Doc.

No: 01 Page No: 1

Test procedure to measure water pH
Date: 12.09.06 Issue No:01

Scope:
To determine the water sample pH
Apparatus Required:
PH meter
Introduction:
With the electrometric method, the pH value is determined from the potential
difference between the measuring electrodes immersed in the liquid under test and
a reference electrode of known potential. For testing water, electrode assemblies
comprising a glass electrode and a calomel reference electrode are suited.
pH meter to be operated in accordance with the instruction supplied with it,
by its manufacturer. To ensure accurate measurements, air must be prevented
from getting to the sample, since pH values are strongly influenced by atmospheric
contaminants such as Carbon dioxide etc.
Where water is very pure, and the pH value and electrical conductivity are being
determined simultaneously, make sure that the pH electrodes are inserted after
the conductivity electrodes if the measuring points are connected in series.
Electrode treatment:
New glass electrodes and those that have been stored dry shall be
conditioned and maintained as recommended by the manufacturer. If the assembly
is in intermittent use, keep the immersed ends of the electrodes, in water between
measurements. For prolonged storage, glass electrodes may be allowed to become
dry, but the junction and filling openings of reference electrodes should be capped
to reduce evaporation.

Procedure:
1. Wash the electrodes by means of a flowing stream from a wash bottle.
2. Place the water sample in a clean glass beaker.
3. Insert the electrode and check temperature.
Doc.No: 01 Page No: 2
Test procedure to measure water pH
Date: 12.09.06 Issue No:01

4. Measure pH in the pH meter.

DO’S:
• Always dip the electrode in water.
• Wash the electrode with distill water before usage.
• Clean the electrode with 1:1 hydrochloric acid once in a week.
• Check pH with standard solution once in two days.
DONT’S:
• Never adjust standardization value during measurement.
• Never take the electrode from the electrode stand.
Record:
Record the pH values in log book.
Doc.No: 02 Page No: 3
Test procedure to measure Conductivity of water
Date: 12.09.06 Issue No:01

Scope:
To measure the conductivity of water
Apparatus Required:
• Conductivity meter
• Conduct bridge (0.5 to 0-5000 micro mho/cm with selector Switch)
• Dip cell (constant 2.0, 1.0, 0.1,0.02)
• Cylinder, rimmed glass, not graduated
• Thermometer, dial type (0-100ºc)
• Measuring cup, brass
Introduction:
The specific conductance of water is a measure of the ability of the water to
conduct an electrical current. This property is of no consequence in itself with
respect to water treatment. However, from a control standpoint, the conductivity
test is important as a direct measure of total ionizable solids in the water.
Specific conductance is inversely proportional to electrical resistance. Pure water is
highly resistant to the passage of an electric current and therefore has a low
specific conductance. However, if the water contains ions, the water becomes a
better conductor of electricity, and the specific conductance is increased. Inorganic
compounds such as sodium chloride and sodium sulfate dissociates into positive
and negative ions, which will conduct electricity in proportion to the amount of ions
present. The conductivity test, therefore, is not specific for any one ion, but rather
a measure of the total ionic concentration.
The conductivity test measures the total ionic concentration; the hydroxide ion
has a much higher conductance that the other ions present. Thus, for accurate
results the sample must be neutralized before measurement.
The basic unit of electrical resistance is the mho or siemen. Since electrical
conductivity is the reciprocal of resistance, the unique term ‘mho’ (“ohm” spelled
backwards) was chosen as the basic unit of conductivity.
Doc.No: 02 Page No: 4
Test procedure to measure Conductivity of water
Date: 12.09.06 Issue No:01

Selection of cell constant:

Selection of Cell constant was based on Sample conductivity that is within
measurable conductivity range.
Cell constant Conductivity range
0.01 0 to 10 µS/cm
0.1 0.1 to 10 µS/cm
1.0 10 to 100 mS/cm
10.0 100 µS to 1S/cm

Procedure:
• Remove the conductivity cell immersed in water.
• Wash cell with distills water before measurement by means of flowing water
stream from a wash bottle.
• Place the water sample in a clean beaker.
• Immerse the conductivity cell in the sample for measurement.
• Press the COND or TDS button for measurement, display shows BUSY.
• Wait for measurement and press ABORT button after measurement.
• Remove conductivity cell and place in the standard solution beaker.
Do’s:
• Wash the cell with distils water before measurement.
• Rinse with 1:1 HCl daily.
• Check temperature at the time of measurement.
• Ensure no air bubbles are present in water sample.
• During low conductivity measurement, ensure the sample is not in contact
with atmosphere.
• Ensure the conductivity cell is always immersed in distill water.
Doc.No: 02 Page No: 5
Test procedure to measure Conductivity of water
Date: 12.09.06 Issue No:01

