Laboratory Manual

Course Code: CI 102

Course name: Chemistry Laboratory I
Integrated M.Sc. 2nd Semester
L-T-P: 0-0-3, Credit = 3

Department of Chemical Sciences

Tezpur University
Nappam, Tezpur - 784028
Assam, INDIA
Introduction:

This manual has been prepared for CI-102 Chemistry Laboratory. This laboratory course
is aimed to provide students a degree of competence in the laboratory skills required for accurate
and precise salt analysis. It is expected that the students will demonstrate proficiency in learning
the underlying reactions involved in identifying acid/basic radicals. Another important purpose
of this laboratory course is to provide students an appreciation for observation of different
physic-chemical property changes. Students should familiarize themselves with the significance
of different changes observed.

Course Policies and Information:

Each student must have a lab Notebook and bring it to the lab every week. You should
keep a good notebook with all the calculations and the results because your instructor will grade
your Lab notebooks at the end of the each experiment.

As per Tezpur University guidelines attendance is required and you are expected to
attend all scheduled laboratory sessions. Should you be sick and cannot come to lab, you need to
bring a doctors excuse from UNIVERSITY HEALTH CENTRE. Please arrive on time or
otherwise you will not be able to complete the experiment as per the schedule.

Format of the Lab Report

You should prepare your lab reports by handwriting. They should include tables and
illustrations where necessary. Typically, a lab report should contain the following sections: Aim,
Theory, Procedure, Calculations and Results.
Laboratory Safety Rules

Laboratories are interesting and potentially dangerous place to work. Laboratory Safety is
a very important aspect of science. Without it, experimentation could result in very serious
injury. To reduce the risks involved with experimentation, there are certain procedures that we
should all follow. Safety is the first priority in our lab.

1. Wear lab coat. A lab coat should be worn during laboratory experiments. It provides
protection at all times.
2. Dress properly. Long hair and loose clothing (such as ties) are a hazard in the laboratory.
They may either catch fire or be chemically contaminated. Long hair must be tied back,
baggy clothing must be secured.
3. Wear shoes. Shoes must completely cover the foot. Sandals are prohibited because of the
hazard from the chemical spills.
4. Wear eye protector. Wear appropriate eye protection (goggles) at all times in the laboratory
and in any area where chemicals are stored or handled. Such protection will protect you
against chemical splashes.
5. Do not wear contact lenses (even with safety goggles). Contact lenses prevent rinsing
chemical splashes from the eye. Vapors in the laboratory (eg. HCl) dissolve in the liquids
covering the eye and concentrate behind the lenses.
6. Behave responsibly. The dangers of spilled acids, chemicals and broken glassware created by
thoughtless actions are not tolerated. Use of cellular phone inside the laboratory is strictly
prohibited.
7. Do not smoke. Smoking is not just an obvious fire hazard; it also draws chemicals in
laboratory air (both vapors and dust) into the lungs.
8. Do not eat or drink. Do not eat food, drink beverages, or chew gum in the laboratory. Do not
use laboratory glassware as containers for food or beverages. Wash your hand thoroughly
with soap and water when leaving the laboratory.
9. Avoid breathing fumes of any kind.
10. Be prepared for your work in the laboratory. Carefully read the experiment before coming to
the laboratory. An unprepared student is a hazard to everyone in the room.
11. KEEP YOUR WORK AREA NEAT AND CLEAN. Clean up spills and broken glass
immediately. Clean up your work space; wipe all surfaces and put away all chemicals and
equipment at the end of the laboratory period.
 Experiment No.

Aim of the experiment:

Systematic qualitative analysis of a given salt mixture for acid and basic radicals. It involves the
identification of the constituents of an inorganic salt mixture.

Preliminary investigation:
Colour

Physical state

Solubility

Preliminary investigation with the dry samples (DRY TEST):

S. Experiment Observation Inference Explanation

No
1 Action of Heat Smell of ammonia and/or May be NH4+
a white sublimate is
A little of the given salt is formed
strongly heated in a dry test
tube. Yellow when hot white May be Zn2+
when cold

Orange red when hot May be Pb2+

yellow when cold

Black residue Salts of Cu2+, Mn2+, Ni2+,

and Co2+ may be present.

Blue color first turns Cu2+ salt may be present.

white, then black.

Reddish brown vapour May be NO3-

evolves

No characteristic change Absence of NH4+, Zn2+,

Pb2+, Cu2+, Mn2+, Ni2+,
 Co2+ and NO3-.

