Fundamentals of Chemistry

CHEM 1101

Laboratory Manual

Prepared by:
Staff Members, Department of Chemistry
Faculty of Science – University of Tabuk
CHEM 1101
Laboratory Manual

Contents

Subject Page

Methods of chemical analysis 1

Qualitative Analysis 2

Investigation for simple salts 4

Investigation for dil. HCl group 5

Investigation for conc. H2SO4 group 15

Investigation for miscellaneous group 23

General scheme of Acidic Radicals 29

Investigation for basic radicals 33

Investigation for group I 34

Investigation for group II 41

Investigation for group III 49

Investigation for group IV 55

Investigation for group V 63

Investigation for group VI 69

General scheme of basic Radicals 76

Presence and absence record 86

CHEM 1101
Laboratory Manual

Methods of Chemical Analysis

Qualitative Chemical Quantitative Chemical

Analysis Analysis

Instrumental Analysis Volumetric Analysis Gravimetric Analysis

Precipitation & Complex Reduction - Oxidation

Neutralization Reactions
Formation Reactions Reactions

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Qualitative Analysis
Deals with the determination of composition of a given sample.

How to make a solution?

≈ 0.1-0.5 gm Solid + ≈ 20ml solvent (e.g., H2O)  clear solution.

Solvents such as :-

1- Cold water then hot water .

2- Cold dil.HCl then hot dil.HCl.

3- Cold conc. HCl then hot conc. HCl.

4- Cold dil. HNO3 then hot dil. HNO3.

5- Cold conc. HNO3 then hot conc. HNO3.

6- Aqua ragia ( 3 conc.HCl :1 conc.HNO3 ). ‫اﻟﻣﺎء اﻟﻣﻠﻛﻰ‬

Solubility of salts

Salts are divided into three groups according to their solubility:

2- Salts that are generally 3- Salts that are generally

1- Salts that are soluble soluble with some insoluble with some
exceptions exceptions

-All salts of alkali metals . -All salts of Cl-, I-, Br –are -All salts of CO3--, PO4---, S--
soluble except those of ,SO3--, S2O3--, are insoluble
-All salts of NH4+.
Ag+ , Pb++, Hg2++. except those of NH4+
-All salts of HCO3- and NO3-
,Na+,K+.
-All salts of SO4- - are
.
soluble except those of
Ca++ , Ba++ ,Sr++ , Pb.++

• Any salt consists of acidic radical (-ve ), anion and basic radical (+ve), cation .

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Strength of acids

Acids are classified into 3 groups according to their strength:

1) weak acids 2) Stronger acids 3) More stronger acids

H2CO3 Carbonic acid HCI Hydrochloric acid H2SO4 Sulphuric acid

Hydrosulphuric
H2S HBr Hydrobromic acid H3PO4 Phosphoric acid
acid

HNO2 Nitrous acid HI Hydroiodic HClO4 Perchloric acid

H2SO3 Sulphurous acid HNO3 Nitric acid

:‫ﻣﻠﺣوظﺔ‬ •

‫ﯾﻣﻛن ﻟﺣﻣض ﻣن أﺣﻣﺎض اﻟﻣﺟﻣوﻋﺔ اﻟﺛﺎﻧﯾﺔ أن ﯾطرد ﺣﻣﺿﺎ ً ﻣن اﻣﻼح اﻟﻣﺟﻣوﻋﺔ اﻷوﻟﻰ‬

Na2S + 2HCI  H2S + 2NaCI

‫ﻛﻣﺎ أﻧﮫ ﯾﻣﻛن ﻟﺣﻣض ﻣن اﻟﻣﺟﻣوﻋﺔ اﻟﺛﺎﻟﺛﺔ أن ﯾطرد ﺣﻣﺿﺎ ً ﻣن اﻣﻼح اﻟﻣﺟﻣوﻋﺔ اﻷوﻟﻰ أو اﻟﻣﺟﻣوﻋﺔ اﻟﺛﺎﻧﯾﺔ‬

2NaCI + H2SO4  2HCI + Na2SO4

‫وﻟﻛن أي ﻣن أﺣﻣﺎض اﻟﻣﺟﻣوﻋﺔ اﻷوﻟﻰ أو اﻟﻣﺟﻣوﻋﺔ اﻟﺛﺎﻧﯾﺔ ﻻ ﯾﺳﺗطﯾﻊ أن ﯾؤﺛر ﻓﻲ أﻣﻼح أﺣﻣﺎض اﻟﻣﺟﻣوﻋﺔ اﻟﺛﺎﻟﺛﺔ‬

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Investigation for simple salts

A. Investigation for anions (acidic radicals):

Example:

NaOH + HCl NaCl + H2O

Since Na+ comes from the base (NaOH), BASIC RADICAL and Cl- comes from the acid (HCl),
ACIDIC RADICAL.

As general

Cations are basic radicals, while anions are acidic radicals

Investigation for acidic radicals

Dil. HCl group Conc. H2SO4 group Miscellaneous group

CO32-
Carbonate
HCO3- Cl-
Bicarbonate Chloride SO42-
S2O32- Br- Sulphate.
Thiosulphate Bromide B4O72-
SO32- I- Borate.
Sulphite. Iodide. PO43-
S2- NO3- Phosphate.
Sulphide. Nitrate.
NO2-
Nitrite.

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1) Dilute HCl group

Introduction

The analysis of acidic radical is based on multi-steps process, so the anions are arranged
in groups and each anions group has its own specific reagent in such way that the reagent
of lower group has no effect on the anions of the higher groups. The anions of this group
(Dil. HCl group) are readily attacked by dilute acids such as dilute hydrochloric acid and
include six anions which are affected by Dil. HCl which are:

1- Carbonates - (CO32- )

2- Bicarbonates – (Hydrogen Carbonates) (HCO3 –)

3- Sulfide- (S2- )

4- Sulfites - (SO32- )

5- Thiosulphates (S2O32- )

6- Nitrites (NO2- ).

The group reagent is dilute hydrochloric acid HCl. All carbonate salts are insoluble in water
except for sodium carbonate, potassium and ammonium are soluble in water. All
bicarbonate salts are soluble in water. All sulfide salts are insoluble in water except for
sulfides sodium, calcium, strontium, ammonium are soluble in water. Bicarbonate
decomposes with heat to insoluble carbonate and CO2 gas.

Goal

To identify acidic radicals of Dil. HCl group; Carbonates - (CO32-), Bicarbonates –

(Hydrogen Carbonates) (HCO3–), Sulfide (S2-), Sulfites - (SO32-), Thiosulphates (S2O32-)
and Nitrites (NO2-).

Apparatus and tools:

• Test tubes • Gas burner

• Test tube holder • Spatula

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• Test tube brushes • Chemical Required: Given Salt and Various

reagents
• Dropper

Theory

This group of acidic radicals includes anions that are readily attacked by dilute acids such
as Dil. HCl. These anions: CO32-, S2-, SO32-, S2O32- and NO2– react with dil. HCl to give
volatile acids or unstable acids which decompose instantaneously to their volatile oxides.
Thus, these acidic radicals; CO32-, S2-, SO32-, S2O32- and NO2–, are identified by Dil. HCl
giving out CO2, H2S, SO2 and NO2 gas respectively which can be identified by certain tests.

Example:

Na2CO3 + 2HCl  2NaCl + H2O + CO2 

Na2S + 2HCl  H2S + NaCl

Na2SO3 + 2HCl  SO2 + H2O + 2NaCl

Procedure:

Conduct the tests of each acidic radical (anion) to confirm it after following up the general scheme
of acidic radical.

a. Carbonate, CO32- and bicarbonate HCO3-

1) Solid + dil. HCl  effervescence of CO2 gas which turbid lime water due to the formation
of insoluble CaCO3.