Don’ts:
• Never keep the conductivity cell dry.
• Never adjust the standardization values without calibration.
• Don’t keep the conductivity cell in measurement mode.
Report:
Record the values in log book.
Doc.No: 03 Page No: 6
Calibration procedure for Conductivity meter
Date: 12.09.06 Issue No:01

Scope:
Calibrate conductivity meter by using standard solution.
Apparatus Required:
• Conductivity meter
• Standard stock solution
Preparation of standard KCl solution:
• Weigh 7.459 gm of dried KCl, dissolve and make up to 1litre in standard
flask. This gives 0.1M kcl solution.
• 0.01 M KCl solution is prepared by diluting 0.1 M KCl solution in the
proportion of 1:10.
Selection of standard calibration solution:
Standard solution chosen for calibration must be closer to the sample
conductivity measured.
Std solution Conductivity at 25 Deg C Temp. variation limit
0.1M KCl 12.88 mS +1.90%
0.01M KCl 1.413 mS +1.94%
0.001M KCl 0.146 MS +2.04%

Procedure:
• Switch on the instrument.
• Press CAL button, Display will show STD Y/N.
• Press CAL button, display will show PUT STD.
• Press PUT STD button to select the required standard for calibration.
• Dip the conductivity cell and temperature probe in standard KCl Solution.
• Press CAL button, display flashes Cal.
• After sometime display Show STD OVER. This indicates that the calibration
done and the instrument was ready for measurement.
Record:
Record the values in the calibration register.
Doc.No: 04 Page No: 7
Test procedure to determine total hardness
Date: 12.09.06 Issue No:01

Scope:
To determine total hardness present in water.
Apparatus Required:
• Graduated 50 ml burette.
• Graduated pipette or std measuring jar.
• 100 ml conical flask.
Reagents required:
• Standard EDTA (0.02N)
• Erichrome black-T Indicator.
• Ammonium buffer solution
Introduction:
Calcium and magnesium ions in water are sequestered by the addition of
sodium ethylene diamine tetra acetate. The end point of the reaction is detected by
means of an indicator, chrome – black T, at an optimum pH of 10.0 – 10.4 which
has a wine red color in the presence of calcium and magnesium, and a blue color
what they are sequestered.
Reagent preparation:
Standard Calcium Chloride Solution (1ml equals 1mg Caco3):
Dissolve 1.00 gm of reagent grade calcium carbonate containing less than
0.04% Mg (dry at 110ºc for one hour) in 10ml 1:1 Hydrochloric acid without
spattering, add 200 ml of distill water and heat to expel co2, cool and add few
drops of methyl orange indicator, transfer and dilute to 1000 ml with distill water.
Buffer solution:
Dissolve 16.9 gms of ammonium chloride in 143 ml of ammonium hydroxide.
Add 1.25 gm of magnesium salt of EDTA and dilute to 250 ml of distill water. Or
dissolve 1.179 g of disodium salt of EDTA and 780 mg of magnesium sulfate
(MgSO4.7H2O) or 644 g magnesium chloride (MgCl.6H2O) in distill water. Add this
solution to 16.9 g of ammonium chloride and 143 ml of conc. ammonium hydroxide
And make up to 250 ml of distill water.
Doc.No: 04 Page No: 8
Test procedure to determine total hardness
Date: 12.09.06 Issue No:01

Chrome Black T Indicator:

