SOP Testing Water Wastewater Treatment Chemicals

MINISTRY OF WATER
WATER QUALITY SERVICES

DIVISION
REVIEWED STANDARD OPERATING PROCEDURE
WATER AND WASTEWATER TREATMENT CHEMICAL

ANALYSIS
MAY 2014
TABLE OF CONTENT
TABLE OF CONTENT.........................................................................................................2
COAGULANTS....................................................................................................................2
1.1 DOSAGE: STANDARD JAR TEST................................................................................2
1.2 DETERMINATION OF ALUMINIUM OXIDE IN ALUMINIUM SULFATE.......................7
1.3 BASICITY OF ALUMINIUM SULFATE SOLUTION.....................................................12
1.4 DETERMINATION OF DENSITY OF ALUMINIUM SULFATE.....................................15
1.6 DETERMINATION OF SOLUBILITY OF ALUMINIUM SULFATE................................21
1.7 pH OF ALUMINIM SULFATE BY POTENTIOMETRIC METHOD................................24
1.8 VISCOSITY OF POLYMERIC CATIONIC COAGULANTS..........................................27
2.0 COAGULANT AID.......................................................................................................30
2.1 DETERMINATION OF PERCENTAGE GRIT IN BENTONITE....................................30
2.2DETERMINATION OF AVAILABLE LIME (HYDRATED LIME)....................................33
3.0 DISINFECTANT...........................................................................................................37
3.1 DETERMINATION OF CHLORINE % IN CALCIUM HYPOCHLORITE.......................37
3.2 DETERMINATION OF CHLORINE % IN SODIUM HYPOCHLORITE.........................41
3.3 DETERMINATION OF MOISTURE CONTENT OF CALCIUM HYPOCHLORITE.......44
3.4 DETERINATION OF DENSITY OF SODIUM HYPOCHLORITE.................................47
3.5 DETERMINATION OF BROMINE................................................................................49
3.5 DETERMINATION OF OZONE IN WATER TREATMENT..........................................53
2
COAGULANTS
1.1 DOSAGE: STANDARD JAR TEST
1.0 INTRODUCTION
Jar tests are used to predict clarification at water works. There are four main factors that can
influence clarification performance, namely the raw water quality, mixing conditions, coagulant
chemistry and dosage rate.
2.0 SCOPE
This method may be used to determine optimum dose of an inorganic coagulant or a

polyelectrolyte for use as a primary coagulant and for comparing the performance of different
coagulants.
3.0 INTERFERENCES
1.1.1 Highly turbid water

1.1.2 Acidity
1.1.3 High concentration of Manganese and Iron
4.0 PRINCIPLE
The removal of turbidity from waters by coagulation and flocculation is the result of several
sequential processes, each of which must work efficiently.
It has been found that almost all foreign matter occurring naturally in waters bears a slight negative
charge. The insoluble colloidal clay particles largely responsible for turbidity are held in suspension
by Brownian motion, being too small to be significantly affected by gravity. The electrostatic
repulsion between such particles prevents them from aggregating by random collisions into
particles large enough to settle. (The colloids themselves will settle given sufficient time without
turbulence, but under natural conditions they are stable as suspensions).
The introduction of a positively charge species to this system destabilizes the colloids by providing
electrostatic attraction greater than interparticle repulsion. The extent of this destabilization
depends on the field strength around the coagulant species and hence on the charge/radius ratio
of a metal ion or the local dipole moment ("charge density") of a polyelectrolyte. Small highly
charged metal ions (A1+++, Fe+++) are the most efficient destabilizers, and polyelectrolytes may
have insufficient charge density for this function in some cases.
5.0 SAFETY
Analyst following and conducting this procedure must wear the appropriate safety personal
protective equipment (PPE). The supervisor must ensure staffs are wearing/using the correct
3
PPE. Ensure that you are familiar with the dangers and treatment associated with these
coagulants.
Table 1
PPE TO BE USED
Laboratory coat; Closed in shoes; Safety glasses – wrap At all stages
around style; Rubber gloves / Latex gloves
MSDS to be read Before analysis
6.0 QUALITY CONTROL
A minimum per QC lot (20 real samples):
6.1 One (1)Method blank (MB) per 20 samples
Water blanks are performed automatically at start-up. Blanks are to be less than the
reporting limit.
6.2 One (1) Laboratory control sample (LCS) per 20 samples
6.3 Two (2) Sample duplicates per 20 samples
Determine the Relative Percentage Deviation (RPD):

RPD = Difference between Duplicate Results x 100
Average of Duplicate Results
7.0 SAMPLING
Water should be a representative sample of the feed water to the process being
investigated, 10 to 20 litres will need to be collected to allow for duplication of results if
needed.
8.0 APPARATUS
8.1 Six place gang stirrer with variable speed control.
8.2 Laboratory stirrer with four-blade impeller, speed capacity from 25-2000 rpm (for
flash mixing).
8.3 Six 1 litre beakers.
8.4 Assorted pipettes and burettes to suit requirements.
8.5 Stop watch
8.6 Turbid meter
8.7 UV Spectrophotometer
8.8 pH meter
4
8.9 Thermometer
9.0 REAGENTS
9.1 Coagulants or Polymers to be assessed.
All solutions are made up in tap or distilled water. Weights and volumes given below
are intended only as a guideline. Different laboratories may choose to use solutions
of different strength with different volumes of water sample.
9.2 Polyelectrolyte coagulant solution

9.2.1 Weigh out 0.8 g of polyelectrolyte solution into a beaker
9.2.2 Transfer to a 1 L volumetric flask and dilute to mark.
9.2.3 May be stored for 1 week.
9.2.4 1 mL polyelectrolyte solution will be equal to 1 mg/L dosage (in 800 mL)
9.3 Inorganic Coagulant Solution

9.3.1 Weigh out 0.8 g (1 mL = 1 mg/L) or 4.0 g (1 mL = 5 mg/L) or 8.0 g (1 mL = 10
mg/L) of aluminium sulphate or ferric chloride (ensure that the weight used
takes into account the concentration of the coagulant solution as supplied,
e.g. to obtain a 4.0g/L as active alum when using a 48% alum solution, 8.33
g/L of 48% alum solution will be required. If the SG has been measured, then
a measured volume can be used instead of a mass).
9.3.2 Transfer to a 1 L volumetric flask and dilute to the mark

9.4 Lime solution
9.4.1 Weigh out 0.8 g (1 mL = 1 mg/L) or 4 g (1 mL = 5 mg/L) of white or
brown lime depending what is used on the works.
9.4.2 Transfer to a 1 L volumetric flask and dilute to mark. May be stored for 1
week.
10.0 ANALYTICAL PROCEDURE

