Lab #1

Topic: Alkanes and Alkenes

Aim: To distinguish between alkane and alkenes

Apparatus and Materials: Beakers, test tubes, test tube racks, pipette droppers, water bath,
KMnO4 (aq), Bromine water(aq), unknown substances A and B (either cyclohexane or
cyclohexene).

Test Observations Inferences

A + KMnO4 (aq)

B+ KMnO4 (aq)

A + Br2 (aq)

B + Br2 (aq)

Note:

 Describe the colour of each solutions before each test is done in the observations
 Mixture may need to be heated in a water bath
 Reactions and mechanism required in inferences
 Explanations for no reaction required in inferences also
 If immiscible mixture results, explanations are required and tell why one liquid
floats on the other interms of density

Lab #2

Topic: Carbonyl Compounds

Aim: To distinguish between aldehydes and ketones

Apparatus and Materials: Beakers, test tubes, test tube racks, pipette droppers, water bath,
Fehling’s solution (or Benedict’s solution), KMnO4(aq), K2Cr2O7(aq), Tollen’s reagent,
Brady’s reagent, unknown substances A and B (propanal or propanone)

Test Observations Inferences

A + Fehlings
Reagent
B + Fehlings
Reagent
A + KMnO4

B + KMnO4

A + K2Cr2O7

B + K2Cr2O7

A + Tollens
Reagent
B + Tollens
Reagent
A + Bradys
Reagent
B + Bradys
Reagent

Lab: 3

Topic: Iodoform Test

Aim: To determine which compound will give a positive iodoform test.

Apparatus and Materials:

Methanol, ethanol, sodium hydroxide solution, iodine solution, test tubes, test tube holders,
distilled water, pipette, dropper.

Procedure

1. Add 1 ml of methanol to a labelled test tube using a pipette.

2. Add 2.5 ml of iodine solution to the test tube followed by 1 ml of sodium hydroxide.

3. Gently swirl the test tube until the dark colour of the iodine fades.
 4. Allow the mixture to settle and observe any changes after 2 minutes.

5. Repeat steps 1-4 using ethanol and water.

Observation and Results

Title:

Test Observations Inferences

Methanol

Ethanol

Propanone

Water

Discussion

Include an explanation for the positive test and the negative test.

Include overall reaction mechanism with state symbols and intermediate products.

Lab: 4

Topic : Qualitative Analysis – Ethanol and Phenol

Aim: To determine which two unknown samples X and Y are ethanol and phenol

Apparatus and Materials:

Ethanol, phenol, iron (III) chloride, bromine water, water

Procedure

Test Observation Inference

3
To 2 cm of sample X, add
few drops of neutral iron
(III) chloride

Add a few drops of neutral

iron (III) chloride to 2 cm3
of sample Y
 Add a few drops of
bromine water to 2 cm3 of
sample X
Add a few drops of
bromine water to 2 cm3 of
sample Y

Add 2 cm3 of water to 2 cm3

sample X

Add 2 cm3 of water to 2

cm3 of sample Y

Add a few drops of conc

sulphuric acid to 2 cm3 of
sample X and heat
Add a few drops of conc
sulphuric acid to 2 cm3 of
sample Y and heat
NB: Include reaction equations in inferences where possible.

Conclusion:

Lab: 5

Title: Saponification

Aim: To prepare a sample of soap using vegetable oil

Apparatus: vegetable oil, measuring cylinder, beaker, tap and distilled water, 20cm 3 of 4M NaOH.

