QC Department Title :Index

Water Analysis Procedures

S.NO PARAMETER PAGE NO

1 pH 1
2 Conductivity 2
3 Total Dissolved Solids 3
4 Total Suspended Solids 4
5 Total Hardness 5
6 Calcium Hardness 6
7 Magnesium Hardness 7
8 Alkalinity 8
9 Chlorides 10
10 Sulphates 11
11 Phosphates 12
12 Silica 13
13 Iron 15
14 Oil and Grease 16
15 Chemical Oxygen Demand 17
16 Ammonical Nitrogen 18

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 QC Department Title :pH Test

Water Analysis Procedures

Procedure :

1) Take sample in a clean beaker.

2) Dip pH electode in the sample.
3) Wait for Stable Reading.
4) Record the pH Value.

Calibration of pH Meter :
The instrument is calibrated as given in instrument manual
With standard pH buffers daily.

Preparation of pH buffers ( 4.0, 7.0, 9.2 ) :

Dissolve one each p H buffer packet/capsule in 100 ml of
distilled water seperatelyand use for one month from the
date of manufacturing.

NOTE: Keep the electrode in 0.1 N H Cl , when not in use

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 QC Department Title : Conductivity

Water Analysis Procedures

Procedure :

1) Take sample in a Clean Beaker.

2) Dip Conductivity Cell in the sample.
3) Wait for Stable Reading.
4) Record the Value.

Calibration of Conductivity Meter :

The instrument is calibrated by checking the conductivity of standard KCl

solution daily

Conc of K Cl Solution Conductivity at 25 Deg C

1.0 N 111.3 ms
0.1 N 12.85 ms
0.01 N 1.408 ms
0.001 N 146.9 ms

Preparation of 1N K Cl :

Dissolve 7.45 g of K Cl in 100 ml of distilled water and use for one month
from the date of manufacturing.

NOTE: Keep the cell in distilled water , when not in use

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 QC Department Title : Total Dissolved Solids

Water Analysis Procedures

Apparatus :
1) Evaporating dish
2) Glass fiber filter paper GF-A (Whatman)
3) Filtration assembly

Procedure :
1) Place the fiber filter paper on the gooch crucible and wet in with the
sample.
2) Record weight of an empty evaporating dish as W1
3) Filter the sample through the crucible and then measure 100ml sample
and transfer to the evaporating dish and evaporate to dryness over a
water bath
4) Dry the evaporating dish in an oven at 110C for 2hrs.
5) Record weight of evaporating dish with solids as W2.

Calculation :

( W2 - W1) X 1000
Total Dissolved solids (ppm) = ----------------------------------------
100

W1 = weight of empty evaporating dish

W2 = weight of evaporating dish + residue

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 QC Department Title : Total Suspended Solids

Water Analysis Procedures

Apparatus :

1.
ooch crucible
2.
lass fiber filter paper GF-A (Whatman)
3. Filtration assembly

Procedure :

Place the fiber filter paper on the gooch crucible and record the weight as W1.

Shake the sample well and filter a known volume of the sample through the
crucible containing the filter paper.

Wash the crucible with distilled water . Dry the crucible for 2hrs. at 105oC in a
oven, cool in a dessicator and record the weight of the crucible as W2.

Calculation :

(W2 –W1) X 1000

Total Suspended Solids = -------------------------------
100

Where W1 = Weight of empty crucible + Filter paper

W2 = Weight of crucible + filter paper + suspended solids after drying.

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 QC Department Title : Total Hardness

Water Analysis Procedures

Reagents :
Buffer Solution :Dissolve 1.179g. sodium salt of EDTA dihydrate and
644mg.MgCl2.6H2O in 50ml distilled distilled water. Add this solution to 16.9g.
of ammonium chloride (NH4Cl) and 143ml liquid ammonia. Dilute it with
distilled water to one litre. Store in a tightly plugged container
Eriochrome black – T indicator : Dissolve 0.5g. of E.B.T. in 100 ml of methyl
alcohol. Keep it in amber coloured bottle.
Standard calcium chloride / Calcium carbonate solution :
Weigh 1.0000g. of CaCO3 or 1.470g. of calcium (CaCl2. 2H2O) and dissolve it in
Approx. 2-5ml of conc. Hydrochloric acid, transfer it to a one liter volumetric flask
and dilute up to the mark with distilled water.
Standard E.D.T.A. solution ( 0.01M ) / 0.02N:
Dissolve 3.723g. of AR – grade Na2EDTA.2H2O in distilled water and dilute to
one litre. Standardize against Standard CaCl2.2H2O / CaCO3 solution.
Inhibitor for Heavy metals: Dissolve 5.0 g sodium sulfide (Na2S.9H2O) in 100
ml Distilled water.