Weigh 0.5 gm of chrome black-T power and dissolve in 100 ml of Tri
ethanolamine.
Standard EDTA solution (0.02N or 0.01M):
Weigh 3.723 gm of EDTA and dissolve in one liter of distil water.
Procedure:
• Take known volume of water sample in a conical flask.
• Add few drops of ammonium buffer to increase pH above 10.2.
• Add Erichrome black-T indicator, color changes to wine red if hardness
present.
• Titrate with standard EDTA.
• Color changes from wine red to sky blue color on addition of EDTA.
• Stop titration when end point appears and note down the titration value.
Calculation:
Total hardness (As CaCO3) ppm= titration value X normality of EDTA X 50 X 1000
Volume of sample
Record:
Record the value in chemical analysis register.
DO’s:
• Clean the conical flask before use.
• Use freshly prepared reagents.
• Ensure ‘0’ before titration in burette.
• Titrate immediately after addition of reagents.
• Note the titration value immediately after titration.
• Take minimum of 10 ml sample for high hardness and 50 ml for low hardness
water.
• Check chemical self-life before usage.
• Discard solution and clean the conical flask after completion.
Don’ts:
• Never use reagents or solution without proper labeling.
Doc.No: 05 Test procedure to determine calcium & magnesium Page No: 9

Date: 12.09.06 hardness Issue No:01

Scope:
To determine calcium hardness present in water.
Apparatus Required:
• Graduated 50 ml burette.
• Graduated pipette or std measuring jar.
• 100 ml conical flask.
Reagents required:
• Standard EDTA (0.02N)
• Pattern reader powder or murexide indicator.
• Ammonium buffer solution
Introduction:
Calcium ions in water are sequestered by the addition of EDTA. The end point
of the reaction is detected by means of an indicator, murexide which is dark purple
in the absence of calcium. However, with calcium forms a light salmon red
complex. The optimum pH range is about 10.4.
Calcium Indicator:
Weigh 0.5 gm of pattern reader powder or ammonium purpurate (Murexide)
and dissolve in 100 ml of Tri ethanol amine.
Sodium hydroxide buffer:
Dissolve 4.0 gms of sodium hydroxide in water and dilute to 100 ml

Standard EDTA solution (0.02N):

Weigh 3.722 gm of EDTA and dissolve in one liter of distil water.
Doc.No: 05 Test procedure to determine calcium & magnesium Page No: 10

Date: 12.09.06 hardness Issue No:01

Procedure:
• Take known volume of water sample in a conical flask.
• Add few drops of sodium hydroxide to increase pH above 10.4.
• Add pattern reader or murexide indicator, color changes to wine red if
hardness present.
• Titrate with standard EDTA.
• Color changes from wine red to sky blue color on addition of EDTA.
• Stop titration when end point appears and note down the titration value.
Calculation:
Calcium hardness = titration value X normality of EDTA X 50 X 1000
(As CaCO3) ppm Volume of sample

Magnesium hardness= total hardness – calcium hardness

Record:
Record the value in chemical analysis register.
DO’s:
• Clean the conical flask before use.
• Use freshly prepared reagents.
• Ensure ‘0’ before titration in burette.
• Titrate immediately after addition of reagents.
• Note the titration value immediately after titration.
• Take minimum of 10 ml sample for high hardness and 50 ml for low hardness
water.
• Check chemical self-life before usage.
• Discard solution and clean the conical flask after completion.
Don’ts:
• Never use reagents or solution without proper labeling.
Doc.No: 06 Test procedure to determine total alkalinity (M Page No: 11

Date: 12.09.06 alkalinity) Issue No:01

Scope:
To determine total alkalinity present in water.
Apparatus Required:
• Graduated 50 ml burette.
• Graduated pipette or std measuring cylinder.
• 100 ml conical flask.
Reagents required:
• Sulphuric acid.
• Methyl orange or methyl red indicator.
Introduction:
The test is based on the determination of the alkaline content of a sample by
titration with a standard acid solution. In this measurements, the end points are
taken as points of change in the color of organic indicators phenolphthalein
(approx. pH 8.3) and methyl orange (approx. pH 4.3) represent definite points to
which the alkalinity of the sample has been reduced by the addition of the standard
acid solution.
Reagent preparation:
N/50 sulphuric acid:
Take 2.77 ml of conc.sulphuric acid in a standard flask and make up to 1000 ml
using distil water to prepare 0.1N solution.
0.02 N solution is prepared from above 0.1N solution by diluting 1:5 times.
Procedure:
• Take known volume of sample in the conical flask.
• Add few drops of methyl orange indicator and yellow color indicates presence
of alkalinity in water.
• Titrate with std sulphuric acid (0.02N) solution.
• Endpoint is the appearance of red color.
• Note down the titration value and discard the solution.
Doc.No: 06 Test procedure to determine total alkalinity (M Page No: 12

