and record the SPL
produced under various conditions of your choice.

10) Measure the sound pressure levels produced by anything else which intrigues you. Use your
imagination, but keep in mind that you may look a bit suspicious walking around with a strange
instrument !!!!!Musical!Acoustics!Lab,!C.!Bertulani 4 taking readings now and then.

11) In general, what differences do you find between your measurements made with A and C
weighting? 12) Why do such differences exist? 13) Based upon the observations you have made
during this experiment, what types of situations have exposed your ears to the highest sound
levels during your life?

14) Do you think any of these situations were hazardous based upon the Table of Permissible
Noise Exposures?

Source of Sound Estimated SPL (dB) A SPL (dB) C Comments on

Distance from weighting weighting Subjective
Meter Loudness
 Experiment 2

Aim: Determine chloride ion concentration in a water sample.

Theory: Chloride in the form of chloride (Cl) ion is one of the major inorganic anions in water
and wastewater. The chloride concentration is higher in wastewater than in raw water because
sodium chloride is a common article of diet and passes unchanged through the digestive system
(Average estimate of excretion: 6 g of chlorides/person/day; additional chloride burden due to
human consumption on wastewater: 15 mg/L). Along the sea coast chloride may be present in
high concentration because of leakage of salt water into the sewage system. It also may be
increased by industrial process. In potable water, the salty taste produced by chloride
concentration is variable and depends on the chemical composition of water. Some waters
containing 250 mg/L Cl may have a detectable salty taste if sodium cation is present. On the
other hand, the typical salty taste may be absent in waters containing as much as 1000 mg/L
when the predominant cations are calcium and magnesium. In addition, a high chloride contents
may harm metallic pipes and structures as well as growing plants.

The measured chloride ions can be used to know salinity of different water sources. For brackish
water (or sea water or industrial brine solution), it is an important parameter and indicates the
extent of desalting of apparatus required. It also interferes with COD determination and thus it
requires a correction to be made on the basis of amount present or else a complexing agent, such
as HgSO4 can be added. Further, chloride ions are used as tracer ions in column studies to model
fate of different contaminants in soil and liquid media.
Procedure: The Mohr Method uses silver nitrate for titration (normality: 0.0141) (method
applicability: 0.15 to 10 mg/L chloride ions). This corresponds to 1 mL of 0.0141 equals to 1 mg
chloride in solution. The silver nitrate solution is standardized against standard chloride solution,
prepared from sodium chloride (NaCl). During the titration, chloride ion is precipitated as white
silver chloride (Eq.1): Ag+ +Cl<=>AgCl (Solubility product constant, Ksp=3×10-10) (1) the
indicator (potassium chromate) is added to visualize the endpoint, demonstrating presence of
excess silver ions. In the presence of excess silver ions, solubility product of silver chromate
exceeded and it forms a reddish-brown precipitate (Eq.2). This stage is taken as evidence that all
chloride ions have been consumed and only excess silver ions have reacted with chromate ions:
2Ag+ +CrO42-<=> Ag2CrO4 (Ksp=5×10-12) (1)

Apparatus: Burette, conical flask, pipette, measuring cylinder Reagents: Potassium chromate
indicator solution, standard silver nitrate titrant.

1. Take 25 ml sample in a conical flask. Measure sample pH.

2. Add 1.0ml indicator solution,

3. Titrate with standard silver nitrate solution to pinkish yellow end point and note down volume
of titrant used. Also measure sample pH.

4. Calculate chloride ion concentration using

Eq.(3): Chloride Ion Concentration (mg/L) = (A×N ×35.45)*1000 / Vsample (3) Where: A =
volume of titrant used, N is normality of silver nitrate (here we used N/71 or 0.0141 N), and
Vsample is volume of sample used (mL).

Result-The chloride ion Concentration of given sample is-------

 Experiment: 3

Solids Analysis (2540 D. Total Suspended Solids Dried at 103-105oC; 2540 E. Fixed and
Volatile Solids Ignited at 550oC)

Objective: To illustrate the various operations involved in gravimetric analysis and to

determine the various categories of solids that are commonly defined in water and
wastewater.