Procedure:

1. Pour approximately 10ml of vegetable oil in a clean beaker using a measuring cylinder.

2. Add 20ml of the NaOH to the oil and boil for 25 minutes.

3. Add a sample of brine solution to the mixture and stir

4. Obtain a sample of the solid and add to both tap water and distilled water. Record
observations.

OBSERVATIONS:

 Describe what is observed at the beginning, during and at the end of the lab
  Describe observations when soap is added to tap water and distilled water

DISCUSSION:

 Define the term saponification

 State what are esters and how to identify the esters from their structures

 Explain alkaline hydrolysis of esters and write the equation for this hydrolysis (structural
equation for the formation of soap)

 Explain why the soap form lather with distilled water and as much with tap water

 Explain why the brine solution was added

Lab: 6

Topic: Alkanoic Acids

Aim: To investigate reactions of alkanoic acids

Apparatus and Materials:

Test tubes, test tube holders, pipette dropper, ethanoic acid, magnesium ribbons, sodium
carbonate, sodium hydroxide, thionyl chloride, ethanol, concentrated sulphuric acid, water
bath, acidified potassium permanganate, filter paper strips, lime water, lighted splints.

Test Observations Inferences

CH3COOH(aq) +
NaOH(aq)

CH3COOH(aq)+ Mg(s)
Test gas with splint
 CH3COOH(aq)
+Na2CO3(s)
Test gas with limewater
CH3COOH(aq)+SOCl2(l)
Test gas with KMnO4
CH3COOH(aq)
+C2H5OH(aq) + conc H2SO4
in hot water bath

Lab: 7

Topic: Monomers & Polymers

Aim: To differentiate between starch and glucose

Apparatus and Materials:

Beakers, test tubes, test tube holders, pipette dropper, distilled water iodine solution,
Benedicts solution, water bath unknown substances A and B (either starch or glucose).

Test Observations Inferences

A + H2O(l)

B + H2O(l)

A + Benedicts Solution + Heat

B + Benedicts Solution + Heat

A + Iodine solution

B + Iodine solution
Lab: 8

Topic: Uncertainties in Measurement

Aim: To calibrate a pipette

Apparatus and Materials:

10cm3 pipette, pipette filler, beaker or crucible, electronic balance, thermometer, distilled
water, paper towels

Procedure:

1. Collect distilled water in a beaker and let it stand for about 15 minutes before determining the
temperature of the water.
2. Weigh the dry empty beaker on the balance.
3. Using the pipette filler, fill and discharge the pipette into the pre-weighed beaker.
4. Determine the mass of water discharged.
5. Repeat steps 3 – 4 until you have results for 7 trials. N.B. You do not need to empty and dry
the beaker between trials.
6. Determine the temperature of the water you have pipetted and take the mean of the two
temperatures you have measured. This value will be used as the temperature of the water
during the calibration.
Calculations

1. Calculate the mean mass of water discharged of the seven trials.

2. Use the following table to determine the density of water at the temperature of your
determination by drawing a calibration curve:
X T/oC 26 28 30 32 34 36

Y Density /gcm-3 0.99678 0.99623 0.99565 0.99503 0.99438 0.99369

3. Using your answer from question 2 determine the mean volume of water discharged from the
pipette.
 4. Calculate the standard deviation of the seven masses from question 1 and convert to volume
as well.
5. State the capacity of the pipette in the format mean volume ± standard deviation
6. State the capacity of the pipette as shown on the pipette you have used.
7. Using the mean volume you have calculated and true mean value stated on the pipette,
calculate the % error via the formula below:
% error = difference between calculated mean value and true mean value x 100
true mean value

8. Discuss any sources of error in your experiment.

Lab: 9

Topic: Phase Separation

Aim: To determine the partition coefficient of citric acid (H3C6H5O7) between water
and diethyl ether (CH3CH2OCH2CH3).

Apparatus and Materials: citric acid about 2.0 g, diethyl ether, 0.50 M potassium hydroxide,
0.10 M potassium hydroxide, phenolphthalein indicator, 100 cm 3 separating funnel, 50 cm 3
measuring cylinder, 100 cm 3 beaker, 100 cm3 conical flask,

Procedure:

A. Setting up of Equilibrium

1. Measure 40.0 cm 3 of distilled water or deionized water using a 50 cm 3 measuring

cylinder. Pour it into a 100 cm 3 beaker.