Na2CO3 + 2HCl 2NaCl + H2O + CO2 

NaHCO3 + HCl NaCl + H2O + CO2 

Ca (OH)2 + CO2 CaCO3 + H2O

2) Soln. + MgSO4 soln.  white ppt., MgCO3 on cold in case of carbonate and after boiling in case
of bicarbonate.

Na2CO3 + MgSO4 MgCO3 +Na2SO4

NaHCO3 + MgSO4 Mg (HCO3)2+ Na2SO4

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Mg (HCO3)2 boiling
MgCO3 + H2O + CO2 

3) Soln. + HgCl2 soln.  reddish brown ppt. Hg2 (OH) 2CO3 basic mercuric carbonate while with
bicarbonate gives the ppt. after boiling.

Na2CO3 + 2HgCl2 Hg2 (OH) 2CO3 + NaCl +H2O

4NaHCO3 + 2HgCl2 heat

Hg2 (OH)2CO3 + 4NaCl + H2O + 3CO2

4) Carbonate soln. + AgNO3  white ppt. Ag2CO3

Bicarbonate soln. + AgNO3 boiling

Ag2CO3

b. Sulphide, S2-

1. Solid. + dil. HCl  H2S gas characterized by its rotten egg odor, blacking of filter paper wetted
with lead acetate solution.

Na2S + 2HCl H2S + NaCl

H2S + Pb(CH3COO)2 PbS + 2CH3COOH

2. Soln. + Pb(CH3COO)2  black ppt. PbS soluble in hot HNO3

Na2S + Pb(CH3COO)2 PbS + CH3COONa

3. Soln. + AgNO3  black ppt. Ag2S soluble in hot HNO3

Na2S + AgNO3 Ag2S + 2NaNO3

c. Sulphite, SO32-

1. Solid. + dil. HCl  SO2 gas with suffocating odor, turns acidic paper wetted with K2Cr2O7 into
green.

Na2SO3 + 2HCl SO2 + H2O + 2NaCl

K2Cr2O7 + H2SO4 + 3SO2 K2SO4 + Cr2(SO4)3 + H2O

2. Soln. + BaCl2  white ppt. BaSO3

Na2S + BaCl2 BaSO3 + NaCl

3. Soln. + AgNO3  White ppt. Ag2SO3 soluble in dil. HNO3

Na2SO3 + AgNO3 Ag2SO3 + 2NaNO3

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d. Thiosulphate, S2O32-

1. Solid. + dil. HCl  Evolution of SO2 gas and yellow ppt. is formed due to separation of sulfur.

Na2S2O3+ dil. HCl NaCl + SO2 + H2O + S

2. Only one drop + excess AgNO3  White ppt. Ag2S2O3 the color changes through yellow to
brown to black (Ag2S)

Na2S2O3 + AgNO3 Ag2S2O3 + 2NaNO3

Ag2S2O3 + H2O Ag2S + H2SO4

3. Soln. + Pb(CH3COO)2  White ppt. PbS2O3 changes into black by boiling giving PbS

Na2S2O3 + Pb(CH3COO)2 PbS2O3 + 2CH3COONa

4. Soln. + FeCl3  Violet color of sod. Ferri-thiosulphate NaFe(S2O3)2 disappears after time
forming Na2S4O6

Na2S2O3 + FeCl3 Na2S4O6 + 2FeCl2 + 2NaCl

e. Nitrite, NO2-

1. Solid. + dil. HCl  Nitric oxide NO gas which combines with oxygen of air giving brown gas
(nitrogen dioxide NO2)

NaNO2 + dil. HCl NaCl + HNO2

HNO2 H2O + HNO3 + 2NO

2NO + O2 2NO2

2. Soln. + AgNO3  White ppt. AgNO2

NaNO2 + AgNO3 AgNO2 + 2NaNO3

3. Black ring test:

Soln. + freshly prepared FeSO4 soln. + drops of conc. H2SO4 Black or brown ring
(FeNOSO4)

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Results:

Lab. 1

1- Carbonate, CO32-

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

Effervescence and evolution of

1. Solid + dil. HCl It may be CO32- or HCO3-
a gas turbid lime water.

2. Soln. + MgSO4 White ppt. It is CO32-

3. Soln. + HgCl2 Reddish brown ppt. It is CO32-

4. Soln. + AgNO3 White ppt. It is CO32-

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2- Bicarbonate, HCO3-

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Solid + dil. HCl

2. Soln. + MgSO4

3. Soln. + HgCl2

4. Soln. + AgNO3

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3- Sulphide, S2-

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Solid + dil. HCl

2. Soln. + Pb(CH3COO)2

3. Soln. + AgNO3

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Lab. 2

4- Sulphite, SO32-

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Solid + dil. HCl

2. Soln. + BaCl2

3. Soln. + AgNO3

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5- Thiosulphate, S2O32-

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Solid + dil. HCl

2. Soln. + AgNO3

3. Soln. + Pb(CH3COO)2

4. Soln. + FeCl3

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6- Nitrite, NO2-

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Solid + dil. HCl

2. Soln. + AgNO3

3. Black ring test

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2) Conc. H2SO4 group

Introduction

The analysis of acidic radical is based on multi-steps process, so the anions are arranged
in groups and each anions group has its own specific reagent in such way that the reagent
of lower group has no effect on the anions of the higher groups. This group is concentrated
sulfuric acid (Conc. H2SO4) group and includes the following radicals: Chloride (Cl-),
Bromide (Br-), Iodide (I-) and Nitrates (NO3-). The anions of this group (Conc. H2SO4 group)
are readily attacked Conc. H2SO4 with liberation of characteristics gases. On the other
hand, Conc. H2SO4 doe does not affect the anions of the next group.

Goal

To identify acidic radicals of Conc. H2SO4 group; Chloride (Cl-), Bromide (Br-), Iodide (I-)
and Nitrates (NO3-).

Apparatus and tools:

• Test tubes • Gas burner

• Test tube holder • Spatula

• Test tube brushes • Chemical Required: Given Salt and

• Dropper Various reagents

Theory

This group is concentrated sulfuric acid (Conc. H2SO4) group and includes the following
radicals: Chloride (Cl-), Bromide (Br-), Iodide (I-) and Nitrates (NO3-). The anions of this
group (Conc. H2SO4 group) are readily attacked Conc. H2SO4 with liberation of
characteristics gases. On the other hand, Conc. H2SO4 doe does not affect the anions of
the next group.

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Example:

2NaCl + H2SO4 Na2SO4 + 2HCl

2KBr + H2SO4 K2SO4 + 2HBr

2KI + conc. H2SO4 K2SO4 + SO2 + H2O + I2

Procedure

Conduct the tests of each acidic radical (anion) to confirm it after following up the general
scheme of acidic radicals.

a. Chloride, Cl-

1. Solid + conc. H2SO4  Evolution of HCl fumes forms white clouds of NH4Cl
when glass rod wetted with NH4OH is held near the top of the test tube.

