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 Silica 12
12 Phosphates 13
13 Iron 14
14 Dissolved Silica ( Low Silica < 2.0 ppm) 16
15 Nitrites 17
16 Nitrates 19
17 Oil and Grease 21
18 Equivalent Mineral Acidity 22
19 Chemical Oxygen Demand 23
20 Ammonical Nitrogen 24
21 Sulphide 25
22 Copper 27
23 Zinc 29

Issue No. : 1.0 Issued By :

Effective Date : 1.4.09 Approved By :

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 by checking the p H of standard 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. Gooch crucible
2. Glass 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 = -------------------------------

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 : 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 : 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 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 .

Issue No. : 1.0 Issued By :

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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

Issue No. : 1.0 Issued By :

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QC Department Title : Nitrites

Water Analysis Procedures

Reagents :
EDTA solution :
Dissolve o.5g. of EDTA in distilled water and dilute it to 100ml.
Sulphanallic acid solution :
Dissolve completely 0.6g. sulphanallic acid in 70ml hot distilled water. Cool and
add 20ml Conc.HCl, dilute to 100ml
Sodium acetate buffer solution :
Dissolve 16.4g. sodium acetate anhydrous or sodium acetate trihydrate in DM
distilled water and dilute to 100ml.
Alpha-naphthylamine hydrochloride solution :
Dissolve 0.6g. amino naphthalene hydrochloride in distilled water containing 1ml
of conc.HCl and dilute to 100ml.
Nitrite stock solution :
Dissolve exactly 493mg. Sodium nitrite in DM distilled water and make up to
1000ml in a volumetric flask.
Nitrite intermediate solution :
Pipet 10ml stock solution of NaNO2 and make up to 100ml.
1ml = 10microgram Nitrite as N
Nitrite working solution :
Dilute above 10ppm solution to 0.5ppm solution.

Calibration :
1) Pipette 1.0, 2.0, 3.0, 4.0 and 5.0ml of nitrite working solution in to 50ml
nessler tube corresponding to 0.5, 1.0, 1.5, 2.0 and 2.5microgram and make
up to the mark with DM distilled water.

2) Add 1ml of sulphanallic acid to blank, standards and mix it thoroughly.

After 10min. add 1ml alphanaphthylamine hydrochloride solution and 1ml
sodium acetate buffer solution and mix thoroughly.

3) After 10min. measure the absorbance spectrophotometrically at 520nm.

Plot a graph of Abs. Vs ug nitrite as N.

Prepare reagent blank using DM distilled water and set the spectrophotometer
to zero abs. Using the blank.

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Procedure :

1) Transfer 50ml of the clear sample or an aliquot diluted to 50ml in a nessler

 tube. Add 1ml EDTA solution and stir well.
2) Add 1ml of sulphanillic acid to blank, sample and mix the thoroughly. After
10min. add 1ml alpha-naphthylamine hydrochloride solution and 1ml
sodium acetate buffer solution and mix thoroughly.
3) After 10min. measure the absorbance of sample spectrophotometrically at
20nm. Find out the conc. of nitrite from the graph.
4) Prepare reagent blank using DM distilled water and set the
spectrophotometer to zero abs. Using the blank.

Method for coloured and turbid samples :

1) If the sample is coloured or contains suspended solids. Place 100ml sample

in a beaker add 2ml of aluminium hydroxide suspension and stir well.
2) Allow the sample to stand for a few min. decant the supernent add filter
through a filter paper and proceed as per above procedure.

