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2nd Year Practical

The document outlines methods for identifying cations and anions through various chemical tests, detailing reagents, expected results, and chemical equations. It also describes the preparation of iodoform from ethyl alcohol and acetone, including the necessary equipment, chemicals, and procedures for each method. Additionally, it provides insights into the properties and applications of iodoform.

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Faiza Yasir
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0% found this document useful (0 votes)
9 views8 pages

2nd Year Practical

The document outlines methods for identifying cations and anions through various chemical tests, detailing reagents, expected results, and chemical equations. It also describes the preparation of iodoform from ethyl alcohol and acetone, including the necessary equipment, chemicals, and procedures for each method. Additionally, it provides insights into the properties and applications of iodoform.

Uploaded by

Faiza Yasir
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Group Reagents: These are chemical solutions that react with specific groups of cations to form precipitates (solid

substances). This allows for the separation of cations into different groups based on their solubility.

Preliminary Tests: These are simple initial tests to narrow down the possible cations present in the solution.

Confirmatory Tests: These are more specific tests used to confirm the presence of a particular cation.

CATIONS
OS: original solution

Group Cation Group Tests Results Equations


Reagent
O NH₄⁺ No group 1. Sodium Hydroxide Pungent NH₄⁺ + OH⁻ → NH₃ (g) + H₂O
(Ammoni reagent Test: Salt + NaOH ammonia
um) smell; white
fumes with
HCl.
2. Nessler’s Reagent Brown/yellow 2[HgI₄]²⁻ + NH₃ + 4OH⁻ →
Test: OS + NaOH + precipitate. HgO·Hg(NH₂)I·H₂O + 7I⁻
Nessler’s reagent
I Pb²⁺ Dilute HCl 1. White Precipitate White Pb²⁺ + 2Cl⁻ → PbCl₂
(Lead) Test: OS + dilute HCl precipitate;
crystals form
on cooling.
2. Potassium Iodide Yellow Pb²⁺ + 2I⁻ → PbI₂
Test: OS + KI precipitate.
3. Potassium Chromate Yellow Pb²⁺ + CrO₄²⁻ → PbCrO₄
Test: OS + K₂CrO₄ precipitate.
II Cu²⁺ Dilute HCl 1. Black Precipitate Black Cu²⁺ + H₂S → CuS + 2H⁺
(Copper) + H₂S Test: OS + dilute HCl + precipitate.
H₂S
2. Ammonium Blue colored Cu²⁺ + 4NH₃ → [Cu(NH₃)₄]²⁺
Hydroxide Test: solution or
Dissolve ppt in dilute precipitate.
HNO₃, then add excess
NH₄OH
3. Potassium Reddish- 2Cu²⁺ + K₄[Fe(CN)₆] →
Ferrocyanide Test: Part brown/chocola Cu₂[Fe(CN)₆] + 4K⁺
2 + acetic acid + te colored
K₄[Fe(CN)₆] precipitate
(difficult to
get).
III Fe²⁺/Fe³⁺ Solid 1. Brown Precipitate Ferric salts: Fe³⁺ + 3OH⁻ → Fe(OH)₃
(Iron) NH₄Cl + Test: Ferric salts give Brown ppt;
Excess brown ppt; Ferrous salts Ferrous salts:
NH₄OH give green ppt Green ppt.
2. Potassium Blue 4Fe³⁺ + 3K₄[Fe(CN)₆] →
Ferrocyanide Test: Part precipitate or Fe₄[Fe(CN)₆]₃ + 12K⁺
1 + K₄[Fe(CN)₆] solution.
3. Potassium Blood red Fe³⁺ + 3SCN⁻ → Fe(SCN)₃
Thiocyanate Test: Part 2 color with
+ KSCN ferric salts.
Al³⁺ 1. Gelatinous White Clear solution. Al³⁺ + 3OH⁻ → Al(OH)₃
(Aluminu Precipitate Blue color
m) with litmus
and NH₄OH.
Cr³⁺ 1. Sodium Hydroxide Dirty green Cr³⁺ + 3OH⁻ → Cr(OH)₃
(Chromiu Test: OS + NaOH precipitate.
m)
2. Sodium Phosphate Green Cr³⁺ + PO₄³⁻ → CrPO₄
Test: OS + Na₃PO₄ precipitate.
IV Mn²⁺ Solid 1. Manganese Test: OS Buff/skin- Mn²⁺ + H₂S → MnS + 2H⁺
(Mangane NH₄Cl + + solid NH₄Cl + excess colored
se) Excess NH₄OH + pass H₂S gas precipitate.
NH₄OH +
H₂S gas
Zn²⁺ 2. Zinc Test: OS + solid White Zn²⁺ + H₂S → ZnS + 2H⁺
(Zinc) NH₄Cl + excess NH₄OH precipitate.
+ pass H₂S gas