Date: 12.09.06 alkalinity) Issue No:01

Calculation:
M alkalinity = titration value X normality of acid X 50 X 1000
(As CaCO3) ppm Volume of sample

Record:
Record the value in chemical analysis register.
DO’s:
• Clean the conical flask before use.
• Use freshly prepared reagents.
• Ensure ‘0’ before titration in burette.
• Titrate immediately after addition of reagents.
• Note the titration value immediately after titration.
• Take minimum of 10 ml sample for high alkalinity and 50 ml for low alkalinity
water.
• Check chemical self-life before usage.
• Discard solution and clean the conical flask after completion.
Don’ts:
• Never use reagents or solution without proper labeling.
Doc.No: 07 Test procedure to determine phenolphthalein Page No: 13

Date: 12.09.06 alkalinity (P alkalinity) Issue No:01

Scope:
To determine phenolphthalein alkalinity present in water.
Apparatus Required:
• Graduated 50 ml burette.
• Graduated pipette or std measuring cylinder.
• 100 ml conical flask.
Reagents required:
• Sulphuric acid.
• Phenolphthalein indicator.
Introduction:
The test is based on the determination of the alkaline content of a sample by
titration with a standard acid solution. In this measurements, the end points are
taken as points of change in the color of organic indicators phenolphthalein
(approx. pH 8.3) and methyl orange (approx. pH 4.3) represent definite points to
which the alkalinity of the sample has been reduced by the addition of the standard
acid solution.
Reagent preparation:
N/50 sulphuric acid:
Take 2.77 ml of conc.sulphuric acid in a standard flask and make up to 1000 ml
using distil water to prepare 0.1N solution.
0.02 N solution is prepared from above 0.1N solution by diluting 1:5 times.
Standardization:
• Weigh accurately 0.22 gm of dried sodium carbonate and transfer to 100 ml
volumetric flask.
• Add few drops of methyl orange indicator.
• Titrate against freshly prepared sulphuric acid.
• End point is appearance of red color.
Doc.No: 07 Test procedure to determine phenolphthalein Page No: 14

Date: 12.09.06 alkalinity (P alkalinity) Issue No:01

Procedure:
• Take known volume of sample in the conical flask.
• Add few drops of phenolphthalein indicator and presence of pink color
indicates P alkalinity.
• Titrate with std sulphuric acid (0.02N) solution.
• Endpoint is appearance of pink to colorless.
• Note down the titration value and discard the solution.

Calculation:
P alkalinity = titration value X normality of acid X 50 X 1000
(As CaCO3) ppm Volume of sample

Record:
Record the value in chemical analysis register.
DO’s:
• Clean the conical flask before use.
• Use freshly prepared reagents.
• Ensure ‘0’ before titration in burette.
• Titrate immediately after addition of reagents.
• Note the titration value immediately after titration.
• Take minimum of 10 ml sample for high alkalinity and 50 ml for low alkalinity
water.
• Check chemical self-life before usage.
• Discard solution and clean the conical flask after completion.
Don’ts:
• Never use reagents or solution without proper labeling.
Doc.No: 08 Test procedure to determine free hydroxyl alkalinity Page No: 15

Date: 12.09.06 (oh alkalinity) Issue No:01

Scope:
To determine free hydroxyl alkalinity present in water.
Apparatus Required:
• 50 ml – measuring cylinder
• 250 ml – Erlenmeyer flask with stopper
• 50 ml – burette – readability 0.1 ml
Introduction:
This method is based on the titration of the hydroxide ion with a standard acid
to the phenolphthalein end point after the carbonate and phosphate ions have been
precipitated with srrantium chloride
Reagent preparation:
Strontium chloride solution:
Dissolves 4.5 g of strontium chloride in water and make up to one litre.
N/50 sulphuric acid:
Take 2.77 ml of conc.sulphuric acid in a standard flask and make up to 1000 ml
using distil water to prepare 0.1N solution.
0.02 N solution is prepared from above 0.1N solution by diluting 1:5 times.