Issue No. : 1.0 Issued By :

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QC Department Title : Nitrates

Water Analysis Procedures

Reagents :

Sulfuric acid solution :

Carefully and slowly add 500ml of conc.sulfuric acid to 75ml of distilled water.
Cool and store in a bottle.
Brucine sulphanillic acid solution :
Dissolve 1g of brucine sulfate and 0.1gm of sulphanillic acid in 70ml of hot distilled
water. Add 3ml of conc. hydrochloric acid cool and dilute to 100ml, with Distilled
water.
Sodium Arsenite solution :
Dissolve 1.83g. of sodium arsenite (NaAsO2) in 1liter of distilled water.
Potassium nitrate Standard solution :
Dissolve 1.631 g. potassium nitrate in 40ml of distilled water and dilute to
one liter. 1ml. = 1mg nitrate

Calibration :

1) Prepare a blank and series of standards using the standard nitrate solution.
The standards should cover the range from 0-50 ppm as N03.
2) In to a clean dry 50ml beaker pipette out 5ml of the standard add 1ml of
of Brucine sulphanalic acid ragent in to a second 50 ml beaker, measure
10ml of sulphuric acid.
3) Mix the contents of the beaker carefully adding the sample with brucine
sulphanilic acid reagent to the beaker containing the acid. Pour from one
beaker to the another six times to ensure mixing.
4) Set aside for 10 min in a dark place.
5) While the color is developing add 10 ml of distilled water to the empty 50
ml beaker. After 10 min interval add to the 10ml distilled water to the
sample and mix as before. Allow to cool for 20-30 min. in a dark place.
6) Measure the absorbance of the above standards at 410 nm. Prepare the
reagent blank using DM distilled water and set the instrument to zero
absorbance using the same.
7) Plot a graph of absorbance Vs the nitrate concentration in ppm.

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Procedure:

1) In to a clean dry 50 ml beaker pipette out 5ml portion of the sample.

 2) Add 1ml of brucine sulphanilic acid reagent.
3) In to a second beaker measure 10 ml of sulfuric acid.
4) Mix the contents of the two beaker by carefully adding the sample with the
brucine sulphanilic acid reagent to the beaker containing acid.Pour from one
beaker to another six times to ensure mixing.
5) Set aside for 10 min in a dark place.
6) While the color is developing add 10 ml of distilled water to the empty 50 ml
beaker. After 10 min interval add to the 10ml distilled water to the sample
and mix as before. Allow to cool for 20-30 min in a a dark place.
7) Measure the absorbance of the sample at 410nm. Prepare a reagent blank
using DM distilled water and set the instrument to zero absorbance using this
solution.
8) Determine the concentration of the sample from the graph.

NOTE : If residual chlorine is present add 0.1ml of arsenite solution to 50ml. portion of
sample for each 0.05ppm of chlorine, add a drop in excess and mix.

Calculation :

Find out nitrate content in ppm from 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 : Equivalent Mineral Acidity

 Water Analysis Procedures

Reagents :

0.02N NaOH :
Mixed indicator :
0.2g. Bromocresol Green & 0.04g. Methyl Red in 100ml. Isopropyl alcohol.
Strong acid cation exchange resin i.e. 225H :

Procedure :

1) Take about 30-40ml of regenerated 225H in a permutit column.

2) Pass about 100ml. Of distilled water sample through the column at a flow rate
of 3-5 ml/min and discard this whole volume.
3) Pass further 100ml of water sample through the resin column and collect in a
conical flask.
4) Pipette out 50ml. of the elute and titrate it against 0.02N NaOH using mixed
indicator. End point is pinkish red to sky blue. Note down the burette reading
R.

Calculation :

R X Normality of NAOH X 50 X 1000

EMA ppm as CaCO3 = ----------------------------------------------------

50

Where R = Burette reading.

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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)

Issue No. : 1.0 Issued By :

Effective Date : 1.4.09 Approved By :

QC Department Title : SULPHIDE

 Water Analysis Procedures

REAGENTS

1. Standard 0.1 N ( App ) Hypo solution

2. Starch Solution
3. 0.1 N ( App ) Iodine solution
4. 6N HCL

PROCEDURE

Pipette out 50 ml of 0.1 N ( App) Iodine solution in a Iodine flask then add about 100 ml
sample to it Shake well. Add 2.0 ml of 6N HCl Close the flask with cap and Keep it in dark
for about 15 minutes and then titrate with Std. Hypo solution using starch as indicator .The
color change is from brownish blue to colorless. Carry out a blank determination in the similar
manner.

