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TECHNICIAN’s HAND BOOK

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 1
April 2009
DETERMINATION OF DENSITY

Students will work in PAIRS – Therefore, there will be 2 SETS of the following placed on
EACH Student Bench:
• 1 - Analytical Balance …………..placed in the middle of the bench

• 1 set placed on the LEFT SIDE & the other placed on the RIGHT SIDE

• 1 - 100mL Beaker with approx 50mL oil kept in the middle of the bench for both groups to
use.
• 1 Thermometer
• 10mL Disposable Pipette
• Pipette filler / pump
• 1 – dry clean 50mL beaker

RIGHT HAND SIDE OF WHITE BOARD

Important Pointers
• Place all books / bags in proper place
• Each GROUP is given:
Thermometer
10mL disposable pipette with pump/filler
50mL beaker
Beaker containing approx 50mL of olive oil
• Wash ALL glasswares and maintain clean work area before leaving the lab

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 2
April 2009
THIN- LAYER CHROMATOGRAPHY

PRE-LAB PREPARATION (Preferably 1 day earlier) :

SPINACH EXTRACT:

• Chop 10g spinach leaves very finely. Transfer to a conical flask containing 100mL 1:1 acetone-
ether solution
• Shake well for 5 mins.
• Filter to remove particulates and concentrate the sample in a water bath
• The extract must be dark green in color and stored in an amber bottle and refrigerated.

REFERENCE COLOR TABLE FOR BANDS ON TLC PAPER

Leaf Pigments Color


Carotenes Golden/ Yellow/ Orange
Pheophytin Olive Green
Chlorophyll – a Blue Green
Chlorophyll – b Yellowish Green
Lutein Yellow
Viola Xanthin Yellow
Neo-Xanthin Yellow

Instructor’s Table Reagent Station :


• Label Large Filter Paper with the following and place the item on top of the filter
paper
o TLC Paper …all cut into thin strips, so as to fit into jar exactly
o 1:1 Acetone-Ether (ELUENT)
o Chromatography Jar + Lid
o Spinach Extract (Sample)
o Capillary Tubes

Students will work in PAIRS – Therefore, there will be 2 SETS of the following placed on table

EACH Set contains


 1 - Chromatography Jar + Lid
 1 - 100 mL (Labelled)Beaker with approx. 50ml of 1:1 acetone-ether solution (Eluent)
 1 – Ruler , pencil
 2 - TLC Paper Strip cut to size to fit inside the jar

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 3
April 2009
DETERMINATION OF BOILING POINTS & MELTING POINTS
OF ORGANIC COMPOUNDS

Each Student Bench will have 1 complete set of the following:


• Table 1: will have 1small weighing boat + 1 small 15mL TT with lid containing solid &
liquid samples- marked UNKNOWN A
• Table 2: will have 1small weighing boat + 1 small 15mL TT with lid containing solid &
liquid samples- marked UNKNOWN B
• Table 3: will have 1small weighing boat + 1 small 15mL TT with lid containing solid &
liquid samples- marked UNKNOWN C and so on ………………… etc………………
** Prepare a KEY of all UNKNOWNS and give it to the Instructor, before the Lab **

Part (I-a): TO DETERMINE MELTING POINT OF A SOLID ORGANIC SAMPLE


• Melting Point apparatus
• Small weighing boat containing UNKNOWN SOLID
• Small weighing Boat containing at least 2 capillary tubes (open at one end)

--------------------------------------------------------------------------------------------------------SPACE-----

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 4
April 2009
Part (I-b): DETERMINE BOILING POINT OF A LIQUID ORGANIC SAMPLE
• 250mL beaker containing some boiling chips + distilled water on a hot plate
• Burette stand with clamp
• 1- 15mL Test-tube with lid containing the liquid organic solvent
• Thermometer

-----------------------------------------------------------------------------------------------------------------

