[Link].
Test Name Procedure
1.0 Description Take about 10 ml of sample in a clean and dry test tube. Visually
examine the sample against the white background.
A Clear, colorless and odourless liquid.
2.0 pH To check the pH, wash the electrode 2 to 3 times with water sample and
transfer about 25 ml water sample in a beaker. Dip the electrode in the
water sample and measure the pH.
3.0 Chlorides To 10 ml of sample in a 250 ml conical flask. Add 5 ml of acetic acid, 50
ml of methanol and 0.15 ml of eosin solution. Stir, preferably with
magnetic stirrer, solution having yellow in color and titrate with the
silver nitrate solution drop wise, end point change as permanently pink
color with white turbid solution. Perform blank with purified water,
replace with water sample.
1 ml of 0.1 M silver nitrate is equivalent to 0.003545 gm of chlorides
Calculation:
(B. R.-Blank) x Normality of 0.1 N AgNO3x 0.003546 x 106
Chlorides =-------------------------------------------------------------
0.1 x Volume of Sample (in ml)
4.0 Sulphate Quantitative Test for Sulphate:
Take 50 ml of water in a 250 ml conical flask. Add 2 to 3 drops of
methyl red indicator solution, Add Hydrochloric acid drop by drop till an
orange red colour appears, Heat the solution to boiling and while stirring
gently, add warm barium chloride solution (10% solution) until
precipitation appears to be complete; then add about 2 ml in excess. If
amount of precipitate is small, add a total of 5 ml of barium chloride
solution. Digest precipitate at 80 to 90°C for at least 2 hours on water
bath. Weight the membrane filter (W 1) (Previously dry in an oven
maintained at 105°C, cool in desiccator). Filter the residue use by
membrane filter, and wash the precipitate with small portions of purified
water. After filtration place the membrane filter on petri dish and dry in
oven maintained at 105°C, Cool in desiccator. Weight the membrane
filter with residue (W2).
Calculate Sulphate content as per below mentioned formula:
(W2-W1) in mg x 411.6
Sulphate Content (ppm) = -------------------------------------
Volume of
Sample (in ml)
5.0 Total Hardness (As Heat the evaporating dish in oven at 105°C for 10 minute and cool in
CaCO3) desiccator and weigh the empty evaporating dish (X). Filter the 100
ml(X) of the water sample through Whatman filter paper No: 42 in
evaporating dish and evaporate the water sample on Waterbath/ Hotplate.
After completely evaporating of water sample, Then Heat the residue at
100-105°C in an oven for 1 hour, Transfer and cool the evaporating dish
with residue in the desiccator. Take final weight of evaporating dish and
residue (Z).
Calculate TDS as per below mentioned formula:
Calculation:
Volume of sample taken in ml = X ml
Weight of Empty evaporating dish = Y gm
Weight of Evaporating dish and residue = Z gm
Weight of residue = (Z – Y) gm
(Z – Y)
Total Dissolved Solid = ------------------ x 1000 x 1000
(in ppm) X
6.0 Total Dissolved Solids Heat the evaporating dish in oven at 105°C for 10 minute and cool in
desiccator and weigh the empty evaporating dish (X). Filter the 100
ml(X) of the water sample through Whatman filter paper No: 42 in
evaporating dish and evaporate the water sample on Waterbath/ Hotplate.
After completely evaporating of water sample, Then Heat the residue at
100-105°C in an oven for 1 hour, Transfer and cool the evaporating dish
with residue in the desiccator. Take final weight of evaporating dish and
residue (Z).
Calculate TDS as per below mentioned formula:
Calculation:
Volume of sample taken in ml = X ml
Weight of Empty evaporating dish = Y gm
Weight of Evaporating dish and residue = Z gm
Weight of residue = (Z – Y) gm
(Z – Y)
Total Dissolved Solid = ------------------ x 1000 x 1000
(in ppm) X
7.0 Total Suspended Solids Dry a whatman filter paper No: 42 by pre heating at specified
temperature 105°C in Hot air oven for 1 hour. Allow to cool in a
desiccator to room temperature. After immediately place on balance and
record the empty whatman filter paper weight (W1). Accurately passing
100 ml of water sample from whatman filter paper No: 42, After passing
sample 100 ml through whatman paper No: 42 dries that whatman filter
paper No: 42 in Hot air oven at 105°C for 1 hour. After drying, allow to
cool in a desiccator to room temperature. After immediately place on
balance and record the residual whatman filter paper No: 42 weight
(W2).
Calculate TSS as per below mentioned formula:
(W2 – W1) x 1000 x 1000
Total Suspended Solids (TSS) = ---------------------------------
Sample Volume (ml)
Where, W2 = Residual Whatman Filter Paper No: 42 Weight
W1 = Empty Whatman Filter Paper No: 42 Weight
8.0 Calcium (As CaO) Transfer 10 ml water sample in to 250 ml conical flask, Add 10 ml of 2M
NaOH, To this add 25 mg of Calcon Indicator Powder and shake well to
dissolve Calcon indicator, Solution having Reddish-Brown in colour and
titrate with 0.05 M EDTA Solution to end point change as permanently
Violet-Black colour.
Each ml of 0.05 M EDTA is eq. to 2.804 mg of CaO.
Calculate Calcium content as per below mentioned formula:
B. R. x Normality of 0.05 M EDTA x 0.002804 x 106
Calcium =---------------------------------------------------------------
(As CaO) 0.05 X 10
9.0 Iron Iron Standard Solution (20 mg/l): Dilute 1 volume of a 0.1726% w/v
solution of ferric ammonium sulphate in 0.05 M sulfuric acid to 10
volumes with water.