2. Weigh about 2.0 g of citric acid and record the mass weighed.

3. Pour the weighed citric acid into the beaker containing 40.0 cm 3 of distilled water.

4. Stir the mixture using a clean and dry glass rod until all citric acid dissolves.

5. Pour the mixture into a clean and dry 100 cm 3 separating funnel.
 6. Measure 50.0 cm3 of diethyl ether using a 50 cm 3 measuring cylinder. Pour it into the
separating funnel.

7. Stopper the funnel and shake vigorously for 2 minutes. Open the tap occasionally to
release the pressure in the funnel. (Caution: Diethyl ether is very volatile and
flammable. Make sure that there is no flame nearby and do not point the tip of the
funnel towards anyone.)

8. Place the separating funnel in the ring. Leave it to stand for several minutes until its
contents separate into 2 clear and steady layers.

9. Measure and record the room temperature using a thermometer.

B. Titration of the aqueous layer

1. Pour 0.50 M potassium hydroxide solution into the burette through a filter funnel.

2. Open the cork of the separating funnel and then the stopcock. Run off the aqueous
layer (lower layer) from the tip into a clean and dry 100 cm 3 beaker. Discard the
fraction just below and above the boundary of the two layers into another beaker.

3. Pipette 10 cm3 of the aqueous layer into a 100 cm3 conical flask.

4. Add 2 drops of phenolphthalein indicator into the conical flask.

5. Record the initial burette reading in Table 1.

6. Titrate the aqueous solution in the conical flask with 0.50 M potassium hydroxide
solution in the burette.

7. Record the final burette reading in Table 1.

8. Repeat steps 3-7 to obtain 2 sets of consistent results.

C. Titration of the Ethereal Layer

1. Pour 0.10 M potassium hydroxide solution into the burette through a filter funnel.

2. Run off the remaining layer (ethereal layer) in the separating funnel into a clean and
100 cm 3 dry beaker.

3. Pipette 10 cm 3 of the ethereal layer into a 100 cm 3 conical flask.

4. Add about 10 cm 3 of distilled water or deionized water into the conical flask.
5. Add 2 drops of phenolphthalein indicator into the conical flask.
6. Record the initial burette reading in Table 2.

7. Titrate the aqueous solution with 0.10 M potassium hydroxide solution.

8. Record the final burette reading in Table 2.

9. Repeat steps 3-8 to obtain 2 sets of consistent results.

3 KOH (aq)  +  H3C6H5O7 (aq)  -->  k2C6H5O7 (aq)  +  3 H2O

Mass of weighing bottle and citric acid:

Mass of weighing bottle:

Mass of anhydrous citric acid used:

 Table 1 (Diether Layer)

Titration 1 (trial) 2 3

Final burette reading (cm3)

Initial burette reading (cm3)

Volume of KOH used (cm3)

Average of potassium hydroxide used =

Table 2 (Aqueous Layer)

Titration 1 (trial) 2 3

Final burette reading (cm3)

Initial burette reading (cm3)

Volume of KOH used (cm3)

Average of potassium hydroxide used =

Discussion

1. Calculate the concentration of citric acid in the diethyl layer in mol dm-3.
2. Calculate the concentration of citric acid in the aqueous layer in mol dm-3.

3. Determine the partition coefficient of citric acid between diethyl ether and water.
Lab: 10

Topic: Paper Chromatography

Aim: To separate the components in a mixture of food colouring dyes.

Apparatus and Materials: Ethanol, distilled water, food dye, pencil, ruler, filter papers,
beakers, watch glass, capillary tube or toothpick.

Procedure:

1. Using a clean ruler and a pencil mark a horizontal line approximately 1.5 cm from the tapered
end of the strip of chromatography paper placed on a clean surface. This line will be the
origin in the developed chromatogram. Mark a small stroke in the centre of the line to
represent the position the spot should be placed.
2. Use the marked strip to estimate the height to which the developing solvent should be poured
into the measuring cylinder. N.B: The solvent should be in contact with the paper but below
the level of the origin at the start of the separation.
3. Remove the strip of paper and pour the solvent (either water or an ethanol/water mixture into
the measuring cylinder (Chromatography tank), stopper the container and leave to stand for a
few minutes.
4. Place the strip of chromatography paper on a clean surface and spot on the mixture to be
separated as follows:
5. Use the toothpick and make a dot roughly 1 mm across on the origin. Repeat this 4 more
times to ensure the spot of mixture is concentrated.
6. Holding the strip by the edge furthest from the origin, place it into the tank so that the tip is
submerged.
7. Replace the cover and leave to stand.
8. Remove the developed chromatogram when the solvent has reached about ¾ to the top of the
paper.
9. Use a pencil to mark the furthest position (solvent front) to which the solvent has moved.
10. Calculate the Rf value for each component in the ink.
11. Paste the chromatogram in your lab book

QUESTIONS

1. a) From your results suggest the number of components that may be present in the dye
b) Using the chromatogram, determine the Rf values of each component.

2. What is the principle on which the separation was based?

3. Why would different Rf values be obtained with the different solvents?

4. What further procedure may be used to obtain a better separation of the components?
Lab: 11

Topic: Gravimetric Analysis

Aim: To determine the value of n and hence the formula of the hydrated salt
CuSO4.nH2O using gravimetric analysis.

Apparatus and Materials:

Hydrated salt CuSO4.nH2O, electronic balance, silica crucible, spatula, crucible tongs, Bunsen burner,
tripod stand, wire gauze, stop clock

Procedure

1. Weigh a clean dry crucible after heating for about three minutes. Record the mass in the table.

2. Half fill the crucible with small crystals of hydrated copper (II) sulphate. Weigh the crucible
and hydrated salt. Record the mass in the table.

3. Place the crucible on the tripod and apply heat gently using the Bunsen flame.

4. Heat more strongly for about 15 minutes but never allow the crucible to become red hot.

5. Remove the flame and use the thongs to remove the crucible from the tripod stand.

6. Allow the crucible to cool to room temperature and record the mass.

7. Repeat the heating for 5 minute intervals until the mass is constant. Record this as the final
mass in table.

8. Record the appearance of the salt after heating.

9. Repeat the procedure two more time.

Results

Title:

Mass Readings

Mass of empty crucible

Mass of crucible and hydrated salt

Mass of hydrated salt

Mass of crucible and salt after heating

Mass of salt after heating

Mass of water of crystallization driven

off during heating

Treatment of Results

Calculate

1. The mass of anhydrous CuSO4

2. The mass of water removed

3. Number of moles of water

4. Number of moles of anhydrous salt

5. The value of n.
Lab: 12

Topic: Redox Titration

Aim: To standardize iron (ii) sulphate using manganate (vii) solution.

Apparatus: Filter funnel, Burette, 25 ml pipette, white paper towel, retort stand, conical
flask, beakers, distilled water, 0.2M potassium permanganate (VII) solution
and iron (II) sulphate solution.

Procedure: 1) CLAMP THE BURETTE ONTO THE RETORT STAND ENSURING IT IS

VERTICAL.

2) PLACE A FUNNEL INTO THE BURETTE THEN ZERO IT WITH MnO -4(aq).
ENSURE THAT NO AIR BUBBLES ARE PRESENT.

3) USE A PIPETTE TO MEASURE 25CM3 OF Fe2+(aq) AND TRANSFER TO A

CONICAL FLASK.

4) PLACE A WHITE PAPER TOWEL AT THE BASE OF THE RETORT STAND AND
PLACE UNDER THE BURETTE.

6) TITRATE MANGANATE (VII) SOLUTION AGAINST THE IRON (II) UNTIL ONE
DROP CAUSES A PERSISTENT PALE-PINK COLOUR.

7) REPEAT STEPS (2) TO (6) THREE TIMES

RESULTS: TABLE SHOWING TITRE VALUES OF VOL OF MnO -4(aq) USED

REACTION Rough Run 1 Run2 Run 3

Final Volume / cm3

Initial Volume / cm3

Volume Used / cm3

SUMMARY: _______ of Fe2+(aq) required _______ of MnO-4 (aq) for complete neutralization.

CALCULATIONS:1) Calculate the # of moles in the volume of MnO -4 (aq) used.

 2) Write a balanced ionic equation for the reaction and hence state the mole
ratio between the MnO-4 (aq) and the Fe2+(aq)

3) Calculate the concentration of the Fe 2+(aq) used.

4) Calculate the concentration in question above in g/dm 3.

CAPE UNIT 2 P&Ds

1. Your father has just done a triple bypass surgery after his recent heart attack. Your
mother wants to find the best type of oil to use in the preparation of his food. She goes to
 the supermarket and sees coconut oil, vegetable oil and corn oil. Plan and design an
experiment to find out which oil would be best to use.

2. The pharmacist at your local drugstore insists on the effectiveness of [Brand A] antacid
over [Brand B] antacid. Plan and design an experiment to establish the truth of the
pharmacist’s claim.
Note: Insert the actual name of the 2 brands antacid that you choose to use

3. Julia suffers from menorrhagia and her doctor recommends she take Iron (II)
supplements. Her mother suggested she takes [Supplement A] whilst her friend suggests
she takes [Supplement B]. Plan and design an experiment to help Julia make an informed
decision.
Note: Insert the actual name of the 2 supplements that you choose to use

4. Christian was a finalist at his first attempt at the JABBFA bodybuilding competition at his
first attempt. He struggles to afford the protein necessary to compete with the other
athletes and his trainer suggested he add lots of peanuts to his diet, however he comes
from a hypertensive family. Plan and design an experiment to help Christian make an
informed decision
Note: Insert the actual name of the 2 brands salted Peanuts that you choose to use

5. Sandra’s electricity bill has skyrocketed and her electrician suggested she could save
money by turning up the temperature inside the refrigerator of which she is skeptic.
Sandra believe the nutrient content of her orange juices (Vitamin C) may be affected if
she follows his advice. Plan and design and experiment to help Sandra make an informed
decision.

DO ANY THREE PDS LABS 13 – 15

INVESTIGATIVE PROJECT

Objectives of the Investigative Project

The Investigative Project must focus on a challenge to be addressed within the environment or

society.

On completion of the Investigative Project students should:

1. Appreciate the use of the scientific method for discovery of new knowledge and to the solution of

problems;

2. Communicate accurately and effectively the purpose and results of research;

3. Apply experimental skills and theory to the solution of problems; and,

4. Synthesise information based on data collected.

Students are encouraged to work collaboratively. Where collaborative work is done, group sizes
must not exceed six (6) persons per group. The teacher is expected to use the group mark for the
project and add it to the marks for the other skills for each individual candidate within the group.

CRITERIA FOR ASSESSING INVESTIGATIVE SKILLS

Lab: 16

Topic: Mass Spectroscopy

Aim: To analyze and interpret a spectrum by mass spectroscopy.

Apparatus: MASS SPECTROMETER, DODECANE,

Method: 1) THE LIQUID SAMPLE WAS INJECTED UNTO THE COLUMN

PRESET AT 175oC

2) THE SPRECTRUM WAS PRINTED & ANALYSED

DATA ANALYS: DRAW FRAGMENTS CORRESPONDING TO ANY 5 PEAKS

DRAW THE FRAGMENT & GIVE THE M/Z RATIO FOR THE
FRAGMENT CORRSEPONDING TO THE BASE PEAK

DRAW FRAGMENT FOR THE PARENT ION & GIVE THE M/Z
RATIO

SKILL ASSESSED A/I (PRINT & PASTE THE SPECTRUM IN YOUR LAB BOOK)

Lab: 17

Topic: Infrared Spectroscopy

Aim: To analyze & interpret an unknown compound by IR spectroscopy.

Apparatus: NICOLET FTIR SPECTROPHOTOMETER, UNKNOWN SAMPLE, NUJOL
MOL, MORTAR & PESTLE, CHEM-WIPE, NaCl PLATES

Procedures: For Liquid Samples

For Solid Samples

RESULTS: FIGURE 1
FIGURE 2
 FIGURE 3

DATA ANALYSIS:

Figures 1,2 and 3 belongs to the compounds 2-propanol, butanoic acid and acetone (2-propanone).
Identify EACH of the compounds from the IR spectra provided. Justify your choice by indicating
which band(s) on the spectra was used to verify the identity of the compounds and indicate the
functional group responsible for the band in EACH case.