RIGHT HAND SIDE OF WHITE BOARD

Important Pointers
• MELTING POINTS OF SOLIDS:
Acetamide : 81 -82C
Phenol: 40- 42C
Benzoic Acid: 122 – 124C
Urea: 132 – 135C
• BOILING POINTS OF LIQUIDS:
Acetone : 56 – 58C
Acetonitrile: 82 – 84C
Ethanol: 78 – 80C
Hexane: 69 – 71C
• Wash All glassware (Do not discard boiling chips) before leaving the lab
• Switch-off and Unplug all Electric Devices

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 5
April 2009
RECRYSTALLIZATION OF IMPURE BENZOIC ACID

▲▲ Keep 500mL beaker with distilled water in the fridge


▲▲ Keep 1 wash bottle containing distilled water in the fridge
This is to be used for Vacuum Filtration and will be done by the technician, for all groups on the
Instructor’s Table
▲▲ Keep large beaker containing distilled water on a hot plate on preparation table

Each Student Bench will have 1 complete set of the following:


• Small weighing boat containing a mixture of 1g Benzoic acid + 1g α - naphthol
• 150mL beakers ………2 Nos
• Watch glass
• Glass Rod
• Small Labels, marker
• Ice Bucket with ice
• Glass sintered Buchner funnel with small filter paper
• Gravity filtration set-up: Large filter funnel, tripod, large filter paper
• Hot plate mounted with 250mL beaker containing distilled water

Instructor’s Table:
• Vacuum Filtration pump fitted with 250mL filter flask and tygon tubing
• Ice bucket containing ice

RIGHT HAND SIDE OF WHITE BOARD

Important Pointers
• Each student is given 2g of the impure benzoic acid mixture
• Gravity Filtration: Fold the filter paper in an ACCORDION shape
• Buchner Filtration: will be done on the Instructor’s Table
• MELTING POINTS and WEIGHTS of your result will be displayed on the notice board
TOMORROW.
• Switch-off and Unplug all Electric Devices
• Wash All glassware before leaving the lab

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 6
April 2009
CHEMICAL & PHYSICAL SEPARATION OF ORGANIC MIXTURES

▲▲ Keep 500mL beaker with distilled water in the fridge


▲▲ Keep 1 wash bottle containing distilled water in the fridge
This is to be used for Vacuum Filtration and will be done by the technician, for all groups on the
Instructor’s Table

Each Student Bench will have 1 complete set of the following:


• 150mL beaker containing 1.5g Benzoic acid + 1.5g Naphthalene in 60mL dichloromethane
Beaker should be labeled “SAMPLE MIXTURE”
• 50mL NaOH (2M) in a labeled 100mL beaker
• 50mL HCl (2M) in a labeled 100mL beaker
• 2g Na2SO4 in a labeled weighing boat (small)
• 150mL conical flask
• Gravity filtration set-up: large filter funnel, large filter paper, tripod stand
• Separatory Filtration Set-up: 250mL Separatory Funnel, stand
• 150mL beakers ….2Nos
• Ice bucket containing ice
• Blue litmus paper strips
• Glass Rod
• Sintered glass buchner funnel, small filter paper
• Large size filter paper

Instructor’s Table:
• Vacuum Filtration pump fitted with 250mL filter flask and tygon tubing
• Ice bucket containing ice
Hood:
• Each hood must be set-up with 2-3 hot plates

RIGHT HAND SIDE OF WHITE BOARD


Important Pointers
Each student is given the following:
• 60mL sample mixture
• 50mL HCl (2M)
• 50mL NaOH (2M)
• 2g Na2SO4
• Gravity Filtration: Fold the filter paper in an ACCORDION shape
• Buchner Filtration: will be done on the Instructor’s Table
• MELTING POINTS and WEIGHTS of your result will be displayed on the notice board
TOMORROW.
• Switch-off and Unplug all Electric Devices
• Wash All glassware before leaving the lab

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 7
April 2009
 Refer Attached Scheme 

CHEMICAL & PHYSICAL SEPARATION OF A MIXTURE OF ORGANIC COMPOUNDS


60 ml of Benzoic Acid and Naphthalene Mixture
dissolved in organic solvent

Add 50 ml of (2M) NaOH and shake

 2 layers will be formed, separate the mixture using separatory funnel

Organic Layer (bottom) in a Aqueous Layer (top) in a beaker


conical flask

Add ∼ 2 g of Add 50 ml of
anhydrous Na2SO4 (2M) HCl, check acidity
and shake (5 minutes) using litmus + stirring

 Weigh the EMPTY beaker Cooling in ice bucket


BEFORE Filtration
Simple Filtration

Filtrate Solid Buchner Filtration


( Liquid) ( Discard)

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 8
April 2009
Liquid Solid
(Discard) Dry & weigh
Next lab
Collect the filtrate in beaker
and place it on hot plate
under the fume hood

Cool and weigh next lab

PREPARATION AND PROPERTIES OF SOAP

Each Student Bench will have 1 complete set of the following:


• Burette Stand with clamp, clamped to 250mL conical flask
• Glass Rod
• 25mL olive oil in a labeled 50 mL beaker
• 30mL ethanol in a labeled 50mL beaker (cover with aluminum foil)
• Hot plate Stirrer
• 100mL saturated NaCl or KCl salt solution in a labeled 150mL beaker
• Ice Bucket with ice
• Red Litmus paper strips
• TT Rack with 1 TT containing equal amounts of oil and water, 3 empty TT
• Distilled Water Wash Bottle
• 5mL disposable pipette and pump ( to draw excess liquid)
• Extra Large Filter Paper (to be used for drying the soap)
• 1 No. 50mL Measuring Cylinders
• 1 No. 150mL beaker

Instructor’s Table / Side Reagent Table should have the following:


• NaOH Reagent Bottle
• Spatula
• Weighing Boats
• At least 2 Analytical Balances, placed at a reasonable distance

RIGHT HAND SIDE OF WHITE BOARD

Important Pointers
Each student is given the following:
• 30mL ethanol
• 25mL olive oil
• 100mL saturated salt solution
• Gravity Filtration: Fold the filter paper in REGULAR shape ; use TWO filter PAPERS
• NaOH is kept on the Reagent Table. Close bottle after use
• Switch-off and Unplug all Electric Devices

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 9
April 2009
• Wash All glassware before leaving the lab

 Refer Attached Scheme 

Preparation of Soap

 Dissolve 10 g NaOH in 50mL H2O in a beaker


 Add 30mL Ethanol
 Transfer this solution to a conical flask

 Add 25mL olive oil & continuously stir, using magnetic stirrer

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 10
April 2009
 Attach the conical flask to a burette stand
and now, place on a hot plate
 Continuously stir for 30 minutes
 Wait for all ethanol to evaporate
 Cool in Ice Bucket for 10 min

 Saturate the mixture with 100mL NaCl / KCl solution

Simple Gravity Filtration

Let the Solid Residue (SOAP) air-dry and discard the filtrate

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 11
April 2009
FROM THE NEXT EXPERIMENT ONWARDS,
FOR EVERY LAB-PREPARATION & STUDENT
SESSION :

LEAVE THE HOT WATER TAPS RUNNING

IDENTIFICATION OF FUNCTIONAL GROUPS


ALKANES , ALKENES & ARENES (SET 1)

Each Student Bench will have 1 complete set of the following:


15mL TT with lids, containing Labels and approx 10mL of:
• ALKANE (on Label) : Hexane or any other alkane
• ALKENE (on Label) : Hexene or any other alkene
• ARENE (on Label) : Benzene or any other arene
TT- Rack containing :
• 3 glass droppers
• 10-12 TT

• Strip of Labels (small)


Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 12
April 2009
• Aluminum Foil
• Wash Bottle containing Distilled Water

Instructor’s Table:
• Dichloromethane / Dichloroethane in a reagent bottle placed on filter paper labeled:
ORGANIC SOLVENT
• Dilute H2SO4 (approx 2N) in a reagent bottle placed on a filter paper labeled: DIL . H2SO4
• Dilute KMnO4 in a reagent bottle placed on a filter paper labeled: DIL . KMnO4
• Dilute NaOH (approx 2N) in a reagent bottle placed on a filter paper labeled: DIL . NaOH

Hood:
• Bromine in CCl4 (Amber Bottle) in a reagent bottle placed on a filter paper labeled:
BROMINE IN CCl4 (With Glass Dropper)
• Conc. H2SO4 in a reagent bottle placed on a filter paper labeled: Conc. H2SO4 (With Glass
Dropper)

RIGHT HAND SIDE OF WHITE BOARD

Important Pointers
Each student is given the following:
• 10mL ALKANE (Hexane or….)
• 10mL ALKENE (Hexene or….)
• 10mL ARENE (Benzene or…)
• Reagents on Instructor’s Table: Dichloromethane (Organic Solvent), KMnO4,Dil NaOH,
Dil H2SO4
• Reagents in the Hood: Bromine Water, Conc. H2SO4
• Wash All glassware before leaving the lab
• For test with conc. H2SO4 , DO NOT wash test-tube. Keep in hood.

 Refer Attached Scheme 

Tests for Alkanes, Alkenes and Arenes - KEY

1- Physical properties
Procedure: a- Comment on the appearance of each test sample
b- Dissolve each of the test sample once in water and other time in
organic solvent and write your observation

Test sample Appearance Solubility


In water In organic
solvent
Alkane : Liquid - Colorless Insoluble-2 layers Soluble
Alkene : Liquid - Colorless Insoluble-2 layers Soluble
Arene : Liquid - Colorless Insoluble Soluble

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 13
April 2009
2- Chemical properties

a- Reaction with bromine


Procedure: 1 -Add about 1 mL of test solution in two separate tubes
2-To each tube add few drops of bromine in CCl4
3-Keep one tube in a dark place and expose the other to sun light and
write your observation.

Test sample In dark Sun light


Alkane : No Reaction Red Color Disappeared
Alkene : Red Color Disappeared Red Color Disappeared

b- Reaction with sulfuric acid


Procedure: 1- diluted acid: 2 ml of test sample + 3 ml diluted H2SO4
2- conc. acid : 2 ml of test solution + 5 drops of conc. H2SO4

Test sample Diluted H2SO4 Conc H2SO4


Alkane : Insoluble-2 layers Insoluble-2 layers
Alkene : Insoluble-2 layers (Soluble) Homogenous – 1
layer
Arene : Insoluble-2 layers Insoluble-2 layers

c- Reaction with potassium permanganate ( Baeyer's Test)


Procedure : 2 ml of test sample + some drops of aq. KMnO4 + some drops of aq. NaOH

Test sample Observation


Alkane : No ppt.
Alkene : Brown ppt.
Arene : No ppt.

IDENTIFICATION OF FUNCTIONAL GROUPS


ALCOHOLS & PHENOLS (SET 2)

Each Student Bench will have 1 complete set of the following:


15mL test tubes with lids containing Labels and approx:
• 10 mL ALCOHOL (on Label) : 1° , 2° and 3° e.g. 1-Propanol, 2-propanol, tert. Butyl alcohol
• PHENOL (on Label) : Phenol (solid)

TT- Rack containing :


• 3 glass droppers

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 14
April 2009
• 1 Spatula
• 10-12 TT

• Strip of Labels (small)


• Wash Bottle containing Distilled Water
• Hot plate Stirrer with a 250mL beaker containing some water (this will be used as a water bath)

Instructor’s Table:
• Dichloromethane / Dichloroethane in a reagent bottle placed on filter paper labeled:
ORGANIC SOLVENT
• Cerric Ammonium Nitrate (solid) in reagent bottle placed on a filter paper labeled:
CERRIC AMMONIUM NITRATE
• 3M NaOH in a reagent bottle placed on a filter paper labeled: 3M NaOH
• Freshly prepared FeCl3 in a reagent bottle placed on a filter paper labeled : FeCl3

Hood:
• Bromine in CCl4 (Amber Bottle) in a reagent bottle placed on a filter paper labeled:
BROMINE IN CCl4 (With Glass Dropper)
• Chromic Acid in a reagent bottle placed on a filter paper labeled: CHROMIC ACID

RIGHT HAND SIDE OF WHITE BOARD

Important Pointers
Each student is given the following:
• 10mL ALCOHOL (1° , 2° and 3° e.g. 1-Prpanol, 2-propanol, tert. Butyl alcohol )
• PHENOL (Phenol )
• Reagents on Instructor’s Table: Dichloromethane (Organic Solvent), Cerric Ammonium
Nitrate , 3M NaOH, FeCl3
• Reagents in the Hood: Bromine Water, Chromic Acid
• Wash All glassware before leaving the lab

 Refer Attached Scheme 

Tests for Alcohols and Phenols - KEY

(1) Results of Alcohol Identification

(A) Physical Properties (B) Chemical Properties

Polar Solvent non-polar solvent Cerric Ammonium Chromic Acid


Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 15
April 2009
(H2O) (1,2dichloroethane) nitrate – 5drops 2 Drops
+5 mins in 60°
water bath

Partially Completely Red Color Losing Initial


indicating –OH Red Color
group to become
Blue-Green

(2) Results of Phenols Identification

(A) Physical Properties (B) Chemical Properties

Polar Solvent non-polar solvent 2 M NaOH FeCl3 Br2/CCl4


(H2O) (1,2dichloroethane) 5 drops

Partially Completely One Violet Brown Color of


Layer Bromine will
disappear &
then yellowish
white ppt.

IDENTIFICATION OF FUNCTIONAL GROUPS


ALDEHYDES & KETONES (SET 3)

Each Student Bench will have 1 complete set of the following:


Vials containing Labels and approx:
• 10 mL ALDEHYDE (on Label) :acetaldehyde or any other aldehyde
• KETONE (on Label) : Acetone or any other ketone

TT- Rack containing :


Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 16
April 2009
• 2 glass droppers
• 10-12 TT
• Hot plate with 250mL beaker containing distilled water & boiling chips
• Strip of Labels (small)
• Wash Bottle containing Distilled Water

Instructor’s Table:
• Dichloromethane / Dichloroethane in a reagent bottle placed on filter paper labeled:
ORGANIC SOLVENT
• 2,4 DNPH in a reagent bottle placed on filter paper labeled: 2,4 DNPH
• Fehling’s A and Fehling’s B in a reagent bottle placed on filter paper labeled: FEHLING’S
A, FEHLING’S B
Hood:
• Chromic Acid in a reagent bottle placed on filter paper labeled: CHROMIC ACID

RIGHT HAND SIDE OF WHITE BOARD

Important Pointers
Each student is given the following:
• 10mL ALDEHYDE
• 10mL KETONE
• Reagents on Instructor’s Table: Dichloromethane (Organic Solvent), 2,4 DNPH ,
Fehling’s A and Fehling’s B
• Reagents in the Hood: Chromic Acid
• Switch off and unplug hot plates after use
• Wash All glassware before leaving the lab

 Refer Attached Scheme 

Tests for Aldehydes & Ketones - KEY

Aldehydes Ketones

2,4
2,4 DNPH
DNPH + + 22 Chromic Fehling’s A + 2,4 DNPH + 2 Chromic Fehling’s A +
drops aldehyde
drops aldehyde Acid + 2 Fehling’s B + drops ketone Acid + 2 Fehling’s B +
Prepared by Ms. Carmen
drops DSouza & Schemes done by Mrs. Mariam
2 drops Al-Asousi2 drops ketone
drops ketone 17
aldehyde aldehyde + April 2009 + water bath
water bath 60C 60C
Yellow to Initial brown Initial blue to Yellow to No Reaction No Reaction
Red ppt to blue-green red Red ppt

IDENTIFICATION OF FUNCTIONAL GROUPS


CARBOXYLIC ACID & AMMONIUM SALTS OF CARBOXYLIC ACIDS (SET 4)

Each Student Bench will have 1 complete set of the following:


Vials containing Labels and approx:
• 10 mL Acetic Acid (on Label)
• Benzoic Acid (on Label)
• Ammonium Acetate (on Label)
TT- Rack containing :
• 1 glass droppers
• 2 Spatula
Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 18
April 2009
• 10-12 TT
• Red Litmus Paper
• Strip of Labels (small)
• Wash Bottle containing Distilled Water

Instructor’s Table:
• Dichloromethane / Dichloroethane in a reagent bottle placed on filter paper labeled:
ORGANIC SOLVENT
• NaHCO3 in a reagent bottle placed on filter paper labeled: NaHCO3
• FeCl3 in a reagent bottle placed on filter paper labeled: FeCl3

Hood:
• 6M NaOH in a reagent bottle placed on a filter paper labeled: 6M NaOH
• Conc. HCl (with glass rod) in a reagent bottle placed on a filter paper labeled: Conc. HCl

RIGHT HAND SIDE OF WHITE BOARD

Important Pointers
Each student is given the following:
• 10mL ACETIC ACID
• BENZOIC ACID
• AMMONIUM ACETATE
• Reagents on Instructor’s Table: Dichloromethane (Organic Solvent), NaHCO3 , FeCl3
• HOOD: 6M NaOH , Conc. HCl
• Wash All glassware before leaving the lab

 Refer Attached Scheme 

Tests for Carboxylic Acid - KEY


Acids used: 1- Acetic acid
2- Benzoic acid

(A) Physical Properties (B) Chemical Properties

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 19
April 2009
Polar Solvent non-polar solvent Test with NaOH Test with NaHCO3
(H2O) (1,2dichloroethane)

1- Acetic Acid: 1- Acetic Acid: 1- Acetic Acid: 1- Acetic Acid:


Soluble Soluble Soluble Effervescence
CO2 gas
2- Benzoic Acid 2- Benzoic Acid
2- Benzoic Acid
Insoluble Soluble 2- Benzoic Acid
Insoluble
Effervescence
CO2 gas

(1) Tests for Ammonium Salts of carboxylic acids


Salt used :Ammonium Acetate

Test with NaOH Test with FeCl3


 NH3 smell Dark Red Color
 Red litmus blue
 White fumes or clouds of NH4Cl with conc HCl

IDENTIFICATION OF FUNCTIONAL GROUPS


AMIDES & DIAMIDES (SET 5)

▲▲ Open the Gas valve and light the Bunsen burner on Preparation Table ( # 6) so as to
carry out Biuret Test. Keep 1 bottle of Biuret Reagent and 1 TT Rack with test-tubes. ▲▲

Each Student Bench will have 1 complete set of the following:


Vials containing Labels:
• ACETAMIDE (on Label)
Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 20
April 2009
• UREA (on Label)
TT- Rack containing :
• 2 spatulas
• 10-12 TT
• Red Litmus Paper
• Strip of Labels (small)
• Wash Bottle containing Distilled Water

Instructor’s Table:
• Dichloromethane / Dichloroethane in a reagent bottle placed on filter paper labeled:
ORGANIC SOLVENT

Hood:
• 6M NaOH in a reagent bottle placed on a filter paper labeled: 6M NaOH
• Conc. HCl with glass rod
• Conc. HNO3 (with glass dropper) in a reagent bottle placed on a filter paper labeled:
Conc. HNO3

RIGHT HAND SIDE OF WHITE BOARD

Important Pointers
Each student is given the following:
• ACETAMIDE
• UREA
• Reagents on Instructor’s Table: Dichloromethane (Organic Solvent)
• Reagents in the Hood: Con. HNO3, 6M NaOH, Conc. HCl
• Biuret Test will be conducted on the LAST BENCH
• Wash All glassware before leaving the lab

 Refer Attached Scheme 

Tests for Amides and Diamides - KEY

1- Physical Properties

Sample Appearance Solubility


Polar solvent Non-polar solvent
Acetamide Solid - Crystalline Soluble Soluble
Urea Solid Amorphous- Soluble Sparingly insoluble

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 21
April 2009
2- Chemical Properties:

A- Tests for Amide ( Acetamide)

 Reaction of acetamide with NaOH

1/2 spatula of acetamide + 3 ml of 6M


NaOH then boil

 NH3 smell
 Red litmus blue
 White fumes or clouds of NH4Cl with conc HCl

(B) Tests for Diamides (Urea)

Biuret Test Reaction with conc. HNO3


Urea in TT, heat to melt, keep heating till
Urea solidifies on flame itself.
Cool TT in TT Rack and then add reagent

Violet Color White ppt.

 IMPORTANT PREPARATIONS 
▲▲ Do your calculations according to no. of students and exact quantity of
reagent required, in order to avoid wastage of chemicals ▲▲

• BIURET REAGENT :
Dissolve about 3.46g of cupric sulfate in 10mL of hot water and allow to cool. This is solution
A.

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 22
April 2009
Dissolve about 34.6g of sodium citrate dihydrate and 20g of sodium carbonate in 80mL hot
water and allow to cool. This is solution B
Mix solutions A and B and dilute with water to 200mL.

This reagent is stable for 6months. Do not use the reagent if it turns turbid or has any
precipitate

• CHROMIC ACID:
Dissolve 140g of sodium dichromate dihydrate in approx 100mL water. Add 2 liters of 98%
conc. Sulfuric acid to a 4-5 liter glass beaker that is sitting in a cold water bath in the fume
cupboard.
Carefully stir the acid gently and pour a few mls of the dichromate solution slowly to the acid.
Keep repeating the addition every few seconds after the previous dose has been dispersed.
As long as the stirring is GENTLE and CONTINUOUS, little or no splattering should occur
BUT the solution will become quite warm.

Allow to cool before storing in a glass stoppered reagent bottle. Always ensure that the stopper
is sufficiently lose to release any gas pressure.

NEVER use a crew caped or similar types of sealed containers

If made gently and correctly, chromic acid should have NO PRECIPITATE and will be deep
red in color and will last for years !

• FEHLING’S SOLUTION A:
Dissolve 17.32g of hydrated copper sulfate crystals in 200mL water and dilute the solution to
250mL

• FEHLING’S SOLUTION B:
Dissolve 86.5g of sodium potassium tartarate and 25g of sodium hydroxide in 100mL water
and dilute the solution to 250mL

• 2,4 DNPH:
Method 1:
1.2g of 2,4 dinitrophenyl hydrazine is immersed in 12mL conc. HCl in the hood. The formed
light yellow hydrochloride is mixed to produce a slurry that is then poured into 600mL of 2N
HCl with continuous stirring. The hydrochloride should is perfectly dissolved

Method 2:
Suspend 2g of 2,4 dinitrophenyl hydrazine in 100mL methanol. Cautiously and slowly add
4mL of conc. Sulfuric acid in the hood. It should be a clear solution
Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 23
April 2009
Method 3:
Dissolve 0.25g of 2,4 dinitrophenyl hydrazine in a mixture of 42mL conc. HCl and 50mL
water, by warming on a water bath. Dilute to 100mL with distilled water.
This reagent is more suitable for water soluble aldehydes and ketones since alcohol is absent.

Method 4: (Brady’s Reagent)


Dissolve 40g of 2,4 dinitrophenyl hydrazine in 80mL conc. sulfuric acid in the hood. Cool and
add 900mL methanol and then 100mL water.

Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 24
April 2009