Koç University Spring 2022

CHEM 103 GENERAL CHEMISTRY LABORATORY

EXPERIMENT 3
Water Analysis

Objective
The aim of the experiment is to analyse and determine by simple methods the most important
property of three different water samples. The investigated properties are freezing temperature,
boiling temperature, pH, chloride amount, total dissolved solid (TDS) amount and conductivity.

I. Introduction
Water is one of the most common compound on earth and composed of hydrogen and oxygen.
Typically high purity water does not have taste or odour and is liquid at room temperature. Its
tastes as drinking water originates from the dissolved salt compounds such as magnesium,
calcium, sodium cations and chloride, sulphate and carbonate, nitrate anions (sodium chloride,
magnesium sulphate, potassium nitrate, and sodium bicarbonate dissolved in water). Water is
commonly described as colourless however it has light blue colour due to the adsorption in the
red region of light. One of the most important property of water is its ability to dissolve
compounds and salts. It is essential for living organisms and it is proposed that life on earth
originates from the oceans. A human body has ~60 wt% water content in the form of body
fluids, blood, digestive juices and so on. Living organisms and human consumption requires
fresh water, however 97,25 % of water found on earth is salty water in oceans. Desalination is
a process to remove the dissolved salt in large quantity in sea water and oceans therefore a very
important industrial process meeting the increasing human life need.

Structure of Liquid Water

Water molecule is built up of two hydrogen atom and one oxygen atom. Between hydrogen and
oxygen there is polar covalent bond, where an electron is shared between hydrogen and oxygen
atom. This electron is located closer to the oxygen nucleus because of higher electronegativity
of oxygen and because of the geometry of the molecule. The geometry of the molecule is shown
on the Figure 1.

Figure 1.
Geometry, electronic structure and electron arrangement of water molecule.
The high electronegativity of oxygen compare to hydrogen results the polar bond in the water
molecule. Free oxygen atoms have six electrons in the valance shell, while the valance shell is
filled to eight when bound to two hydrogen atoms. Among these electrons two is shared
between the hydrogen and the oxygen atoms. The dots on Figure 1 represent the unshared
electrons of oxygen. The polarity difference occurs as a partial negative change (δ−) on oxygen
and partial positive charge (δ+) on hydrogen atoms in water. The weak attraction between the
partially negative and partially positive parts of the water molecules called hydrogen bonding
and is one of the most important intermolecular force. This relatively weak interaction between
water molecules is the source of the unusual property of water. Water has melting point of 0 °C
(32 °F), and boiling point, 100 °C (212 °F) which is significantly higher compare to similar
compounds like hydrogen sulphide.
The polarity of water molecules is also the reason why water is an effective solvent for ionic
compounds, salts. The most important property of water is summarized in table 1.

Table 1. Physical properties of water

Mw 18.02 g/mol

Melting point 0.00 °C

Boiling point 100.00 °C

Density
1.00 g/cm3
(maximum at 3.98 °C)

heat of fusion (0 °C) 6.010 kJ/mol

heat of vaporization (100 °C) 40.65 kJ/mol

heat of formation (25 °C) –285.85 kJ/mol

Water can be both a proton donor (acid) and a proton acceptor (base). This behaviour is
characteristic for amphiprotic molecules. The chemical equilibrium in water can be written as
follows:

H2O(l) + H2O(l) ⇌ H3O+(aq) + OH−(aq)

where the (l) corresponds to the liquid state and (aq) to the aqueous state.
The hydronium or oxonium ion (H3O+) is the hydrated form of H+. The concentration of H3O+
and hydroxide ion (OH-) is equal to each other and is 10−7 moles per liter (M). According to the
simplest acid-base theory (Arrhenius theory) an acid is a substance when dissociates in water
produces one or more hydrogen ions (H+) and a base is a substance which dissociates in water
to produce one or more hydroxide ions (OH-). The acidity of water is described by the amount
of dissolved hydronium ions concentration in logarithmic scale.
pH = −log [H+],
The pH of freshwater is changing between 6,0 – 8,2 and is the optimum level for most
organisms.

Selected EPA Drinking Water

Contaminant Standard
pH=6.5-8.5
Total Dissolved Solids (TDS) < 500 mg/L
Turbidity < 5 Nephelometric Turbidity Units (NTU)
Chloride < 250 mg/L
Nitrate < 10 mg/L
Copper < 1.3 mg/L
Lead < 0.015 mg/L

In theory, deionized water, having negligible amount of dissolved ions except OH- and H3O+
and should have a pH=7. However, the pH reading of DI water is 5,5-6,0. The low pH is the
effect of dissolved atmospheric carbon dioxide which is absorbed and produces carbonic acid
in water.
Chlorination of water is a method to disinfect water by chlorine (Cl2) which is a highly toxic
compound and will result the death of certain bacteria and microbes in tap water. When
dissolved in water the following reaction occurs:
Cl2+ H2O ⇌ HOCl + HCl.
On the other hand, the chloride concentration is a result of the dissolved salts such as NaCl,
CaCl2 and MgCl2 in drinking water. The recommended chloride amount in drinking water is
below 250 mg/l concentration. The NaCl concentration of sea water is 3.5 wt% (~0.6 M), which
means 3.5 g NaCl is dissolved in 100 g solution (be careful, not 100 g water!). The chloride
concentration can be determined by simple analytical chemistry methods (titration in the
presence of Ag+ ions) or by probes (Ion Selective Electrodes).

The total dissolved solids (TDS) is the amount of dissolved salts and organic compounds
appearing in drinking water dissolved or in molecular and microgranular form (such as sand or
clay particles less than 2 micrometer size). The main source of TDS in freshwater is calcium,
phosphates, nitrates, sodium, potassium and chloride ions. Determination of TDS level of
drinking water is a common method to classify water quality.

Water classification based on TDS level:

Fresh water: <500 mg/l
Brackish water: 500 to 30.000 mg/l
Saline water: 30,000 to 40.000 mg/l
Hypersaline: >40.000 mg/l

Conductivity is an other frequently used method to determine ionic content of a water sample.
It can be connected to the TDS value of water. The conductivity of deionized water water is
~5.5 μS/m, while drinking water has 5–50 mS/m conductivity and sea water around
5 S/m. The electrical conductivity of an electrolyte solution can be measured by resistance
measurements. For this purpose two usually cylindrical electrodes separated by a known
distance is dipped into the solution and a conductometer having alternating voltage measures
the resistance between these two electrodes. Strong electrolytes are containing compounds
dissociating completely, while weak electrolytes only partially due to the equilibrium between
ions and complete molecules of the compound. Kohlrausch found that the limiting conductivity
of anions and cations are additive: the conductivity of a solution of a salt is equal to the sum of
conductivity contributions from the cation and anion. Therefore increased amount of same type
salts in a water sample increases also the conductivity of the solution.

The solute concentration (amount of dissolved compound) can be shown as follows:

Molarity, M = moles solute/liter of solution
Weight % (wt %) = (mass of solute/100 g of solution)
Parts per million, ppm = (mass of solute/mass of solution) x 106 = mg solute/1 kg or l
solution
Mass per volume, mg/L = mass of solute/liter of solution
molality, = moles of solute/mass of solvent
mole fraction, χ = moles of solute/total moles

II. Experimental methods

Three different samples will be investigated:
• deionized water (DI water),
• drinking water and
• 0.6 M NaCl solution.
Part 1. Preparation of 0.6 M NaCl solution
Take a clean 250 ml volumetric flask. Calculate the mass of NaCl needed to prepare 500 ml 0.6
M solution, by converting the molarity (M) to weight% (wt%) concentration. Use a clean dry
beaker and measure the amount of NaCl on the balance. Use deionized water to dissolve the
sample in roughly 100 ml water. Transfer this solution to the volumetric flask. By rinsing the
beaker with 30-50 ml water portion slowly fill up till the mark on the volumetric flask.
Homogenize the sample by inverting the flask several times. Save the solution for the analysis.
Part 2. Freezing temperature, boiling temperature of deionized (DI) water
a) Place an immersion type thermometer into a water sample having 5-6 ice cubes in ~250
ml water. Wait ~5 min for the system to equilibrate (ice and water are in equilibrium).
Mix it frequently! Record the temperature when there is still some ice in the water.
b) Place 250 ml water on the hot plate and immerse a thermometer on such a way that it
does not touch the bottom of the beaker. Observe the formation of bubbles and record
the temperature when continuous bubble formation is observed. Read the temperature
for both case with 0,1 oC precision.
Part 3. Determination of the pH of water samples
Rinse the electrodes before measurements with DI water. Use a pH meter and dip into the
solution of the three different water sample. Rinse the electrode when you dip into a different
solution. Determine the pH of the solutions by reading the pH checkers. Record your results in
the data sheet.
Part 4. Detection of chloride amount
The chloride amount of the three samples will be compared visually using AgNO3 solution.
The reaction with Ag+ (0.1 M AgNO3) in nitric acid solution yields white insoluble AgCl, this
compound is soluble in dilute NH3.
AgCl + 2NH3  [Ag(NH3)2]+ + Cl−
The reaction must be carried out in 6 M HNO3 acidic solution, because several other Ag
compounds such as Ag2[CO3], Ag2[SO4], Ag3[PO3] etc. are also insoluble or slightly soluble in
neutral or basic medium. Acidify about 5 ml of your sample with 6 M HNO3 and add 3 drops
of AgNO3 solution. If a precipitate is formed (insoluble particles), check whether it is soluble
in 6 M NH3 solution.
Part5. Determination of total dissolved solid (TDS) amount
Use a large 250 ml beaker and warm it before the experiment to 104 °C for 1 h. Keep it in a
desiccator till used. Weigh it immediately before use. To assure homogeneous sampling, stir
sample with a magnetic stirrer and measure 100 g water sample into the pre-weighed beaker
(described above). Record the exact amount of the solution to your data sheet. Place the
evaporating dish (beaker) on a hot plate in a good ventilated hood bring it to boiling heat. Avoid
intense boiling as it can result small droplets escape from the solution! Evaporate to dryness in
30-60 minutes and continue to heat in the oven at 104 °C for 20 min. Cool in a desiccator and
weigh! Calculate TDS of your sample.

Part 6. Determination of the electric conductivity

There will be two conductometer given to you one with S/cm and one with mS/cm resolution.
Rinse the electrodes before measurements with DI water. Pipette with graduated pipette exactly
10 ml NaCl solution to a pre-weight beaker. Place the sample on the balance and add water
until the total weight of the sample is 100 g (10 ml solution and the water together). Dip into
the sample the conductometer and make sure that the water level is between the minimum and
maximum level of the conductometer. Read the value measured and record into the data sheet.
Measure also DI water and tap water after rinsing the electrode! The electric conductivity of
NaCl solution is shown on Figure 2. Electric conductivity of the solution increases non-linearly
with the increase of NaCl concentration for non-dilute solutions.

Figure 2. Electric conductivity of water as a function of 0-25 wt% NaCl concentration.

 Report 3: CHEM103

Water analysis

Name: Date:

Partner’s name:

Part 1. Preparation of 0.6 M NaCl solution

Calculate the mass of NaCl needed to prepare 250 ml 0.6 M solution:

- convert molarity (M) to wt% concentration:

- amount of NaCl needed for 250 ml solution:

Part 2. Freezing temperature, boiling temperature of deionized (DI) water

Tfreezing=

Tboiling=

How is the Celsius scale defined ie.: how does it depend on the water boiling temperature and
freezing temperature?

Part 3. pH determination of the water samples

pH
Measured with DI water Drinking water 0.6 M NaCl solution
pH meter

Why is the pH different than 7 for

b) drinking water?
a) pure water
Part 4. Detection of chloride amount
Observations: write your observation into the table.
Is the precipitate amount in line with the expectation? Comment in the table!

Cl- detection: amount of ppt.

DI water Drinking water 0.6 M NaCl solution
+ Ag+

Effect of 6 M NH3 solution

+ NH3 solution

Part5. Determination of total dissolved solid (TDS) amount

mbeaker2= mdrinking water= mbeaker2 with residue =
mbeaker3= mNaCl solution= mbeaker3 with residue =

Calculate the TDS based on your mass measurements for 100 ml water sample.

TDS drinking water=

TDS NaCl water=

Part 6. Determination of the electric conductivity

mbeaker=
Electric conductivity
DI water Drinking water 0.06 M NaCl
solution
Conductivity*

NaCl - -
concentration
(wt%)
*Indicate the units!
a) Using the electric conductivity for diluted NaCl concentrations Figure 3, determine the
concentration of NaCl in the solution and write it into the table! How does it correlated to the
0.06 M concentration?

b) Why is it not possible to estimate the NaCl amount in drinking water based on only
conductivity measurements?

Figure 3. Electric conductivity of water as a function of NaCl concentration (below 1.2 wt%
concentration).