Procedure:
• Take known volume of sample in the conical flask.
• Add few drops of phenolphthalein indicator and presence of pink color
indicates P alkalinity.
• Titrate with std sulphuric acid (0.02N) solution.
• Endpoint is appearance of pink to colorless.
• Note down the titration value and discard the solution.
Doc.No: 08 Test procedure to determine free hydroxyl alkalinity Page No: 16

Date: 12.09.06 (OH alkalinity) Issue No:01

Calculation:
P alkalinity = titration value X normality of acid X 50 X 1000
(As CaCO3) ppm Volume of sample

Record:
Record the value in chemical analysis register.
DO’s:
• Clean the conical flask before use.
• Use freshly prepared reagents.
• Ensure ‘0’ before titration in burette.
• Titrate immediately after addition of reagents.
• Note the titration value immediately after titration.
• Take minimum of 10 ml sample for high alkalinity and 50 ml for low alkalinity
water.
• Check chemical self-life before usage.
• Discard solution and clean the conical flask after completion.
Don’ts:
• Never use reagents or solution without proper labeling.

Method II

OH Alkalinity, ppm as CaCO3 = 2P - M

P – Phenolphthalein alkalinity, ppm as CaCO3

M – Methyl Orange alkalinity, ppm as CaCO3
Doc.No: 09 Page No: 17
Test procedure to determine sulphite in water
Date: 12.09.06 Issue No:01

Scope:
To determine sulphite as SO3 present in water.
Principle:
An acidified sample containing sulfite is titrated against potassium iodide –
iodate. Free iodine liberated by the iodide iodate reagent reacts with sulfite ion.
Formation of blue color with starch indicator indicates excess iodine present in
water.
Apparatus Required:
• 100 ml – measuring cylinder
• 250 ml – Conical flask
• 50 ml – burette – readability 0.1 ml
Reagent preparation:
Iodide Iodate preparation:
Weigh accurately 0.713 gm of potassium iodate and dissolve in 150 ml of distill
water and add 7 gms of potassium iodide, 0.5 gms of sodium hydrogen Carbonate
(Na2CO3) and make up to one liter.
Starch indicator:
Weigh 0.5 gm of starch to boiling water.
Hydrochloric acid:
Prepare 1:1 hydrochloric acid.
Procedure:
 • Take 100 ml of sample in a conical flask.
• Add 2 ml of 1:1 hydrochloric acid.
• Add few drops of freshly prepared starch indicator.
• Titrate against potassium iodide iodate solution.
• End point is appearance of blue color.
• Stop titration and note down the endpoint.

Doc.No: 09 Page No: 18

Test procedure to determine sulphite in water
Date: 12.09.06 Issue No:01

Precaution:
• To prevent oxygen absorption from the atmosphere, titration need to done
immediately after sampling.
• Sampling to be done in a closed bottle, prevent oxygen entry into it.

Calculation:

Sulphite (as SO3) ppm = Titration value X normality of KI-KI2 X 40 X 1000

Volume of sample

Record:
Record the value in chemical analysis register.
DO’s:
• Clean the conical flask before use.
• Use freshly prepared reagents.
• Ensure ‘0’ before titration in burette.
• Titrate immediately after addition of reagents.
• Note the titration value immediately after titration.
• Check chemical self-life before usage.
• Discard solution and clean the conical flask after completion.
Don’ts:
• Never use reagents or solution without proper labeling.
Doc.No: 10 Page No: 19
Test procedure to determine chloride in water
Date: 12.09.06 Issue No:01

Scope:
To determine chloride content in water.
Apparatus Required:
• 100 ml –conical flask.
• 50 ml –graduated burette.
• 100 ml –measuring jar.
Reagent preparation:
Potassium dichromate:
Take 5 gm of potassium dichromate and dissolve in 100 ml of water.
0.02N Silver nitrate solution:
Weigh 3.45 gm of silver nitrite and dissolve in 1 liter distil water.
Procedure:
• Take known volume of sample in a conical flask.
• Add few drops of freshly prepared potassium chromate indicator.
• Titrate against 0.02N silver nitrate solution.
• End point is appearance of reddish brown precipitate.
• Stop titration and note down the endpoint.
Calculation:

Chloride (as Cl) ppm = Titration value X normality of AgNO3 X 35.45 X 1000
Volume of sample
Record:
Record the value in chemical analysis register.

End point is the sharp color change from bluish green to reddish brown .
Doc.No: 13 Test procedure to determine total dissolved solids in Page No: 24

Date: 12.09.06 water Issue No:01

Scope:
To determine dissolved solids present in water.

SOLIDS INTRODUCTION:

The term “solids” is generally used when referring to any material suspended or
dissolved in wastewater that can be physically isolated either through filtration or
through evaporation.
Solids can be classified as either filterable or nonfilterable. Filterable solids may
either be settleable or nonsettleable. Solids can also be classified as organic or
inorganic.
“Filterable” solids are so small that they will pass through a standard laboratory
filter, while “nonfilterable” solids are large enough to be captured on a standard
filter pad. The nonfilterable solids are termed “settleable” if the solids settle out in
a standard laboratory settling container within a specified period of time. They are
called “non-settleable” if they fail to settle out within that time period. If solids are
“organic”, the material is carbon-based and will burn. “Inorganic” solids, on the
other hand, are mineral based and generally will not burn. Any material that was
at one time living (for example: body wastes, starches, sugars, wood, bacteria and
cotton) are all organic while limestone, iron and calcium are inorganic.
The amount of solids in wastewater is frequently used to describe the strength
of the waste. The more solids present in a particular wastewater, the stronger that
wastewater will be. If the solids in wastewater are mostly organic, the impact on a
treatment plant is greater than if the solids are mostly inorganic.
Normal domestic wastewater contains a very small amount of solids when
compared to the amount of water that carries it, generally less than 0.1%. This
can be misleading, however, because it may take only a very small amount of
organic residue to create large pollution problems. The number and severity of
pollution problems will depend on the type of solids that are involved.
Doc.No: 13 Test procedure to determine total dissolved solids in Page No: 25

Date: 12.09.06 water Issue No:01

As a rule, large quantities of organic solids will create more pollution problems
than will the same quantity of inorganic solids. Therefore, not only is it important
to know how much solids are present in the waste, but also the type of solids that
are present. The test procedures for solids provide essential information about the
level and type of solids coming into the treatment plant and whether the solids are
actually being removed in the plant processes.
SAMPLE COLLECTION:
Samples used for solids determinations can be either grab or composite. The
type of sample used will depend on the monitoring requirements, plant operating
procedures and the testing and sample storage capabilities of individual plants.
Whichever type is used, samples should be representative of the plant’s flow.
APPROVED METHODS:
The approved methods for total solids, total dissolved solids, total suspended
solids, fixed and volatile solids, and settleable solids are specified in the Federal
Register Part 1“Guidelines Establishing Test Procedures for the Analysis of
Pollutants.”

The parameter method and temperature if applicable are noted below

Parameter Procedure Temperature °C

Total Solids Gravimetric 103-105

Total Dissolved Solids Gravimetric 180
Total Suspended Solids Gravimetric 103-105
Volatile Solids Gravimetric 550
Settleable Solids Volumetric (Imhoff Cone)
Doc.No: 13 Test procedure to determine total dissolved solids in Page No: 26

Date: 12.09.06 water Issue No:01

TOTAL SOLIDS ANALYSIS:

DESCRIPTION OF TEST:
A well-mixed sample of wastewater is evaporated in a weighed dish and dried to
a constant weight at 103-105°C. The increase in weight of the dish and solids
compared to the empty dish represents the total solids (TS).

EQUIPMENT AND REAGENTS:

EQUIPMENT:
1. Evaporating dishes, 100 mL capacity, constructed from porcelain, platinum,
or high-silica glass
2. Drying oven, for operation at 98 and 103-105°C
3. Desiccator, with indicating desiccant
4. 100 mL graduated cylinders
5. Analytical Balance, 160-200 g capacity, capable of weighing to 0.0001 g
(0.1mg) *
6. Dish tongs
REAGENTS:
1. Distilled Water
Preparation of Evaporating Dish:
1. If volatile solids are to be determined, ignite a clean evaporating dish at 550
+/-50°C for 1 hour. If only total solids are to be determined, heat a clean dish
for 1 hour at 103-105°C.
2. Remove dish from muffle furnace or drying oven and place in a desiccator
until needed.
3. Weigh the cooled dish immediately before use.
Doc.No: 13 Test procedure to determine total dissolved solids in Page No: 27

