Professional Documents
Culture Documents
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
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
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.
Students will work in PAIRS – Therefore, there will be 2 SETS of the following placed on table
Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 3
April 2009
DETERMINATION OF BOILING POINTS & MELTING POINTS
OF ORGANIC COMPOUNDS
--------------------------------------------------------------------------------------------------------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
-----------------------------------------------------------------------------------------------------------------
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
Instructor’s Table:
• Vacuum Filtration pump fitted with 250mL filter flask and tygon tubing
• Ice bucket containing ice
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
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
Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 7
April 2009
Refer Attached Scheme
Add ∼ 2 g of Add 50 ml of
anhydrous Na2SO4 (2M) HCl, check acidity
and shake (5 minutes) using litmus + stirring
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
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
Preparation of Soap
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
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 :
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)
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.
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
Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 13
April 2009
2- Chemical properties
Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 14
April 2009
• 1 Spatula
• 10-12 TT
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
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
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
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
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
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
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
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)
▲▲ 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. ▲▲
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
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
1- Physical Properties
Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 21
April 2009
2- Chemical Properties:
NH3 smell
Red litmus blue
White fumes or clouds of NH4Cl with conc HCl
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.
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.
Prepared by Ms. Carmen DSouza & Schemes done by Mrs. Mariam Al-Asousi 24
April 2009