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1.

0 Introduction

First of all, as for environmental laboratory we had been given a task to come out with
proposal before begin all the lab’s experiment. The objectives of this lab is to analyse the
water quality of selected water resources according to Malaysia Water Quality Index (WQI)
and to determine the suitable application of the water resources. Besides, it is also to identify
the class of the certain area chosen whether it is suitable for any human activities or not.

As a group 3, we had discuss and agreed that we will do the experiment by taking a
sample from FKAAS’s lake. Generally, we can see that this area is one of the favourite area
for fishing activities. In addition, they have a lots of lotus flowers planted in this lake. So, by
conducting the lab experiment from this area’s water sample we are able to know the class of
water and automatically can identify whether it is suitable or safe for fishing activities and
also planting lotus flowers or not in that area.

Moreover, biochemical oxygen demand (BOD, also called biological oxygen demand)
is the amount of dissolved oxygen needed (i.e. demanded) by aerobic biological organisms to
break down organic material present in a given water sample at certain temperature over a
specific time period. The BOD value is most commonly expressed in milligrams of oxygen
consumed per litre of sample during 5 days of incubation at 20 °C and is often used as a
surrogate of the degree of organic pollution of water.
2.0 Methodology

2.1 Sampling Procedure (According To APHA Standard Or Any Related Standard)

1) Find any location that we are going to conduct an experiment, by taking a water sample
and also consider about human activities around the area.

2) Find polyethylene bottle and wash it using acid nitrate for 1 night or we also just can wash
it 3 times by using the water at the location of sample that need to be taken.

3) Bring 1 litre polyethylene bottle to the location chosen.

4) Then, take the sample as needed (1 litre) by using the bottle.

2.2 On-Site Measurement (According To APHA Standard Any Related Standard)

1. Before taking a sample of water, make sure that we are not taking a sample with bubble.

2. In order to avoid or reduce the bubble, we need to take the water's sample slowly.

3. Make sure that the amount of sample water should be enough to conduct all of the
experiment test in lab.

4. Next, bring the sample of water into the lab.

5. Then, continue with the lab experiment by using the sample water taken.
2.3 Laboratory Procedure (According To APHA Standard Any Related Standard)

2.3.1 Experiment 1: Chemical Oxygen Demand (COD)


1. Add substances to the round bottom flask (labeled as Blank (B) and Sample (S):

BLANK SAMPLE

BLANK (B) SAMPLE (S)


1) 20 ml distilled water 1) 20 ml water sample
2) 10ml potassium dichromate 2) 10ml potassium
K2C2O7 dichromate K2C2O7
3) 30ml Sulfuric acid reagent 3) 30ml Sulfuric acid reagent
(H2SO4 + Ag2SO4 (H2SO4 + Ag2SO4

2. Reflux /Boil the mixture for 2 hours (chemical digestion)


C (Organic matter) + Cr2O72- H+ CO2 + H2O + Cr3+

Cr6+
6+
* Oxidizing agent ,Cr
3+
is reduced to Cr
during digestion
* Organic matter are oxidized by
oxidizing agent.

COD Open Reflux Unit


 At a meantime prepare for standard ferrous ammonium sulfate (FAS) titrant.
a). Add substances into the conical flask

1.90 ml distilled water


2. 10ml potassium dichromate K2C2O7
3. 30ml Concentrated Sulfuric acid reagent
(H2SO4 )

b). Cool the solution to room temperature.


c). Titrate solution with ferrous ammonium sulfate (FAS)

 TITARTION
a) Jot down first reading of burette.
b) b. Titrate FAS until the color change from blue – green to reddish brown
c) Stop titration.
d) Jot down last reading.

Compute the Normality (N) for the FAS standard using formula given :

3. After 2 hours, disconnect reflux condenser.


4. Transfer the solution to the cone flask and dilute the mixture up to 150 mL with distilled
water.
5. Cool the solution to room temperature.
6. Add with 3 drops of ferroin indicator.
7. Place the magnetic bars and stir it with magnetic stirrer.
8. Titrate K2Cr2O7 with ferrous ammonium sulfate (FAS)

Compute the COD concentration in mg/L for the samples using formula given :

2.3.2 Experiment 2: Biochemical Oxygen Demand (BOD)


1. Label separately 6 unit of 300 mL BOD bottle as followed:

BLANK 1
BLANK2
BLANK3
SAMPLE1
SAMPLE2
SAMPLE3

BOD bottle

2. Measure out the proper volume of sample size and into BOD bottle.
3. Completely fill the BOD bottle with dilution water.
4. For BLANK bottle, completely fill the bottle with only dilution water.
5. Measure the initial DO for each bottles using DO meter.
Dilution water DO meter

6. Insert the bottle cap.


7. Place the bottles in the incubator at 20oc and incubate for 5days @ 30oc for 3 days.
8. Measure final DO (for triplicate samples) and get the average.