Iron free citric acid (20%w/v): Take 100 ml of volumetric flask,
dissolve 20 gm of citric acid anhydrous into it and make up the volume
up to the mark.
Ammonia solution, Iron free: Dilute 425 ml of strong ammonia
solution to 1000 ml with water.
Test Procedure:
Sample: Take 50 ml of water sample into a 100 ml Nessler cylinder.
Standard: Take 5 ml of standard solution (20 mg/l) into a 100 ml
Nessler cylinder, add 45 ml of iron free water.
Follow below procedure for Standard and Sample:
Procedure: Add 2 ml of a 20% w/v solution of iron-free citric acid and
0.1 ml of thioglycolic acid into a 100 ml Nessler cylinder. Make alkaline
with iron-free ammonia solution, dilute to 100 ml with water and allow to
stand for 5 minutes.
Observation: Any color produced in sample solution is not more than
that obtained by standard solution
10.0 Nitrate Preparation Standard solution (1000 ppm): Dissolve 163 mg of
Potassium nitrate in 100 ml volumetric flask and make up volume 100
ml with water (1000 ppm).
Preparation Standard solution (500 ppm): Dilute 25 ml of 1000 ppm
of nitrate standard solution and make 50 ml volume with water. (500
ppm).
Preparation Standard solution (100 ppm): Dilute 10 ml of 500 ppm of
nitrate standard solution and make 50 ml volume with water. (100 ppm).
Preparation Standard solution (5 ppm): Dilute 1 ml of 100 ppm of
nitrate standard solution and make 20 ml volume with water. (5 ppm).
Preparation Standard solution (2 ppm): Dilute 1 ml of 100 ppm of
nitrate standard solution and make 50 ml volume with water. (2 ppm).
Standard: Prepare reference standard using a mixture of 4 ml of nitrate
free water and 1 ml nitrate standard solution (500 ppm). Immerse it in an
ice water.
Sample: Take 5 ml of water sample in a test tube as test solution.
Immerse it in an ice water.
Follow below procedure for Standard and Sample:
Add 0.4 ml of a 10% w/v solution of potassium chloride, 0.1 ml of
diphenylamine solution (0.1% w/v solution in sulphuric acid) and, add
drop wise with shaking, 5 ml of nitrogen free sulphuric acid. Transfer the
tube to a water-bath at 50°C and allow to stand for 15 minutes.
Observation: Any blue color in the test solution should not be more
intense than that in a reference standard solution.
11.0 Ammonium Preparation of Ammonium Standard solution (2 ppm): Dissolve 74.1
mg of ammonium chloride in to 100 ml with water. Dilute 10 ml of
resulting solution in to 25 ml volumetric flask and make up to volume
with purified water. Dilute 2 volume of the above resulting solution to
100 volume with ammonium free water immediately before use.
Standard: To 20 ml of ammonium standard solution (2 ppm) and 10 ml
of ammonium-free water.
Sample: To 20 ml of water.
Follow below procedure for Standard and Sample:
Add 1 ml of alkaline potassium tetraiodomercurate solution. After 5 min,
Examine the standard solution and sample solution down the vertical
axis of the tube.
Observation: The sample solution is not more intensely colored than a
standard solution
12.0 Heavy Metal Reagent Preparation:
1. Lead standard solution (100 ppm Pb): Dissolve 0.400 gm of lead
nitrate in purified water containing 2.0 ml of nitric acid and add
sufficient purified water to produce 250.0 ml. Dilute 1 volume of
this solution to 10 volumes with purified water.
2. Lead standard solution (10 ppm Pb): Dilute 1 volume of lead
standard solution (100 ppm Pb) to 10 volumes with purified
water.
3. Lead standard solution (1 ppm Pb): Dilute 1 volume of lead
standard solutions (10 ppm pb) to 10 volumes with purified
water.
4. Acetate buffer pH 3.5: Dissolve 25.0 gm of ammonium acetate in
25.0 ml of purified water and add 38.0 ml of 7 M hydrochloric
acid. Adjust the pH to 3.5 with either 2 M hydrochloric acid or 6
M ammonia and dilute with purified water to 100.0 ml.
5. 7 M Hydrochloric acid: Dilute 59.5 ml of hydrochloric acid to
100.0 ml with purified water.
6. 2 M Hydrochloric acid: Dilute 17.0 ml of hydrochloric acid to
100.0 ml with purified water.
7. 6 M Ammonia: Dilute 45.0 ml of ammonia to 100.0 ml with
purified water.
8. Thioacetamide solution: Dissolve 4.0 gm of thioacetamide in
100.0 ml with purified water.
9. Thioacetamide reagent: Add 1.0 ml of a mixture of 15.0 ml of 1
M sodium hydroxide, 5.0 ml of purified water and 20.0 ml of
glycerin (85%) to 0.2 ml of thioacetamide solution, heat in a
water bath for 20 seconds cool and use immediately.
10. 1 M sodium hydroxide: Dissolve 40.0 gm of sodium hydroxide in
purified water to produced 1000.0 ml.
Procedure:
Standard Solution: Into a small nessler cylinder pipettes 10.0 ml of lead
standard solution (10 ppm Pb) and add 2.0 ml of the test solution and
mix.
Test Solution: Evaporate 150.0 ml to 15.0 ml on a water bath; pipette
12.0 ml of this solution into a small Nessler cylinder.
To each of the cylinder add 2.0 ml of acetate buffer pH 3.5, mix, add 1.2
ml of thioacetamide reagent, allow to stand for 2 min and view
downward over a white surface.
Observation: The color produced with the test solution is not more
intense than that produced with the standard solution.