Background: Solids analysis provides one of the fundamental measurements used for control of
the activated sludge process and for the regulation of wastewater discharges. Gravimetric
analysis is based on the determination of constituents or categories of materials by measurement
of their weight. The experiment illustrates the principles of weighing and demonstrates
separation and categorization techniques used to define the various types of solids in waters and
wastewaters. These techniques involve three analytic operations in addition to weighing. These
are: filtration, evaporation, and combustion. Filtration is used to separate suspended or
particulate (nonfilterable) fraction from dissolved or soluble (filterable) fractions. Evaporation
separates water from material dissolved or suspended in it. Combustion differentiates between
organic and inorganic matter. Organic matter will be destroyed completely by burning at 550oC
for 30 min.

Procedure: Samples: (1) A turbid water 1. Weigh filters (mass=B g).

2. Filter samples (50 ml).

3. Run each sample in duplicates. You will have a total of 4 samples.

4. Oven dry at 103o C for 30 min (please note that standard methods recommend 1 hour). At this
stage all water will be evaporated and only suspended solids will be retained on filter. Weigh
filters now (mass =A g).

5. Calculate concentration of total suspended solids mg total suspended solids =1000*(A-B)/

(sample volume in mL) (1)

6. Weight crucibles (mass=C) and then weight crucible and filter (total mass=E).
7. Put crucibles with filter paper in muffle furnace and Ignite at 550o C for 15 min. At this stage
all volatile components of solids will be volatilized and only fixed inert solid materials will be
left in crucible. Weigh crucible after proper cooling (mass=D g).

8. Calculate concentration of volatile suspended solids (F) : mg volatile suspended solids/L

=1000*(E-D)/(sample volume in mL) (2)

9. Calculate concentration of fixed suspended solids (G) : mg volatile suspended solids/L

=1000*(D-C)/(sample volume in mL) Sample Questions to Answer: 1. Why solid determination
is important? 2. What do you expect about volatile and fixed suspended solids in drinking water
and in raw wastewater? Discuss using their solid characteristics.

Result- Total Suspended Solid of sample is---------------

Volatile Solid-----------
 Experiment 4

Objective: Determine DO content of a given sample

Background: Dissolved oxygen (DO) levels in environmental water depend on the

physiochemical and biochemical activities in water body and it is an important useful in
pollution and waste treatment process control. Two methods are commonly used to determine
DO concentration: (1) The iodometric method which is a titration-based method and depends on
oxidizing property of DO and (2) The membrane electrode procedure, which works based on the
rate of diffusion of molecular oxygen across a membrane. In the Iodometric method, divalent
manganese solution is added to the solution, followed by addition of strong alkali in a glass-
stopper bottle. DO rapidly oxidize an equivalent amount of the dispersed divalent manganese
hydroxide precipitates to hydroxides of higher valence states. In the presence of iodide ions in an
acidic solution, the oxidized manganese reverts to the divalent state, with the liberation of iodine
equivalent of the original DO content. The iodine is then titrated with a stranded solution of
thiosulfate. The titration end point can be detected visually with a starch indicator. Some
oxidizing and reducing agents present in solution can interfere with the iodometric method.
Oxidizing agents liberate iodine from iodides (positive interference) and some reducing agents
reduce iodine to iodide (negative interference). Also, organic matter present in solution can be
oxidized partially in the presence of oxidized manganese precipitate, thus causing negative
errors. Thus some modification of procedure is required.

Lab Procedure Method: The Azide Modification (For nitrite-N < 0.05 mg/L and Ferrous iron

The azide modification is used to minimize the effect of interfering materials. It removes
interference caused by nitrite which is most commonly found interference in biologically treated
effluents and in incubated BOD samples. Collection of Samples for DO Determination Samplers
are designed to ensure that air cannot enter into the sample. Most samplers are designed to retain
3-4 times the volume of samples which is required for analysis purposes. As oxygen values
change with time due to any biological activity, it is important to fix it in field immediately after
collection. This is done using reagents using in DO test and then the titration is done in
laboratory. This method gives low results for samples with high iodine demand and in this case it
is better to preserve sample using 0.7 mL concentrated sulfuric acid and 0.02 g sodium azide.
When this is doe it is necessary to add 3 mL of alkali-iodide reagent rather than the usual 2 mL
because of the extra acid the sample contains. Better results are also obtained if the sample is
fixed and stored in the dark and on the ice until the analyses are conducted. The final titration
should not be delayed more than 6 hours.

