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Environmental Engineering Laboratory, Civil Engineering Department, Bengal Engineering & Science University

Determination of Alkalinity of water


Principle: Alkalinity of water is its acid-neutralising capacity and is the sum of all the titratable bases.
Alkalinity values provide guidance in applying proper doses of chemicals in water and wastewater
treatment processes, particularly in coagulation, softening and operational control of anaerobic
digestion. The alkalinity of natural water is primarily a function of CO 3=, HCO3-, and OH- content and
thus the alkalinity is taken as an indication of the concentration of these constituents. Titration to pH 8.3
or a sharp change from purple to yellow colour of metacresol purple indicator will show complete
neutralisation of OH- & ½ of CO3=. This portion of alkalinity is known as "Phenolphthalein Alkalinity".
Similarly, titration to pH 4.5 or a sharp change of colour from blue to green of bromocresol green
indicator will indicate complete neutralisation of OH -, CO3= & HCO3-, which constitute "Total
Alkalinity".
Apparatus & Reagents:
i) Standard N/50 sulphuric acid.
ii) Bromocresol green & metacresol purple indicators.
iii) Burettes & 250 mL Erlenmeyer flasks.
Procedure:
(a) For Total Alkalinity (T): Take 50 mL of sample (or aliquot) in a 250 mL flask. Add 4 drops of
bromocresol green indicator. Titrate with N/50 H 2SO4 till the blue colour changes to green and
record the volume of titrant used.
(b) For Phenolphthalein Alkalinity (P): Take 50 mL sample (or aliquot) in a flask. Add 4 drops of
metacresol purple indicator and titrate with N/50 H 2SO4 till the purple colour changes to yellow
and record the volume of titrant used.
Result: Date of Analysis:

Volume Total Alkalinity(TA) Phen. Alkalinity(PA)


of Volume Volume
Sample Date of PA Remark
No.
Location Source Collection
Sample of N/50
H2SO4
Mean TA
(mg/l as
of N/50
H2SO4
Mean (mg/l as s
taken
(ml) used(ml (ml) CaCO3) used(ml (ml) CaCO3)
) )

Calculation: Total Alkalinity (T) or Phenolphthalein Alkalinity (P) will be calculated as follows
Volume (mL) of N H 2 SO 4  1000
Alkalinity, mg/L as CaCO 3  50
mL of sample
Caustic Alkalinity : Caustic alkalinity is the alkalinity corresponding to the OH - present in water
and calculated using the following Table. Carbonate and bicarbonate Alkalinity also can be
calculated using the same Table.

Value of P and T Caustic Carbonate Alkalinity Bicarbonate Alkalinity


Alkalinity

P=0 0 0 T

P < T/2 0 2P T-2P

P = T/2 0 2P 0

P > T/2 2P - T 2 (T - P) 0
P=T
P 0 0

Discussion on Result:
Environmental Engineering Laboratory, Civil Engineering Department, Bengal Engineering & Science University