2NaCl + H2SO4 Na2SO4 + 2HCl

2. Soln. + AgNO3  White ppt. AgCl insoluble in dil. HNO3 but soluble in NH3

NaCl + AgNO3 NaNO3 + AgCl

3. Soln. + Pb(CH3COO)2  White ppt. PbCl2 soluble by heating and returns

back after cooling

2NaCl + Pb(CH3COO)2 PbCl2 + 2CH3COONa

4. Soln. + Hg2 (NO3)2  white ppt. Hg2Cl2

2NaCl + Hg2 (NO3)2 Hg2Cl2 + 2NaNO3

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b. Bromide, Br-

1. Solid. + conc. H2SO4  Orange vapor of HBr and Br2 which detected by
changing starch paper into yellow.
2KBr + H2SO4 K2SO4 + 2HBr
2HBr + H2SO4 Br2 + SO2 + 2H2O
2. Soln. + Pb (CH3COO)2  white ppt. PbBr2 soluble by heating and returns
after cooling.
2KBr + Pb (CH3COO)2 PbBr2 + 2CH3COOK
3. Soln. + AgNO3  pale yellow ppt. AgBr soluble in hot HNO3
KBr + AgNO3 AgBr + KNO3
AgBr + 2NH3 [Ag (NH3)2] Br
4. Soln. + MnO2 + conc. H2SO4  Br2 Bromine vapor which detected by
changing starch paper into yellow.

c. Iodide, I-

1. Solid. + conc. H2SO4  I2 Violet vapor which turns starch paper into blue.
2KI + conc. H2SO4 K2SO4 + SO2 + H2O + I2
2. Soln. + Pb (CH3COO) 2  yellow ppt. PbI2 soluble by heating.
2KI + Pb (CH3COO) 2 PbI2 + 2CH3COOK
3. Soln. + AgNO3  yellow ppt. AgI insoluble in ammonia
KI + AgNO3 AgI + KNO3
4. Soln. + HgCl2  red ppt. HgI2 soluble in excess KI giving Nessler’s solution
[K2HgI4]
2KI + HgCl2 HgI2 + KCl
HgI2 +2KI K2HgI4

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d. Nitrate, NO3-

1. Solid. + conc. H2SO4 heat

NO2 reddish brown vapor.

NaNO3 + conc. H2SO4 NaHSO4 + HNO3

4HNO3 2H2O + 4NO2 + O2

2. Solid + Cu + H2SO4 heat

NO2 reddish brown vapor and the solution
become blue.

3. Black ring test:

Soln. + excess freshly prepared FeSO4 soln. + drops of conc. H2SO4  black
or brown ring (FeSO4.NO)

NaNO3 + H2SO4 NaHSO4 + HNO3

6FeSO4 + 2HNO3 + 3H2SO4 Fe2(SO4)3 + 4H2O + 2NO2

FeSO4 + NO FeSO4.NO

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Results:

Lab. 3

1- Chloride, Cl-

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

Evolution of fumes form white clouds

1. Solid + conc. H2SO4 of NH4Cl when glass rod wetted with It may be Cl-
NH4OH is held near the test tube

2. Soln. + AgNO3 White ppt. It is Cl-

3. Soln. + Pb(CH3COO)2 White ppt. It is Cl-

4. Soln. + Hg2(NO3)2 White ppt. It is Cl-

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2- Bromide, Br-

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Solid + conc. H2SO4

2. Soln. + AgNO3

3. Soln. +Pb(CH3COO)2

4. Soln. + MnO2 + conc.

H2SO4

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3- Iodide, I-

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Solid + conc. H2SO4

2. Soln. + AgNO3

3. Soln. + Pb(CH3COO)2

4. Soln. + HgCl2

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4- Nitrate, NO3-

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Solid + conc. H2SO4

2. Solid +Cu+ conc.H2SO4

3. Black ring test

3)

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3) Miscellaneous group

Introduction

The analysis of acidic radical is based on multi-steps process, so the anions are arranged
in groups and each anions group has its own specific reagent in such way that the reagent
of lower group has no effect on the anions of the higher groups. This group is the last
group, and it includes anions that are not affected by any of the acids known. It includes
sulfates; SO42-, Borates; B4O72- and phosphates; PO43-. No volatile products are obtained
on treatment with acids. The main reagent of this group is barium chloride solution which
results in white ppt. in all case but with different stability. Thus, this group of anions are
called Miscellaneous group or BaCl2 group.

Goal

To identify acidic radicals of Miscellaneous group sulfates; SO42-, Borates; B4O72- and
phosphates; PO43-

Apparatus and tools:

• Test tubes • Gas burner

• Test tube holder • Spatula

• Test tube brushes • Chemical Required: Given Salt and

Various reagents
• Dropper

Theory

This group is the last group, and it includes anions that are not affected by any of the acids
known. It includes sulfates; SO42-, Borates; B4O72- and phosphates; PO43-. No volatile
products are obtained on treatment with acids. The main reagent of this group is barium
chloride solution which results in white ppt. in all case but with different stability. Thus, this
group of anions are called Miscellaneous group or BaCl2 group.

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Example:

Na2SO4 + BaCl2 BaSO4 white ppt.+ 2NaCl

Soln. + BaCl2  White ppt. BaHPO4 soluble in ammonia.

Procedure:

Conduct the tests of each acidic radical (anion) to confirm it after following up the general
scheme of acidic radicals.

a. Sulphate, SO42-

1. Soln. + BaCl2  white ppt. BaSO4 soluble in HCl and HNO3 or excess BaCl2

Na2SO4 + BaCl2 BaSO4 + 2NaCl

2. Conc. soln. + AgNO3  White ppt. Ag2SO4 insoluble in dil. HNO3 but soluble
in NH3

K2SO4 + 2AgNO3 KNO3 + Ag2SO4

3. Soln. + Pb (CH3COO) 2  White ppt. PbSO4 insoluble in acids but soluble

in NaOH.

K2SO4 + Pb (CH3COO) 2 PbSO4 + 2CH3COOK

b. Borate, B4O72-

1. Soln. + BaCl2 White ppt. Ba (BO2)2 soluble in dil. acids and excess of
BaCl2.

2. Soln. + AgNO3  White ppt. silver metaborate AgBO2 which changes into
brown ppt. (Ag2O) after boiling.

Na2B4O7 + 3H2O + 2AgNO3 2AgBO2 + 3H3BO3 + 2NaNO3

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AgBO2 boiling
Ag2O + 2H3BO3

3. Soln. + HgCl2  Red ppt. Hg (BO2)2 soluble in dil. acids.

c. Phosphate, PO43-

1. Soln. + BaCl2  White ppt. BaHPO4 soluble in ammonia.

Na2HPO4 + BaCl2 BaHPO4 + 2NaCl

2. Soln. + AgNO3  yellow ppt. Ag3PO4 soluble in dil. HNO3

Na2HPO4 + AgNO3 Ag3PO4 + NaNO3

3. Soln. + FeCl3  Yellowish white ppt. FePO4 soluble in mineral acids

Na2HPO4 + FeCl3 FePO4 + NaCl + HCl

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Results:

Lab. 4

1- Sulphate, SO42-

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

White ppt. soluble in HCl, HNO3

1. Soln. + BaCl2 It may be SO42-
or excess BaCl2

2. Conc. soln. + AgNO3 White ppt. It is SO42-

3. Soln. + Pb(CH3COO)2 White ppt. It is SO42-

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2- Borate, B4O72-

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + BaCl2

2. Soln. + AgNO3

3. Soln. + HgCl2

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3- Phosphate, PO43-

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + BaCl2

2. Soln. + AgNO3

3. Soln. + FeCl3

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Lab. 5

General Scheme of Acidic Radicals

1- Test for dil. HCl group (Solid + dil. HCl)

Gas with
suffocating Gas with
Rotten odor
odor (SO2) suffocating
Effervescence (H2S) turns a
and turns odor (SO2)
and evolution paper Evolution of
acidic paper and turns No specific
of a colorless moistened colorless gas
moistened acidic paper result. Dil.HCl
gas (CO2) with lead turns brown.
with K2Cr2O7 moistened group is
A.R my be acetate to A.R may be
into green and with K2Cr2O7 absent.
CO3- - or black NO2-
a yellow ppt is into green
HCO3- A.R may be S-
- formed. A.R may be
A.R may be SO3- -
S2O3- -

2- Test for conc. H2SO4 group (Solid + conc. H2SO4)

Colourless gas orange gas turns Brown vapor

Violet vapor turns
gives white a paper wetted increases after No specific result.
a paper wetted
clouds with with starch to adding copper Conc. H2SO4
with starch blue
ammonia . yellow turnings . group is absent.
A.R . may be I-
A.R may be Cl- A.R may be Br- A.R may be NO3--

3- Test for miscellaneous group (Soln. + AgNO3)

White ppt from conc. soln not White ppt . changes into black
yellow ppt .
affected by heating.. after boiling.
A.R may be PO4---
A.R may be SO4-- A.R may be B4O7--

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Unknown 1

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

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Unknown 2

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

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Unknown 3

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

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B. Investigation for basic radicals

Basic radicals divided into six groups:

Group
Group reagent Type of precipitate Basic radical
No.