Di = initial DO
Df = final DO
Vs = sample volume
Vb = sample bottle volume, 300m
3 or 5 days
2.3.3 Experiment 3: Total Suspended Solid

1. Total Solid Determination

2. Total Suspended Solid Determination


3. Total Dissolved Solid Determination
4. Total Volatile Solid Determination

2.3.4 Experiment 4: Jar Test


1. Prepare the wastewater sample
2. Measure temperature, pH and turbidity of water sample
3. Add 1 - 5 ml of coagulant (alum/ferrous sulfate) by using a measuring pipette into beaker
1,2,3,4 and 5 while in beaker 6, no alum was added as it acts as a control sample.
 JAR TEST 1: Set up the variation of coagulant dose at selected pH (shown in
Table 1 lab sheet)
 JAR TEST 2: Set up the variation of coagulant dose at a fixed pH=6 (shown in
Table 2 in lab sheet)
4. Measure the pH and turbidity of each beaker by using pH and turbidity meter.
5. Start stirring rapidly (60 to 80 rpm) for 3 minutes.
6. Reduce the speed (30 rpm) for about 20 minutes.
7. Observe the flocculation process and record the floc formation in final 10 minutes by
referring to the chart of particle sizes provided as in lab sheet.
8. After the stirring period is over, stop the stirrer and allow the flocs to settle for about 5
minutes.
9. Separate out 500 mL of settled water into another beaker.
10. Determine the temperature, pH and turbidity of the clarified water.
 Please record the qualitative characteristics of flocs as bad, moderate, good and
very good.
 Cloudy samples indicate bad coagulation while good coagulation refers to rapid
floc formation resulting in clear water formation on the upper portion of the
beaker.

2.3.5 Experiment 5: Bacteria Counting


1. Preparing nutrient media
a) Mix peptone (5g), beef extract (3g), agar (15g) and distilled water in 600mL beaker
and boil it.
b) Cool the agar up to 45-50C. (so that the pours can be made without killing the
bacteria). (Since our digital thermometer has been out of service, use traditional
method. As long as the liquefied agar can move and flow easily and you can hold the
beaker with your hand, it is consider safe for your bacteria too.)
c) For the Spread Plate test, pour the nutrient media into half of the six petri plates.
(agar preparation procedures should be performed under laminar flow to keep the
samples sterile. Use gloves to prevent contamination of the samples).

2. Preparing bacteria dilution


3. Spread Plate method
4. Pour Plate method

5. Bacteria counting
a) After being incubate for 1 day, take out the petri plates.
b) Place the petri plate on the counting chamber.
c) At the end of the incubation period, select all of the petri plates containing between 30
and 300 colonies. Plates with more than 300 colonies cannot be counted and are
designated too many to count (TMTC). Plates with fewer than 30 colonies are
designated too few to count (TFTC).
d) Count the colonies on each plate.
2.3.5 Experiment 6: AN, Nitrogen, Ammonia
Before starting :
1. Hold the reagent droppers and dropper bottles vertically, not at an angle, when the
reagent is added.
2. The reagents that are used in this test contain mercury. Collect the reacted samples for
safe disposal.
3. If the Pour-Thru Cell is used, clean the cell periodically. To clean, add several crystals
of sodium thiosulfate pentahydrate into the cell funnel. Add deionized water to
dissolve the crystals. Rinse fully with deionized water.
4. Review the Safety Data Sheets (MSDS/SDS) for the chemicals that are used. Use the
recommended personal protective equipment.
Test Procedure:
1. Start program 380 N, Ammonia, Ness. For information about sample cells, adapters or
light shields, refer to Instrument specific information on page 1.
2. Prepare the sample: Fill a mixing cylinder to the 25mL line with sample.
3. Prepare the blank: Fill a mixing cylinder to the 25‑mL line with deionized water.
4. Add 3 drops of Mineral Stabilizer to each mixing cylinder.
5. Put the stopper on the mixing cylinders. Invert the mixing cylinders several times to
mix.
6. Add 3 drops of Polyvinyl Alcohol Dispersing Agent to each mixing cylinder.
7. Put the stopper on the mixing cylinders. Invert the mixing cylinders several times to
mix.
8. Use a pipet to add 1.0 mL of Nessler Reagent to each mixing cylinder.
9. Put the stopper on the mixing cylinders. Invert the mixing cylinders several times to
mix.
10. Start the instrument timer. A 1-minute reaction time starts.
11. Pour 10 mL from the blank cylinder into a sample cell.
12. When the timer expires,clean the blank sample cell.
13. Insert the blank into the cell holder.
14. Push ZERO. The display shows 0.00 mg/L NH3–N.
15. Pour 10 mL from the sample cylinder into a second sample cell.
16. Clean the prepared sample cell.
17. Insert the prepared sample into the cell holder.
18. Push READ. Results show in mg/L NH3–N.

2.4 Water Sampling & Sample Preservation


1. Collect samples in clean glass or plastic bottles.
2. If the sample contains chlorine, add one drop of 0.1 N sodium thiosulfate for each 0.3
mg/L chlorine in 1 liter of sample.
3. To preserve samples for later analysis, adjust the sample pH to less than 2 with
concentrated sulfuric acid (approximately 2 mL per liter). No acid addition is
necessary if the sample is tested immediately.
4. Keep the preserved samples at or below 6 °C (43 °F) for a maximum of 28 days.
5. Let the sample temperature increase to room temperature before analysis.
6. Before analysis, adjust the pH to ~7 with 5 N sodium hydroxide solution.
7. Correct the test result for the dilution caused by the volume additions.