2 Flame Test Persistent golden-yellow Na+-saltmay present

flame
A clean platinum wire is first
dipped in conc. HCl then salt is Violet (lilac) flame K-salt may present
touched with it and it is put in
the non-luminous Bunsen flame. Carmine-red flame Li-salt may present

Brick-red (yellowish) Ca-salt may present

flame

Crimson flame Sr-salt may present

Yellowish-green flame Ba/Mo -salt may be present

Green flame Borates/copper/thalium

may present

Blue flame Lead/ Arsenic/

Bismuth/Copper may
present

3 Charcoal Reduction Test No residue, smell of NH4+ may be present.

ammonia.
The salt is mixed with Na2CO3
(1:2 ratios). The mixture is taken Yellow when hot, white Zn2+ may be present.
in charcoal cavity and heated when cold.
with the help of a blowpipe.
Red flakes Cu2+ may be present.

Yellow incrustation with Pb2+ may be present.

greenish metallic bead.

Grey metallic particles. Fe3+, Ni2+ and Co2+ salt

may be present.

White residue; glows on Al3+, Zn2+ and Mg2+ salt

heating. may be present.

4 Cobalt Nitrate Test Blue residue Al3+ salt may be present.

1-2 drop of cobalt nitrate is Green residue Zn2+ salt may be present.
 added to the white residue Pink residue Mg2+ salt may be present.
and is heated with a
blowpipe.

(Note: The test is to be

performed if white infusible
residue is obtained in
charcoal cavity test)

5 Borax Bead Test: Deep blue when hot and Co2+ salt may be present.
cold
(Note: This test is done if
the salt is colored) Green when hot, blue Cu2+ salt may be present.
when cold
For this test a small loop is
made in the platinum wire. Yellow when hot and cold Fe3+ salt may be present.
The loop is heated with a
small amount of borax in the Violet when hot and cold Mn2+salt may be present.
non-luminous flame. Now
salt is touched with the hot Reddish brown when cold Ni2+ salt may be present.
bead and then it is heated in
the oxidizing flame.

Reactions of anions or acid radicals:

The methods available for the detection of anions/acid radicals are not as systematic as those for
cation/basic radicals. The following scheme of classification has been found to work well in
practice; it is not a rigid one since some of the anions/acid radicals belong to more than one of
the subdivisions. Essentially the process employed may be divided into Class A, those involving
the identification by volatile products obtained on treatment with acids, and Class B, those
dependent upon reactions in solution. Class A is subdivided into (1) gases evolved with dil. HCl
or dil. H2SO4, and (2) gases or vapours evolved with conc. H2SO4. Class B is subdivided into (1)
precipitation reactions and (2) oxidation and reduction in solution.
Class A

Class B
Preliminary test for anions or acid radicals:

S. Experiment Observation Inference Explanation

No.

1 Salt + Dil.H2SO4 Evolution of colorless Carbonate (CO32-)

odourless gas which turns or bicarbonate
lime water milky. (HCO3-) may be
present

Evolution of a colorless S 2- may be

gas which smells like present.
rotten egg.

Evolution of a colorless SO32- may be

gas with smells of burning present
sulphur which turns
acidified potassium
dichromate paper green.

Evolution of a reddish NO2 may be

brown fume which can present.
turn ferrous sulphate
solution black.

2 Potassium Pink colour is discharged I- may be

Permanganate Test with the evolution of present
violet iodine vapours that
(Salt + dil. H2SO4 turns starch paper blue.
boil to expel all the
gases completely Pink colour is discharged Br- may be present
then add few drops of with the evolution of
potassium brown bromine vapours
permanganate that turns starch paper
solution) yellow.

Pink colour is discharged Cl- may be present

with the evolution of
yellowish-green chlorine
gas which has pungent
odour and bleaches litmus
 paper.

Pink colour does not Cl-, Br-, I-, Oxalate

discharge at all. and Tartarate may
be absent.

3 Salt + conc.H2SO4 Evolution of brown fume NO3 may be

(Warm the mixture if which can turn FeSO4 present.
necessary) black.

Evolution of brown fume. Br- may be

present.

Colourless gas with Cl may be

pungent odour present.

Evolution of violet vapour I may be present.

which can turn moist
starch paper blue.

4 Salt + MnO2 + Evolution of greenish Cl may be

conc.H2SO4 + Heat yellow gas with pungent present.
smell

Evolution of dense reddish Br may be

brown fume present.

