2.

3 ANALYTICAL METHOD

2.3.1 pH Test

Apparatus: Portable multi-parameter

Procedure:

1) Calibrate the pH meter.

2) Take the water sample and put it into a clean beaker.
3) Rinse the probe thoroughly with distilled water to prevent any carry-over.
4) Switch to pH mode.
5) Immerse the probe in the sample.
6) Establish equilibrium between probe and sample by stirring to ensure
homogeneity. Gently drop a stirring bar into the sample and place the
beaker on magnetic stirrer.
7) Start the magnetic stirrer and adjust the speed to give through but gentle
mixing.
8) Read and record the pH value.
9) Rinse the electrode thoroughly with distilled water.
10) When not in use, the electrode should be replaced in the beaker containing
water.
2.3.2 Dissolved oxygen (DO)

Apparatus: Portable multi-parameter

Procedure:

1) ·Rinse the probe with distilled water.

2) ·Put the probe in a beaker that contains the solution. Do not let the probe
touch the stir bar, bottom or sides of the container.
3) Remove the air bubbles from under the probe tip. Stir the sample at a
slow to moderate rate.
4) Push ‘Read’ and a progress bar is shown. When the measurement is stable,
the reading is taken.
5) When the value is stable, record the mV value and the temperature value.
2.3.3 Total Suspended Solid

Apparatus:

1) Evaporating dishes
2) Dishes of 100-mL capacity made of one of the following materials:
o Porcelain, 90-mm diam.
o Platinum—Generally satisfactory for all purposes.
o High-silica glass
o Muffle furnace for operation at 550°C.
o Steam bath.
o Desiccator, provided with a desiccant containing a color indicator of moisture
concentration or an instrumental indicator.
o Drying oven, for operation at 103 to 105°C.
o Analytical balance, capable of weighing to 0.1 mg.
o Magnetic stirrer with TFE stirring bar.
o Wide-bore pipets.
o Graduated cylinder.

Procedure:

Preparation of glass-fiber filter disk:

1) Insert disk with wrinkled side up in filtration apparatus. Apply vacuum and wash
disk with three successive 20-mL portions of reagent-grade water.
2) Continue suction to remove all traces of water, turn vacuum off, and discard
washings. Remove filter from filtration apparatus and transfer to an inert
aluminium weighing dish. If a Gooch crucible is used, remove crucible and filter
combination.
3) Dry in an oven at 103 to 105°C for 1 h. If volatile solids are to be measured,
ignite at 550°C for 15 min in a muffle furnace.
4) Cool in desiccator to balance temperature and weigh. Repeat cycle of drying or
igniting, cooling, desiccating, and weighing until a constant weight is obtained or
 until weight change is less than 4% of the previous weighing or 0.5 mg,
whichever is less. Store in desiccator until needed.

Selection of filter and sample sizes:

1) Choose sample volume to yield between 2.5 and 200 mg dried residue. If volume
filtered fails to meet minimum yield, increase sample volume up to 1 L. If
complete filtration takes more than 10 min, increase filter diameter or decrease
sample volume.

Sample analysis:

1) Assemble filtering apparatus and filter and begin suction.

2) Wet filter with a small volume of reagent-grade water to seat it. Stir sample with a
magnetic stirrer at a speed to shear larger particles, if practical, to obtain a more
uniform (preferably homogeneous) particle size.
3) Centrifugal force may separate particles by size and density, resulting in poor
precision when point of sample withdrawal is varied.
4) While stirring, pipet a measured volume onto the seated glass-fiber filter.
5) For homogeneous samples, pipet from the approximate midpoint of container but
not in vortex. Choose a point both mid depth and midway between wall and
vortex. Wash filter with three successive 10-mL volumes of reagent-grade water,
allowing complete drainage between washings, and continue suction for about 3
min after filtration is complete. Samples with high dissolved solids may require
additional washings.
6) Carefully remove filter from filtration apparatus and transfer to an aluminium
weighing dish as a support.
7) Alternatively, remove the crucible and filter combination from the crucible
adapter if a Gooch crucible is used. Dry for at least 1 h at 103 to 105°C in an
oven, cool in a desiccator to balance temperature, and weigh.
8) Repeat the cycle of drying, cooling, desiccating, and weighing until a constant
weight is obtained or until the weight change is less than 4% of the previous
 weight or 0.5 mg, whichever is less. Analyse at least 10% of all samples in
duplicate. Duplicate determinations should agree within 5% of their average
weight. If volatile solids are to be determined, treat the residue according to
2540E.