Apparatus: Incubation bottle 300mL volume; Air compressor

Procedure 6. Make dilution water by adding 2mL/L of following reagents in distilled water: a.
Phosphate buffer solution b. Magnesium sulfate solution c. Calcium chloride solution d. Ferric
chloride solution e. Sodium Sulfite solution 7. Take 300 mL sample in BOD bottle. Prepare two
sets of this sample. Keep one set for DO analysis for day 0 (i.e., Sample0Day) and another
sample in BOD incubator for 5 days at 20° C (Sample5Day) (this is how 5-day BOD experiment
is done). Here you will prepare duplicate samples and analyze at Day 0 (i.e., Sample0Day_A and
Sample0Day_B). 8. For a given sample bottle, add 1 mL of alkali azide and then 1 mL
manganous sulfate solution. Shake well the bottle and keep it open for 5 minutes to settle the
precipitate. Add 2 mL concentrated H2SO4 and place the cap on the bottle. Shake well the bottle
till all the precipitate is dissolved. 9. Take 203 mL of sample in conical flask and titrate with
standard sodium thiosulfate solution (0.025N) till the colour changes from dark yellow to light
yellow. Then add few drops of starch indicator and continue to titrate till the color of the solution
becomes either colorless or changes to its original sample colour. Note down volume of 0.025N
sodium thiosulfate consumed. 10. Calculate DO value of the sample. Remember that in 200 mL
sample, 1 mL of sodium thiosulfate of 0.025N equals to 1 mg/L dissolved oxygen: =>Dissolved
oxygen (DO) (in mg/L) = mL of sodium thiosulfate (0.025N) consumed.

Result- DO of give water sample---------

 Experiment No. 4

Objective: To determine BOD value for determining biodegradability of solution.

Background: The most widely used test indicating organic pollution of both wastewater and
surface water is the 5-day BOD (BOD5). This determination involves the measurement of the
dissolved oxygen used by microorganisms in the biochemical oxidation of organic matter. BOD5
is the total amount of oxygen consumed by microorganisms during the first five days of
biodegradation. Oxygen demand is associated with the biodegradation of the carbonaceous
portion of wastes and oxidation of nitrogen compounds such as ammonia. The following
equations simplify the process of biodegradation: Organic matter + O2 + microorganisms CO2
+ H2O + new microbial cells Ammonia + O2 + microorganisms NO3 + H2O + new microbial
cells

Apparatus: Incubation bottle 300mL volume; Air compressor, 20°C incubator Reagents for DO
measurement:

Steps:

DO measurement: 11. Make dilution water by adding 2mL/L of following reagents in distilled
water: a. Phosphate buffer solution b. Magnesium sulfate solution c. Calcium chloride solution d.
Ferric chloride solution e. Sodium Sulfite solution 12. For a given sample bottle, add 1 mL of
alkali azide and then 1 mL manganous sulfate solution. Shake well the bottle and keep it open for
5 minutes to settle the precipitate. Add 2 mL concentrated H2SO4 and place the cap on the
bottle. Shake well the bottle till all the precipitate is dissolved. 13. Take 203 mL of sample in
conical flask and titrate with standard sodium thiosulfate solution (0.025N) till the colour
changes from dark yellow to light yellow. Then add few drops of starch indicator and continue to
titrate till the color of the solution becomes either colorless or changes to its original sample
colour. Note down volume of 0.025N sodium thiosulfate consumed. 14. Calculate DO value of
the sample. Remember that in 200 mL sample, 1 mL of sodium thiosulfate of 0.025N equals to 1
mg/L dissolved oxygen: =>Dissolved oxygen (DO) (in mg/L) = mL of sodium thiosulfate
(0.025N) consumed.

BOD: 1. Prepare BOD dilutions. Use dilution water (it contains nutrients, the exact contents are
described in Standard Methods):Blank (only dilution water);5 mL sample in 300 mL BOD bottle, fill up
with dilution water;15 mL sample in 300 mL BOD bottle, fill up with dilution water;20 mL sample in 300
mL BOD bottle, fill up with dilution water 2. Take 300 mL sample in BOD bottle. Prepare two sets of this
sample. Keep one set for DO analysis for day 0 (i.e., Sample0Day) and another sample in BOD incubator
for 5 days at 20° C (Sample5Day). 3. Measure DO in different samples at t=0. 4. Incubate samples in 20oC
for 5 days. 5. Come back in the lab after 5 days and record dissolved oxygen. 6. Record data in following
manner.