Group I Dil. HCl Chlorides Ag+, Hg22+, Pb2+

Sulphides in acidic
Group II Dil. HCl + H2S Hg2+, Cu2+, Cd2+, Bi3+
medium

Group III NH4Cl + NH4OH Hydroxides Al3+, Fe2+, Fe3+, Cr3+

Sulphides in basic
Group IV NH4Cl + NH4OH + H2S Zn2+, Mn2+, Co2+, Ni2+
medium

NH4Cl + NH4OH +
Group V Carbonates Ca2+, Sr2+, Ba2+
(NH4)2CO3

Group VI No Specific Reagent ------- Mg2+, Na+, K+, NH4+

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1. Group I

Introduction

The analysis of basic radicals (Cations) is based on multi-steps process as the acid
radicals, so the cations are arranged into six groups, and each cation group has its own
specific reagent group which will precipitate the members in each group. The reagent of
the lower group does not precipitate the cations of higher groups. The precipitation of the
group cations depends upon the solubility of their salts e.g., chloride, sulfide, hydroxide
and carbonate. Hence, the separation of the basic radicals into various groups is based on
the knowledge of solubility product. For example, in 2nd and 4th groups of basic radicals,
the solubility product of sulfides of 2nd group is lesser than 4th group so that the 2nd group
need acidic medium and hence only those metal sulfides are precipitated which have low
solubility product. On other hand cations in the 4th group need alkaline medium to
precipitate.

The basic radicals of Group I (Ag+, Pb2+, Hg22+) are precipitated as chlorides in using Dil.
HCl without affecting the cations of the other groups.

Goal

To identify the basic radicals of Group I (Ag+, Pb2+, Hg22+)

Apparatus and tools:

• Test tubes • Gas burner

• Test tube holder • Spatula

• Test tube brushes • Chemical Required: Given Salt and

Various reagents
• Dropper

Theory

The basic radicals of Group I (Ag+, Pb2+, Hg22+) are precipitated as chlorides in using Dil.
HCl without affecting the cations of the other groups.

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Example:

AgNO3 + HCl AgCl + HNO3

Pb(NO3)2 + 2HCl PbCl2 + 2HNO3

Procedure:

1. To identify the cations in their simple salts or in a mixture of them you must have a
soluble salt by preparing a solution by trying to dissolve the salt in the following solvents
(water and Acids) in the order given below:

1) Cold water then hot water .

2) Cold dil.HCl then hot dil.HCl.

3) Cold conc. HCl then hot conc. HCl.

4) Cold dil. HNO3 then hot dil. HNO3.

5) Cold conc. HNO3 then hot conc. HNO3.

6) Aqua ragia ( 3 conc.HCl :1 conc.HNO3 )‫اﻟﻣﺎء اﻟﻣﻠك‬

2. Conduct the following tests for each cation to confirm it.

a. Silver ion, Ag+

1. Soln. + dil. HCl  White ppt. AgCl which turns violet on exposure to light and easily
soluble in NH4OH, but insoluble in dil. HNO3

AgNO3 + HCl AgCl + HNO3

AgCl+ NH4OH [Ag(NH3)2]Cl + 2H2O

2. Soln. + KI  Yellow ppt. AgI insoluble in mineral acids and in NH4OH

AgNO3+ KI AgI + KNO3

3. Soln. + K2CrO4  Red ppt. Ag2CrO4 soluble in both NH4OH and dil. HNO3

2AgNO3 + K2CrO4 Ag2CrO4 + 2KNO3

4. Soln. + NaOH  Brown ppt. Ag2O insoluble in excess reagent.

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AgNO3 + NaOH AgOH + NaNO3

2AgOH Ag2O + H2O

5. Soln. + NH4OH  Brown ppt. complex dissolves in excess reagent.

AgNO3 + 2NH4OH [Ag(NH3)2]NO3 + 2H2O

b. Lead ion, Pb2+

1. Soln. + dil. HCl  White ppt. PbCl2 which soluble in hot water and precipitates on cooling
and insoluble in NH4OH.

Pb(NO3)2 + 2HCl PbCl2 + 2HNO3

2. Soln. + KI  Yellow ppt. PbI2 soluble in boiling and returns on cooling.

Pb (NO3)2 + 2KI PbI2 + 2KNO3

3. Soln. + K2CrO4  yellow ppt. PbCrO4 insoluble in NH4OH

Pb (NO3)2 + K2CrO4 PbCrO4 + 2KNO3

4. Soln. + NaOH  White ppt. Pb (OH)2 soluble in excess reagent.

Pb (NO3)2 + NaOH Pb (OH)2 + NaNO3

Pb (OH)2 + 2NaOH NaPbO2 + 2H2O

5. Soln. + NH4OH  White ppt. Pb (OH)2 insoluble in excess reagent.

Pb (NO3)2 + 2NH4OH Pb (OH)2 + 2NH4NO3

c. Mercurous ion, Hg22+

1. Soln. + dil. HCl  White ppt. Hg2Cl2which insoluble in mineral acids and turns black on
adding NH4OH.

Hg2(NO3)2 + 2HCl Hg2Cl2 + 2HNO3

2. Soln. + KI  Yellowish-green ppt. Hg2I2 which dissolves in excess reagent yielding

Nessler’s reagent.

Hg2(NO3)2 + 2KI Hg2I2 + 2KNO3

3. Soln. + K2CrO4  Brown ppt. Hg2CrO4 which turns red on heating

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Hg2(NO3)2 + K2CrO4 Hg2CrO4 + 2KNO3

4. Soln. + NaOH  Black ppt. of Hg2O.

Hg2(NO3)2 + NaOH Hg2O + 2NaNO3 + H2O

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Results

Lab. 6

1- Silver ion, Ag+

Physical properties:

Solubility: ………………………………………….

