Experiment 9:

Impurities in
Natural Water

Purpose
To learn some techniques for the purification of
natural water.
To learn how to test for the contaminants of natural
water (mostly ions).
To learn the technique of softening using an ionexchange resins.
To learn about the properties of phosphate salts
and their role as contaminants of natural water.
To determine quantitatively (by spectrophotometric
means), the phosphate content in a number of
water samples and in an unknown.

Contaminants in natural
water
Very little of Earth water is fresh water
(less than 3%).
Impurities any substance other the
H2O molecule.
Classified into five major categories.

Types of Contaminants

Suspended solids: sand, clay, silt, organic

material, (bits of leaves).

Dissolved gases: O2, N2, NH3, H2S, oxides of

nitrogen (NOx).

Dissolved ionic substances (salts):

a. Cations: H+, Li+, Na+, Mg2+, Mn2+, Fe3+, Ca2+
b. Anions: Cl, F, OH, NO3, SO42, HCO3,
PO43

Types of Contaminants
Dissolved organic substances:
vegetables and animal matter and their
decay products.
Microorganisms: bacteria, viruses,
protozoa, algae.

Theory and
Procedure

Distillation
Dissolve few crystals of cobalt chloride in water and distill.
Co2+(anhydrous)
blue

Co(H2O)62+, 2Cl
pink

CoCl4
blue

- Note the color of the distillate

- Save the distillate; Label A1.
Add concentrated NH3 to water and distill.

- Note the odor of the distillate

ammonia?

is the distillate free of

- Test with phenolphthalein

- Save the remainder of the distillate; Label A2.

Minerals in tap water: cations

Hardness in Ca2+ and Mg2+
Complex with EDTA:
M2+ + Y4

MY2

Determine water hardness by titration with EDTA

Report the total [Ca2+, Mg2+] in mol/L (M)

convert to mg CaCO3/L solution.

Minerals in tap water: anions

Chloride ion
Silver ion test:
Ag+ (aq) + Cl (aq)
AgCl (s)
test on tap water and distillates A1 and A2
Sulfate ion
Barium ion test:
Ba2+ (aq) + SO42 (aq)

BaSO4 (s)

test on tap water and distillates A1 and A2

Carbonate
Evaporation to dryness

scale

Ca(HCO3)2 (aq) CaCO3 (s) + H2O (l) + CO2 (g)

Mg(HCO3)2 (aq) MgCO3 (s) + H2O (l) + CO2(g)

At high T, solubility of CO2 decreases: equilibrium
driven to the right.
Test for the carbonates: HCl

Test for carbonate

CaCO3 (s) + 2 HCl (aq)
Ca2+ + 2Cl + CO2 (g) + H2O
MgCO3 (s) + 2 HCl (aq)
Mg2+ + 2Cl + CO2 (g) + H2O
Treat the solid with HCl

fizzing

Water Softening using ionexchange resins

Resins are polymers with cross-linking (connections between
long C chains in a polymer).
A resin has active groups in the form of electrically charged
sites.
Ions are attracted at these sites, and are replaced by other ions.

Two key factors:

affinity for a specific ion

number of active
sites for exchange

Structure of a resin

Ion-exchange
polymeric resin
with cross-linking
Cross-linking agent

Binding sites for cations

Properties of resins
Maximize the number of active sites; significant
surface areas are desirable (frequently cast in
the form of porous beads).

pH
Activity (efficiency) depends on:
Temprature

Types of resins
Household type:
The resin captures all metal ions and releases Na+
ions in their place
Na2R + CaCl2
CaR + 2 NaCl
- R represents the negatively charged site of the
cation exchange resin.
DOWEX: made of spherical (round) particles,
yielding optimal flow kinetics
highly efficient.

Water Softening using Deionizing

type resins
De-ionizing type (both cation and anion
exchange resins):
Cations taken and replaced by H+
Anions taken and replaced by OH
H+ + OH

H2O

De-ionization less expensive than

distillation due to lower energy
requirements.

Phosphate
Contamination
in Water

Phosphate: A Major
Contaminant*
Phosphate ion
serious contaminant in water (deprives living species
from sufficient oxygen).
enters water from agricultural run-off, biological and
industrial waste.
used in the manufacture of soap and detergents (major
ingredient, 50% in domestic sewage!).
contributes to excess growth of algae Eutrophication.

Quantitative determination
Complexation of PO43 with:
6

molybdate Mo7 O 24

vanadate VO 3

Reaction:

6
24

H 2 PO4 6 VO Mo7 O 13 H

H 9 Mo6O 40PV6 1 MoO3 3 H 2O

Mo 6 V6 (OH) 9 O 27 (PO 4 )

Vanadomolybdo
phosphoric acid

Calibration curve
Prepare 5 standard phosphate solutions:
From a stock KH2PO4 solution 3.230103 M,
prepare five standards:

6.460 10-5 M
1.292 10-4 M
1.938 10-4 M
2.584 10-4 M
3.230 10-4 M

420 nm

(1:50)
(2:50)
(3:50)
(4:50)
(5:50)

Determine b (M1)
from slope

Analysis of water samples

Determine the concentration (M) of
phosphate, [PO43] in three water
samples:
Tap water
Sea water
Unknown

Convert to mg P/L solution (ppm)

Procedure and report

Procedure
Report
Assigned questions: 1, 2 and 4
Useful links (applications)