Water Effluent Analysis Procedure 1. PH Principle

WATER EFFLUENT ANALYSIS PROCEDURE
1. pH
Principle
The term “pH” stands for the power of Hydrogen and is the measurement of the hydrogen ion activity in a solution. The hydrogen ion
concentration is very difficult to measure directly. Instead, its activity is measured indirectly by the use of specific electrodes in the solution. These
electrodes are conveniently put together to make our pH probes. The electrical potential between these two electrodes in a sample is measured,
and by comparing this with the potentials of known pH samples (buffers) we can approximate the hydrogen ion activity of the solution. In the
wastewater field pH analyses are important for neutralization, corrosion control, precipitation, coagulation, and biological treatment.
pH is measured on a scale of 0 to 14 with the lower values indicating high hydrogen ion activity (more acidic) and high values indicating low
hydrogen ion activity (less acidic). A pH of 7 is neutral. Every whole unit of pH change represents a ten-fold change in the hydrogen ion activity. For
example, a pH of 5 is ten times more active than a pH of 6 and a pH of 4 is one hundred times more active than a pH of 6.
Reagents
pH 4 buffer solution Reagents needed are for the calibration of the pH meter only.
pH 7 buffer solution No reagents needed in the actual testing of the sample.
pH 9 buffer solution
Procedure
Sample 100 mL (placed in Dip the pH probe into the

glass or plastic container Mix the sample Record pH meter reading.
solution
Note: pH meter should be calibrated before every analysis.

Samples should be tested within 15 minutes of collection.
There should be no headspace in the sample container.
Rinse the pH probe with distilled water and blot it dry before dipping it into the solution.
Temperature of the sample tested should be the same with the temperature of the buffer solution used during calibration.
2. Chemical Oxygen Demand (COD)

Principle
Chemical Oxygen Demand (COD) test is commonly used to indirectly measure the amount of organic compounds in water. Most applications of
COD determine the amount of organic pollutants found in surface water making COD a useful measure of water quality. It is expressed in
milligrams per liter (mg/L), which indicates the mass of oxygen consumed per liter of solution. The basis for the COD test is that nearly all
organic compounds can be fully oxidized to carbon dioxide with a strong oxidizing agent under acidic conditions. The method used in
determining the Chemical Oxygen Demand is the Open Reflux Method.
Reagents
a. Standard potassium dichromate solution, 0.025N (0.004167M)
Dissolve 1.225 g K2Cr2O7, primary standard grade, previously dried at 150°C for 2h, in distilled water and dilute to L.
b. Sulfuric acid reagent, 18M
Measure 1L sulfuric acid and add 0.1 g Ag2SO4.
c. Ferroin indicator solution
Dissolve 1.485 g 1,10-phenanthroline monohydrate and 695 mg FeSO4·7H2O in distilled water and dilute to 100 mL. This indicator solution
may be purchased already prepared.*
d. Standard ferrous ammonium sulfate (FAS) titrant, approximately 0.025M
Dissolve 9.8 g Fe(NH4)2(SO4)2·6H2O in distilled water. Add 20 mL conc H2SO4, cool, and dilute to 1000 mL.
e. Mercuric sulfate, HgSO4, crystals or powder.
f. Potassium hydrogen phthalate (KHP) standard, HOOCC6H4COOK
Lightly crush and then dry KHP to constant weight at 110°C. Dissolve 425 mg in distilled water and dilute to 1000 mL. If practical, prepare
and transfer solution under sterile conditions. Weekly preparation usually is satisfactory.
Procedure
Standardization of Ferrous Ammonium Sulfate
Dilute 10 mL standard K2Cr2O7 Add 30 mL concentrated Titrate with FAS titrant using 0.10 to
to about 100 mL. H2SO4 and cool 0.15 mL (2 to 3 drops) ferroin indicator
*Read volume when solution turns red at end point.
1
COD Determination
Add 25 mL 0.004167M
Mix the sample well and pipet 50 mL Add 1g HgSO4, glass beads and 5 mL H2SO4 reagent
K2Cr2O7 solution and
into 500-mL refluxing flask with mixing to dissolve HgSO4.
mix.
Cover open end of condenser Add remaining H2SO4 reagent (20 mL) through open
with a small beaker. end of condenser. Continue swirling and mixing while Attach flask to condenser and
adding H2SO4 turn on cooling water.
Disconnect reflux condenser and dilute mixture to

Cool and wash condenser with
Reflux for 2 hours about twice its volume with distilled water
distilled water
Titrate excess K2Cr2O7 with FAS, using 0.10 to 0.15 mL (2 Cool to room temperature and dilute to a final volume of
to 3 drops) ferroin indicator approximately 300mL with distilled water.
Note: Mix reflux mixture thoroughly before applying heat to prevent local heating of flask bottom and a possible blowout of flask contents.
Take as the end point of the titration the first sharp color change from blue-green to reddish brown that persists for 1 min or longer.
Calculation
Normality of FAS solution
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐾2 𝐶𝑟2 𝑂7 , 𝑚𝐿
𝑚𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 𝐹𝐴𝑆 = 𝑥 0.2500
𝑣𝑜𝑙𝑢𝑚𝑒 𝐹𝐴𝑆 𝑢𝑠𝑒𝑑 𝑖𝑛 𝑡𝑖𝑡𝑟𝑎𝑡𝑖𝑜𝑛, 𝑚𝐿
Chemical Oxygen Demand