ANIONS
Group Anion Group Tests Results Equations
Reagent
Group CO₃²⁻ Dilute 1. Carbonate Test: WE White CO₃²⁻ + Mg²⁺ →
I (Carbonate) H₂SO₄ + MgSO₄ precipitate. MgCO₃
(dilute
H₂SO₄
group)
2. Barium Chloride White ppt CO₃²⁻ + Ba²⁺ →
Test: WE + BaCl₂ (aq) soluble in BaCO₃
dilute HCl.
SO₃²⁻ Dilute Sulphite Test: Colorless - SO₃²⁻ + 2H⁺ → SO₂
(Sulphite) H₂SO₄ gas with pungent smell (g) + H₂O
S²⁻ Dilute Sulphide Test: Colorless - S²⁻ + 2H⁺ → H₂S (g)
(Sulphide) H₂SO₄ gas with pungent smell
NO₂⁻ Dilute Starch-Iodide Test: WE Deep blue NO₂⁻ + 2I⁻ + 2H⁺ →
(Nitrite) H₂SO₄ + dilute H₂SO₄ (or dilute coloration. I₂ + NO + H₂O
acetic acid), boil, then
add solid KI + fresh
starch
CrO₄²⁻ Dilute 1. Barium Chloride Yellow ppt. CrO₄²⁻ + Ba²⁺ →
(Chromate) H₂SO₄ Test: WE + BaCl₂ (aq) BaCrO₄
2. Lead Nitrate Test: Yellow ppt. CrO₄²⁻ + Pb²⁺ →
WE + Lead nitrate PbCrO₄
Group Cl⁻ Concentrated 1. Silver Nitrate Test: White ppt Cl⁻ + Ag⁺ → AgCl
II (Chloride) H₂SO₄ WE + AgNO₃ soluble in
(conc NH₄OH.
H₂SO₄
group)
2. Chromyl Chloride Orange/red 4Cl⁻ + Cr₂O₇²⁻ + 6H⁺
Test: Salt + solid fumes of → 2CrO₂Cl₂ (g) +
K₂Cr₂O₇ + 2-3 drops conc chromyl 3H₂O
H₂SO₄ chloride.
Br⁻ Concentrated 1. Silver Nitrate Test: Yellow ppt Br⁻ + Ag⁺ → AgBr
(Bromide) H₂SO₄ WE + AgNO₃ partially
soluble in
NH₄OH.
2. Organic Layer Test: Lower layer Br₂ + CCl₄ →
WE + CCl₄ + 1 drop conc organic of Orange/Brown color
HNO₃ orange/brown
color.
I⁻ (Iodide) Concentrated 1. Silver Nitrate Test: Yellow ppt I⁻ + Ag⁺ → AgI
H₂SO₄ WE + AgNO₃ insoluble in
NH₄OH.
2. Organic Layer Test: Lower layer I₂ + CCl₄ → Violet
WE + CCl₄ + 1 drop conc organic of color
HNO₃ violet color.
NO₃⁻ Concentrated Brown Ring Test: WE + Brown ring NO₃⁻ + 4Fe²⁺ + 4H⁺
(Nitrate) H₂SO₄ freshly prepared FeSO₄ + formed at → NO + 3Fe³⁺ +
1 drop conc HNO₃ junction of 2H₂O
solution and
acid.
Group SO₄²⁻ No group Barium Chloride Test: White ppt SO₄²⁻ + Ba²⁺ →
III (Sulphate) reagent WE + BaCl₂ (aq) insoluble in BaSO₄
(special conc HCl.
group)
Notes:

• WE refer to the "Water Extract" of the salt being tested.


• Each test is designed to detect a specific anion based on its unique chemical behavior when treated
with certain reagents.

lists the colors of various salts along with the corresponding inferences about their chemical composition.

Colour Inference Example


Blue Cupric salts (Cu²⁺)copper sulfate (CuSO₄·5H₂O).
Light green Ferrous salts (Fe²⁺)
ferrous sulfate (FeSO₄·7H₂O).
Yellow / Brown Ferric salts (Fe³⁺)ferric chloride (FeCl₃).
Green / Blue Hydrated copper sulfate (CuSO₄·5H₂O)
Hydrated copper salts
where water molecules are part of the
crystal structure.
Pale pink Manganese salts (Mn²⁺) manganese (II) sulfate (MnSO₄).
Dark green / Purple Chromic salts (Cr³⁺) chromium chloride (CrCl₃).
Summary:

These colors arise due to the electronic transitions within the metal ions when they interact with light. The
specific color depends on the metal ion's electronic configuration, oxidation state, and the nature of the
surrounding ligands (in the case of hydrated salts).
Experiment 22: Prepare Iodoform
Method No. 1 (From Alcohol)
Equipment:
• Test tubes • Test tube rack • Safety goggles
• Test tube holder • Bunsen burner
Chemicals:
• Alcohol • Sodium carbonate
• Solution of iodine in potassium iodide • Water
Chemicals Required:
1. Ethyl alcohol (20 ml): The starting material for the iodoform reaction.
2. Sodium carbonate (20 g): Acts as a base to neutralize the acidic byproduct of the reaction and
maintain an alkaline environment.
3. Iodine (5 g): The primary reagent that reacts with the alcohol to form iodoform.
Reaction:
C₂H₅OH + 4I₂ + 3Na₂CO₃ → CHI₃ + 5NaI + HCOONa + 3CO₂ + 2H₂O
ethyl alcohol reacts with iodine and sodium carbonate to produce iodoform (CHI₃), sodium iodide (NaI),
sodium formate (HCOONa), carbon dioxide (CO₂), and water (H₂O).

Procedure:
1. Dissolve Sodium Carbonate: Dissolve 20 g of sodium carbonate in 100 ml of distilled water in a
round-bottom flask.
2. Warm the Solution: Warm the sodium carbonate solution
to 60°C using a water bath.
3. Add Ethyl Alcohol: Add 20 ml of ethyl alcohol to the
warmed sodium carbonate solution.
4. Add Iodine Crystals: Gradually add iodine crystals to the
mixture while shaking continuously. The brown color of the
iodine solution will disappear as it reacts with the alcohol.
Continue adding iodine until the brown color persists,
indicating that the reaction is complete. A pale-yellow
crystalline precipitate of iodoform will form.
5. Isolation of Iodoform: Filter the reaction mixture to collect
the iodoform crystals. Wash the crystals with cold water to
remove impurities.
6. Recrystallization: To purify the iodoform, dissolve the
crystals in a small amount of hot alcohol and then allow the
solution to cool slowly. Pure iodoform crystals will form as
the solution cools.
7. Melting Point Determination: The melting point of pure
iodoform is 119°C.

Method No. 1 (From Acetone)


Chemicals Required:
1. Acetone (10 mL) 3. Iodine (5.0 g)
2. Sodium carbonate (10.0 g):
Reaction:
CH₃COCH₃ + 3I₂ + 2Na₂CO₃ → CHI₃ + 3NaI + CH₃COONa + 2CO₂ + H₂O
acetone reacts with iodine and sodium carbonate to produce iodoform (CHI₃), sodium iodide (NaI), sodium
acetate (CH₃COONa), carbon dioxide (CO₂), and water (H₂O).
Procedure:
1. Dissolve Sodium Carbonate: Dissolve 10.0 g of sodium carbonate in 100 mL of distilled water in a 250
mL round bottom flask.
2. Add Acetone: Add 10 mL of acetone to the sodium carbonate solution.
3. Warm the Solution: Warm the solution to a temperature between 60-70°C.
4. Add Iodine Crystals: Gradually add iodine crystals to the warm solution with frequent shaking. The
brown color of the iodine solution will disappear as it reacts with the acetone. Continue adding iodine
until the brown color persists, indicating that the reaction is complete. A pale yellow crystalline
precipitate of iodoform will form.
5. Isolation of Iodoform: Filter the reaction mixture to collect the iodoform crystals. Wash the crystals
with cold water to remove impurities.
6. Drying: Dry the iodoform crystals.
Feature From Alcohol From Acetone
Starting Material Ethyl Alcohol (Ethanol) Acetone
Initial Step Oxidation of ethanol to acetaldehyde Direct halogenation of acetone
Reaction Involves multiple steps including oxidation Involves primarily alpha-halogenation
Mechanism and alpha-halogenation
Overall Reaction C₂H₅OH + 4I₂ + 3Na₂CO₃ → CHI₃ + 5NaI + CH₃COCH₃ + 3I₂ + 2Na₂CO₃ → CHI₃ + 3NaI +
HCOONa + 3CO₂ + 2H₂O CH₃COONa + 2CO₂ + H₂O
Extra information:
• Iodoform is a crystalline pale-yellow material that is highly flammable. It is insoluble in water but
soluble in ethyl alcohol and ether. Iodoform has a chemical behavior that is nearly identical to that
of chloroform. The iodoform test detects the presence of an aldehyde or ketone in which a methyl
group is one of the groups immediately linked to the carbonyl carbon. It is also used as an antiseptic
and in the manufacture of pharmaceuticals, among other uses. The Iodoform tests can also be used
to identify several pairs of compounds.
• Iodoform has tetrahedral molecular geometry. The iodoform molecule
contains 4 bonds, of which 3 are C–I bonds, and one is a C–H bond.

Experiment 23: Prepare Glucosazone
Equipment:
• Beakers • Balance • Funnel
• Test tube • Bunsen burner • Filter papers
• Measuring cylinders • Match box
Chemicals:
• Glucose solution • Acetic acid
• 2,4-Dinitrophenylhydrazine solution
• Distilled water
Material Required:
• Phenylhydrazine hydrochloride (2 g)
• Glucose (1.0 g)
• Sodium acetate (3 g)
Chemical Reaction:

Glucose reacts with three molecules of phenylhydrazine to form glucosazone, aniline, and water.
Procedure:
1. Prepare Phenylhydrazine Solution: Take 2 g of phenylhydrazine hydrochloride in a small round bottom
flask. Add 3 g of sodium acetate crystals and about 20 mL of water. Shake the mixture thoroughly to
obtain a clear solution.
2. Add Glucose: To this solution, add 1.0 g of glucose dissolved in about 5 mL of water.
3. Heat the Mixture: Heat the flask on a water bath for about an hour.
4. Cool and Collect Crystals: Cool the flask and observe the formation of yellow crystals of glucosazone.
5. Purification:
• Filter the mixture to collect the yellow crystals.
• Wash the crystals with dilute acetic acid to remove impurities.
• Recrystallize the crystals from hot alcohol to obtain pure glucosazone.
Result:
Pure yellow crystals of glucosazone are obtained with a melting point of 205°C.
Extra information:
• Glucosazone is a characteristic derivative of glucose and is used to identify and characterize sugars.
• The reaction of glucose with phenylhydrazine is known as the osazone formation reaction.
Experiment 33: Identify Carboxylic Acids Using Sodium Carbonate Test
Apparatus:
• Test tubes • Spatula • Delivery tube
• Test tube rack • Burner • Corks
• Test tube holder • Match box
Chemicals:
• Acetic acid solution • Distilled water
• Solid sodium carbonate • Lime water
Chemical Reaction:
CH₃COOH + Na₂CO₃ → CH₃COONa + H₂O + CO₂

Acetic acid reacts with sodium carbonate, it produces sodium acetate, water, and carbon dioxide gas.
Procedure:
1. Take acetic acid: A small amount of dilute acetic
acid is taken in a test tube.
2. Add sodium carbonate: A few crystals of solid
sodium carbonate are added to the acetic acid
solution.
3. Observe reaction: The reaction between acetic
acid and sodium carbonate produces carbon
dioxide gas (CO₂), which is observed as
effervescence.
4. Test for CO₂: The evolved gas is passed through
lime water (a clear solution of calcium
hydroxide). If carbon dioxide is present, the lime
water will turn milky due to the formation of
insoluble calcium carbonate (CaCO₃).

Result:
The evolution of carbon dioxide gas (confirmed by the lime water test) indicates the presence of a carboxylic
acid.
In Summary:
This experiment demonstrates a simple chemical test to identify carboxylic acids based on their reaction with
sodium carbonate, which produces carbon dioxide gas.

Carboxylic Acids
Definition: Carboxylic acids are organic compounds that contain the carboxyl functional group (-COOH). This
group consists of a carbonyl group (C=O) bonded to a hydroxyl group (-OH).
It interact easily with polar compounds and contributes to many important chemical reactions.
Carboxylic acids have a tendency to donate protons and act as acids. It is this property which is helpful in
the identification of a -COOH group.
Examples of Carboxylic Acids
• Formic Acid (HCOOH): Found in ants.
• Acetic Acid (CH₃COOH): Commonly known as vinegar.
• Oxalic Acid (HOOC-COOH): Found in spinach.
• Citric Acid: Found in citrus fruits (lemons, oranges).
• Tartaric Acid: Found in grapes.
• Malic Acid: Found in apples and pears.
Formation of Acetic Acid (Ethanoic Acid)
• Oxidation of Ethyl Alcohol: Acetic acid is produced by the oxidation of ethyl alcohol (ethanol) with air.
• Role of Bacteria: In this process, tiny microorganisms called bacteria play a crucial role in the
oxidation of ethyl alcohol.
Chemical Equation:
C₂H₅OH + O₂ → CH₃COOH + H₂O
Uses of Acetic Acid
• Vinegar: Vinegar, which contains 5% acetic acid, is used as a preservative and flavoring agent in food.
• Industrial Uses: Acetic acid is an important industrial chemical used in the manufacture of various
products, including:
o Drugs
o Dyes
o Paints
o Insecticides
o Plastics
• Ester Formation: Acetic acid is used to make esters, which are a class of organic compounds with a
wide range of applications, such as fragrances and flavors.

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