Bottle no. Wastewater sample Initial DO (mg/L) DO at 5-day (mL)

(mL) (DO0) (DO5)

Calculate 5-day BOD value of the sample at 20°C: t-day BOD= [DOt-DO0]/(P) (1) where P=
Dilution factor = 300mL/(sample volume in mL)

Result- BOD of given water sample is ---------

 Experiment 5

Aim- To determine COD value for determining organic strength of solution

Background: Chemical oxygen demand (COD) is termed as the amount of a specific oxidizing
agent that reacts with sample under controlled conditions and it is expressed as oxygen
equivalence. This parameter indicates the extent of organic matter contamination of water and is
always higher than the biochemical oxygen demand (BOD). It is used to indicate organic matter
contamination and it helps in knowing overall organic load to the receiving body

Apparatus: Digestion vessels; block heater; microburet; ampule sealer. Borosilicate culture
tubes (16mm*100 mm or 20 mm*150mm) with TFE lined-screw caps are used. The block heater
is required to operate at 150±2°C with holes to accommodated digestion vessels. Do not use an
oven because of the possibility of leaking samples generating corrosive and explosive
atmosphere.

Reagents: a. Standard potassium dichromate digestion solution, 0.01667M: Add to about 500
mL distilled water 4.903 g K2Cr2O7, primary standard grade, previously dried at 150°C for 2 h,
167 mL conc. H2SO4, and 33.3 g HgSO4. Dissolve, cool to room temperature, and dilute to
1000 mL.b. Sulfuric acid reagent: c. Ferroin indicator solution: Dilute it by a factor of 5 as
required. This indicator is used to indicate change in oxidation-reduction potential of the
solution. d. Standard ferrous ammonium sulfate titrant (FAS), approximately 0.10M: Dissolve
39.2 g Fe(NH4)2(SO4)2.6H2O in distilled water. Add 20 mL conc H2SO4, cool, and dilute to
1000 mL. Standardize solution daily against standard K2Cr2O7 digestion solution as follows:
Pipet 5.00 mL digestion solution into a small beaker. Add 10 mL reagent water to substitute for
sample. Cool to room temperature. Add 1 to 2 drops diluted ferroin indicator and titrate with FAS
titrant. Molarity of FAS solution = [VK2Cr2O7 ×0.1] / (VFAS) (3) Where: VK2Cr2O7 = volume
of K2Cr2O7 (mL); VFAS = volume of FAS (mL)

Steps: 4. Wash culture tubes and caps with 20% H2SO4 before using to prevent contamination.
5. Place sample in culture tube or ampule and add digestion solution. Carefully run sulfuric acid
reagent down inside of vessel so an acid layer is formed under the sample-digestion solution
layer and tightly cap tubes or seal ampules, and invert each several times to mix completely. 6.
Place tubes or ampules in block digester preheated to 150°C and reflux for 2 h behind a
protective shield. CAUTION: These sealed vessels may be under pressure from gases generated
during digestion. Wear face and hand protection when handling and dangerous pressures will be
generated at 150°C. 7. Cool to room temperature and place vessels in test tube rack. Some
mercuric sulfate may precipitate out but this will not affect the analysis. 8. Remove culture tube
caps and add small TFE-covered magnetic stirring bar. If ampules are used, transfer contents to a
larger container for titrating. 9. Add 0.05 to 0.10 mL (1 to 2 drops) ferroin indicator and stir
rapidly on magnetic stirrer while titrating with standardized 0.10M FAS. The end point is a sharp
color change from blue-green to reddish brown, although the bluegreen may reappear within
minutes. In the same manner reflux and titrate a blank containing the reagents and a volume of
distilled water equal to that of the sample. 10. COD is given by

COD as mg/L O2/L = [(A-B)× M ×8000) / (Vsample) (4)

Where: A = volume of FAS used for blank (mL); B= volume of FAS used for sample (mL);
M=molarity of FAS; 8000= miliquivalent weight of oxygen ×1000 mL/L

Result- COD of given water sample-------------