Date: 12.09.06 water Issue No:01

Sample Analysis Procedure

1. Select a sample volume that will yield between 2.5 and 200 mg.
2. Mix sample well and measure into a graduated cylinder to the selected
volume.
3. Pour the measured volume into the preweighed dish.
4. Rinse any residue from the graduated cylinder into the evaporating dish with
a small amount of distilled water.
5. Evaporate to dryness in a drying oven at 98°C.
NOTE: If the selected volume exceeds the capacity of the evaporating dish,
repeat steps 2-5 in the same dish after evaporation until the selected volume
has been evaporated. Also, when evaporating in a drying oven, the temperature
should be lowered to approximately 98°C to prevent splattering.
6. Dry evaporated dish and residue for at least 1 hour at 103-105°C.
7. Remove dish from drying oven and cool in a desiccator to room temperature.
8. Weigh dish and residue and record weight.
9. Repeat steps 6-8 until a constant weight is obtained or until the weight loss
is less than 0.5 mg or 4% of previous weight.
NOTE: For most wastewater samples, drying to constant weight can be
accomplished in one step. The cycle of drying, cooling and weighing to achieve
constant weight should be performed at least one time for each sample source
to establish the drying time for that source. The established drying time should
be documented and maintained in the laboratory’s permanent records.
Calculation:

Total solids = (solids+dish wt)-(empty dish wt) x106 mg

(Weight of sample) lit
Doc.No: 15 Page No: 29
Test procedure to determine sulphate
Date: 12.09.06 Issue No:01

Scope:
To determine sulphate present in water by turbid metric method.
Principle:
Sulphate present in water is precipated in acetic medium with barium chloride to
from barium sulphate. The light absorbance of the barium sulphate suspension
is measured by spectro photometer.
Apparatus Required:
1. Conical flask
2. Spectrophotometer at 420 nm
Reagents:
1. Buffer solution: dissolve 30 gm magnesium chloride and 5 gm of sodium
acetate, 1.0 gm of potassium nitrate and 20 ml of acetic acid in 500 ml distill
water and make up to 1000 ml.
2. Barium chloride: 20% solution.
Standardization: 1ml =100 micro gram of SO4
1. Weigh 0.1479 gm of anhydrous sodium sulphate and dissolve it in 500 ml of
distill water and make up to 1000 ml standard flask.
2. Prepare intermediate standard solution of 100, 250, 500, 1000, 1500, 2000
ppm from stock solution.
3. Note the absorbance at 420 nm.
4. Plot graph to calculate slope.
Procedure:
1. Take 50 ml of sample in a 250 ml conical flask.
2. Take 50 ml of distill water in separate conical flask.
3. Add 10 ml of buffer solution to each flask.
4. Add 5 ml of 20% barium chloride solution and stir continuously for one min.
5. Measure the absorbance in spectro meter at 420 nm wavelength.
6. Estimate the sulphate content present in water using standard graph
available.
Doc.No: 16 DETERMINATION OF SOLUBLE SILICA IN Page No: 29
HIGH PURITY WATER
Date: 12.09.06 Issue No:01

SUMMARY OF METHOD
This calorimetric method depends of forming molydbi – silicic acid by reacting
the silica and ammonium molybdate in acid solution 1 – amino 2 – napthol –4-
sulfonic acid is then added to reduce the molybdisilicic complex. Oxalic acid is
added to destroy molybdophosphonic acid. This method is designed to determine
soluble silica with high accuracy in the range of 5 to 1000 mg/litre (ppb).

APPARATUS REQUIRED
§ 5 ml – pipette
§ 100 ml – polyethylene container
§ 1 ml pipette (for 1:1 HCI)
§ 2 ml pipette (for Ammonium molybdate solution)
§ 2 ml pipette (for oxalic acid solution)
§ 2 ml pipette (for 1,2,4 ANS solution)
§ Spectrophotometer at 815 nm
REAGENTS:
§ Amino – Napthol –Sulfonic Acid solution. Dissolve (0.5 g of 1 –amino-
2napthol-4sulfonic acid in 50 ml of a solution containing 1 g of sodium
sulphite (Na2So3). After dissolving, add the solution to 100 ml of a solution
containing 30 g of sodium hydrogen sulphite (NaHSO3). Make up to 200 ml
and store in a dark, plastic bottle. Prepare a fresh solution every 2 weeks.
§ Ammonium molybdate solution – (100 g/litre) Dissolve 10 grams of
ammonium molybdate tetrahydrate in 100 ml of deionized water. Filter this
solution each day before using.
§ Hydrochloric Acid (1:1) – Dilute 1 volume of concentrated hydrochloric
acid (HCL, sp gr. 1.19) with 1 volume of deionized water.
§ Oxalic Acid solution – (100 g/litre) – dissolve 10 grams of oxalic acid
dihydrated (H2C2O4 2H2O) in 100 ml of deionizedwater.
§ Silica, Standard Solution (1ml – 1 mg SiO2) – Dissolve 4.732 g of sodium
metasilicate (Na2SiO3 9H2O) – in water and dilute to 1 litre. Check the
Doc.No: 16 DETERMINATION OF SOLUBLE SILICA IN Page No: 29
HIGH PURITY WATER
Date: 12.09.06 Issue No:01

Concentration of this solution in accordance with Referee Method A. (ASTM 859).