CALCULATION

( A * B C * D ) * 160000
Sulphide = -------------------------------------------
( ppm ) Sample Volume(ml)

A = Normality of IODINE
B = Vol. Of IODINE
C= Normality of HYPO
D=Vol. Of HYPO

Issue No. : 1.0 Issued By :

Effective Date : 1.4.09 Approved By :

 QC Department Title : Determination Of Chlorides

Water Analysis Procedures

Reagents :

Standard NaCl solution: (0.0141N)

Dry NaCl AR grade in oven at approx. 140oC weight and dissolve 0.824 gm of
dried NaCl into DM water to a final volume of 100mls.

Standard Silver nitrate solution : (0.0141N)

Dissolve 2.395 gm of AgNO3 in distilled water and dilute to 1000 ml. Standardise
against Standard NaCl. Store in a brown bottle.
Potassium chromate indicator :
Dissolve 50 gms of K2CrO4 in a small amount of distilled water. Add AgNO3
solution untill a definite red precipitate is formed. Stand for 12 hours , filter and
dilute to 1 lit distilled water.

Procedure :

1) Take suitable aliquot of t he sample in the PH range 7 -10. Adjust the sample PH to
7- 10 with very dilute HNO3 or Dil NaOH. Add 1ml K2CrO4 indicator solution.
Titrate with standard AgNO3 to a brick red end point. Run AgNO3 titrant blank ..

Calculations:

Chlorides as Cl (ppm) = TV * Normality of AgNO3 * 1000 * 35.5

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

Issue No. : 1.0 Issued By :

Effective Date : 1.4.09 Approved By :

 QC Department Title : Phosphates by SnCl2
(O-PO4, Pyro PO4 and Organic
Water Analysis Procedures phosphates)

Reagents :
Stannous chloride :
Dissolve 2.5g. SnCl2 2H2O in a 100ml Glycerol. Heat in a water bath with stirring
to Hasen dissolution.
Ammonium Molybdate Solution :
Dissolve 25g. ammonium molybdate in 175ml distilled water(A)
280ml 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 50 ml sample in 100ml volumetric flasks, add 1ml (1+2)H2SO4 and 0.5g
Ammonium persulfate and digest for 15-30min. while boiling Add distilled water
and do not allow to dry. Cool the solution and add 4 ml of ammonium molybdate
solution& 0.5ml of Stannous chloride solution .Make up to 100ml and find
concentration after 15-20 min. at 650nm.
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 + 4ml Amm.molybdate and 0.5 ml of Stannous chloride
solution makeup
to 100 ml with D.Water
2) Wait for 15-20 minutes , record the absorbencies by Spectrophotomet
at 650 nm and plot the graph absorbance Vs Concentration

Issue No. : 1.0 Issued By :

Effective Date : 1.4.09 Approved By :

 QC Department Title : Copper D1688 Neocuproine Method-B

Water Analysis Procedures

INTRODUCTION
This method covers the determination of total copper in the 2 to 2,000 ppb ranges. This
method is based upon the yellow colour produced y the neocuproine cuprous complex. A
buffer solution maintains the pH between 4.0 to 6.0 bur full colour developments takes place
over the range of 2.3 to 9.0. The hydroxylamine hydrochloride reduces the copper to the
cuprous state.
SAMPLING
Although samples may be taken in polyethylene bottles, meticulously clean 500-ml glass
bottles with plastic caps are preferred. Prepare bottles by soaking in (HNO 3 1:9) for several
hours prior to use. Then rinse bottles with distilled water and drain before sampling. Take the
sample from the sample point, which has been continuously running for at least four hours.
Do no overflow or rinse bottle. Do not touch valve or jar line.
STANDARDS
Prepare a series of copper standards in 250 ml separatory funnels using the standard copper
solution (1ml=4mg Cu) add 1.0 ml of 1:1 HCL. Dilute each to 200 ml. Includes a blank and
treat similarly.
Application Range of Apparatus
Set spectrophotometer at 454nm (isoamyl)
1.0 cm cell 20 to 1000 ppb
1. cm cell 2 to 100 ppb