Color: ……………………………….………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

White ppt. which turns violet on

1. Soln. + dil. HCl exposure to light and easily soluble in It may be Ag+
NH4OH, but insoluble in dil. HNO3

Yellow ppt. insoluble in mineral acids

2. Soln. + KI It is Ag+
and in NH4OH

Red ppt. soluble in both NH4OH and

3. Soln. + K2CrO4 It is Ag+
dil. HNO3

Brown ppt. insoluble in excess

4. Soln. + NaOH It is Ag+
reagent (NaOH)

Brown ppt. soluble in excess reagent

5. Soln. + NH4OH It is Ag+
(NH4OH)

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2- Lead ion, Pb2+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + dil. HCl

2. Soln. + KI

3. Soln. + K2CrO4

4. Soln. + NaOH

5. Soln. + NH4OH

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3- Mercurous ion, Hg22+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + dil. HCl

2. Soln. + KI

3. Soln. + K2CrO4

4. Soln. + NaOH

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Group II

Introduction

The analysis of basic radicals (Cations) is based on multi-steps process as the acid
radicals, so the cations are arranged into six groups, and each cation group has its own
specific reagent group which will precipitate the members in each group. The reagent of
the lower group does not precipitate the cations of higher groups. The precipitation of the
group cations depends upon the solubility of their salts e.g., chloride, sulfide, hydroxide
and carbonate. Hence, the separation of the basic radicals into various groups is based on
the knowledge of solubility product. For example, in 2nd and 4th groups of basic radicals,
the solubility product of sulfides of 2nd group is lesser than 4th group so that the 2nd group
need acidic medium and hence only those metal sulfides are precipitated which have low
solubility product. On other hand cations in the 4th group need alkaline medium to
precipitate.

Goal

To identify the basic radicals of Group II (Ag+, Pb2+, Hg22+)

Apparatus and tools:

• Test tubes • Gas burner

• Test tube holder • Spatula

• Test tube brushes • Chemical Required: Given Salt and

• Dropper Various reagents

Theory

The basic radicals of Group II (Hg2+, Bi3+, Cu2+, Cd2+) are precipitated as sulfides in acidic
medium using Dil. HCl to avoid affecting the cations of the next groups specially group IV
cations.

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Example:

Soln. + dil. HCl + excess H2S  the ppt. is firstly yellow then brown and finally black HgS.

Hg(NO3)2 + H2S HgS + 2HNO3

Procedure:

1. To identify the cations in their simple salts or in a mixture of them you must have a
soluble salt by preparing a solution by trying to dissolve the salt in the following solvents
(water and Acids) in the order given below:

1) Cold water then hot water .

2) Cold dil.HCl then hot dil.HCl.

3) Cold conc. HCl then hot conc. HCl.

4) Cold dil. HNO3 then hot dil. HNO3.

5) Cold conc. HNO3 then hot conc. HNO3.

6) Aqua ragia ( 3 conc.HCl :1 conc.HNO3 )‫اﻟﻣﺎء اﻟﻣﻠك‬

2. Conduct the following tests for each cation to confirm it.

a. Mercuric ion, Hg2+

1. Soln. + dil. HCl + excess H2S  the ppt. is firstly yellow then brown and finally black
HgS.

Hg(NO3)2 + H2S HgS + 2HNO3

2. Soln. + KI  Red-crimson ppt. HgI2 soluble in excess reagent.

Hg(NO3)2 + 2KI HgI2 + 2KNO3

HgI2 + 2KI K2HgI4

3. Soln. + NaOH  Yellow ppt. HgO

Hg(NO3)2 + NaOH HgO + 2NaNO3 + H2O

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b. Bismuth ion, Bi3+

1. Soln. + dil. HCl + H2S  Blackish-brown ppt. Bi2S3 which soluble in hot HNO3

Bi(NO3)3 + 2H2S Bi2S3 + 6HNO3

2. Soln. + KI  Black ppt. BiI3 soluble in excess reagent.

Bi(NO3)3 + 3KI BiI3 + 3KNO3

BiI3 + KI KBiI4

3. Soln. + NaOH  White ppt. Bi(OH)3 soluble in dil. HNO3

Bi(NO3)3 + 2NaOH Bi(OH)3 + 3NaNO3

Bi(OH)3 + 3HNO3 Bi(NO3)3 + 3H2O

c. Copper ion, Cu2+

1. Soln. + dil. HCl + H2S  Black ppt. CuS soluble in hot HNO3

Cu(NO3)2 + H2S CuS + 2HNO3

2. Soln. + KI  White ppt. CuI and iodine liberating which turns the solution brown.

Cu(NO3)2 + 2KI CuI + I2 + 4KNO3

3. Soln. + NaOH  Blue ppt. Cu(OH)2 turns black on boiling due to formation of CuO

Cu(NO3)2 + 2NaOH Cu(OH)2 + 2NaNO3

Cu(OH)2 CuO + H2O

4. Soln. + NH4OH  Bluish-green ppt. Cu(OH)2 soluble in excess NH4OH yielding deep
blue soln. [Cu(NH3)4](OH)2

Cu(NO3)2 + 2NH4OH Cu(OH)2 + 2NH4NO3

Cu(OH)2 + 4NH4OH [Cu(NH3)4](OH)2 + 4H2O

5. Soln. + K4[Fe(CN)6]  Brown chocolate ppt. Cu2[Fe(CN)6].

2Cu(NO3)2 + K4[Fe(CN)6] Cu2[Fe(CN)6] + 4KNO3

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d. Cadmium ion, Cd2+

1. Soln. + dil. HCl + H2S  yellow ppt. CdS soluble in excess reagent.

Cd(NO3)2 + H2S CdS + 2HNO3

2. Soln. + NaOH  White ppt. Cd(OH)2 soluble in mineral acids and excess of NH4OH

Cd(NO3)2 + 2NaOH Cd(OH)2 + 2NaNO3

Cu(OH)2 + NH4OH [Cd(NH3)4](OH)2 + 2H2O

3. Soln. + NH4OH  White ppt. Cd(OH)2 soluble in excess reagent.

Cd(NO3)2 + 2NH4OH Cd(OH)2 + 2NH4NO3

Cd(OH)2 + 4NH4OH [Cd(NH3)4](OH)2 + 4H2O

4. Soln. + K4[Fe(CN)6]  White ppt. Cd2[Fe(CN)6]

2Cd(NO3)2 + K4[Fe(CN)6] Cd2[Fe(CN)6] + 4KNO3

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Lab. 7

1- Mercuric ion, Hg2+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

When H2S is added in excess to

the acid soln. the ppt. is firstly
1. Soln. + dil. HCl+H2S It may be Hg2+
yellow then brown and finally
black.

Red-crimson ppt. soluble in excess

2. Soln. + KI It is Hg2+
reagent.

Yellow ppt. soluble in excess

3. Soln. + NaOH It is Hg2+
reagent (NaOH)

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2- Bismuth ion, Bi3+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + dil. HCl + H2S

2. Soln. + KI

3. Soln. + NaOH

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3- Copper ion, Cu2+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + dil. HCl + H2S

2. Soln. + KI

3. Soln. + NaOH

4. Soln. + NH4OH

5. Soln. + K4[Fe(CN)6]

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4- Cadmium ion, Cd2+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + dil. HCl + H2S

2. Soln. + NaOH

3. Soln. + NH4OH

4. Soln. + K4[Fe(CN)6]

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Group III

Introduction

The analysis of basic radicals (Cations) is based on multi-steps process as the acid
radicals, so the cations are arranged into six groups, and each cation group has its own
specific reagent group which will precipitate the members in each group. The reagent of
the lower group does not precipitate the cations of higher groups. The precipitation of the
group cations depends upon the solubility of their salts e.g. chloride, sulfide, hydroxide and
carbonate. Hence, the separation of the basic radicals into various groups is based on the
knowledge of solubility product. For example, in 2nd and 4th groups of basic radicals, the
solubility product of sulfides of 2nd group is lesser than 4th group so that the 2nd group need
acidic medium and hence only those metal sulfides are precipitated which have low
solubility product. On other hand cations in the 4th group need alkaline medium to
precipitate.

The basic radicals of Group III (Fe3+, Cr3+, Al3+) are precipitated as hydroxides in using
(NH4Cl + NH4OH) without affecting the cations of the next groups, where NH4Cl control the
concentration of hydroxide ion (OH-) through the common ion effect.

Goal

To identify the basic radicals of Group III (Fe3+, Cr3+, Al3+)

Apparatus and tools:

• Test tubes • Gas burner

• Test tube holder • Spatula

• Test tube brushes • Chemical Required: Given Salt and

Various reagents
• Dropper

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Theory

The basic radicals of Group III (Fe3+, Cr3+, Al3+) are precipitated as hydroxides in using
(NH4Cl + NH4OH) without affecting the cations of the next groups, where NH4Cl control the
concentration of hydroxide ion (OH-) through the common ion effect.

Example:

Soln. + NH4Cl + NH4OH  Brown gelatinous ppt. Fe(OH)3

FeCl3 + 3NH4OH Fe(OH)3 + 3NH4Cl

Procedure:

1. To identify the cations in their simple salts or in a mixture of them you must have a
soluble salt by preparing a solution by trying to dissolve the salt in the following solvents
(water and Acids) in the order given below:

1) Cold water then hot water .

2) Cold dil.HCl then hot dil.HCl.

3) Cold conc. HCl then hot conc. HCl.

4) Cold dil. HNO3 then hot dil. HNO3.

5) Cold conc. HNO3 then hot conc. HNO3.

6) Aqua ragia ( 3 conc.HCl :1 conc.HNO3 )‫اﻟﻣﺎء اﻟﻣﻠك‬

2. Conduct the following tests for each cation to confirm it.

a. Ferric ion, Fe3+

1. Soln. + NH4Cl + NH4OH  Brown gelatinous ppt. Fe(OH)3 dissolves in mineral acids
and insoluble in excess NH4OH

FeCl3 + 3NH4OH Fe(OH)3 + 3NH4Cl

2. Soln. + K4[Fe(CN)6]  Dark blue ppt. Fe4[Fe(CN)6]3 insoluble in dil. HCl

4FeCl3 + 3K4[Fe(CN)6] Fe4[Fe(CN)6]3 + 12KCl

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3. Soln. + K3[Fe(CN)6]  Brown color or ppt. Fe3[Fe(CN)6]

FeCl3 + K3[Fe(CN)6] Fe3[Fe(CN)6] + 3KCl

4. Soln. + Na2HPO4  Yellowish-white ppt.

FeCl3 + 2Na2HPO4 FePO4 + 3NaCl + NaH2PO4

5. Soln. + NH4SCN  Blood red coloration Fe(SCN)3.

FeCl3 + 3NH4SCN Fe(SCN)3 + 3NH4Cl

b. Chromium ion, Cr3+

1. Soln. + NH4Cl + NH4OH  Green ppt. Cr(OH)3 dissolves in excess NH4OH

CrCl3 + 3NH4OH Cr(OH)3 + 3NH4Cl

2. Soln. + NaOH  Green ppt. Cr(OH)3

CrCl3 + 3NaOH Cr(OH)3 + 3NaCl

3. Soln. + Na2HPO4  Yellow ppt. CrPO4dissolves in mineral acids.

CrCl3 + Na2HPO4 CrPO4 + 3NaCl + NaH2PO4

4. Soln. + Na2CO3  Green ppt. Cr2(CO3)3

CrCl3 +2Na2CO3 Cr2(CO3)2 + NaCl

c. Aluminum ion, Al3+

1. Soln. + NH4Cl + NH4OH  White gelatinous ppt. Al(OH)3 dissolves in NaOH

Al2(SO4)3 + 6NH4OH Al(OH)3 + 3(NH4)2SO4

Al(OH)3 + NaOH NaAlO2 + 2H2O

2. Soln. + Na2HPO4  White gelatinous ppt. Al PO4

3. Soln. + Na2CO3  White gelatinous ppt. of Al(OH)3

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Lab. 8

1- Ferric ion, Fe3+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

Brown gelatinous ppt. soluble in

1. Soln. +NH4Cl+NH4OH mineral acids and insoluble in It may be Fe3+
excess NH4OH

2. Soln. + K4[Fe(CN)6] Dark blue ppt. insoluble in dil. HCl It is Fe3+

3. Soln. + K3[Fe(CN)6] Brown color or ppt. It is Fe3+

4. Soln. + Na2HPO4 Yellowish-white ppt. It is Fe3+

5. Soln. + NH4SCN Blood red coloration. It is Fe3+

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2- Chromium ion, Cr3+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + NH4Cl +NH4OH

2. Soln. + NaOH

3. Soln. + Na2HPO4

4. Soln. + Na2CO3

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3-Aluminum ion, Al3+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + NH4Cl +NH4OH

2. Soln. + Na2HPO4

3. Soln. + Na2CO3

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Group IV

Introduction

The analysis of basic radicals (Cations) is based on multi-steps process as the acid
radicals, so the cations are arranged into six groups, and each cation group has its own
specific reagent group which will precipitate the members in each group. The reagent of
the lower group does not precipitate the cations of higher groups. The precipitation of the
group cations depends upon the solubility of their salts e.g. chloride, sulfide, hydroxide and
carbonate. Hence, the separation of the basic radicals into various groups is based on the
knowledge of solubility product. For example, in 2nd and 4th groups of basic radicals, the
solubility product of sulfides of 2nd group is lesser than 4th group so that the 2nd group need
acidic medium and hence only those metal sulfides are precipitated which have low
solubility product. On other hand cations in the 4th group need alkaline medium to
precipitate.

Goal

To identify the basic radicals of Group IV (Zn2+, Mn2+, Ni2+, Co2+)

Apparatus and tools:

• Test tubes • Gas burner

• Test tube holder • Spatula

• Test tube brushes • Chemical Required: Given Salt and

• Dropper Various reagents

Theory

The basic radicals of Group IV (Zn2+, Mn2+, Ni2+, Co2+) are precipitated as sulfides in
alkaline medium using (NH4Cl + NH4OH + H2S) as reagent without affecting the cations of
the next groups.

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Example:

Soln. + NH4Cl + NH4OH + H2S  White ppt. ZnS

ZnSO4 + H2S ZnS + H2SO4

Procedure:

1. To identify the cations in their simple salts or in a mixture of them you must have a
soluble salt by preparing a solution by trying to dissolve the salt in the following solvents
(water and Acids) in the order given below:

1) Cold water then hot water .

2) Cold dil.HCl then hot dil.HCl.

3) Cold conc. HCl then hot conc. HCl.

4) Cold dil. HNO3 then hot dil. HNO3.

5) Cold conc. HNO3 then hot conc. HNO3.

6) Aqua ragia ( 3 conc.HCl :1 conc.HNO3 )‫اﻟﻣﺎء اﻟﻣﻠك‬

2. Conduct the following tests for each cation to confirm it.

a. Zinc ion, Zn2+

1. Soln. + NH4Cl + NH4OH + H2S  White ppt. ZnS

ZnSO4 + H2S ZnS + H2SO4

2. Soln. + NaOH  White ppt. Zn(OH)2 soluble in excess NaOH

ZnSO4 + NaOH Zn(OH)2 + Na2SO4

Zn(OH)2 + 2NaOH Na2ZnO2 + H2O

3. Soln. + NH4OH  White ppt. Zn(OH)2

ZnSO4 + NH4OH Zn(OH)2 + (NH4)2SO4

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b. Manganese ion, Mn2+

1. Soln. + NH4Cl + NH4OH + H2S  Buff ppt. MnS soluble in diluted acids.

MnCl2 + H2S MnS + 2HCl

2. Soln. + NaOH  White ppt. Mn(OH)2which turns in air to pink due to formation of
manganic acid (H2MnO3).

MnCl2 + NaOH Mn(OH)2 + 2NaCl

Mn (OH)2 + O H2MnO3

3. Soln. + NH4OH  White ppt. Mn(OH)2

MnCl2 + 2NH4OH Mn(OH)2 + 2NH4Cl

c. Nickel ion, Ni2+

1. Soln. + NH4Cl + NH4OH + H2S  Black ppt. NiS soluble in hot conc. HNO3 and insoluble
in dil. HCl.

NiCl2 + H2S NiS + 2HCl

2. Soln. + NaOH  Green ppt. Ni(OH)2

NiCl2 + 2NaOH Ni(OH)2 + 2NaCl

3. Soln. + NH4OH  Green ppt. Ni(OH)Cl the basic salt soluble in excess NH4OH

NiCl2 + NH4OH Ni(OH)Cl + NH4Cl

4. Soln. + Dimethyl glyoxim (D.M.G.)  Red ppt. Ni (DMG)2

NiCl2 + D.M.G. Ni (DMG)2 + 2HCl

d. Cobalt ion, Co2+

1. Soln. + NH4Cl + NH4OH + H2S  Black ppt. CoS soluble in hot conc. HNO3 and
insoluble in dil. HCl.

Co(NO3)2 + H2S CoS + 2HNO3

2. Soln. + NaOH  Blue ppt. Co (OH) NO3 the basic salt soluble in excess reagent

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Co(NO3)2 + 2NaOH Co(OH)NO3 + NaNO3

3. Soln. + NH4OH  Blue ppt. Co (OH) NO3 the basic salt soluble in excess NH4OH
yielding red color

Co(NO3)2 + NH4OH Co(OH)NO3 + NH4NO3

4. Soln. + NH4SCN  Violet-blue color (NH4)2[Co(SCN)4] appears due to the formation of

[Co(SCN)4]2+ ion

Co(NO3)2 + NH4SCN (NH4)2[Co(SCN)4] + 2NH4NO3

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Results

Lab. 9

1- Zinc ion, Zn2+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + NH4Cl + NH4OH + White ppt. soluble in mineral

It may be Zn2+
H2S acids.

White ppt. soluble in excess

2. Soln. + NaOH It is Zn2+
NaOH.

White ppt. soluble in excess

3. Soln. + NH4OH It is Zn2+
reagent.

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2- Manganese ion, Mn2+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + NH4Cl + NH4OH +

H2S

2. Soln. + NaOH

3. Soln. + NH4OH

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3- Nickel ion, Ni2+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + NH4Cl + NH4OH +

H2S

2. Soln. + NaOH

3. Soln. + NH4OH

4. Soln. + D.M.G.

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4- Cobalt ion, Co2+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + NH4Cl + NH4OH +

H2S

2. Soln. + NaOH

3. Soln. + NH4OH

4. Soln. + NH4SCN

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Group V

Introduction

The analysis of basic radicals (Cations) is based on multi-steps process as the acid
radicals, so the cations are arranged into six groups, and each cation group has its own
specific reagent group which will precipitate the members in each group. The reagent of
the lower group does not precipitate the cations of higher groups. The precipitation of the
group cations depends upon the solubility of their salts e.g., chloride, sulfide, hydroxide
and carbonate. Hence, the separation of the basic radicals into various groups is based on
the knowledge of solubility product. For example, in 2nd and 4th groups of basic radicals,
the solubility product of sulfides of 2nd group is lesser than 4th group so that the 2nd group
need acidic medium and hence only those metal sulfides are precipitated which have low
solubility product. On other hand cations in the 4th group need alkaline medium to
precipitate.

Goal

To identify the basic radicals of Group V (Ba2+, Sr2+, Ca2+)

Apparatus and tools:

• Test tubes • Gas burner

• Test tube holder • Spatula

• Test tube brushes • Chemical Required: Given Salt and

Various reagents
• Dropper

Theory

The basic radicals of Group V (Ba2+, Sr2+, Ca2+) are precipitated as carbonates in alkaline
medium using (NH4Cl + NH4OH + (NH4)2CO3) as reagent without affecting the cations of
group VI.

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Example:

Soln. + NH4Cl + NH4OH + (NH4)2CO3  White ppt. BaCO3

Soln. + NH4Cl + NH4OH + (NH4)2CO3  White ppt. SrCO3

Procedure:

1. To identify the cations in their simple salts or in a mixture of them you must have a
soluble salt by preparing a solution by trying to dissolve the salt in the following solvents
(water and Acids) in the order given below:

1) Cold water then hot water.

2) Cold dil.HCl then hot dil.HCl.

3) Cold conc. HCl then hot conc. HCl.

4) Cold dil. HNO3 then hot dil. HNO3.

5) Cold conc. HNO3 then hot conc. HNO3.

6) Aqua ragia (3 conc.HCl :1 conc.HNO3 )‫اﻟﻣﺎء اﻟﻣﻠك‬

2. Conduct the following tests for each cation to confirm it

a. Barium ion, Ba2+

1. Soln. + NH4Cl + NH4OH + (NH4)2CO3  White ppt. BaCO3soluble in dil. HCl and acetic
acids.

BaCl2 + (NH4)2CO3 BaCO3 + 2NH4Cl

2. Soln. + dil. H2SO4  White ppt. BaSO4 insoluble in mineral acids.

BaCl2 + H2SO4 BaSO4 + 2HCl

3. Soln. + CaSO4  White ppt.

4. Flame test: Apple green color.

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b. Strontium ion, Sr2+

1. Soln. + NH4Cl + NH4OH + (NH4)2CO3  White ppt. SrCO3soluble in dil. HCl.

SrCl2 + (NH4)2CO3 SrCO3 + 2NH4Cl

2. Soln. + dil. H2SO4  White ppt. SrSO4insoluble in ammonium sulphate.

SrCl2 + H2SO4 SrSO4 + 2HCl

3. Soln. + CaSO4  White ppt. SrSO4 forms slowly on cold and rapidly on boiling

4. Flame test: Crimson red color.

c. Calcium ion, Ca2+

1. Soln. + NH4Cl + NH4OH + (NH4)2CO3  White ppt. CaCO3soluble in dil. HCl.

CaCl2 + (NH4)2CO3 CaCO3 + 2NH4Cl

2. concentrated Soln. + dil. H2SO4  White ppt. CaSO4

CaCl2 + H2SO4 CaSO4 + 2HCl

3. Soln. + CaSO4  No ppt.

4. Flame test: reddish-brown color.

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Results:

Lab. 10

1- Barium ion, Ba2+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + NH4Cl + NH4OH + White ppt. soluble in dil.

It may be Ba2+
(NH4)2CO3 HCl and acetic acids.

White ppt. insoluble in

2. Soln. + dil. H2SO4 It is Ba2+
mineral acids.

3. Soln. + CaSO4 White ppt. It is Ba2+

4. Flame test Apple green color It is Ba2+

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2- Strontium ion, Sr2+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + NH4Cl + NH4OH +

(NH4)2CO3

2. Soln. + dil. H2SO4

3. Soln. + CaSO4

4. Flame test

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3- Calcium ion, Ca2+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + NH4Cl + NH4OH +

(NH4)2CO3

2. Soln. + dil. H2SO4

3. Soln. + CaSO4

4. Flame test

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Group VI

Introduction

The analysis of basic radicals (Cations) is based on multi-steps process as the acid
radicals, so the cations are arranged into six groups, and each cation group has its own
specific reagent group which will precipitate the members in each group. The reagent of
the lower group does not precipitate the cations of higher groups. The precipitation of the
group cations depends upon the solubility of their salts e.g. chloride, sulfide, hydroxide and
carbonate. Hence, the separation of the basic radicals into various groups is based on the
knowledge of solubility product. For example, in 2nd and 4th groups of basic radicals, the
solubility product of sulfides of 2nd group is lesser than 4th group so that the 2nd group need
acidic medium and hence only those metal sulfides are precipitated which have low
solubility product. On other hand cations in the 4th group need alkaline medium to
precipitate.