Determination of pH of Water

Introduction: Measurement of pH is one of the most important and frequently used tests in.
Practically every phase of water supply and wastewater treatment, e.g., acid base neutralization,
water softening, precipitation, coagulation, disinfection and corrosion control, is pH dependent. pH
is used in alkalinity and carbon dioxide measurements and many other acid–base equilibria. At a
given temperature, the intensity of the acidic or basic character of a solution is indicated by pH or
hydrogen ion activity. It is expressed on a scale ranging from 0 to 14, which is the common
logarithm of the reciprocal of the hydrogen ion concentration. Completely neutral water measures
7.0 on the scale. The values of pH lower than 7.0 indicate the hydrogen ion concentration is greater
than the hydroxyl ion concentration, and the water is termed acidic. The opposite condition is
implied when the pH exceeds 7.0, and water is termed basic.
Acidic range Alkaline range
|______________________|______________________|
pH 0 7 14
pH may be represented by
pH = log 101/[H+] or, pH = - log10 [H+]
similarly, pOH = - log 10[OH-]
where, [H+] & [OH-] are the molar concentrations of hydrogen and hydroxyl ions,
respectively.
Pure water is slightly ionized and at equilibrium the ion product is
[H+][OH-] = Kw where Kw is the ion product of water,
= 10-14 at 250C
i.e., log10[H+] + log10[OH-] = log10Kw
or, – pH –pOH = -14
or, pH + pOH = 14
or, pOH = 14 - pH
Apparatus & Reagents: pH meter and 7.0 & 4.0 or 9.2 Buffer Solutions
Procedure :
1. Connect the instrument to 230V AC main. Display shown "SYS - 361 Ready".
2. Connect the pH electrodes to back panel.
3. Press “STD” key:
a) If standardization is not in memory; display shows "Put 7.00 pH".
b) If standardization is already in memory, display shows "RE-STD". The system is as
such ready for measurement. [However, if re-standardization is desired, press “STD”
key again and display will show. Put 7.00 pH.]
c) Put /dip electrodes in standard pH 7.00 buffer solution. Press “STD” key again.
Display will show "SYS BUSY", then finally will show -"Put pH 4.00 or pH 9.2".
d) Clean electrodes and dip in either pH 4.00 or pH 9.2 buffer solution. Press “STD”
key
again. Display would show "SYS BUSY" and finally "STD” over.
4. Clean, dry and dip electrodes in unknown solution.
5. Press "pH" key and display will show temperature and pH of the water to be tested.
Result: Date of Analysis: - ___________

Sample No. Location Source Date of Collection pH Remarks

Discussion on Result:
Environmental Engineering Laboratory, Civil Engineering Department, Bengal Engineering & Science University

Determination of Turbidity of water by Nephelometric Method.

Introduction: Turbidity is defined as an expression of the optical property that causes light to be
scattered and absorbed rather than transmitted in straight lines through the sample. This scattering
and absorption are caused by the interaction of light with suspended particles in the samples.
Turbidity is caused by the suspended solids including silt, clay, algae and other plankton, microbes,
and other fine insoluble particles. The higher the intensity of scattered light, the higher the
turbidity. However, turbidity is not a direct measure of suspended particles in water. Turbidity is
expressed in Nephelometric Turbidity Units (NTU).
Apparatus & Glassware:
Turbiditymeter (Nephelometer), Sample cell.
Reagents:
Preparation of Formazin suspension which is used as standard turbidity suspension is as
follows:
1) Solution I – Dissolve 1.0 g hydrazine sulfate [(NH 2)2.H2SO4], in distilled water and
dilute to 100 ml in a volumetric flask.

2) Solution II – Dissolve 10.0 g hexamethylenetetramine [(CH2)6N4], in distilled water and


dilute to 100 ml in a volumetric flask.

3) In a 100 ml volumetric flask, mix 5.0 ml Solution I and 5.0 ml Solution II. Let it stand
for 24 h at 25 0C, dilute to mark, and mix. The turbidity of this suspension is 400 NTU.
Operation of Nephelometer:
a) Switch the instrument ON and allow 10/15 minutes for warm up.
b) Select appropriate RANGE: (insert the CELL RISER for the 0-1000 NTU Range.)
c) Set STANDARDIZE CONTROL(CAL knob)to maximum and insert Sample Cell with
distilled water into cell holder and cover with shield. Using "SET ZERO CONTROL" adjust the
meter reading to zero.
d) Remove the above Cell and replace with another Cell containing standard solution
( Formazin).
e) Adjust "STANDARDIZE CONTROL" to get the desired turbidity reading on the scale.
Repeat steps from (c) to (e) twice.
4

f) Instrument is now ready for test samples. Insert the cell containing samples of unknown
turbidity in the cell holder and note the readings on meter.
g) Standardize the instrument when using other RANGES.