Procedure :
Take 25ml sample add 1ml ammonia buffer solution in 250ml conical flask, and
add 2 drops E.B.T. indicator. Titrate with E.D.T.A. Solution until the reddish
colour converts to blue colour.

Calculations :
Total Hardness as CaCO3 (ppm) = TV * Normality of EDTA * 1000 * 50
--------------------------------------------------
Sample volume

Note: If heavy metals like Iron are high, add 1 ml of inhibitor solution in hardness
test.
If alkalinity is more than 300ppm, take 25ml water sample add 1ml HCl and boil
for half an hour and proceed for hardness analysis.

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 QC Department Title : Calcium Hardness

Water Analysis Procedures

Reagents :

Indicator : Weigh 0.5g. of Calcon indicator mix in a pestle mortar with 5g. of
sodium sulphate or 5g. of Potassium Chloride until the mixture becomes
uniform.
Potassium Hydroxide or Sodium Hydroxide solution :
Dissolve about 225g. of KOH in 500ml. of distilled water or 40g. of sodium
hydroxide in 500ml. distilled water and keep the solution in polyethylene bottle for
preservation.
Standard Calcium solution : Follow the procedure mentioned in the method of
measuring total hardness.
Standard EDTA solution : Follow the procedure mentioned in the method of
measuring total hardness.
Inhibitor for Heavy metals: Dissolve 5.0 g sodium sulfide (Na2S.9H2O) in 100
ml Distilled water.

Procedure:
Take 25ml sample add 1ml NAOH buffer solution in 250ml conical flask, and add
1 spec of calcon . Titrate with E.D.T.A. Solution until the reddish colour converts
to blue colour.

Calculations:
Calcium Hardness as CaCO3 (ppm) = TV * Normality of EDTA * 1000 * 50
--------------------------------------------------
Sample volume

Note: If heavy metals like Iron are high, add 1 ml of inhibitor solution in hardness
test.
If alkalinity is more than 300ppm, take 25ml water sample add 1ml HCl and boil
for half an hour and proceed for hardness analysis.

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 QC Department Title : Magnesium Hardness

Water Analysis Procedures

Calculation :

Magnesium Hardness in ppm as CaCO3 =

Total hardness (ppm as CaCO3) - Calcium hardness (ppm as CaCO3)

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 QC Department Title : P – Alkalinity & M - Alkalinity

Water Analysis Procedures

Reagents :

Phenolphthalein indicator :
Dissolve 0.5g. of phenolphthalein in 50 ml IPA and 50 ml distilled water.
Mixed methyl red indicator :
Dissolve 0.02g. of methyl red and 0.1g. of bromocresol green in 100ml of
alcohol (95% v/v)
0.1N Sodium carbonate solution ( For standardisation):
Heat in advance sodium carbonate (Na2CO3) for 40- 50 min. Cool it in the
desiccator, weigh out 5.3000g. of 100% Na2CO3 and dissolve in distilled water.
Place the mixture in a 1litre volumetric flask and add distilled water up to the
mark.
0.1N H2SO4 :
Add 3ml sulphuric acid to the beaker in which 100ml of distilled water has been
placed before hand shake the solution thoroughly after cooling it, add distilled
water to increasing it to 1litre.
0.02N H2SO4 :
Place 200ml of 0.1N sulfuric acid in 1litre volumetric flask, add distilled water
that is free of carbonic acid to get one litre.Determine exact concentration factor
(f) by standardizing with std. Sodium Carbonate solution.

Procedure:

Take 50 ml of sample to be tested in a conical flask add 4drops phenolphthalein

indicator. If solution is Colorless P-Alkalinity is nil. If pink color appears
titrate the solution with 0.02N sulphuric acid until it turns colorless.

Calculations:

P-Alkalinity as CaCO3 (ppm) = TV * Normality of H2SO4 * 1000 * 50

-------------------------------------------------
Sample volume

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M – Alkalinity :

For above solution (from P-Alkalinity) add 4 drops mixed indicator and titrate
0.02N H2SO4 again.Take burette reading from the beginning. Solution until the
blue color converts to reddish purple color.