𝑚𝑔 𝑂2 (𝐴 − 𝐵) 𝑥 𝑀 𝑥 8000
𝐶𝑂𝐷 𝑎𝑠 =
𝐿 𝑚𝐿 𝑠𝑎𝑚𝑝𝑙𝑒
where: A = mL FAS used for blank,

B = mL FAS used for sample,
M = molarity of FAS
8000 = milliequivalent weight of oxygen X 1000 mL/L.
3. Biochemical Oxygen Demand (BOD)

Principle
BOD refers to the measure of the approximate quantity of dissolved oxygen that will be required by bacteria to stabilize organic matter in
wastewater or surface water. It is a semi-quantitative measure of the wastewater organics that are oxidizable by bacteria. It is also a standard
test in assessing wastewater strength and quality of water. If the oxygen level in the water drop too much, fish and other aquatic life may not
survive. There are two recognized methods for the measurement of BOD; the dilution method and manometric method. The method
recognized by Environmental Management Bureau is the Dilution Method.
Reagents
a. Phosphate buffer solution
Dissolve 8.5 g KH2PO4 (monopotassium phosphate), 21.75 g K2HPO4 (dipotassium phosphate), 33.4 g Na2HPO4·7H2O (disodium phosphate
heptahydrate), and 1.7 g NH4CI in about 500 mL distilled water and dilute to 1L. The pH should be 7.2 without further adjustment.
b. Magnesium sulfate solution
Dissolve 22.5 g MgSO4·7H2O in distilled water and dilute to 1L.
c. Calcium chloride solution
Dissolve 27.5 g CaCI2 in distilled water and dilute to 1L.
d. Ferric chloride solution
Dissolve 0.25 g FeCI·6H2O in distilled water and dilute to 1L.
e. Acid and alkali solutions, 1N for neutralization of caustic or acidic waste samples.
Acid-Slowly and while stirring, add 28 mL concentrated sulfuric acid to distilled water. Dilute to 1L.
Alkali-Dissolve 40 g sodium hydroxide in distilled water. Dilute to 1L.
2
Procedure
Preparation of Dilution Water:
Add 1mL phosphate buffer, magnesium

sulfate, calcium chloride, ferric chloride Add distilled water up to 1L
into 1L volumetric flask.
Test Procedure:
Add 1mL wastewater Add dilution water up to Adjust pH value to 6.5-7.5 by

sample into 500mL beaker 300mL into the same beaker adding acid/alkali
Measure DO for each sample by Put all prepared samples and Prepare 300mL dilution
using Dissolved Oxygen Meter control in 300mL-incubation bottle water as control
Put all the bottles in BOD incubator for Measure final DO value after 5 days.
5days. Set temperature at 20oC.
Calculation
BOD5, mg/L = (D1 – D2) x Dilution factor
Where: Dilution factor = Bottle volume (300mL) / Sample volume
D1 = DO value in initial sample
D2 = DO value in final sample
4. Total Suspended Solids (TSS)

Principle
Total suspended solids is a water quality measurement usually abbreviated TSS. The amount of particles that suspend in a sample of water is
called total suspended solids (TSS). To remain permanently suspended in water, particles have to be light in weight, be relatively small in size,
and/or have a surface area that is large in relation to their weight. The greater the TSS in the water, the higher its turbidity and the lower its
transparency (clarity).
TSS can be estimated from measurements of turbidity or transparency, but an accurate TSS measurement involves carefully weighing the
amount of suspended material from a water sample. The method is called gravimetric analysis.
Reagents
No reagents needed. Only filter paper is used in this test.
Procedure
Weigh 1 filter Take 100mL sample. Mix well and filter using the Dry the filtered sample in an
paper weighed filter paper oven @ 103-105oC.
Dry the weighed sample again and weigh again after an hour and dry again. Weigh the dried sample after
Repeat this step until constant weight is reached. 1 hour
Calculation
(𝐹2 −𝐹1 ) 𝑚𝑔
𝑇𝑆𝑆 = = where: F2 = Weight of dried sample with filter paper
𝑉 𝐿
F3 = weight of filter paper
V = volume of sample

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WATER EFFLUENT ANALYSIS PROCEDURE

Sample 100 mL (placed in Dip the pH probe into the

Note: pH meter should be calibrated before every analysis.

2. Chemical Oxygen Demand (COD)

*Read volume when solution turns red at end point.

Disconnect reflux condenser and dilute mixture to

Chemical Oxygen Demand

where: A = mL FAS used for blank,

3. Biochemical Oxygen Demand (BOD)

Add 1mL phosphate buffer, magnesium

Add 1mL wastewater Add dilution water up to Adjust pH value to 6.5-7.5 by

4. Total Suspended Solids (TSS)

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