Silica standards may be purchased from several chemical supply houses

PROCEDURE:
§ Pipette 5 ml of clear sample into a 100-ml polyethylene container.
§ Add 1 ml of 1:1 HCI solution
§ Add 2 ml of ammonium molybdate solution
§ Wait 5 minutes. The sample should be swirled during this period.
§ Add 2.0 ml of oxalic acid solution.
§ Add 2.0 ml of 1-amino-2napthol-4sulfonic acid solution and swirl.
§ Wait 5 minutes. Read on spectrophotometer at 815 mm. Transmittance of
the reagent blank versus deionized water should not be less than 98.8%
Calculation:

Soluble silica as SiO2: titre value x normality of Na2SO3 X 35.45 X 1000

Volume of sample
Doc.No: 17 Page No: 29
Test procedure to determine IRON
Date: 12.09.06 Issue No:01

Method: Phenanthroline
Principle:
Iron brought into solution,reduced to the ferrous state by boiling with acid and
hydroxylamine, and treated with 1,10 phenanthroline at pH 3.2 to 3.3.three
molecules chealate with each atom of ferrous iron to form an orange red complex.

Reference: Standard Methods for the Examination of Water and Wastewater

Preservation and Handling: Refrigerate, add HNO3 to <2. Max. 6 mos.

Concentration Range: 0.05 to 4.0 mg/l

Procedure (Total Iron):

(1) Mix the sample thoroughly and measure 50.0 ml into a 100 ml Erlenmeyer
flask. Run a blank concurrently.

(2) Add 2 ml conc HCL and 1 ml hydroxylamine soln.

(3) Heat the content; continue boiling until the volume reduces to 15 to 25 ml.

(4) Cool to room temperature and transfer to volumetric flask

(5) Add 10 ml ammonium acetate buffer soln and 4 ml phenanthroline soln and
dilute to 100 ml with distilled water.

(6) Mix thoroughly and allow at least 10 to 15 min for maximum color development.

(7) Read absorbance at 510 nm.

(8) Compare absorbance with standard curve prepared with standard solutions.

Procedure (Ferrous Iron):

(1) Acidify a separate sample with 2 ml conc. HCL/100 ml sample at the time of
collection.

(2) Immediately before analysis, withdraw a 50 ml portion; add 20 ml

phenanthroline soln and 10 ml ammonium acetate buffer. Dilute to 100 ml and
measure color intensity within 5 to 10 min.
Apparatus

(1) Spectrophotometer at 510 nm.

(2) Pipets, erlenmeyer flasks, beakers, and graduated cylinders.

Reagents

(1) Hydroxylamine solution: Dissolve 10 g NH2OH. HCl in 100 ml water.

(2) Conc HCl

(3) Ammonia acetate buffer soln: Dissolve 250 g NH4C2H3O2 in 150 ml water. Add
700 ml con (glacial) acetic acid.

(4) Phenanthroline soln: Dissolve 100 mg 1,10 - phenanthroline monohydrate,

C12H8N2 H20, in 100 ml water by stirring and heating to 80oC. Do not boil.
(Heating is unnecessary if 2 ml of conc HCl is added).

(5) Sodium acetate solution: Dissolve 200 g NaC2H302.

3H20 in 800 ml distilled water.

Stock solution:

Slowly add 20 ml of conc. Sulphuric acid to 50 ml of distill water and dissolve 1.404
gm of ferrous ammonium sulfate fe(NH4)2(so4)2.6h2o . Add 0.1N potassium
permanganate drop wise until faint pink color appears. Dilute to 1000 ml this is 200
microgram Fe per ml

Interferences:

(1) Strong oxidizing agents - excess of hydroxylamine is added.

(2) Metals (Cr, Zn, Co, Cu, Ni,) in high concentrations - add excess hydroxylamine
or extract as per reference.

(3) Organic matter - ash.