Evolution of dense violet I may be present.

vapour

5 Salt + conc. H2SO4 + Green edged flame is BO33- present.

Ethanol + Heat obtained

6 Salt + conc. HNO3 + Canary yellow precipitate PO43- present.

ammonium molybdate
solution. Boil the
mixture if necessary.
 7 Special test for S2- Lead acetate paper turns S 2- is confirmed.
black.
(Lead acetate paper
test)

Salt + dil.H2SO4 ---

the evolved gas is
treated with lead
acetate paper

Special test for NO2 - Ferrous sulphate solution NO2 is

turns black. confirmed.
(Starch iodide paper
test)
8
Salt + dil.H2SO4 - the
evolved fume can turn
ferrous sulphate
solution black

Special test for NO3- Evolution of dense brown NO3- is confirmed.

fume.
(Copper- turnings test)
9
Salt + conc.H2SO4
+Cu-turnings + Heat

Special test for Cl Dense white fume is Cl - is confirmed.

obtained
Salt + conc.H2SO4
10 the evolved fume is
treated with a glass
rod wetted with
ammonia solution.

Chromyl Chloride Yellow precipitate which Cl - is confirmed.

Test for Chloride: is soluble in NaOH
solution.
Salt + K2Cr2O7 + conc.
11 H2SO4. Heat the test
tube and pass the red
vapors through dil.
NaOH solution which
will lead to a yellow
colour solution.
 Acidify the yellow
solution with acetic
acid and then add 1-2
mL of Lead acetate
solution

Wet test for anions or acid radical:

For water insoluble salt a Na2CO3 extract is prepared.

[Preparation of Na2CO3 extract:

About 1g of the sample is mixed with 4-5 times its weight of anhydrous Na2CO3 and 50mL
distill water are taken in a conical flask. A funnel is put at the mouth of the conical flask and the
flask is heated for 10 min, then it is filtered. The filtrate is called Na2CO3 extract and is used for
wet test for acid radical. ]

S. No. Experiment Observation Inference Explanation

1. Barium Chloride Test: White precipitate SO32-, SO42-

insoluble in conc. HNO3 may present.
Salt solution/Na2CO3 or conc. HCl.
extract +dil HNO3 + BaCl2
solution

2. Lead acetate test: White precipitate SO32-, SO42-

present.
Salt solution/Na2CO3
extract +dil HNO3 + Lead
acetate solution

3 Salt solution/Na2CO3 Decolourization of SO32-

extract + dil. H2SO4+ KMnO4 colour confirms
KMnO4 solution

4 Salt solution/Na2CO3 Green colouration SO32-

extract + dil. H2SO4+ confirms
K2Cr2O7 solution

3 Salt solution + MgSO4 White ppt obtained in CO32-

solution cold confirms
 If no ppt. appears in HCO3-
cold but white ppt. confirms
obtained while heating

4 Salt solution/Na2CO3 White precipitate Cl - present.

extract + dil. HNO3 + soluble in NH4OH
AgNO3 solution solution.

Pale yellow precipitate Br present.

partially soluble NH4OH
solution.

Yellow precipitate I present.

insoluble in NH4OH
solution.

5 Salt solution/ Na2CO3 Orange coloured organic Br present.

extract + dil. HCl (boil the layer is formed
solution to expel CO2) +
CCl4 + conc. HNO3. Shake Violet coloured organic I present.
the mixture vigorously. layer is formed

6 Salt solution/Na2CO3 Canary yellow PO43- present.

extract +conc. HNO3 + precipitate
Ammonium molybdate
solution. Boil the mixture
if necessary.

Salt solution/Na2CO3 Yellow-white PO43- present.

extract + FeCl3 solution precipitate

7 Salt solution/Na2CO3 Purple coloration S2- present.

extract + Sodium
nitroprusside solution.

8 Salt solution/Na2CO3 Black precipitate S2- present.

extract + dil. CH3COOH
+Pb(CH3COO)2 solution

Salt solution/Na2CO3 Black ppt. insoluble in S2- present

cold, but soluble in hot
 extract + AgNO3 solution dil. HNO3

9 Brown Ring Test: A brown ring is formed NO3- is

(Ring test for NO3-) between the two layers confirmed
Salt solution in water + of the liquid.
Freshly prepared FeSO4
solution + 3-5 drops of
conc. H2SO4 is added
slowly.

10 Salt solution + AgNO3 White precipitate CO32-

solution soluble in dil. HNO3 confirmed

11 Salt solution + BaCl2 White precipitate CO32-

solution soluble in dil. HNO3 confirmed

12 Boil salt solution/ Na2CO3 Formation of white Either F- or

extract + CH3COOH until Precipitate C2O4- is
effervescence of CO2 present
diminishes and then add
CaCl2 solution.