PROCEDURE
1. Place acidified sample bottle (with top off) in a hot water bath at 90c for one hour. (see
note)
2. Cool to room temperature and transfer 200 ml of the sample to a 250 ml separator funnel
3. Add 1 ml of NH2OH HCI (Hydroxyl Amine Hydrochloride) solution and mix by shaking.
4. Add 10 ml of NaC2 H3O2 (Sodium Acetate-Try hydrated) solution and mix again.
5. Then add 2 ml of neocuproine solution (4 ml for greater than 100 ug of Cu in sample).
6. Add 25-ml isoamyl alcohol and shake for one minute. Allow standing five minutes and
permitting aqueous phase to separate from alcohol phase. Alcohol phase will be at top
and aqueous phase can be drained off.
7. Collect alcohol layer and add 10 ml of isopropyl alcohol to clear solution. Swirl to mix
thoroughly.
8. Read in the appropriate cell at 454nm.

REAGENTS
1. Copper, standard solution (1 ml = 0.02 mg Cu) weigh 0.200 g of electrolytic copper.
Place it in a 250ml beaker under a hood, add 3 ml of water and 3 ml of HNO 3, (spgr 1.42),
and cover the beaker with a watch glass. After the metal has completely dryness. Do not
bake the residue. Cool the residue, wash down the sides of the beaker and the bottom of the
watch glass, and again evaporate the solution early to dryness to expel the HNO 3. Cool the
residue dissolves it in water, and dilutes the solution to 1 liter with water. One milliliter of the
standard contains 0.02 mg Cu or when diluted to 50 ml with water it represents a 0.4 mg/liter
(ppm) Cu solution.
2. Copper standard solution (1 ml, 4 ug Cu) Dilute 200 ml of copper solution (1ml/0.02 mg
Cu) to 1 liter with water. One milliliter of this std. Solutions contains 4 ug of copper or, when
diluted to 200 ml with water, it contains 20 ug/liter (ppb).
3. Hydrochloric acid (sp gr. 1.19)- concentrated hydrochloric acid (HCl).
4. Hydroxylamine hydrochloride solution (200 g/liter) remove traces of copper from the
solution prepared by treating in a separator funnel with neocuproine solution and isoamyl
alcohol solvent in accordance with procedure. Discard the organic extract.
5. Isoamyl alcohol, copper-free.
6. Isopropyl alcohol, copper-free.
7. Neocuproine solution (1g/litre)-dissolve 0.1 g of neocuproine (2.9-dimethyl-1, 10-
phenanthroline) in 50 ml of isopropyl alcohol. Dilute the solution to 100ml with water.
8. Sodium acetate solution (275 g/liter)-dissolve 55g of sodium acetate trihydrate (NaC 2H3O2).
3H3O) in water and dilute to 200 ml. Remove traces of copper from the solution by treating in
a separatory funnel with NH2OH.HCl, neocuproine, and isoamyl alcohol solvent solutions in
accordance with procedure. Discard the organic extract.
NOTE: -Copper analysis should be run prior to iron. The copper in boiler
feedwater is generally in the form of the soluble copper-ammonium
complex and the acidified sample (approximately pH 1.5) will prevent
plating out of elemental copper. The preliminary digestion step in the
above procedure will generally assume complete solubility of low
concentrations of copper (less than 50 ppb).
APPARATUS REQUIRED
1. 500 ml glass bottles with plastic caps with sample extraction hose.
2. 250 ml separating funnels.
3. 1 ml pipette (for 1:1 HCl)
4. 1 ml pipette (for NH2OH.HCl)
5. 10 ml pipette (for NaC2H3O2 solution)
6. 2 ml & 4 ml pipettes (for neo cuproine)
7. 25 ml pipette (for isoamyl alcohol)
8. 10 ml pipette (for isopropyl alcohol)
9. Spectrophotometer at 454nm (isoamyl)
10. 1.0 cm cell 20 to 1,000 ppb
11. 10.0 cm cell 2 to 100 ppb
12. Water bath suitable for heating(thermostat)

Issue No. : 1.0 Issued By :

Effective Date : 1.4.09 Approved By :

QC Department Title : Determination Of Zinc

 Water Analysis Procedures

1.REAGENTS

1. ACETATE BUFFER: Dissolve 67.5 gm Sodium Acetate and 30 ml of Acetic Acid

(Glacial) in 250 ml distilled water.

1.2 SODIUM THIOSULPHATE SOLUTION: 2.5 % in distilled water.

1.3 DITHIAZONE: 0.001% solution in carbon tetra chloride. This solution should always be
freshly prepared and should be kept in cold.

1.4 STANDAR ZINC SOLUTION: dissolve 1 gm of pure zinc in 10 ml of 1:1 HCI and
transfer to a 1 lt. Volumetric flask and make it up to the mark with distilled water. Mix well.
Keep this as stock solution 1 mg of zinc.

Transfer 10 ml of the stock solution by means of pipette to another 1 lt. volumetric flask. Add
5ml 1:1 Hcl and make it up to 1 lt. Mix well. This solution should be used as standard
solution. (1ml = 0.01 mg of zinc.)

II. APPARATUS: Separating funnels - 6nos.

III PROCEDURE: Take 1,2,3,4 and 5 ml of standard zinc solution in 5 separating funnels.
Add 5ml of acetate buffer 2 ml of Sodium Thiosulphate solution to each funnel. Mix. Add
10ml of Dithiazone reagent to each funnel and shake vigorously for 2 min. occasionally
releasing the pressure. Allow separating. Wipeout any water from the funnel by means of
filter papers. Run a blank side by side with this standard. Using distilled water. Measure the
optical density the carbon tetra chloride layer in 1-cm cell at 530nm. Draw a graph of OD vs.
mg of zinc.
Take sample containing 0.02 to 0.03 mg of zinc and test as mentioned above (i.e. take sample
in place of standard solution). Measure optical density and calculate ppm of zinc against
graph

VOLUMETIRC ESTRIMATION OF ZINC

THEORY;-Zinc reacts with dithiozone indicator weakly acid medium to form a red
compound. The zinc dithiozone reaction is extremely sensitive. Most interference
can be overcome by adjusting the PH to 4.0-5.5 by adding sufficient sod. Thiosulphate
The zinc is estimated by complexometric titration using disodium salt of EDTA & dithiozone
indicator in an acetate buffer medium.
REAGENTS
1.Acetate buffer soln..:-Dissolve 270gm.sodium acetate in distilled water Add 225ml of
glacial acetic acid(And one excelar grade).Mix it well and make up to 100ml with distilled
water.
2.Dithiozone indicator:-Dissolve 0.05gm of dithizone indicator powder in 100ml acetone.
Keep the soln. in a Stoppard bottle to avoid loss of acetone(carbon tetra chloride may used in
place of acetone).
3.0.02N EDTA;-Dissolve 3.7224gm of Edta(triplex) in 1000ml distilled water.
4.Isoprpyl alcohol:-Analar/execlar grade.
4.Sodium thio sulphate:- Dissolve 49.7gm sod.thiosulphate in distilled water. Add 0.1gm sod.
carbonate and make up to1000ml with distilled water.

PROCEDURE:-1.pippete out 100ml filtered water sample in conical flask.

2.Add 5ml of acetate buffer soln. followed by 1ml sod. Thiosulphite,mix it well.
3.Add 50ml of isopropyl alcohol and 1ml dithiozone indicator soln. mix it well.
4.A pink co lour indicate of zinc.
5. Titrate with EDTA soln. until the co lour changes from pink to blue violet.

CALCULATION:-Zinc mg/lit. As Zn =BR*0.02*32.75*1000/Volume of sample

Zinc mg/lit. As CaCO3 =BR*0.02*50*1000/Volume ofsample

Issue No. : 1.0 Issued By :

Effective Date : 1.4.09 Approved By :