SKILL ASSESSED A/I (PRINT AND PASTE THE SPECTRUM IN YOUR LAB BOOK)
Lab: 18

Topic: Spectrophotometric Determination of iron Tablets

In this experiment, iron from a tablet is dissolved in acid, converted to Fe 2+ with hydroquinone, and
complexed with o- phenanthrolineto form an intensely red coloured complex.
Reagents

Hydroquinone: Freshly prepared solution containing 10g/L. Store in an amber or dark coloured
bottle to prevent decomposition by light.

Trissodium citrate: 25g/L

O – phenathroline: Dissolved 2.5g in 100 mL of ethanol and add 900mL of water. Store in an amber
bottle.

Standard iron (II) solution (0.04 mg Fe/L) Prepared by dissolving 0.2810g of reagent grade
Fe(NH4)2(SO4)2.6H2O in water in a 1 L volumetric flask containing 1 mL of 98% wt%H 2SO4.

Procedure

1. Place one of the iron – containing tablets in a 125mL flask or 100mL beaker and boil gently
( in a fume hood) with 25mL of 6M HCl for 15 minutes. Filter the solution directly into a
100mL volumetric flask. Wash the beaker and filter several times with small portions of
water to complete a quantitative transfer. Allow the solution to cool, dilute to the mark, mix
well. Dilute 5.00 mL of this solution to 100.0 mL in a fresh volumetric flask. If the tablet
contains < 15 mg of Fe, use 10.00mL instead of 5.00mL
2. Pipette 10.00mL of standard Fe solution into beaker and measure the pH (with pH paper or a
glass electrode). Add sodium citrate solution 1 drop at a time until a pH of 3.5 is reached.
Count the drops needed ( it will require about 30 drops)
3. Pipette a fresh 10.00 mL aliquot of Fe standard into 100mL volumetric and add the same
number of drops of citrate solution as required in Step 2. Add 2.00 mL hydroquinone
solution and 3.00mL of o – phenanathroline solution, dilute to the mark with water, and mix
well.
4. Prepare three more solution from 5.00, 2.00 and 1.00 mL of Fe standard and prepare a blank
containing no Fe. Use sodium citrate solution in proportion to the volume of Fe solution. (if
10 mL of Fe requires 30 drops of citrate solution, 5mL of Fe requires 15 drops of citrate
solution).
 5. Find out how many drops of citrate solution are needed to bring 10.00mL of iron tablet
solution from Step 1 to pH 3.5. This will require about 3.5 or 7mL of citrate, depending on
whether 5 to 10 mL of unknown was diluted in the second part of Step 1.
6. Transfer 10.00mL of solution from Step 1 to a 100mL volumetric flask. Add the required
amount of citrate solution determined in Step 5, then add 2.00mL of hydroquinone solution
and 3.0mL of o-phenanthroline solution; dilute to the mark and mix well.
7. Allow the solution to stand for at least 10 minutes. Then measure the absorbance of each at
508nm. ( The colour is stable, so all solution may be prepared and all the absorbance
readings measured at once). Use distilled water in the reference cuvette and subtract the
absorbance of the blank from the absorbance of the standards.
8. Plot a graph of absorbance versus micrograms of Fe in the standards. Determine the slope
and intercept ( and standard deviations) by the method of least squares.

Calculations

i. The molarity of the Fe ( o- phenanathroline) 32+ in each solution

ii. The average molar absorptivity ( in Beer’s Law) from the four absorbance readings
taken. Remember that all the iron has been converted of the phenanathroline
complex.
iii. Using the calibration curve ( or its least squares parameters), calculate the number of
milligrams of Fe the tablet.

Table for calibration Curve:

(Fe)/ppm Absorbance reading