Treat the white precipitate White ppt. remains F- is present

with hot dil. H2SO4 in
which CaC2O4 is soluble.

If a clear solution is Decolourization of C2O42- is

obtained, add few drops of KMnO4 present.
KMnO4.

Special test for sulphites:

To the salt solution/ Na2CO3 extract add excess of BaCl2 solution. If white precipitate appears it
may be due to sulphite, sulphate or excess sodium carbonate present in the solution. Filter the
precipitate and divide it into four parts:
a) To part I add dil. HCl. If there is evolution of SO2 which turns acidified dichromate paper
green, it confirms sulphite.
b) To part II add a few drops of potassium permanganate solution followed by addition of 3 mL
of dil. H2SO4. If the colour of permanganate gets discharged, the presence of sulphite
confirmed.
c) To part III, add bromine water. On warming this solution the colour of bromine gets
discharged and a white ppt. insoluble in acids is obtained. This confirms sulphite.
d) To part IV, add I2 solution. If iodine colour decolorizes sulphite is confirmed.

Special test for sulphates:

Take 1-2 mL of BaCl2 solution in a test tube. To this add 0.5 mL of freshly prepared 0.1 %
aq. Rhodizonate solution. A red colour in the test tube is formed. To this add 1-2 mL of salt
solution/ Na2CO3 extract. If red colour disappears, it identifies sulphates.

Wet test for basic radicals or cations:

If the salt contains BO33- or PO43- as interfering radical then BO33- should be removed before
performing wet test for basic ions and PO43- should be removed after group II analysis.
Otherwise a salt solution is prepared either in water or dilute/concentrated HCl.

Removal BO33-:

BO33- is removed as boric acid from the salt by volatile heating with conc. HCl (3-4 times).

Removal of PO43-:

The PO43- radical is removed after group II analysis. The removal of PO43- consists of following
steps

i. To the salt solution NH4Cl and ammonia solution is added till a precipitate obtained.
ii. To the above solution dil. HCl is added dropwise till precipitate just disappears.
iii. To the small amount of the above solution K4 [Fe(CN)6] solution is added.
If deep blue precipitate obtained. Fe3+ present.
iv. To the remaining solution NH3 solution is added drop wise till precipitate just
disappears.
v. To the above solution half test tube acetic acid and half test tube ammonium acetate are
added as buffer solution.
vi. Neutral FeCl3 solution is added to the above solution till solution becomes tea coloured.
 The solution is then boiled and filtered. Residue is rejected and filtrate is taken for further
analysis.

Classification of the cations:

For analytical purposes cations are classified into six groups to their reactivity and precipitated
by common reagents. It is important that one group should be completely precipitated (in a
mixture of cation) before precipitation of the next group is attempted. Otherwise, the desired
group will be contaminated by metals from the preceding groups, and misleading results will be
obtained.

1. The first group: contains those metal cations that precipitate as chlorides. This group
includes Pb2+, Ag+ and Hg+.
2. The second group: contains those mmetal cations which forms insoluble sulphides in
acidic conditions. The group consists of group IIA and IIB. Group IIA includes Pb2+,
Cu2+, Bi3+, Cd2+, Hg2+. Group IIB includes: Sb3+, Sb5+, As3+, As5+, Sn2+, Sn4+.
3. The third group: contains those metal cations that will precipitate as their hydroxides,
Fe2+, Fe3+, Al3+, Cr3+ are the cations for this group.
4. The fourth group: contains those metal cations that precipitate as sulphides under basic
conditions. This includes Zn2+, Co2+, Ni2+ and Mn2+.
5. The fifth group contains Ba2+, Ca2+ and Sr2+ which are precipitated as carbonate.
6. The sixth group: Unprecipitated after removal of the other groups. This group includes:
Na+, K+ and Mg2+.

Preparation of original solution:

1. For Nitrate, Chloride and Sulphate: The given salt is dissolved in distilled water. The
solution obtained will be termed as Original solution.
2. For carbonates: The original solution is prepared by dissolving the substance in dilute
hydrochloric acid and dilute Nitric acid.
Test for zero group cations:

Before proceeding for the separation of cations into various groups, one should perform a test for
NH4+ radical. Heat a small quantity of the substance with NaOH. Liberation of ammonia indicate
the presence of NH4+ (Caution: To identify the gas do not smell it). The gas evolved may be
identified by the following test: Dip a glass rod in conc. HCl and then place it at the opening of
the test tube. Evolution of dense white fumes confirms the presence of NH4+.