Group VI is the last one of the basic radicals and it has no specific reagent and cations of
this group are not affected by the precipitation reagents of the previous groups.

Goal

To identify the basic radicals of Group VI (NH4+, Mg2+, K+, Na+)

Apparatus and tools:

• Test tubes • Gas burner

• Test tube holder • Spatula

• Test tube brushes • Chemical Required: Given Salt and

• Dropper Various reagents

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Theory

Group VI is the last one of the basic radicals and it has no specific reagent and cations of
this group (NH4+, Mg2+, K+, Na+) are not affected by the precipitation reagents of the
previous groups.

Example:

Solid + NaOH  Ammonia gas (NH3) evolved

Soln. +NH4Cl+NH4OH+Na2HPO4 white ppt. Mg3(PO4 )2

Procedure:

1. To identify the cations in their simple salts or in a mixture of them you must have a
soluble salt by preparing a solution by trying to dissolve the salt in the following solvents
(water and Acids) in the order given below:

1) Cold water then hot water .

2) Cold dil.HCl then hot dil.HCl.

3) Cold conc. HCl then hot conc. HCl.

4) Cold dil. HNO3 then hot dil. HNO3.

5) Cold conc. HNO3 then hot conc. HNO3.

6) Aqua ragia ( 3 conc.HCl :1 conc.HNO3 )‫اﻟﻣﺎء اﻟﻣﻠك‬

2. Conduct the following tests for each cation to confirm it.

a. Ammonium ion, NH4+

1. Solid + NaOH  Ammonia gas (NH3) evolved characterized by its odor and forming
white fumes with dil. HCl.

NH4Cl + NaOH NH4OH + NaCl

2. Soln. + Nessler's solution.  Yellowish brown color or ppt. according to the

concentration of salt.

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b. Magnesium ion, Mg2+

1. Soln. +NH4Cl+NH4OH+Na2HPO4 white ppt. Mg3(PO4 )2

2. Soln. + NaOH  White ppt. Mg(OH)2 soluble in excess NaOH

MgSO4 + NaOH Mg(OH)2 + Na2SO4

3. Soln. + Na2CO3  white ppt. MgCO3

MgSO4 + Na2CO3 MgCO3

c. Potassium ion, K+

1. Concentrated Soln. + tartaric acid  White ppt. of potassium hydrogen tartarate, the
ppt. is easily formed by shaking the tube or scratching the inner walls of the tube.

2. Soln. + sodium cobaltinitrite  Yellow ppt. of potassium cobaltinitrite insoluble in acetic

acid.

3. Flame test: Violet color.

d. Sodium ion, Na+

1. Soln. + sodium cobaltinitrite  No ppt.

2. Flame test: Golden yellow color.

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Results:

1- Ammonium ion, NH4+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

Ammonia gas evolved characterized

1. Solid + NaOH by its odor and forming white fumes It may be NH4+
with dil. HCl

2. Soln. + Nessler's
yellowish brown color or ppt. It is NH4+
solution

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2- Magnesium ion, Mg2+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + NH4Cl + NH4OH +

Na2HPO4

2. Soln. + NaOH

3. Soln. + Na2CO3

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3- Potassium ion, K+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + tartaric acid

2. Soln. + sodium
cobaltinitrite

3. Flame test

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4- Sodium ion, Na+

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

1. Soln. + sodium
cobaltinitrite

2. Flame test

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General scheme for basic radicals

NH4+ Group I Group II Group III Group IV Group V Group VI

presence
(Ag+, Hg22+& (Cu2, Hg2, (Al3+, Fe3+& (Zn2+, Mn2+, (Ca2+, Sr2+& (Mg2+, K+ &
test
pb2+) Bi3+& Cd2+) Cr3+) Co2+& Ni2+) Ba2+) Na+)

Solid + NaOH Soln. + dil. HCl Soln.+ dil. HCl+ Soln.+ NH4Cl+ Soln. + NH4Cl + Soln. + NH4Cl + Soln. + NH4Cl +
H2S NH4OH NH4OH + H2S NH4OH + NH4OH +
(NH4)2CO3 Na2HPO4
NH3 evolved White ppt.
sol. in Yellow ppt. White gel White gel White ppt. with White ppt.
∴ NH4+ present
NH4OH ppt. ppt. all radicals.
∴ (Cd2+) ∴ (Mg2+)
∴ (Ag+) ∴ (Al3+) ∴ (Zn2+)

Soln + CaSO4
White ppt. Flame test:
White ppt. changes into Grayish- Buff ppt.
changes into yellow then to green ppt.
∴ (Mn2+) No ppt.
black by black Golden
∴ (Cr )3+

NH4OH ∴ (Ca )2+

yellow.
∴ (Hg2+)
∴ (Hg22+) Black ppt. ∴ (Na+)
Brown ppt.
May be Co2+ or White ppt.
Black ppt.
∴ (Fe )3+ Ni2+
White ppt. May be Bi3+ or May be Sr2+ or Violet.
dissolves by Cu2+ So, to differ Ba2+
∴ (K+)
heating & between them:
So, to differ
returns by
between 1. Soln. +
cooling So, to differ
them: NH4SCN
between them:
∴ (Pb2+)
Soln. + KI
Soln. + dil
Violet color
K2CrO4
∴ (Co2+)
Black ppt.

∴ (Bi3+) No ppt.
2. Soln. + DMG
Brown ppt. ∴ (Sr2+)
+ NH4OH
disappear by
Na2S2O3
Red ppt. Yellow ppt.
∴ (Cu2+)
∴ (Ni )2+
∴ (Ba2+)

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Unknown 1

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

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Unknown 2

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

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Unknown 3

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

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Unknown 4

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

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Unknown 5

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

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Unknown 6

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

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Unknown 7

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

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Unknown 8

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

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Unknown 9

Physical properties:

Solubility: ………………………………………….

Color: ………………………………………………

Shape: ……………………………………………...

Chemical properties:

Experiment Observation Result

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‫ﺳﺟل ﺣﺿور وﻏﯾﺎب اﻟطﺎﻟب‬

‫اﺳم اﻟطﺎﻟب‪ .................................................................... :‬اﻟرﻗم اﻟﺟﺎﻣﻌﻲ‪.................................. :‬‬

‫اﻟﻘﺳم‪ .......................................................................................... :‬اﻟﺷﻌﺑﺔ‪.......................... :‬‬

‫اﻟﯾوم‪ .................................... :‬اﻟﺳﺎﻋﺔ‪......................................... :‬‬

‫ﻣﻼﺣظﺎت‬ ‫اﻟﺗﺎرﯾﺦ‬ ‫ﺗوﻗﯾـــﻊ اﻟﻣﺣــــﺎﺿر‬ ‫اﻷﺳﺑوع‬

‫اﻷول‬

‫اﻟﺛﺎﻧﻲ‬

‫اﻟﺛﺎﻟث‬

‫اﻟراﺑﻊ‬

‫اﻟﺧﺎﻣس‬

‫اﻟﺳﺎدس‬

‫اﻟﺳﺎﺑﻊ‬

‫اﻟﺛﺎﻣن‬

‫اﻟﺗﺎﺳﻊ‬

‫اﻟﻌﺎﺷر‬

‫اﻟﺣﺎدي ﻋﺷر‬

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