Calculations:

M-Alkalinity as CaCO3 (ppm) = TV * Normality of H2SO4 * 1000 * 50

--------------------------------------------------
Sample volume

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 QC Department Title : Determination Of Chlorides

Water Analysis Procedures

Reagents :

0.2N NaCl solution:

Dry NaCl AR grade in oven at approx. 105oC weight and dissolve 1.17gm of
dried NaCl into DM water to a final volume of 100mls.
0.02N NaCl solution :
Pipette out 10ml of 0.2N NaCl solution to 100mls with DM water.
0.02N Hg (NO3)2 solution :
7.46 ±0.02 gms of Mercuric Nitrate AR grade are dissolved in DM water along
with 6 mls of conc. Nitric acid LR. The final solution is made up to 2000
±10mls shake well and standardize against 0.02N NaCl solution.
0.2% w/v Diphenyl Carbonate indicator (DPC):
Dissolve 2 ±0.02gms of DPC in 1 liter of methanol LR.
Nickel Nitrate Buffer Solution:
Dissolve 500 ±5gms of Nickel Nitrate LR grade along with 21 ± 1 mls conc.
Nitric acid. Make the total volume to 420 mls with DM water.

Procedure :

1) Take suitable aliquot of t he sample add Diphenyl Carbozone indicator solution

and Nickel Nitrate buffer solution (each 1 ml for every 50ml of sample).
2) Titrate with 0.02N Hg (NO3)2 till colour of solution changes from green violet.
3) Take burette reading (BR) and calculate the chloride contents from formula
given below.

Calculations:

Chlorides as Cl (ppm) = TV * Normality of H2SO4 * 1000 * 35.5

--------------------------------------------------
Sample volume

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 QC Department Title :Sulphates ( By Turbidity Method )

Water Analysis Procedures

Interference :
If sample is coloured, make colour blank.

Reagents :
Standard sulphate solution :
Dissolve 0.1479g. anhydrous sodium sulphate in distilled distilled water and dilute
to 1000ml.

Buffer Solution A :
Dissolve 30g. of magnesium chloride MgCl2. 6H2O, 5g. of sodium acetate
CH3COONa 3H2O, 1g. KNO3 and 20ml. acetic acid. in 1lit. distilled water.

Buffer solution B: ( required when the sample contains less than 10ppm sulphate
ions.)
Dissolve 30g. of magnesium chloride MgCl2. 6H2O, 5g. of sodium acetate
CH3COONa 3H2O, 1g. KNO3, 0.111g. of sodium sulphate anhydrous and 20ml.
acetic acid.in1lit. distilled water.

Barium Chloride :
Barium chloride crystals of mesh size 20 – 30

Procedure :

Calibration and Analysis :

Take 2, 4, 6, 8, 10 ppm standard sulphate ion solutions in 100ml standard flasks.

To each flask add 25ml. of buffer solution add 0.5gm of barium chloride crystals
and measure absorbance at 420nm after 15 min diluting it to 100ml. Prepare
calibration curve of SO4 in ppm Vs Abs.

Repeat the above procedure using suitable aliquot of sample instead of standard
sulphate solution. Measure absorbance at 420nm and find out content of ions from
standard graph. Run blank simultaneously.

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 QC Department Title : Phosphates by Metol Method
(O-PO4, Pyro PO4 and Organic
Water Analysis Procedures phosphates)

Reagents :
Metol :
Dissolve 20g. metol in a 200ml distilled water -1
100g. sodium meta bisulphite dissolved in 200 ml distilled water –2
20g. citric acid dissolved in a 200ml distilled water.---3
Mix (1), (2) and (3) in 1liter standard flask and dilute to one litre.
Ammonium Molybdate Solution :
Dissolve 50g. ammonium molybdate in 200ml distilled water(A)
50ml conc.H2SO4 in 400ml distilled water(B).
Cool mix (A) & (B) and dilute to one litre
(1+2) H2SO4 :
One part of sulfuric acid mix carefully and slowly in two parts of distilled water.

Procedure for Total PO4:

Take 25 ml sample in 100ml volumetric flasks, add 1ml (1+2)H2SO4 and
0.5g Ammonium persulfate and digest for 15-30min. Add distilled water and
do not allow to dry. Cool the solution and add 5ml of metol solution& 5ml of
ammonium molybdate solution. Make up to 100ml and find concentration
after 30min. at 720nm.
A) Ortho phosphate procedure is same as above without adding ammonium
persulphate and digestion.
B) For total inorganic ( ortho & Pyro ) PO4, add acid and digest but do not
add ammonium persulphate.
C) Pyro/phosphate as PO4 = Total inorganic phosphate – Ortho phosphate
D) Organic phosphate as PO4 = Total phosphate – Total inorganic phosphate.

Calibration :
A) Dissolve 1.4325 gm of KH2 PO4 in 1 lit of DMwater , it is equivalent to
1000 ppm of PO4.
B) Dilute 10 ml solution (from A ) to100 ml with DMWater. it is equivalent
to100 ppm of PO4
Take 1,2 ,3 ,4,5,,6,7,8,9, and 10 ml From solution B separately in to a 100
ml volumetric flask ,
1) Add 1 ml of H2SO4 + 5 ml METOL + 5ml Amm.molybdate and makeup
to 100 ml with D.Water
2) Wait for 20 to 30 minutes , record the absorbencies by Spectrophotomet
at 720 nm and plot the graph absorbance Vs Concentration
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 QC Department Title : Dissolved Silica

Water Analysis Procedures

Reagents:

1:1 HCl

10% Ammonium molybdate:

Dissolve 10 grams of ammonium molybdate approximately in 100 ml of DM
distilled water(solution A).

10 % oxalic acid solution :

Add 100g of Oxalic Acid LR to 1000 ml of DM water.Stri till it dissolves

Reducing agent:
A) 30 grams of sodium metabisulphite is dissolved in approximately 150 ml
of DM distilled water
B) Grind 0.5 grams of 1-amino, 2-napthal 4 -sulphonic acid with 1.0g of
Sodium Sulphite and dissolve in 50 ml DM water.
Solution (A) and (B) are mixed together
Procedure:

Take 25 ml of sample in PVC cylinder and make it upto 50 ml. Then add 1 ml
1:1 HCl, 2 ml Ammonium Molybdate solution,Wait for 5 minutes.Then add
1.5 ml Oxalic Acid & 2 ml Reducing reagent . The silica content is analyzed on
spectrophotometer, at 650nm wavelength after 10 Minutes.

Note : Before starting analysis prepare silica standards and draw calibration
graph ( Abs. Vs SiO2 Conc. in ppm ).
This procedure follows Beer - Lambert's law .

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 QC Department Title : Dissolved Silica(Low Silica <
2.0ppm)
Water Analysis Procedures

Reagents:

Ammonium molybdate:
Dissolve 75 grams of ammonium molybdate approximately in 500 ml of DM
distilled water(solution A).
Add 100 ml of concentrated sulphuric acid in 260 ml of DM distilled water
while stirring constantly. Cool and add 320 ml of this solution to solution A, and
adjust the volume to 1 liter.

10 % oxalic acid solution :

Add 100g of Oxalic Acid LR to 1000 ml of DM water.Stri till it dissolves

Reducing agent:
A) 90 grams of sodium metabisulphite is dissolved in approximately 500 ml
of DM distilled water
B) 5 grams of 1-amino, 2-napthal 4 -sulphonic acid is dissolved in 100 ml of
DM distilled water with 7 grams of sodium sulphite.

Solution (A) and (B) are mixed together and dilute it to 1 liter with DM
distilled water.

Procedure:

Take 25 ml of sample in pvc cylinder add 2.0 ml of acid molybdate. Wait for 5
minutes.Then add 4 ml of oxalic acid and 1.0 ml of reducing agent. Wait for 10
minutes. The silica contents is analyzed on spectrophotometer, at 815nm
wavelength (on HACH 2010 – program no. 651)

Note : Before starting analysis prepare silica standards and draw calibration
graph ( Abs. Vs SiO2 Conc. in ppm ).
This procedure follows Beer - Lambert's law in the range of 0 to 2 ppm only

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 QC Department Title : Dissolved Iron

Water Analysis Procedures

Reagents:

Hydroxyl Ammonium Chloride:

Dissolve 10gm NH2OH. HCL in 100ml dist. Water.

Ammonium Acetate Buffer Solution : Dissolve 100g NH4C2H3O2

(Ammonium Acetate) in 60ml distilled water. Add 280ml conc. (glacial) acetic
acid.

Phenanthroline Solution : Dissolve 100mg 1, 10-phenanthroline monohydrate,

C12H8N2.H2O in 100ml distilled water by stirring.

Stock Iron Solution : Add slowly 20ml conc. H2SO4 to 50 ml distilled water
and dissolve 1.404g Fe(NH4)2 (SO4)2.6H2O. add 0.1N KMnO4 dropwise until a
faint pink colour persists. Dilute to 1000ml with iron free distilled water. 1ml =
200 ppm Fe.

Standard Iron Solution : (Prepare daily) Dilute 50ml stock solution to 1000ml
in a volumetric flask with iron free distilled water. 1ml = 10ppmFe.

Procedure :
Take 50 ml sample in a standard flask add 5 ml Hydroxyl ammonium chloride
10 ml Acetate buffer 4 ml phenonthraline and wait for 20 minutes.Record
obsorbance at 510 nm by spectrophotometer.

Calibration procedure :

Take 1 ml ,2,3,4,5,6,7,8,9,10 ml standards from 10 ppm Fe standard in 100 ml

vol.flasks seperately and proceed as per the above procedure and plot the graph
.

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 QC Department Title : Oil and Grease

Water Analysis Procedures

Reagents:

Sulphuric acid [1:1] :

Add slowly and carefully 250 ml conc. sulfuric acid to 250 ml distilled water
and cool
Petroleum ether :

Procedure:

1) Place 1 liter or appropriate volume of the sample in a suitable separating funnel.

2) Add 5 ml sulphuric acid per liter of sample.
3) Rinse the sample bottle with 15 ml petroleum ether. Add further 25 ml ether to
the funnel and shake vigorously for 5 minutes.
4) Draw the aqueous phase in to a clear container and transfer the ether layer
through a whatman no 40 filter paper in to a clean previously weighed 100 ml
beaker.
5) Continue the extraction twice and add the ether extracts to the beaker.
6) Distill off the ether over a water bath.
7) Cool in a dessicator and weigh.

Calculations :

Residue in the beaker(mg) X 1000

Oil and grease(ppm) = --------------------------------------------
Sample taken(ml)

Note : The method does not determine volatile fraction.

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 QC Department Title : Chemical Oxygen Demand

Water Analysis Procedures

Reagents :

Standard potassium dichromate digestion solution, 0.0417M (0.25N):

Dissolve 12.259g. of K2Cr2O7( previously dried at 1030C for 2hrs.) in 500ml
distilled water and dilute to 1000ml.
Sulphuric acid reagent :
Add Ag2SO4 powder to the standard sulphuric acid at the rate of
5.5g./Kg.H2SO4 . Let stand for a day to dissolve Ag2SO4.
Ferroin indicator Solution :
Dissolve 1.485g. of 1,10-phenanthroline mono hydrate and 695mg.
FeSO4.7H2O in distilled water and dilute to 100ml.
Standard Ferrous Ammonium Sulphate FAS ( 0.1 M ) :
Dissolve 39.2g. Fe(NH4)2(SO4)2.6H2O in distilled water. Add 20ml sulphuric
acid, cool and dilute to 1000ml. Standardize daily against 0.25N standard
K2Cr2O7 solution.
Mercuric sulphate :
Sulfamic acid :
Required only to remove nitrite interference.

Procedure :

Take 5 ml of sample in a 100ml round bottom flask add 0.4gms of mercuric

sulphate and 10ml of K2Cr2O7 and 15ml distilled water and 30ml of H2SO4
and keep for reflux for 2 hours. After cooling add 90ml of distilled water, add 3
drops of ferroin indicator and tirate with 0.1N FAS.
Run blank using distilled water in place of sample.

Caculation :

(Blank – titer value ) X Normality of FAS X 8000

COD ( ppm ) = ----------------------------------------------------------------
Sample Volume (ml)

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 QC Department Title : Ammonical Nitrogen For ETP

Water Analysis Procedures

Reagents:

Borate Buffer Solution:

Add 88 ml 0.1N NaoH to 500 ml approximately 0.025M Sodium tetraborate
(Na2B4O7) Solution (9.5 grams Sodium tetra borate and 88 ml 0.1 N NaoH
Solution Dilute to 1 liter.
Mixed Indicator Solution:
Dissolve 0.2 grams Methyl red indicator in 100 ml 95% ethyl or isopropyl
alcohol . Dissolve 0.1 grams methylene blue in 50 ml 95% ethyl or isopropyl
alcohol.
Indicating boric acid Solution:
20 grams Boric acid in Ammonia free distilled water, add 10 ml mixed indicator
Solution ,add dilute to 1 liter prepare monthly.

Procedure :

Take 500 ml Sample to a distillation flask and add 25 ml borate buffer Solution
and adjust to p H 9.5 with 6 N NaoH Using a p H meter.
Titrate ammonia in distillate with Standard 0.02 N H2SO4 titrant until indicator
turns a pale lavender.

Caculation :

Titer value of H2SO4 X Normality of H2SO4 X 1000 X 14

Ammonical Nitrogen = -------------------------------------------------------------------------
( ppm ) Sample Volume(ml)

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