Calculation:

( A−B ) X 1000
Mg total suspended solid/L =
Sample volume , mL

Where:

A = weight of filter + dried residue, mg

B = weight of filter, mg
2.3.4 Ammonia

Apparatus:

Description Quantity/tes Unit

t
Mixing cylinder, graduated, 25ml with 1 Each
stopper
Pipet, serological, 1ml, glass 1 50kg/pkg
Pipet filler, safety bulb 1 each

Reagents:

Description Quantity/test Unit

Ammonia Nitrogen Reagent Set,
includes:
Nessler Reagent 2ml 500ml
Mineral Stabilizer 6drops 50ml
SCDB

Procedure:
1) Start program 380 N, Ammonia, Ness. For information about sample cells,
adapters or light shields.
2) Prepare the sample: Fill a mixing cylinder to the 25- mL 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. Put the
stopper on the mixing cylinders. Invert the mixing cylinders several times to mix.
 9) Start the instrument timer. A 1-minute reaction time starts.
10) Pour 10 mL from the blank cylinder into a sample cell.
11) When the timer expires, clean the blank sample cell.
12) Insert the blank into the cell holder.
13) Push ZERO. The display shows 0.00 mg/L NH3–N.
14) Pour 10 mL from the sample cylinder into a second sample cell.
15) Clean the prepared sample cell.
16) Insert the prepared sample into the cell holder.
17) Push READ. Results show in mg/L NH3–N.

2.3.5 Biochemical Oxygen Demand (BOD)

Apparatus
 1) Incubation bottles: Use glass bottles having 60 mL or greater capacity (300-mL
bottles having a ground-glass stopper and a flared mouth are preferred).
2) Clean bottles with a detergent, rinse thoroughly, and drain before use.
3) Air incubator or water bath, thermostatically controlled at 20 ±1°C. Exclude all
light to prevent possibility of photosynthetic production of DO.

Procedure:

River water samples:

1) Preferably fill large BOD bottle (>2 L, or alternatively 6 or more 300-mL BOD
bottles) with sample at 20°C. Add no nutrients, seed, or nitrification inhibitor if
in-bottle decay rates will be used to estimate in-stream rates. Do not dilute sample
unless it is known by pretesting or by experience to have a high ultimate BOD
(>20 mg/L).
2) Measure DO in each bottle, stopper, and make an airtight seal. Incubate at 20°C in
the dark. Measure DO in each bottle at intervals of at least 2 to 5 day over a
period of 30 to 60 day (minimum of 6 to 8 readings) or longer under special
circumstances.
3) After five days (± 3 hours) the DO meter is used again to measure a final
dissolved oxygen concentration (mg/L), which ideally will be a reduction of at
least 4.0 mg/L.
4) The final DO reading is then subtracted from the initial DO reading and the result
is the BOD concentration (mg/L). If the wastewater sample required dilution, the
BOD concentration reading is multiplied by the dilution factor
2.3.6 Chemical Oxygen Demand (COD)

Apparatus: Digestion vessels, Block heater, Microburette

Reagents:

1) Standard potassium dichromate digestion solution

2) Potassium hydrogen phthalate
3) Ferroin indicator solution
4) Sulphuric acid reagent
5) Standard ferrous ammonium sulphate titrant (FAS)

Procedure:

1) Collect samples in clean bottles. Use plastic bottles only if they are known to be free of
organic contamination.
2) Test biologically active samples as soon as possible.
3) Homogenize samples that contain solids to get a representative sample.
4) To preserve samples for later analysis, adjust the sample pH to less than 2 with
concentrated sulphuric acid (approximately 2 ml per litre). No acid addition is necessary
if the sample is tested immediately.
5) Keep the preserved samples at 2-6 ℃ (36-43 ℉) for a maximum of 28 days.
6) Correct the test result for the dilution caused by the volume additions.