Result: Date of Analysis:-

Sampl Location Source Date of Range Turbidit Remarks


e No. Collection y
(NTU)

Discussion on Result:
Environmental Engineering Laboratory, Civil Engineering Department, Bengal Engineering & Science University

Light Shield

Scattered Light

Sample Cell

Photo Cell

Lenses

Lamp

Schematic Diagram of Nephelometric Light Path


Environmental Engineering Laboratory, Civil Engineering Department, Bengal Engineering & Science University

DETERMINATION OF HARDNESS IN WATER


Principle:
Hardness is caused by divalent metallic cations. Such ions are capable of reacting with soap
to form precipitates and with certain anions present in the water to form scale. The principal
hardness-causing cations are calcium and magnesium; however, strontium, ferrous and manganous
ions, which are normally present in trace quantities in natural waters, also cause hardness
In alkaline condition, EDTA reacts with Ca++ and Mg++ ions to form a soluble chelated
complex. Ca++ and Mg++ ions develop wine red colour with Eriochrome Black T under alkaline
condition. When EDTA is added as a titrant, the Ca++ and Mg++ divalent ions get chelated and sharp
change of colour from wine red to blue which indicates complete chelation. The pH for this
titration has to be maintained at around 10.0. At a higher pH, i.e., about 12.0, the Mg ++ ions
precipitate and only Ca++ ions remain in solution. At this pH, Murexide indicator forms a pink
colour with Ca++ ion. When EDTA is added, Ca++ ion gets chelated and a change from pink to
purple colour indicates complete chelation.
Reagents:
1. Buffer solution (Do not store more than 1 month): In the absence of Mg++ salts of EDTA,
dissolve 1.179 g disodium salt of EDTA and 780 mg MgSO4,7H2O or 644 mg MgCl2,6H2O in 50
mL distilled water. Add this solution to 16.9 g NH4Cl and 143 mL conc. NH4OH (sp. gr.
0.90-0.91) with mixing and dilute to 250 mL with distilled water. Keep the solution in a plastic
container.
2. Standard EDTA solution: Dissolve 3.723 g of disodium salt of EDTA in 1 L distilled water
(This solution may be standardised against standard calcium Solution).
3. Eriochrome Black T (EBT) : Mix 0.5 g dye with 4.5 g hydroxylamine hydrochloride.
Dissolve this mixture in 100 mL of 95% ethyl or isopropyl alcohol or, grind together in a mortar
200 mg EBT powder and 100 g solid NaCl.
4. Murexide (ammonium perpurate) Indicator: Prepare by mixing 200 mg murexide with 100
g NaCl and grinding the mixture.
5. 2N NaOH solution: Dissolve 20 g NaOH in 250 mL distilled water & store in polyethylene
bottles.
Procedure:
 Total Hardness (TH):
Take 50 mL of sample (or aliquot) in an Erlenmeyer flask. Add 1 or 2 mL buffer solution
and one pinch of Eriochrome Black T powder. Titrate with Standard EDTA solution till wine red
colour changes to blue. Record the volume of titrant used.
 Calcium Hardness (Ca H):
Take similar volume of sample (or aliquot) in an Erlenmeyer flask. Add 2 mL of 2N NaOH
to raise pH to 12, and one pinch of Murexide Indicator. Titrate with Standard EDTA solution till
pink colour changes to purple. Record the volume of titrant used.

Result: Date of Analysis:-

Calcium Hardness(Ca
Volume Total Hardness(TH)
Sa H)
of
Date of Volume Remark
mple Location Source Sample Ca H
No.
Collection
taken
of
EDTA
Mean TH
(mg/l as
Volume
of EDTA
Mean (mg/l as
s
(ml) (ml) (ml)
used CaCO3) used (ml) CaCO3)
(ml)
Environmental Engineering Laboratory, Civil Engineering Department, Bengal Engineering & Science University
mL of EDTA  1000
Calculation: Hardness, mg/L as CaCO 3 
mL of sample

Discussion on Result:

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