After the of zero group elements has been performed proceed as outlined below to separate
cations of different groups:
Table for group separation:

Experiment Observation Inference

Original solution +dilute HCl White / black Group I (Pb2+, Ag+ and Hg22+)
precipitate. present.

No precipitate Group II, III, IV, V, VI may

present.

Original solution/filtrate + dil. HCl Black/yellow Group II (Hg2+, Bi3+, Pb2+,

+ H2S precipitate Cu2+, Cd2+, As3+, Sb3+ and
Sn2+) present.

No precipitate Group III, IV, V, VI may

present.

Original solution / filtrate (boiled Gelatinous white / Group III (Fe3+, Cr3+ and Al3+ )
off H2S), Conc. HNO3, Boil, Add pink / brown present.
NH4Cl, add NH3 solution (excess) precipitate

No precipitate Group IV, V, VI may present.

Above solution / filtrate + H2S Black / Pink / flesh Group IV (Ni2+, Co2+, Zn2+ and
color precipitate Mn2+ ) present.

No precipitate Group V, VI may present.

Above solution / filtrate (boiled off White precipitate. Group V (Ba2+, Sr2+, and Ca2+)
H2S), concentrate and add present.
(NH4)2CO3 + NH4OH and filter
No precipitate Group VI and/or NH4+ may
present.

Above solution / filtrate + Na2HPO4 White precipitate Group VI (Mg2+) present.

solution
No precipitate Group VI (Na+, K+) and NH4+
may present.
Flow chart for group separation:

Original Solution

Add dilute HCl in slight

excess and filter

Precipitate Filtrate
Ag+, Hg+, Pb2+ Group II, III, IV, V, VI
Group I

Original solution/filtrate + Dil.

HCl + H2S

Precipitate Filtrate
Hg , Pb2+, Bi3+, Cu2+,
2+
Group III, IV, V, VI
Cd2+, As3+, Sb3+, Sn3+
Group II
Original solution / filtrate (boiled off H2S),
Conc. HNO3, Boil, Add NH4Cl, add NH3
solution (excess)

Precipitate Filtrate
Al3+, Cr3+ and Fe3+ Groups IV, V and VI
Group III
Above solution / filtrate + H2S

Precipitate
Filtrate
Zn2+, Mn2+, Ni2+ and Co2+
Groups V and VI
Group IV

Above solution / filtrate (boiled off

H2S), concentrate and add
(NH4)2CO3 + NH4OH and filter

Precipitate Ba2+, Filtrate

Sr2+, Ca2+ Group VI
Group V
Above solution / filtrate
+ Na2HPO4 solution

Precipitate Filtrate
Mg2+ Na+, K+, NH4+
Analysis of group I precipitate:
The formation of white precipitate upon addition of dilute HCl to the original solution of the
sample infers the presence of Group I radicals. Filter the precipitate and then wash with cold
water to remove traces of HCl present. The precipitate is transferred to a test tube, boiled with
water and subsequently filtered when hot.

Analysis of group II precipitate:

Wash the precipitate with hot water on filter paper.
Analyses of group II A precipitate:
Wash the precipitate for group IIA (insoluble in yellow ammonium sulphide) with hot water.
Heat the precipitate with 5 mL 50 % HNO3 and filter.
Analysis of group IIB Cations:
Acidify the filtrate reserved for group IIB with dil. HCl. A coloured precipitate shows the presence of
arsenic, antimony and tin. [ A white ppt. shows the absence of group IIB].

Filter and wash the colourd precipitate with distilled water. Transfer the precipitate to a boiling tube and
boil with about 10 mL of HCl for 5 min. Cool and filter.
Analyses of Group III precipitate:

Analyses of group IV precipitate:

Analysis of group V precipitate:

If Ba2+ is present:

If Ba2+ is abesent:
Analysis of group VI precipitate:

Special tests for NH4+, K+ and Na+ :

Fresh solution of salt in water / Na2CO3 extract is prepared

Experiment Observation Inference

Salt solution + Nesslers Brown precipitate NH4+ present & confirmed

reagent + NaOH solution till
alkaline

Salt Solution + tartaric acid Crystalline precipitate K+ present

Flame test with solid salt Golden yellow flame Na+ present

Results:

The given salt mixture contains:

Acid radicals:

Basic radicals: