Name

: Kavisha a/p Sundraraj

ID

: 1205675

Name of partners

: Ryan Annasdass, Rita Sharmila Dewi, Jothy Priyaa

Practical Group

:3

Experiment

: 1- QUALITATIVE ANALYSIS QUALITATIVE

INVESTIGATION OF WATER SAMPLES

Date

: 2nd June 2016

Lecturer

: Miss Chang Chew Cheen

Submission Date

: 16th June 2016

Title: Qualitative investigation of water samples

Objectives:
i.

To investigate the quality of water samples

ii.

To identify the ions present in standard solution, tap water and unknown water

Introduction:
The list of the main dissolved mineral components of natural waters include the ions
Na+, K+, Ca2+, Mg2+, H+, Cl-, HCO3-, CO32-, SO42- and gases O2, N2, CO2 and H2S. In small
amounts such ions contain: Fe2+, Fe3+, Mn2+, Br-, I-, F-, BO2-, HPO42-, SO32-, HSO4-, S2O32-, HS-,
HSiO3-, HSO3- and gases CH4, Ar, He, Rn. Other substances are in water in the smaller
amounts. Water always contains ions H+ and OH- in small amounts. The active concentration
of hydrogen ions in natural and waste water is usually characterized by pH.
Hydrocarbonic ions occur in natural waters owing to dissolution the limestone by the
carbonic acid. These anions are in all waters, except for soft waters with pH lower than 4. In
fresh sources they dominate. The level of pH of the majority of natural waters is caused just
by the presence of these ions in them. The contents of hydrocarbonic ions in superficial
waters usually do not exceed 250 mg/l, and in waters of northern reservoirs and number of
the mountain rivers their concentration is about 50 mg/l. The concentration of ions SO42- in
natural waters containing the ions Ca2+, does not exceed 1500 mg/l owing to small solubility
of CaSO4, however in well mineralised waters as a result of reduction of activity of ions the
concentration of ions SO42- is frequently higher. So, in sea water with the contents of salts of
35 g/kg and Ca2+ - 0,0104 mole/kg the concentration of SO42- achieves 2,7 g/kg. Galogenic
ions are submitted in natural waters mainly by chloride ion. The contents of chloride ions in
water of natural reservoirs varies over a wide range. In river and lake waters, the

concentration of them is insignificant. However with increase of the mineralisation water

absolute and relative quantity of Cl- increases; it is the main anion in the seas and greater part
of hydrochloric lakes; in sea water the chlorid-ions make 87 % of weights of all anions. The
wide dispersion of ions of chlorine is promoted by industrial and physiological activity of the
man: the ion Cl- is not acquired by living beings.
The concentration of fluorine in superficial waters is usually insignificant - below
sanitary norm (0,7-1,5 mg/l); in underground waters the contents of fluorine sometimes
considerably exceeds these norms.
The ions of alkaline metals - magnesium and calcium, determine general rigidity of
water. From ions of alkaline metals in natural, especially in sea, waters there are in plenties
ions of Na, in smaller - K, and also Rb (about 0,2 mg/l) and Li (about 0,1 mg/l). On
prevalence in natural waters Na+ occupies the first place, making more half of all the cations
contained in them. The amount of K+ usually makes 4-10 % of number of the Na+ (ions,
present in water. In fresh waters the concentration of Na+ + K+ usually does not exceed
several milligrammes on litre. The reason of occurrence of connections of nitrogen in water
except for biological pollution is also direct fixing of nitrogen from an atmosphere by
bacteria. The concentration of NO3- in water is significant more, in earth waters of the top
horizons the amount of it achieves sometimes several tens of milligrammes on litre.
Other metals meet in natural water in very insignificant concentration. The more
detailed items of information are available for sea water. In waters of the rivers and fresh
lakes on the average contains, mg/l: Co - 0,0048, Ni - 0,001, Zn - 0,02. Cu - from 0,0001 up
to 0,01. The large concentration of metals in water is the result of industrial pollution. The
radioactive elements are extremely rarely met in all waters, that is caused by their distribution

in mountain breeds. In water of the rivers about 2*10-8 g/l of uranium, about 10-9 mg/l of
radium.
Materials:

Standard solution

Tap water

1 M NH4OH

NH4Cl

(NH4)2C2O4

Na2HPO4

1 M HCl

K4Fe(CN)6

K3Fe(CN)6

0.2 M AgNO3

0.25 M (NH4)2MoO4

20 % NaOH

Apparatus:

Test tubes

Litmus paper

Test tube rack

Beaker

Hot plate

Measuring cylinder

Dropper

Procedure:
Part 1: Standard. Solutions containing all the ions were used to familiarize you with the tests.
A blank sample of demineralized water was run alongside it.
Part 2: Tap water. 200 250 cm3 of tap water was evaporated to about one- third of the
original volume. Ions present were analyzed. If test is very faint, it indicates a trace.
Part 3: Unknown. A sample of solution was obtained in a small, clean beaker. The results
were analyzed and recorded.
Tests:
Ca2+

1 mole dm-3 NH4OH was added until blue to litmus into 4 cm3 of water sample. When dark
precipitate formed, it was filtered off, a little NH4Cl and (NH4)2C2O4 were added. It was
placed in water bath and warmed for a minute. A white precipitate indicates calcium in the

Mg2+

form of calcium oxalate.

The calcium oxalate was filtered off from above sample and a little NH4OH and NH4Cl were
added to the filtrate and then a few grains of Na2HPO4. The formation of white crystalline
precipitate, ammonium magnesium phosphate, upon shaking, indicates magnesium.

Fe3+

A few drops of 1 mole dm-3 HCl and a little [K4Fe(CN)6] were added to a fresh sample of

Fe2+
Cl-

water. A dark blue precipitate (Prussian blue) shows presence of Fe3+.

HCl and [K3Fe(CN)6] were added and a similar dark blue precipitate signifies Fe2+.
0.2 mole dm-3 AgNO3 solutions were added. A cloudy white turbidity develops which will

3-

PO4

turn purplish in sunlight.

Litmus paper was used to check if sample is either strongly basic or acidic. It was
neutralized with 1 mole dm-3 NH4OH if acidic, or 1 mole dm-3 HNO3 if basic, then about 1-2
cm3 of 0.25 mole dm-3 (NH4)2MoO4 solution was added, it was warmed in water bath and

NH4-

NO3

checked for the formation of a bright yellow precipitate.

3 cm3 sample of water was placed in a boiling tube. 10 drops 20 % NaOH solution and an
anti-bumping chip were added, then boiled.
All the ammonia was boiled off, and then 5 mg Devardas alloy was added and boiled again.
Emission of ammonia at this stage indicates nitrate.
The test for ammonia:
i.

Smell

ii.

A drop of HCl

Results:
Ions

Standard solution

Tap water

Lake water

Ca2+

White precipitate

No precipitate formed.

No precipitation was

formed. Positive

Clear solution.

formed. Clear solution.

Formation of white

No crystalline formed.

Traces of white

Mg2+

Fe3+

crystalline precipitate.

crystalline precipitate

Positive

formed.

From yellow to dark

Clear to dark yellow

Clear to dark yellow

blue solution.

solution.

solution.

Dark blue precipitate

No changes

No changes

Clear to yellow solution.

Clear to yellow solution.

formed. Positive.
Fe2+

From yellow to dark

blue solution.
Dark blue precipitate
formed. Positive.

Cl-

Solution turns from light White cloudy solution

White turbidity remains

yellow to cloudy.

unchanged.

Under sunlight, purple

turns purple when being

exposed to sunlight.

solution formed.
Positive.
PO43-

red litmus paper turns

Blue litmus paper

blue before adding

remained unchanged.

HNO3. Bright yellow

precipitate formed.

No changes.

Bright yellow precipitate

formed.

Positive.

NH4+

Gas evolved while

Gas evolved while

Gas evolved while

boiling. Red litmus

boiling. Red litmus paper

boiling. Red litmus paper

paper turns blue.

remains unchanged.

remains unchanged.

NO3-

Gas evolved while

No changes to red litmus

No changes to red litmus

boiling. Red litmus

paper.

paper.

Gas evolved.

Gas evolved.

paper turns blue.

Positive.

Discussion:
Water sample is the main objective in this experiment to determine the ions are
present in a standard solution, tap water and unknown sample. These ions are detected by the
formation of a coloured solution or a precipitate when special reactants are added to the water
samples such as NH4Cl, (NH4)2C2O4, Na2HPO4, AgNO3, potassium hexacyanoferrate(II),
potassium hexacyanoferrate(III) and (NH4)2MoO4.

For standard solution which contains all the ions was tested to get used with the test
and to observe and compare the results. For calcium ion test in standard solution contains
high calcium ions contents due to the formation of white precipitate after reacted with NH4Cl
and (NH4)2C2O4. The precipitating agent for Ca2+ is the oxalate anion, C2O42-. Initially, the
solution was acidic with containing undissociated oxalic acid, H2C2O4. The calcium ion will
not be precipitated in this form. After heating, the urea, (NH2)2CO, decomposed slowly to
form -OH, which it neutralized the oxalic acid to release the oxalate anion. Thus, forming
white calcium oxalate precipitate. In tap water and unknown samples, it is found to have no
trace amount of white precipitate which indicated that there is no concentration of calcium
ions.
NH4OH + H2O NH3 + 2H2O............( red litmus to blue)

NH4Cl + H2O NH4OH + HCl

Cl- + (NH4)2C2O4 C2O42- + NH4Cl
Ca2+ + C2O42- Ca(C2O4)........... (white precipitate)

The traces of white crystalline precipitate, ammonium magnesium phosphate indicate

the presence of magnesium in unknown sample while for the tap water there is no formation
of precipitate which shows that there is no presence of magnesium ions in the boiled tap
water.
NH4Cl + H2O NH4OH + HCl
Na2HPO4 3Cl- PO43- + 2NaCl + HCl
Mg2+ + PO43- + NH4+ NH4MgPO46H2O
Potassium hexacyanoferrate(III) is the inorganic salt of the coordination complex of 6.
This salt forms lemon-yellow monoclinic crystals. The reaction involves treatment with ferric
salts to give Prussian blue. Prussian blue, the deep blue is generated by the reaction of
K3[Fe(CN)6] with ferrous (Fe2+) ions. Potassium hexacyanoferrate(II) is used to test the
presence of Fe3+ in water sample. There is no blue precipitate for both tap and unknown thus
there are no Fe3+ and Fe2+ in both the water sample. However, there is presence of Fe3+ and
Fe2+ in the standard solution.
6 HCl + K4[Fe(CN)6] 6 HCN + FeCl2 + 4 KCl
6 HCl + K3[Fe(CN)6] 6 HCN + FeCl3 + 3 KCl

AgNO3 ions were dissociated in order to test the presence of chloride ions each of the
water samples that were added with AgNO3. Then, the Ag+ ions reacted in the presence of Clions. AgCl is insoluble in water and it precipitated to become solid. The colour of AgCl solid
is cloudy white and turns purplish under sunlight. This shows that the standard solution and
boiled tap water contains chloride ions whereas for unknown solution there is no changes in
solution which the white turbidity does not turns into purple solution.
AgNO3 Ag+ + NO3Ag+ + Cl- AgCl
For the phosphate test, the red litmus paper was changed into blue before adding the
HNO3. After experiment conducted, the standard solution and the tap water contained
phosphate. The solution turns bright yellow after added by (NH4)2MoO4 and let to be boiled.
The phosphate react with Ammonium Molybdate, I2(NH4)2MoO4 to form Ammonium
Phosphomolybdate (NH4)3PO4.12MoO3 obtained as a yellow precipitate. It is more commonly
called as the Ammonium Molybdate Phosphomolybdic Acid or the Ammonium Phosphomolybdate. For the unknown solution pale yellow precipitate formed indicating it is the trace
amount of phosphate presence in the water sample. In unknown water sample, there was no
change in the water sample therefore eliminating for the presence of phosphate in the sample.
PO43- + I2(NH4)2MoO4 + 24H2O (NH4)3PO4.12MoO3 + 2INH4 + 12H2O
For the ammonium ions only the standard solution contains ammonium when it reacts
with sodium hydroxide. The litmus paper turn red to blue which indicate the gas is alkaline.
For the nitrate test, there was no nitrate ions present in tap water and unknown
solution except the standard solution. Devarda's alloy (Cu/Al/Zn) is a reducing agent. When

reacted with nitrate in sodium hydroxide solution, ammonia is liberated. The ammonia
formed may be detected by its characteristic odor, and by moist red litmus.
3 NO3- + 8 Al + 5 OH- + 18 H2O 3 NH3 + 8 [Al(OH)4]There are some precaution steps that need to be considered during the experiment was
being carried out. Firstly, gloves are worn and HCl was carefully handled as it is corrosive
and cause irritation to skin. Potassium hexacyanoferrate(II) is a bit toxic, thus it must be
handle carefully as well. Inhalation of high concentration of ammonia gas was being avoided
as it may cause damage to lung. Lastly, goggles were worn to protect eyes from being directly
contacts with chemical.

Conclusion:
In this experiment, tap water contains chlorine ions and phosphate ions only while the
unknown sample (lake water) contains a small amount of magnesium ions. This shows that
different water samples have different concentration of ions. Thus, I am able to investigate
the quality of water samples and identified the ions present in tap water and the unknown
water samples with comparing to the standard solution.
References:

UK Essays. 2016. Qualitative Investigation Of Water Samples Biology Essay.

[ONLINE] Available at https://www.ukessays.com/essays/biology/qualitativeinvestigation-of-water-samples-biology-essay.php . [Accessed 7 June 2016].

Qualitative Data Analysis, Quantitative Chemical Analysis |

Chemistry@TutorVista.com. 2016. Qualitative Data Analysis, Quantitative Chemical
Analysis | Chemistry@TutorVista.com. [ONLINE] Available at:
http://chemistry.tutorvista.com/analytical-chemistry/qualitative-analysis.html.
[Accessed 7 June 2016].

Systems, A.I. (2010) Lab 4 - qualitative analysis. Available at:

http://www.webassign.net/question_assets/ncsugenchem102labv1/lab_4/manual.html
[Accessed: 7 June 2016].

Ions in water. Available at: http://water157.narod.ru/clear/ion_e.htm

[Accessed: 7 June 2016].