10.1 Obtain a raw water sample from the raw water inlet before addition of any
chemicals and excluding filter wash water return.
10.2 Determine the turbidity, pH, temperature and any other relevant treatment
measurement on the raw water sample and record results on report sheet.
10.3 Measure out 800 mL aliquots of raw water into the number of beakers on the
jar test machine and number them accordingly. The volumes provided here are
intended only as a guideline. Different laboratories may choose to use solutions
of different strength with different volumes of water sample.
10.4 Set the flashmix speed at a speed which best simulates the conditions on the
plant (this is generally between 100 and 300 rpm) and start the stirrer.
10.5 Add coagulant solution to all the beakers simultaneously or within as short a
time as possible, in a range of doses based on previous experience. Coagulant
can be added using a specially designed manifold apparatus in which the
5
coagulant dose for each jar can be added to a small beaker or test tube and
then the manifold tipped so that the coagulant dose for each jar is added
simultaneously. Alternatively, one can use a separate syringe or beaker for the
coagulant dose for each jar. If the syringes or beakers are filled first, it is
possible to add the coagulant to each of the jars within a very short period of
time.
10.6 If the water is unfamiliar, commence with a dosage range of 1 to 6 mg/L for
polyelectrolyte, or 5 to 30 mg/L for ferric chloride, or 10 to 60 mg/L for alum,
and adjust for further jar tests if necessary for less turbid waters. Higher doses
may be required for more turbid waters.
10.7 If using alum or ferric chloride add lime at a dosage of 1/4 or 1/3 the coagulant
dosage respectively
10.8 Stir for 2 minutes
10.9 After 2 minutes reduce the speed to 40 rpm for a further 15 minutes.
10.10 Turn off the stirrer and record the floc size, based on the standard floc sizes
shown on the 'Floc comparator' at the bottom of the jar test worksheet.
10.11 Record the settling rate, i.e. slow, moderate or rapid settling.
10.12 If required, allow the water to settle for specific period of time and then
carefully withdraw sufficient water from just below the surface using a pipette,
syringe or similar and measure the turbidity or whichever parameter is used for
meeting the treatment objectives.
10.13 Filter each sample through 24 cm MN615 filter papers or Whatman No. 1 filter
papers or equivalent into 1 L conical flasks.
10.14 Collect about 200 mL of filtrate in the flask and rinse. Discard the washings.
10.15 Filter the remaining sample.
10.16 Measure the filtered sample for pH, turbidity or any other parameter important
in terms of the treatment objectives.
10.17 Record the results on report sheets.
10.18 If the turbidity (or any other treatment parameter) is greater than the specified
maximum, repeat the exercise starting at a higher or lower dose as relevant,
until the optimum dose is achieved.
11.0 CALCULATION AND REPORT OF RESULTS
11.1 The turbidity should be less than the specified maximum (generally 0.5 NTU or
1 NTU
11.2 If color, total organic carbon or any other parameter is important in meeting
the treatment objectives, measure these too and choose the lowest coagulant
dose which reduces the relevant parameter to below the specified maximum
value
11.3 Based on treatment requirements, performance and cost, the optimum dose
and most suitable coagulant can be determined.
6
12.0 REFERENCES
12.1 Freese, S. D., Trollip, D. L and Nozaic, D. J (2003), Manual for Testing of Water
and Wastewater Treatment Chemicals, Umgeni Water, Water Research
Commission, South Africa.
12.2 Franson M.A. H (1998), Standard Method for Water and Wastewater
Examination 20 Edition. American Public Health Association 1015 Fifteenth ,NW
Washington, DC 20005-2605
12.3 Indian Standards: 260-1969
7
1.2 DETERMINATION OF ALUMINIUM OXIDE IN ALUMINIUM SULFATE
1. INTRODUCTION
Aluminium sulfate, is a chemical compound with the formula Al2(SO4)3. It is soluble in water
and is mainly used as a flocculating agent/coagulant in the purification of drinking water
and wastewater treatment plants, and also in paper manufacturing. Aluminium sulphate
used to be added to the water in lump or slab form and is prepared from aluminium
hydroxide, alumina trihydrate, or alumina-bearing ores, such as clay and bauxite. Aluminum
sulfate is determined as a aluminium oxide (Al 2O3) % by weight. In Liquid Aluminium
Sulphate, 8% w/w (as Al2O3) is an inorganic, acidic chemical
2. SCOPE
This method will be used to determine Alluminium Oxide in Aluminium Sulfate
3. INTERFERENCES
The solubility of Al (OH)3 is a function of the pH. As the degree of acidity increases (the pH
decreases) the alumina concentration at any particular density would be lower than the
alumina concentration at the same density of neutral acidic liquid alum.
4. PRINCIPLE
The compound decomposes to γ−alumina and sulfur trioxide when heated between 580
and 900 °C. It combines with water forming hydrated salts of various compositions.
Aluminium sulfate reacts with sodium bicarbonate to which foam stabilizer has been added,
producing carbon dioxide for fire-extinguishing foams:
Al2(SO4)3 + 6 NaHCO3 → 3 Na2SO4 + 2 Al(OH)3 + 6 CO2
The carbon dioxide is trapped by the foam stabilizer and creates thick foam which will float
on top of hydrocarbon fuels and seal off access to atmospheric oxygen, smothering the fire.
Chemical foam was unsuitable for use on polar solvents such as alcohol, as the fuel would
mix with and break down the foam blanket. The carbon dioxide generated also served to
propel the foam out of the container, be it a portable fire extinguisher or fixed installation
using hoselines.
5. SAFETY
protective equipment (PPE). The supervisor must ensure staff are wearing / using the
correct PPE. Corrosive, wear gloves, aprons, goggles masks and protective shoes when
handling.
Table 1
8
PPE TO BE USED
Laboratory coat; Closed in shoes; Safety glasses – wrap around At all stages
style; Rubber gloves / Latex gloves
Breathing Aluminum Sulfate can irritate the nose, throat and lungs causing coughing,
wheezing and/or shortness of breath
6. QUALITY CONTROL
reporting limit.

7. SAMPLING, SAMPLE STORAGE AND HANDLING

7.1 Prior to working with Aluminum Sulfate you should be trained on its proper
handling and storage
7.2 Sampling and preparation shall be conducted as expeditiously as possible in
order to avoid undue exposure of the material to the air, thus avoiding
contamination and evaporation.
7.3 The sampling method must give a gross sample that is representative of the
material, and which may be divided to provide representative samples for
analysis. Samples for analysis shall be provided in triplicate. Samples shall
be sealed in airtight moisture proof containers.
7.4 Samples may be collected in plastic bag
7.5 Each sample shall be labelled to identify it by such information as the
name of the purchaser package number, and date received. Each label shall
be signed by the sampler.
9
7.6 If the alum is packaged, 5% of the number of the packages shall be
sampled. No sample shall be taken from a broken package.
7.7 Care shall be taken to include a proportional amount of lumps and fines, to
obtain representative material.
7.8 Ground aluminium sulphate shall be sampled using a sampling tube or other
effective device that measures at least 2 cm in diameter.
7.9 Kibbled alum (or lumps) shall be sampled from the container by removing an
assortment of different sized lumps by hand (wearing clean gloves).
8. SAMPLE PREPARATION
8.1 Nitric Acid - Sulphuric Acid digestion or Nitric - Hydrochloric Acid (Aqua
Regia) digestion is adequate for samples with readily oxidisable organic
matter.
8.2 Nitric - Perchloric Acid digestion or Nitric - Perchloric - Hydrofluoric Acid
digestion is necessary for samples containing difficult to oxidise organic
matter or minerals.
9. APPARATUS/ EQUIPMENTS
Analytical balance, volumetric flask, Measuring cylinder, burette, spatula, sucker crucible,
petri dishes, beaker, wash bottles
10. REAGENTS AND STANDARDS

10.1 Disodium ethylenediaminetetraacetate (EDTA) solution -0.1M
Disolve 37.225g of EDTA dehydrate in water and make the volome to
1L in a volumetric flask.
10.2 Absolute alcohol
10.3 Dithiozone Indicator - 0.025% in absolute alcohol. It shall be prepared
afresh
10.4 Acetic acid –Amonium buffer solution
Dissolve 7.709g of ammonium acetate in 100mlof water. Mix 6.005 g
acetic acid in 100ml of water. Mix both the solutions together. The
final solution is in the concentration of 1M of ammonium acetate and
1M of acetic acid per litre
10.5 Standard zinc chloride solution -0.1M
11. PROCEDURES
11.1 Dissolve 2g of prepared sample in 25ml of water
11.2 Add 50ml of EDTA solution followed by 10ml of buffer solution and then
85ml of absolute alcohol and 3ml of dithiozone indicator.
10
11.3 Titrate the excess of EDTA solution with standard zinc chloride solution
until the color change from blue to reddish purple
12. CALCULATION AND REPORTING OF RESULTS
Calcute the Aluminium content of the material on the assumption that, one milliliter of 0.1M
EDTA solution is equivalent to 0.0051g of Aluminium (as Al2O3)
1ml of 0.1M EDTA solution Ξ 0.0051g of Aluminium (as Al2O3
13. REFERENCES
13.1 Freese, S. D., Trollip, D. L and Nozaic, D. J (2003), Manual for Testing of
Water and Wastewater Treatment Chemicals, Umgeni Water, Water Research
Examination 20 Edition. American Public Health Association 1015
Fifteenth ,NW Washington, DC 20005-2605
13.3 Indian Standards: 260-1969
11
1.3 BASICITY OF ALUMINIUM SULFATE SOLUTION
1.0 INTRODUCTION
As early as the 17th century various forms of aluminium sulphate have been used for the
coagulation of suspended and colloidal particles in water. Alum solutions are acidic. For
instance, a 1% solution has a pH of around 3. Ionic species present in alum solutions are
highly dependent on the degree of reaction with hydroxyl ions. It is tempting to say that "the
composition is pH-dependent. Basicity is important because of its effect in controlling the
dissociation of biologically active substances. Increasing basicity coagulants gives less
acidity to the treated water.
2.0 SCOPE
This method will be used to confirm the basicity or free acid of liquid Aluminium Sulphate.
3.0 INTERFERENCES
The degree of basicity is the function of temperature and therefore all measurement shall
refer to the operating temperature.
4.0 PRINCIPLE
This method is based on the decomposition of aluminium salts by an excess of neutral
potassium fluoride to form two stable compounds neutral to phenolphthalein, whereas any
free acid remains unaltered.
Basic alumina exists if the sodium hydroxide back titration is less than the amount of
sulphuric acid added (i.e. less than 10 mL). Free acid exists if the sodium hydroxide back
titration is more than the amount of sulphuric acid added (i.e. is greater than 10 mL). The
sample is neutral if the sodium hydroxide back titration is equal to the sulphuric acid added.
5.0 SAFETY
correct PPE. Ensure that you are familiar with the dangers and treatment associated with
these coagulants.
Table
PPE TO BE USED

12
6.0 QUALITY CONTROL
Water blanks are performed automatically at start-up. Blanks are to be less than
the reporting limit.

7.0 SAMPLING, SAMPLE STORAGE AND HANDLING

7.2 Sample should be store in a low humid and dry place
8.0 APPARATUS/ EQUIPMENTS
Analytical balance, volumetric flasks 50 mL (Erlenmeyer flask), measuring Cylider, Spatula,
burette, pipette
9.0 REAGENTS AND STANDARDS

9.1 Phenolphthalein indicator
9.2 Potassium Fluoride solution
9.2.1 Dissolve 1000 g of pure potassium fluoride in 1 200 mL of hot, carbon
dioxide free distilled water and 0.5 mL of phenolphthalein solution.
9.2.2 Neutralize with potassium hydroxide or sulphuric acid. To confirm that
the neutralization is correct, add 1 mL of solution to 10 mL of distilled
water, a faint pink colour should be observed.
9.2.3 Upon neutralization, filter out the insoluble matter without washing and
dilute to 2 L, with carbon dioxide free water. Store in a plastic bottle. 3.
0,5 N Sulphuric acid solution
9.2.4 Filter about 500 mL of distilled water into a 1 L volumetric flask. Add 14
mL of concentration sulphuric acid and dilute to 1 L with distilled water.
4. 0,5 N Sodium Hydroxide solution
9.2.5 Weigh out 20 g of sodium hydroxide pellets in to a beaker, dissolve in
distilled water and pour into a 1 L volumetric flask and dilute to 1 L.
13
Standardize the sodium hydroxide against the sulphuric acid in 40 mL of
distilled water to which 10 mL of potassium fluoride solution has been
added, use phenolphthalein as the indicator. Standardize against
benzoic acid or potassium acid phthalate before using.
10.0 PROCEDURES
10.1 Weigh out 7 g of liquid alum into an Erlenmeyer flask. Record the exact weight.
10.2 Add 100 mL of distilled water to the flask and heat to boiling.
10.3 Add 10 mL of 0.5 N Sulphuric acid to the hot solution.
10.4 Cool to room temperature
10.5 Add 18 to 20 mL of potassium fluoride solution and 0.5 mL of phenolphthalein
indicator.
10.6 Titrate against 0.5N sodium hydroxide, dropwise, until a slight pink colour
persists for 1 minute.
11.0 CALCULATION AND REPORTING OF RESULTS

The fomular below will be used to calculate percentage free alumina and percentage free sulphuric
acid
% Free alumina (Al2O3) = (mL 0.5N H2SO4 - mL 0.5N NaOH) x 0.0085 x100………………..eqn 1
Weight of sample
% Free sulphuric acid (H2SO4) = (mL 0.5NaOH - mL 0.5N H2SO4) x 0.0245 x 100…………..eqn 2
Weight of sample
Results are reported in percentage ( % Free alumina (Al2O3) or/and % Free sulphuric acid (H2SO4)
12.0 REFERENCES
14
1.4 DETERMINATION OF DENSITY OF ALUMINIUM SULFATE
1.0 INTRODUCTION
The density of an object is described as its mass per unit volume and is expressed as: D =
M/V. Since density is characteristic of a substance, it can be helpful in identifying it, as well
as being useful in determining the concentration of the substance in solution form.
2.0 SCOPE
This method is used to determine the density of Aluminium Sulfate solutions in mass per
unit volume. This result can be used to assist in determining the volume required to relate
to a mass per volume measurement.
3.0 INTERFERENCE
Change in temperature can interfere measurement of density therefore density should be
measured at specific temperature
4.0 PRINCIPLE
This analysis can be done in two ways. The first is a weight method. This is done by
determining the density of your sample by using density bottle.
The second is called the hydrometer method. The instrument used is called a
Hydrometer, it is floated in the sample and the Specific Gravity can be read directly off the
instrument.
5.0 SAFETY
these coagulants.
Table
PPE TO BE USED
15
6.0 QUALITY CONTROL
reporting limit.


8.0 APPARATUS
8.1 Analytical Balance (capable of weighing to the nearest

0.0001g).
8.2 Gay Lussac Flask.
8.3 Hydrometer (different ranges depending on the range

expected of the sample).
9.0 PROCEDURE
9.1 Specific Gravity by Weight method
9.1.1 Obtain Density bottle. Prepare flask by washing and drying the outside of
the bottle. Let the bottle sit upside down on a rack so that it can dry at
room temperature.
16
9.1.2 After drying, weigh bottle on its own and record mass (M1).
9.1.3 Fill bottle so that it overflows. Lower stopper into bottle and make sure
that the bottle fills the hole all the way to the top of the stopper. Dry the
outside of the bottle so that there is no water or residue of any kind on
the flask. After drying make sure that the water level is still to the very
top of the stopper.
9.1.4 Weigh the bottle containing the solution to be determined and record
mass (M2).
Measure the temperature of the sample and record this temperature (this
temperature. will be used when calculating the result).
9.2 Hydrometer Method
Fill a 250ml volumetric cylinder with well mixed sample. If you can estimate
what range your sample will fall into, then select the Hydrometer that
covers that range. Gently lower the bulb end of the Hydrometer into the
sample and wait until it reaches a steady equilibrium. Reading off the scale
on the side of the instrument, read from the top of the meniscus. Record
the reading.
10.0 CALCULATIONS (FOR WEIGHT METHOD) RESULTS
Density of the sample will be calculated by using the following formula

Density = Weight of sample  F
Volume of density bottle at TC
F = Temperature Correction Factor (Temperature of sample)
This value is a mass per volume number.
Results are report in mass per volume number to the nearest two decimal places.
17
In the case of a solution, the density (in g/mL) is numerically equal to the specific gravity (SG).
Refer to Table below for the conversion of SG to % aluminium sulphate.
Specific %Aluminum Sulphate Specific %Aluminium Sulphate

Gravity Gravity
1.01 1.88 1.19 30.2
1.02 3.68 1.20 31.6
1.03 5.44 1.21 32.9
1.04 7.18 1.22 34.2
1.05 8.94 1.23 35.6
1.06 10.6 1.24 37.0
1.07 12.3 1.25 38.4
1.08 13,9 1.26 39.7
1.09 15.4 1.27 41.0
1.10 17.0 1.28 42.3
1.11 18.5 1.29 43.7
1.12 20.1 1.30 45.0
1.13 21.5 1.31 46.2
1.14 23.0 1.32 47.5
1.15 24.4 1.33 48.8
1.16 25.9 1.34 50.1
1.17 27.4 1.35 51.3
1.18 28.8
11.0 REFERENCES
11.1 Standard Methods for the Examination of Water and Wastewater, 20 Edition
(2710 F: 2-82).
18
1.5 DETERMINATION OF INSOLUBLE MATTER IN ALUMINIUM SULPHATE
1.0 INTRODUCTION
Water-insoluble matter in liquid alum should be kept to a minimum, since it does not take
part in the coagulation reaction, adds to sludge formation and may introduce undesirable
particulates into the water.
2.0 SCOPE
This method may be used to confirm the water insoluble matter of liquid Aluminium
Sulphate.
3.0 INTERFERENCES
No significant interference
4.0 PRINCIPLE
A well- mixed sample is filtered through a weighed standard glass-fibre filter and the
residue retained on the filter is dried to a constant weight at 103oC to 105oC.
5.0 SAFETY
these coagulants.
Table
PPE TO BE USED
Laboratory coat; Closed in shoes; Safety glasses At all stages
– wrap around style; Rubber gloves / Latex gloves
6.0 QUALITY CONTROL


19


Samples may be collected in plastic bag
Analytical balance, Gooch crucibles, Filter papers, Tongs
Dilute Sulphuric Acid – approximately 1N
10.0 PROCEDURES
10.1 Crush about 200g of a material to pas 1.00mm IS Sieve
10.2 Into a Gooch crucible place a glass-fibre filter paper, dry at 105° C to 110° C
for at least an hour.
10.3 Cool in desiccator and record weight when cool.
10.4 Weigh out 10 g of liquid alum or 5 g of dry alum sulphate and dilute to 150
mL with dilute sulphuric acid or hot distilled water and stir.
10.5 Filter through the prepared crucible. Rinse the residue with dilute sulphuric
acid or hot distilled water until the filtrate is free of sulphates. This should be
at least 3 washings of 25 mL each.
10.6 Return the crucible to the oven and for at least 1 hour or to a constant
weight.
10.7 Cool in desiccators and weigh, record weight

Insoluble matter will be determined by using the formula below
% Insoluble matter = weight of insoluble residue x 100
Weight of sample
Results are expressed in % Insoluble matter to two the nearest
12.0 REFERENCES
(2710 F: 2-82).
20
1.6 DETERMINATION OF SOLUBILITY OF ALUMINIUM SULFATE
1.0 INTRODUCTION
Aluminium sulfate (Al2 (SO4)3), commonly called alum, is produced as white crystals which
are non-combustible and soluble in water. This dry hydrate (Al 2 (SO4)3.14H2O) is 17% Al2O3
and is also sold as a 47% w/w Aluminium Sulfate solution which is 8% Al 2O3. It is also sold
in solid form as kibbled, ground or dust.
2.0 SCOPE
This method will be used in determine solubility of Aluminium Sulfate (Al2 (SO4)3) in
water.
3.0 INTERFERENCES
At pHs below 6.0, Al+3 solids containing sulfate, silica or potassium are thermodynamically
favored versus amorphous Al(OH)3. At pHs above 9, aluminum and magnesium were
discovered to form complex solid phases of approximate composition AlMg 2(OH)7,
AlMg2SiO2(OH)7 or Al(SiO2)2(OH)3 dependent on circumstance. Formation of these solids
provide a mechanistic explanation for enhancements to precipitative softening obtained in
practice by dosing Al+3 salts; that is, improved flocculation/settling and removal of silica
from water that interferes with calcium precipitation. The solids also maintain residual
aluminum below regulatory guidelines at high pH >9.5.
High concentration of Silica
4.0 PRINCIPLE
When a chemical species is classified as “insoluble”, this does not mean that none of the
compound dissolves in the given solvent or solution system. In reality, a measurable level
of material does go into solution, but it is sometimes considered negligible relative to the
total amount of the chemical. Perhaps a better name for such salts is “sparingly soluble.”
The dissolving of a solid monovalent-monovalent salt, represented as MX, in an
appropriate solvent is represented by the general equation:
21
MX(s) l M+ (aq) + X– (aq).
where the subscripts “(s)” and “(aq)” represent the solid and aqueous solution physical
states, respectively. For a set of given conditions, the precipitate has a definite solubility (or
maximum amount that will dissolve) expressed in units of grams/liter or moles/liter.
5.0 SAFETY
these coagulants.
Table
PPE TO BE USED
6.0 QUALITY CONTROL




Sample should be stored in a cool, dry, well ventilated place, in securely closed original
container
22
Product should be used in accordance with good industrial principles for handling and
storing of hazardous chemicals. Avoid creating or raising dust. Avoid contact with skin or
eyes.

Beaker, stirrer, motor and pestle, balance, spatula

Not applicable
10.0 PROCEDURES
10.1 Take 10.g of finely grinded aluminum sulfate and dissolve using distilled water in
100ml beaker
10.2 Filter the solution in a pre-weighed filter paper
10.3 Dry the filter paper to a constant weight

Percentage solubility will be determined by using the formula below
% solubility = weight of filter paper after filtration- weight of filter paper before filtration X 100
Weight of filter paper after filtration
Results will be expressed in percentage solubility with acceptance
12.0 REFERENCES
12.3 http://en.wikipedia.org/wiki/Aluminium_sulfate
12.4 http://www.ulm.edu/chemistry/courses/manuals/chem1010/experiment_10.pdf.
23
1.7 pH OF ALUMINIM SULFATE BY POTENTIOMETRIC METHOD
1.0 INTRODUCTION
The Aluminim Sulfate pH is a measure of the acidity or alkalinity in Aluminium Sulfates. pH
is defined as the negative logarithm (base 10) of the activity of hydronium ions (H+ or, more
precisely, H3O+aq) in a solution. In water, it normally ranges from 1 to 14, with 7 being
neutral. A pH below 7 is acidic and above 7 is alkaline. Aluminim Sulfate pH is considered a
master variable in Aluminium Sulfate as it controls many chemical processes that take
place.
2.0 SCOPE
This method is the procedure for determining the pH of Aluminium Sulfate samples by use
of a pH meter.
3.0 INTERFERENCES
The glass electrode is relatively free from interference from colour, turbidity, colloidal
matter, oxidants, reductants and salinity however samples should be dilute solutions
[<0.2M] of simple salts to ensure that the pH is due only to the hydrogen ion activity.
4.0 PRINCIPLE
A pH meter provides a value as to how acidic or alkaline a liquid is. The basic principle of
the pH meter is to measure the concentration of hydrogen ions. Acids dissolve in water
forming positively charged hydrogen ions (H+). The greater this concentration of hydrogen
ions, the stronger the acid is. Similarly alkali or bases dissolve in water forming negatively
charged hydrogen ions (OH-). The stronger a base is the higher the concentration of
negatively charged hydrogen ions there are. The amount of these hydrogen ions present
solution is dissolved in some amount of water determines the pH
5.0 SAFETY
24
these coagulants.
Table
PPE TO BE USED
MSDS to be read
6.0 QUALITY CONTROL



6.4 Acceptance criteria

± 10% of the QC samples

Samples should be collected in plastic bag
8.1 pH meter
8.2 Plastic beakers
8.3 Magnetic Stirrer

Buffer solution (pH 4.00 and pH 7.00), deionised water
9.1 Standard Buffer Solution pH 4.00

9.1.1 Dry potassium hydrogen phthalate [COOH.C6H4.COOK] for 2 hours at
120oC, cool to room temperature in desiccators.
25
9.1.2 Dissolve 10.12g potassium hydrogen phthalate in deionised water then
dilute to 1 litre in a volumetric flask.
9.2 Standard Buffer Solution pH 7.00

9.2.1 Dry potassium dihydrogen orthophosphate [K2PO4] and disodium
hydrogen phosphate [Na2HPO4] for 2 hours at 110oC. Cool to room
temperature in a desiccators.
9.2.2 Dissolve 3.387g KH2PO4 and 3.533g Na2HPO4 in deionised water then
dilute to 1 litre in a volumetric flask.
10.0 PROCEDURES
10.1 Set up instrumentation/software as per manufacturer’s instruction
10.2 Rinse probe/s thoroughly with deionised water.
10.3 Calibrate the pH system according to manufacturer’s instructions for measuring

pH using at least two buffer solutions with traceable pH values. When practical,
the pH of the buffer solutions should bracket the expected pH of the samples.
10.4 Calibrate meter using pH 7.00 and pH 4.00 Buffers. (Note: Different meters may
require the use of alternate buffers e.g. pH 7.00, pH 10.00. Check the
manufacturer’s procedures.) Check slope values are between 97%-102%.
10.5 Check calibration with a fresh portion of 9.18 buffer. Alternatively check with a
pH 4 buffer if calibration was performed using a pH 7 and pH 10.
10.6 Print, or record the calibration details and calibration check control results with
each day’s sample results. Use controlled form to record the check calibration
control. Inform supervisor if control fails.
10.7 Allow samples and buffers to come to room temperature. Fill cups with about
30mL (ensure volume is at least sufficient to cover probe electrodes; refer
manufacturer’s instructions) and place in positions on the auto sampler. Analyse
a blank, duplicates and pH buffer check with each batch of samples as per QC
requirements.

Direct reading from the instrument and results reported to two nearest decimal
places
12.0 REFERENCES
26
(4500-H+A: 4-86).
1.8 VISCOSITY OF POLYMERIC CATIONIC COAGULANTS
1.0 INTRODUCTION
Viscosity is the ability of a liquid to resist various internal and external movements, such as
flow. In the case of polymeric coagulants, the viscosity is affected by a number of factors, such
as the degree of polymerization and the concentration of the active ingredient. Viscosity can
therefore be a good quality control indicator, indicating consistency in the product and whether
changes, which may affect the activity of the coagulant, might have occurred.
2.0 SCOPE
This method may be used to determine the viscosity of a polymeric cationic coagulant.
3.0 INTERFERENCES
Temperature Polymeric cationic coagulants are thixotropic, such that their viscosity will
decrease with increasing spindle speed.
4.0 PRINCIPLE
The dynamic viscosity, η of a (Newtonian) fluid is given by η = τ ÷ dv/dr; τ = shearing stress

between two planes parallel with the direction of flow, dv/dr = velocity gradient at right angles to
the direction of flow. The dimensions of dynamic viscosity are ML−1T−1, and the SI unit is Pa s.
Kinematic viscosity, ν, is the ratio of the dynamic viscosity to the density, ρ. The dimensions
of kinematic viscosity are L2T−1 and the SI unit is m2 s−1.
Fluidity is the reciprocal of the dynamic viscosity, η. The dynamic viscosity of liquids
decreases with the temperature approximately according to the equation log η = A + B/T,
where A and B are characteristic constants and T is the absolute temperature. Values of A and
B for a large number of liquids
5.0 SAFETY
protective equipment (PPE). The supervisor must ensure staff are wearing / using the correct
coagulants.
27
Table
PPE TO BE USED
6.0 QUALITY CONTROL




7.0 SAMPLE COLLECTION

Samples may be collected in either glass or plastic containers.
8.0 APPARATUS
8.1 Viscometer
8.2 Brookfield
8.3 Model LVT
8.4 Tall form 250 mL beaker
9.0 REAGENTS
Distilled water
28
10.1 Set up the viscometer and level the instrument. These instructions are for a
Brookfield Model LVT. For other viscometers, follow the manufacturer's
instructions.
10.2 Attach the spindle specified by the polymer supplier. (NOTE: Left-handed
threads.)
10.3 Pour enough samples into the beaker to cover the spindle up to the groove.
10.4 Lower the viscometer with the spindle attached into the sample until the surface
of the sample meets the groove on the spindle shaft. The spindle should not
touch the bottom of the beaker.
10.5 Set the viscometer to chosen revolutions per minute.
10.6 Turn on the viscometer motor.
10.7 After the needle reaches a steady reading, and after at least 10 revolutions,
depress the clutch lever on the back of the viscometer to "freeze" the needle on
the scale.
10.8 With the clutch depressed, stop the viscometer motor when the needle is visible
in the viscometer window.
10.9 Read and record the position of the needle on the scale.
10.10 Repeat the procedure until you have three readings.
10.11 If the manufacturer does not specify a spindle, start with spindle number 1 and
follow the procedure. If the needle is not near the middle of the of the
viscometer's scale range, use the next spindle size up and repeat until a correct
reading has been obtained.
11.0 CALCULATION AND RESULTS

Direct reading from the equipment and follow manufacture specification
Results are reported to two nearest decimal places
12.0 REFERENCES
12.1 David Moonay, Sales Engineer/Rheology Laboratory Supervisor, Brookfield
Engineering Laboratories, Inc., Middleboro, Mass
12.2 David Moonay at 508-946-6200, or visit www.brookfieldengineering.com.
12.3 Barrer (1943) Trans. Farad., 39, 48.
29
2.0 COAGULANT AID
2.1 DETERMINATION OF PERCENTAGE GRIT IN BENTONITE
1. INTRODUCTION
The grit content of bentonite needs to be minimized in order to avoid damage occurring to
pumps and feed equipment. Ideally, the grit content should not exceed 5% when the
bentonite is passed through a 53 µm sieve. The physical and chemical properties of
bentonites typically vary both within and between deposits due to differences in the degree
of chemical substitution within the smectite structure and the nature of the exchangeable
cations present, and also due to the type and amount of impurities present
2. SCOPE
This method describes a procedure for the determination of percentage grit content in
bentonite.
3. INTERFERENCES
Presence of high concentration of exchangeable cations
4. PRINCIPLE
The existing smectite clay-minerals in the bentonite (i.e.montmorillonite) generate a huge
reactive surface when disperged. The clay minerals ́ weak negative charge enables it to
adsorb changeable cationic components
By exchange of ions with higher valence against ions with weaker charge the silica layers
of montmorillonite show a negative charge. This is compensated by adsorption of counter
ions in the interlayers. The charge of the layers is so weak that the interlayer cations are
exchangeable. Furthermore the weak charge effects an expansion of the inter layers,
enabling the counter ions to be integrated with their hydrate shell (inner crystalline swelling
5. SAFETY
30
these coagulants.
Table
PPE TO BE USED
Laboratory coat; Closed in shoes; Safety glasses – At all stages
wrap around style; Rubber gloves / Latex gloves
6. QUALITY CONTROL

reporting limit.

7. SAMPLING, SAMPLE STORAGE AND HANDLING

Samples may be collected in either plastic or glass containers or packets.
8. APPARATUS/ EQUIPMENTS
Blender, Analytical balance, Evaporating dish or metal crucible, Sieve of pore size 53 µm,
beakers
9. REAGENTS AND STANDARDS

Di - Sodium Dihydrogen Pyrophosphate (Na2H2P2O7), AR grade.
10. PROCEDURES
10.1 Record the mass of the empty crucible or evaporating dish.
10.2 Weigh out 50.0g of bentonite into a 500 mL glass beaker and to it add 300.0
mL of distilled water. Add approximately 5g of di-sodium dihydrogen
pyrophosphate and mix at a high speed until the solution is well blended.
31
10.3 Brush the suspension through a 53 µm sieve with a fine stream of water.
10.4 Continue brushing until the water passing through the sieve is clear.
10.5 Transfer the residue retained on the sieve to a metal crucible or evaporating
dish and dry to a constant mass.
10.6 Record the mass of the residue.
11. CALCULATION AND REPORTING OF RESULTS

The percentage grit content will be obtained by using the formula below.
% Grit = (M2-M1) x 100

50
Where:
M1 = mass of empty dry crucible or dish (g).
M2 = mass of crucible or dish plus dry residue (g).
Results are presented in percentage grit content to two nearest decimal place
12. REFERENCES
12.1 Freese, S. D., Trollip, D. L and Nozaic, D. J (2003), Manual for Testing of Water and
Wastewater Treatment Chemicals, Umgeni Water, Water Research Commission,
South Africa
12.2 Inglethorpe S D J, D J Morgan, D E Highley A J Bloodworth (1993) Industrial

Minerals Laboratory Manual BENTONITE Keyworth, Nottingham, British Geological
Survey, Britain
32
2.2 DETERMINATION OF AVAILABLE LIME (HYDRATED LIME)
1.0 INTRODUCTION
When quicklime is slaked to produce slaked or hydrated lime, calcium oxide is converted to
calcium hydroxide. Determination of the calcium oxide content gives an indication of the
purity of the hydrated lime, but gives no indication of the conversion to calcium hydroxide that
occurred during slaking. It is important to ensure that the lime has been properly slaked
before using it for treatment applications. This method is also not suitable for dolomite lime,
except as an approximation.
2.0 SCOPE
This method describes a procedure for the determination of available lime content of
hydrated lime.
3.0 INTERFERENCES
High salinity
4.0 PRINCIPLE
Calcium oxide is a white crystalline solid with a melting point of 2572°C. It is manufactured
by heating limestone, coral, sea shells, or chalk, which are mainly CaCO3, to drive off
carbon dioxide.
CaCO3(s) 500–600°C
CaO(s) + CO2(g)
This reaction is reversible; calcium oxide will react with carbon dioxide to form calcium
carbonate. The reaction is driven to the right by flushing carbon dioxide from the mixture as
it is released.
33
5.0 SAFETY
these coagulants.
Table
PPE TO BE USED
6.0 QUALITY CONTROL

Water blanks are performed automatically at start-up. Blanks are to be less
than the reporting limit.


7.0 SAMPLE COLLECTION AND PRESERVATION

Samples may be collected in either plastic or glass containers or packets.
8.0 APPARATUS
8.1 50 mL Burette
8.2 250 mL Erlenmeyer flasks
8.3 Analytical balance
8.4 A grade glass pipettes
8.5 1 L glass Schott bottles or equivalent for shaking.
34
8.6 Mechanical shaker
A: IODINE METHOD
9.0 REAGENTS:
9.1 Standard sodium thiosulphate solution, 0.1N recently standardized.
9.2 Standard Iodine Solution 0.1 N recently standardized against standard sodium
thiosulphate solution.
9.3 Starch indicator solution. : titrate 5 gms of starch and 0.01gm of mercuric iodide with
30 ml of cold water and slowly pour it with stirring into 1 litre of boiling water. Boil for
three minutes. Allow the solution to cool and decant off the supernatant liquid.
10.0 PROCEDURE:
10.1 Take 1g of the material, accurately weighed, in a glass stopper conical flask
and add about 30 ml of boiling water.
10.2 Shake for 5 to 10 min.
10.3 Cool the solution and an amount of iodine solution sufficient to provide an
excess of about 5 ml and stir occasionally until the lime has gone in the
solution.
10.4 Any insoluble silica present in easily distinguished from the milky appearing
lime.
10.5 When the solution of lime is complete (about 10 min are required), dilute the
solution in a volumetric flask to 500ml.
10.6 Pipette out 25 ml of the solution and titrate the excess iodine with standard
sodium thiosulphate solution.
10.7 Adding starch indicator towards the end of the titration.
10.8 Carry out a blank determination of the same amount of iodine solution as
with the sample.
11.0 CALCULATION
Available lime as CaO = 56.08 * (V1 – V2) N / (M)
V1 = Volume in ml. Of the standard sodium thiosulphate solution used in the blank
V2 = Volume in ml. Of standard sodium thiosulphate solution used with the material
N = Normality of the standard sodium thiosulphate solution
M = mass in gms. Of the material taken for the test
35
B: Determination of Available Lime (as CaO) by Sugar method
9.0 REAGENTS
9.1 Rectified spirit
9.2 Standard hydrochloric acid, 0.1 N.
9.3 Standard sodium hydroxide solution, 0.1 N
9.4 Sugar solution, approximately 15%, in CO2 free water.
9.5 Phenolphthalein indicator solution: Dissolve 0.5 g of Phenolphthalein in 100 ml of
rectified spirit.
10.0 PROCEDURE
10.1 Weigh accurately about 1 g of the finely powdered material into a 500ml volumetric
flask and wet it with the minimum amount of rectified spirit.
10.2 Shake with about 400 ml of sugar solution for 3 hours and dilute to the mark.
10.3 Filter through a coarse dry filter paper (Whatman No. 40 of it’s equivalent) into a dry
flask.
10.4 Discard the first 25 ml of the filtrate.
10.5 Pipette out 50 ml from the filtrate into another flask, add 50 ml of standard
hydrochloric acid and titrate with standard sodium hydroxide solution using
Phenolphthalein as indicator.
10.6 Run a blank using 50 ml of sugar solution and 50 ml of standard hydrochloric acid.
11.0 CALCULATION
Available Lime (as CaO)% by mass =28.04*(A – B) * N / M
Ca(OH)2 = Available Lime as CaO * 1.32
A = volume, in ml, of standard sodium hydroxide solution used in blank.
36
B = volume, in ml. of standard sodium hydroxide solution used with the material.
N = normality of standard sodium hydroxide solution.
M = mass, in g, of the material taken for the test
12.0 REFERENCES
12.1 South African Bureau of Standard 459-1955 Standard Specification of lime for
chemical and Metallurigical purposes
3.0 DISINFECTANT
3.1 DETERMINATION OF CHLORINE % IN CALCIUM HYPOCHLORITE
1.0 INTRODUCTION
Percent active chlorine is a unit of concentration used for hypochlorite-based bleaches. One
gram of 100% active chlorine bleach has the same bleaching power as one gram of chlorine.
The term "active chlorine" is used because most commercial bleaches contain substantial
amounts of chlorine in the form of chloride ions, which have no bleaching properties. Calcium
Hypochlorite (bleaching powder) sold for use in water treatment is typically 65–70% chlorine or
30% to 35% active chlorine.
2.0 SCOPE
This method is used for the routine sampling and analysis of chlorine % in calcium hypochlorite
3.0 INTERFERENCE
3.1 High Ferric and nitrate ion concentration
3.2 Oxidized forms of manganese
3.3 Organic sulphides
3.4 Sulphuric acid
4.0 PRINCIPLE
In chemistry, hypochlorite is an ion composed of chlorine and oxygen, with the chemical
formula ClO−. It can combine with a number of counter ions to form hypochlorites, which may
also be regarded as the salts of hypochlorous acid. Common examples include sodium
37
hypochlorite (household bleach) and calcium hypochlorite (bleaching powder, swimming pool
"chlorine").
Hypochlorites are frequently quite unstable in their pure forms and for this reason are normally
handled as aqueous solutions. Their primary applications are as bleaching, disinfection and
water treatment agents but they are also used in chemistry for chlorination
5.0 SAFETY
coagulants.
Table
PPE TO BE USED
All hypochlorite are corrosive to some degree and will affect the skin and eyes upon contact. Any
affected area should be washed with copious amount of water. When handling it is advisable to
wear protective gear such us gloves, aprons, goggles and suitable nap our mask.
6.0 QUALITY CONTROL



7.0 SAMPLING, STORAGE AND HANDLING.

7.1 Samples may be collected in either sealed plastic container
38
7.2 Preferably stored in the dark and analysed as soon as possible.
7.3 If analysis cannot be conducted immediately, store in the dark.
7.4 Exercise caution when handling chlorine.
7.5 It is recommended that gloves be worn.
7.6 It is recommended that the sample be handled in a fume cupboard with the extractor
fan running.
8.0 APPARATUS AND EQUIPMENT
8.1 Burette
8.2 Volumetric flask
8.3 Measuring Cylinder
8.4 Motor and pestle
9.0 REAGENT
9.1 Glacial acetic acid concentrated

9.2 Potassium iodide
9.3 0.1 N Sodium thiosulphate
Dissolve 25g of Na2S2O3. 5H2O in 1 L of freshly boiled distilled water.
9.4 0.1 N Potassium dichromate
Dissolve 4,904 g of previously dried at 110 +/- 50C to are constant weight K2Cr2O7 in
1 000 mL of distilled water.
Store in an amber bottle with a glass-stoppered lid
9.5 Starch indicator

Dissolve 5 to 15 g of soluble starch in 500 mL of distilled water.
Note; All prepared solutions are made up in volumetric flasks and are stored in glass
containers, unless otherwise indicated. Use only distilled water.
9.6 Standardization of Na2S2O3.5H20
To 80.0 ml distilled water, add with constant stirring, 1ml conc H 2SO4, 10.0ml 0.1N
K2cr2O7 and 1.0 gm KI. Titrate immediately with 0.1N Na 2S2O3.5H20. Titrate until a
yellow color of liberated iodine almost is discharged. Add 1.0 ml starch indicator
solution and continue titrating until the blue disappears.
Normality of Na2S2O3=1.0/ml Na2S2O consumed.
9.7 Standardization of Na2CO3

Heat Na2CO3 for half an hour at 260 0C – 270 0C and cool in a desiccators or NaHCO 3
heat at the same temperature for 60-90 minutes. The temperature must not be allowed
to exceed 270˚C for above this temperature the sodium carbonate may lose CO2.
Place 5-10g of A.R. Sodium carbonates in a porcelain nickel or platinum crucible.

Spread along the walls of the crucible to have a uniform thick layer. When cooling in a
39
desiccators before it is quite cold, transfer the material to a worm dry glass stoppered to
be or battle, out of which when cold, it may be weighed rapidly as required.
Normality Na2CO3 = 1.0 /mls of IN HCL used

IN of Na2CO3 =53g Na2CO3 + 1000mls dist
53g =gram equivalent not

0.1N = 53 x0.1 = 5.3g
1
NB.
Anhydrous sodium carbonate is hydroscopic and exhibits a tendency to pass into
monohydrate. After weighing your test sample adds 50mls distilled water indicator
(monophenol) and titrate against TN HCL.
10.0 PROCEDURE
10.1 Weigh accurately 2.5g of the sample and grind in a mortal with water till a smooth
paste is formed.
10.2 Add 15 to 25ml of water and decant of the fine part into a 250ml flask.
10.3 Again grind the material left behind and repeat the process of decanting off till no
gritty material is left.
10.4 Wash the pastel and mortal in the same flask; make the solution to 250ml.
10.5 Take 25ml of the solution, add 2g of potassium iodide crystals and 100ml water
and then add 2ml of glacial acetic acid and titrate it against the standardized
sodium thiosulphate solution till the pale yellow colour is left.
10.6 At this stage add starch indicator and continue the addition of standard sodium
thiosulphate solution till the blue colour discharges.
The percentage available chlorine will be calculated by using the formula below
Available chlorine, % by weight = AxNxM

W
Where
A = Volume in ml of standard thiosulphate solution used.
N = Normality of standard thiosulphate solution
W = Weight in g of sample taken for the tested rapidly.
M = Chlorine Atomic Weight
The results are presented in available chlorine %

12.0 REFERENCE
40
12.2 Indian Standard 1975
3.2 DETERMINATION OF CHLORINE % IN SODIUM HYPOCHLORITE
1.0 INTRODUCTION
Chlorination of water supplies serves primarily to destroy or deactivate disease producing
micro-organisms and to improve water quality by reaction with ammonia, iron, manganese,
sulphide and some organic substances. Chlorination can also produce adverse effects, for
example the taste and odour characteristics of phenols and other organic compounds present
in a water supply may be intensified.
2.0 SCOPE
The iodometric titration procedure described in this method is ideal for waters and solutions in
which the chlorine concentration is at least 1 mg/L
3.0 INTERFERENCES
3.1 High Ferric and nitrate ion concentration
3.2 Oxidized forms of manganese
3.3 Organic sulphides
3.4 Sulphuric acid
4.0 PRINCIPLE
41
In chemistry, hypochlorite is an ion composed of chlorine and oxygen, with the chemical
formula ClO−. It can combine with a number of counter ions to form hypochlorites, which may
also be regarded as the salts of hypochlorous acid. Common examples include sodium
hypochlorite (household bleach) and calcium hypochlorite (bleaching powder, swimming pool
"chlorine").
Hypochlorites are frequently quite unstable in their pure forms and for this reason are normally
handled as aqueous solutions. Their primary applications are as bleaching, disinfection and
water treatment agents but they are also used in chemistry for chlorination
5.0 SAFETY
coagulants.
Table
PPE TO BE USED
Laboratory coat; Closed in shoes; Safety glasses – At all stages
wrap around style; Rubber gloves / Latex gloves
6.0 QUALITY CONTROL




7.0 SAMPLING STORAGE AND HANDLING

7.1 Samples may be collected in either sealed plastic container
7.2 Preferably stored in the dark and analysed as soon as possible.
7.3 If analysis cannot be conducted immediately, store in the dark.
7.4 Exercise caution when handling chlorine.
42
7.5 It is recommended that gloves be worn.
7.6 It is recommended that the sample be handled in a fume cupboard with the extractor
fan running.
8.0 APPARATUS
8.1 Burette
8.3 Measuring Cylinder
8.4 Motor and pestle
9.0 REAGENT AND STANDARDS
10.0 PROCEDURE
10.1 Weigh accurately 2.5g of the sample and grind in a mortal with water till a smooth
paste is formed.
10.2 Add 15 to 25ml of water and decant of the fine part into a 250ml flask.
10.3 Again grind the material left behind and repeat the process of decanting off till no
gritty material is left.
10.4 Wash the pastel and mortal in the same flask; make the solution to 250ml.
10.5 Take 25ml of the solution, add 2g of potassium iodide crystals and 100ml water and
then add 2ml of glacial acetic acid and titrate it against the standardized sodium
thiosulphate solution till the pale yellow colour is left.
10.6 At this stage add starch indicator and continue the addition of standard sodium
thiosulphate solution till the blue colour discharges.
11.0 CALCULATION
12.0 REFERENCES
12.2 Water and waste water standard method 20th Edition
12.3 Indian Standard 1975
43
3.3 DETERMINATION OF MOISTURE CONTENT OF CALCIUM HYPOCHLORITE
1.0 INTRODUCTION
Calcium Hypochlorite is by far the most common disinfecting agent used in water treatment.
Its use is almost universal and has been practiced for approximately a hundred years. In its
natural state chlorine is a greenish yellow gas with a specific weight of about 2/4 times that of
air, an atomic weight of about 35, and a boiling point of about minus 34°C at atmospheric
pressure
2.0 SCOPE
This method describes a procedure for the determination of the moisture content of calcium
hypochlorite
3.0 INTERFERENCES
Calcium hypochlorite is mildly hygroscopic and should therefore be stored in a dry place.
4.0 PRINCIPLE
The moisture content is determined by measuring the mass of a material before and after the
water is removed at temperature between 103-115oC.
44
5.0 SAFETY
these coagulants.
Table
PPE TO BE USED
6.0 QUALITY CONTROL CRITERIA



7.0 SAMPLING, STORAGE AND HANDLING

7.1 Samples may be collected in either amber or clear glass containers, preferably
stored in the dark and analysed as soon as possible.
7.2 7.2 If analysis cannot be conducted immediately, chill and store in the dark.
7.3 It is recommended that the sample be handled in a fume cupboard with the
extractor fan running.
8.0 APPARATUS
8.1 Aluminium crucibles with covers

8.2 Oven
8.3 Weighing balance
8.4 Spatula
45
8.5 Desiccators with self indicating silica gel
8.6 Tongs
9.0 REAGENTS
Not applicable

10.1 Weigh porcelain dish and record the mass. (M1)
10.2 Weigh 10 g of calcium hypochlorite into porcelain dish and record mass (M2).
10.3 Dry for 2 hours at 1050C to 110° C oven.
10.4 Allow to cool in a desiccators and weigh and record weight (M3).
11.0 CALCULATIONS
% Moisture = (M2 - M3) x100
M2 - M1
MI= Weigh porcelain dish and record the mass

M2= Weigh 10 g of calcium hypochlorite into porcelain dish and record mass
M3= Weigh of dry sample with Crucible
Results are presented in percentage moisture content
12.0 REFERENCES
12.2 AWWA ANS/AWWA B4
46
3.4 DETERINATION OF DENSITY OF SODIUM HYPOCHLORITE
1.0 INTRODUCTION
The density of a substance is measured as the mass per unit volume measured at specific
temperature. The density of a substance can be therefore be defined as its mass per unit
volume.
2.0 SCOPE
This method is used to determine the density of solutions. This result can be used to assist
in determining the volume required to relate to a mass per volume measurement.
3.0 INTERFERENCES
Temperature
4.0 PRINCIPLE
47
This analysis can be done in two ways. The first is a weight method. This is done by
determining the density of the sample by using density bottle.
The second is called the hydrometer method. The instrument used is called a Hydrometer,
it is floated in the sample and the Specific Gravity can be read directly off the instrument.
5.0 SAFETY
correct PPE.
PPE TO BE USED
6.0 QUALITY CONTROL


Water blanks are performed automatically at start-up. Blanks are to be less
than the reporting limit.


8.0 APPARATUS
8.1 Analytical Balance (capable of weighing to the nearest 0.0001g).
8.2 Gay Lussac Flask.(density bottle)
8.3 Hydrometer (different ranges depending on the range expected of the sample).
48
9.0 REAGENTS
Not applicable
10.0 PROCEDURE
10.1 Density by Weight method
10.1.1 Obtain Density bottle Prepare flask by washing and drying the outside of the bottle.
Let the bottle sit upside down on a rack so that it can dry at room temperature.
10.1.2 After drying, weigh bottle on its own and record mass (M1).
10.1.3 Fill bottle so that it overflows. Lower stopper into bottle and make sure that the
bottle fills the hole all the way to the top of the stopper. Dry the outside of the bottle
so that there is no water or residue of any kind on the flask. After drying make sure
that the water level is still to the very top of the stopper.
10.1.4 Weigh the bottle containing the solution to be determined and record mass (M2).
10.1.5 Measure the temperature of the sample and record this temperature (this temp. will
be used when calculating the result).
10.2 Hydrometer Method (Specific Gravity)
10.2.1 Fill a 250ml volumetric cylinder with well mixed sample. If you can
estimate what range your sample will fall into, then select the
Hydrometer that covers that range.
10.2.2 Gently lower the bulb end of the Hydrometer into the sample and
wait until it reaches a steady equilibrium.
10.2.3 Reading off the scale on the side of the instrument, read from the
top of the meniscus. Record the reading
11.0 CALCULATIONS AND RESULTS (FOR WEIGHT METHOD)

The density of Sodium Hypochlorite is calculate by using the formula below
Density = Weight of sample
Volume of density bottle at TC
T = Temperature Correction Factor (Temperature of sample)
Results are reported in mass per volume number to two nearest decimal places.
12.0 REFERENCE
49
12.1 Freese, S. D., Trollip, D. L and Nozaic, D. J (2003), Manual for Testing of
Water and Wastewater Treatment Chemicals, Umgeni Water, Water Research
12.2 Standard Methods for the Examination of Water and Wastewater, 20th
Edition (2710F: 2-82)
3.5 DETERMINATION OF BROMINE
1.0 INTRODUCTION
Use of bromine in potable water is rare, but it is used for wastewater disinfection. The fact that
bromine reacts more quickly than chlorine does however allow for shorter contact times when
using bromine. Bromine has also been found to form trihalomethanes more readily than
chlorine, which has negative implications for potable water treatment.
2.0 SCOPE
This method will be used to measure total bromine residual, including bromamines. This
method is more suitable for measuring mg/L levels of bromine
3.0 INTERFERENCES
All other strong oxidants (chlorine or hydrogen peroxide) will interfere in this procedure.
4.0 PRINCIPLE
Bromide is added in conjunction with chlorine, which in turns oxidizes bromide to bromine. The
greater reactivity of bromine with natural organic matter in water can be attributed to the
greater solubility of bromine in water when compared to chlorine.
5.0 SAFETY
PPE.
PPE TO BE USED
6.0 QUALITY CONTROL
50



7.1 Samples may be collected in either amber or clear glass containers, preferably
stored in the dark and analyzed as soon as possible.
7.2 If analysis cannot be conducted immediately, chill and store in the dark.
8.0 APPARATUS AND EQUIPMENT

8.1 Burette
8.3 A-grade glassware.
8.4 Pipette
Use only distilled water. All prepared solutions are made up in volumetric flasks and are stored
in glass containers, unless otherwise indicated.
9.1 Glacial acetic acid concentrated
9.2 Sulphuric acid concentrated
Dissolve 25 g of Na2S2O3. 5H2O in 1 L of freshly boiled distilled water.
This should be stored for two weeks before use.
Dilute 100 mL of 0.1 N Na2S2O3 (10 x) into 1 000 mL of freshly boiled distilled water.
Dissolve 4,904 g of previously dried K2Cr2O7 in 1 000 mL of distilled water.
Store in an amber bottle with a glass-stopped lid
Dilute 100 mL of 0.1N K2Cr2O7 (10 x) into 1 000 mL of distilled water. Store in an
amber bottle
51
Dissolve 5 to15 g of soluble starch in 500 mL of distilled water. Keep refrigerated.

10.1 For percentage strength bromine solutions, dilute the sample 10 times
10.2 Pipette 10.0 mL of the 10 times dilution solution into a 1000 mL volumetric flask and
dilute to the mark using distilled water. Otherwise dilute as appropriate.
10.3 Store diluted solutions in a dark cupboard.
10.4 Standardization of 0.01 N Na2S2O3.
10.4.1 Into a 250 mL conical flask pipette 10.0 mL of 0.01 N K2Cr2O7.
10.4.2 Add 1 mL of concentrated sulphuric acid.
10.4.3 Add a spatula full of potassium iodide (KI) crystals.
10.4.4 Place in dark cupboard for 6 minutes.
10.4.5 Titrate against 0.01 N sodium thiosulphate until a pale straw colour is visible.
10.4.6 Add approximately 1 to 2 mL of starch indicator and the solution will turn
deep blue-black. Titrate until colourless.
10.4.7 Record the volume of thiosulphate (mL).
10.4.8 Run blank titrations together with the standardization titrations that contain
all the reagents, except replace the 10.0 mL K2Cr2O7 with distilled water.
10.5 Standardization of bromine sample.

10.5.1 Dilute the sample as described in (8)1 above.
10.5.2 Into a 500 mL conical flask measure 250 mL of the diluted bromine sample.
10.5.3 Add 5 mL of glacial acetic acid.
10.5.4 Add a spatula full of KI crystals.
10.5.5 Immediately titrate against standardised 0.01 N sodium thiosulphate until a
pale straw colour.
10.5.7 Record volume of thiosulphate.
10.5.8 Run blank titrations together with the standardization titrations, replacing the
250 mL bromine sample with 250 mL distilled water.
10.5.9 Low concentrations of bromine can also be read using the N, N - diethyl-
pphenylenediamine (DPD) method (see Method 6.8.7.).

11.1 Normality of Sodium Thiosulfate
N (Na2S2O3) = 10 x 0.01
Titre Na2S2O3 (mL)
11.2 Concentration of bromine solution mg/L =
Titre Na2S2O3 (mL) x 79 900 x dilution x N (Na2S2O3)

Volume Br2 sample (mL)
52
Results are expressed in concentration of bromine in mg/l to the nearest two decimal places
12.0 REFERENCES
12.1 White, G. C.: “Hand book of chlorination and Alternative Disinfectants”, 3 rd Edition,
Pub. Van No strand Reinhold, 1992.
12.2 Standard Method for the Examination of water and waste water”, 20 th Edittion,
Edited by L. S.Clesceri, A. E Green Berg and A.D. Eaton, Pub. APHA. AWWA WEF
1998. Processes Services, Umgeni water.
3.5 DETERMINATION OF OZONE IN WATER TREATMENT
1.0 INTRODUCTION
Ozone is an extremely powerful oxidant and disinfectant. Its side effects and reaction products
have not been researched as thoroughly as those of chlorine and the effects of its by-products
are not as well known. It is important that, ozone concentrations to be measured since process
ozone levels must be accurate in the water purification environment in order to ensure reliable
and efficient product addition.
2.0 SCOPE
This method is used to determine the concentration of ozone produced by an ozone generator.
3.0 INTERFERENCES
High concentration of bromine
4.0 PRINCIPLE
Ozone is one of the strongest oxidizing agents and disinfectants known. It is generated by
electric discharge at relatively high frequencies in dry air or dry oxygen, and efficient
generators can produce up to 14% ozone in an oxygen stream. Generation from air requires
53
very careful air filtration and drying of the air as a dew point of -60°C to -70°C is required if
arcing of electrodes in the ozone generator is to be avoided. Ozone is a gas at ambient
temperatures and is highly reactive and toxic.
Addition to the water is usually through diffusers or at the throat of a venturi on a recycle side
stream. Efficient contacting with the water is essential if the production of large quantities of
waste ozone requiring destruction is to be avoided. Unreacted ozone represents wastage of
generation capacity and an additional cost to the treatment process.
5.0 SAFETY
Analysit following and conducting this procedure must wear the appropriate safety personal
PPE.
PPE TO BE USED
6.0 QUALITY CONTROL


reporting limit.


7.0 SAMPLE COLLECTION

Samples must be titrated immediately after being collected.
54
8.0 APPARATUS
8.1 Burette
8.2 Volumetric equipment.
8.3 Pipette.
8.4 Conical flask
9.0 REAGENTS
All prepared solutions are made up in volumetric flasks and are stored in glass containers,
unless otherwise indicated. Use only distilled water.
9.1 Sulphuric acid conc.

9.3 Starch indicator (soluble)
Dissolve 25 g Na2S2O3. 5H2O in 1 L of freshly boiled distilled water.
This should be stored for two weeks before use.
9.5 0.01 N Sodium thiosulphate.
Dilute 100 mL of 0.1 N Na2S2O3(10 x) into 1 000 mL of freshly boiled distilled water.
Dissolve 4.904 g of previously dried K2Cr2O7 in 1 000 mL of distilled water.
Store in an amber bottle with a glass-stoppered lid
Dilute 100 mL of 0.1N K2Cr2O7 (10 x) into 1 000 mL of distilled water.
Store in an amber bottle.
Dissolve 5 to 15 g of soluble starch in 500 mL of distilled water.
Keep refrigerated.

10.1 Standardization of 0.01 N Na2S2O3
10.1.1 Into a 250 mL conical flask pipette 10.0 mL of 0.01 N K2Cr2O7.
10.1.2 Add 1 mL of concentrated sulphuric acid.
10.1.3 Add a spatula full of potassium iodide (KI) crystals.
10.1.4 Place in dark cupboard for 6 minutes.
10.1.5 Titrate against 0.01 N sodium thiosulphate until a pale straw colour is visible.
10.1.7 Record the volume of thiosulphate.
10.1.8 Run blank titrations together with the standardization titrations, replacing the
10.0 mL K2Cr2O7 with 10.0 mL distilled water.
10.2 Standardization of Ozone sample
10.2.1 Dilute the sample if necessary.
10.2.2 Into 500mL glass conical flask measure 2mL of glacial acetic acid and 1 g of
potassium iodide.
10.2.3 Add the volume of ozone sample to be titrated.
55
10.2.4 Immediately titrate against standardized 0.01 N or 0.1 N sodium thiosulphate
until a pale straw colour.
10.2.5 Add approximately 1 to 2mL of starch indicator and the solution will turn
10.2.6 Record the volume of thiosulphate.
10.2.7 Run blank determinations together with the standardization titrations,
replacing the ozone sample with an equal volume of distilled water.
10.2.8 Low concentrations of ozone can also be read using the N, N - diethyl-
pphenylenediamine (DPD) method. To convert the reading to mg/L ozone
divide the reading by 1.48
11.0 CALCULATION
11.1 Normality of Sodium Thiosulfate
N (Na2S2O3) = 10x0.01N
Titre N Na2S2O3 (mL)
11.2 Concentration of ozone solution mg/L = Titre N a2S2O3 (mL) x 24,000 x dilution x N (Na2S2O3)
Volume ozone sample (mL)
12.0 REFERENCES
12.1 White, G. C.: “Hand book of chlorination and Alternative Disinfectants”, 3 rd Edition,
Pub. Van No strand Reinhold, 1992.
12.2 Standard Method for the Examination of water and waste water”, 20 th Edittion,
Edited by L. S.Clesceri, A. E Green Berg and A.D. Eaton, Pub. APHA. AWWA WEF
1998.Processes Services, Umgeni water.
56

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MINISTRY OF WATER

WATER QUALITY SERVICES

REVIEWED STANDARD OPERATING PROCEDURE

WATER AND WASTEWATER TREATMENT CHEMICAL

1.1 DOSAGE: STANDARD JAR TEST

This method may be used to determine optimum dose of an inorganic coagulant or a

1.1.1 Highly turbid water

6.0 QUALITY CONTROL

A minimum per QC lot (20 real samples):

6.1 One (1)Method blank (MB) per 20 samples

6.2 One (1) Laboratory control sample (LCS) per 20 samples

6.3 Two (2) Sample duplicates per 20 samples

Determine the Relative Percentage Deviation (RPD):

9.2 Polyelectrolyte coagulant solution

9.3 Inorganic Coagulant Solution

9.3.2 Transfer to a 1 L volumetric flask and dilute to the mark

10.0 ANALYTICAL PROCEDURE

11.0 CALCULATION AND REPORT OF RESULTS

12.3 Indian Standards: 260-1969

Al2(SO4)3 + 6 NaHCO3 → 3 Na2SO4 + 2 Al(OH)3 + 6 CO2

6.1 One (1)Method blank (MB) per 20 samples

6.2 One (1) Laboratory control sample (LCS) per 20 samples

6.3 Two (2) Sample duplicates per 20 samples

Determine the Relative Percentage Deviation (RPD):

7. SAMPLING, SAMPLE STORAGE AND HANDLING

10. REAGENTS AND STANDARDS

1ml of 0.1M EDTA solution Ξ 0.0051g of Aluminium (as Al2O3

13.3 Indian Standards: 260-1969

Laboratory coat; Closed in shoes; Safety glasses – wrap At all stages

MSDS to be read Before analysis

6.1 One (1)Method blank (MB) per 20 samples

6.2 One (1) Laboratory control sample (LCS) per 20 samples

6.3 Two (2) Sample duplicates per 20 samples

Determine the Relative Percentage Deviation (RPD):

7.0 SAMPLING, SAMPLE STORAGE AND HANDLING

9.0 REAGENTS AND STANDARDS

11.0 CALCULATION AND REPORTING OF RESULTS

6.1 One (1)Method blank (MB) per 20 samples

6.2 One (1) Laboratory control sample (LCS) per 20 samples

6.3 Two (2) Sample duplicates per 20 samples

Determine the Relative Percentage Deviation (RPD):

7.0 SAMPLING, SAMPLE STORAGE AND HANDLING

8.1 Analytical Balance (capable of weighing to the nearest

8.2 Gay Lussac Flask.

8.3 Hydrometer (different ranges depending on the range

9.1 Specific Gravity by Weight method

9.2 Hydrometer Method

Density of the sample will be calculated by using the following formula

This value is a mass per volume number.

Specific %Aluminum Sulphate Specific %Aluminium Sulphate

6.0 QUALITY CONTROL

6.1 One (1)Method blank (MB) per 20 samples

Determine the Relative Percentage Deviation (RPD):

7.0 SAMPLING, SAMPLE STORAGE AND HANDLING

11.0 CALCULATION AND REPORTING OF RESULTS

Results are expressed in % Insoluble matter to two the nearest

1.6 DETERMINATION OF SOLUBILITY OF ALUMINIUM SULFATE

6.0 QUALITY CONTROL

6.1 One (1)Method blank (MB) per 20 samples

Determine the Relative Percentage Deviation (RPD):

7.0 SAMPLING, SAMPLE STORAGE AND HANDLING

8.0 APPARATUS/ EQUIPMENTS

9.0 REAGENTS AND STANDARDS

11.0 CALCULATION AND REPORTING OF RESULTS

Available Lime (as CaO)% by mass =28.04(A – B) N / M