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PRINCES 

TOWN WEST SECONDARY
CAPE UNIT 2
CHEMISTRY LABS
2011 - 2012

 Princes Town West Secondary Unit 2 Chemistry Labs 1|Page


# Title Skills

Lab # 1 Organic Compounds : To determine which organic compound is contained in the


 bottles labelled A, B, C and D
Lab # 2 Organic Compounds: To determine which organic compound is contained in the
 bottles labelled P, Q, R and S.
Lab # 3 Plan and Design : Organic Chemistry
Lab # 4 Organic Chemistry: To investigate the relative acidities of alcohols, phen ols and
carboxylic acids
Lab # 5 Analytical Chemistry : The degree of uncertainty
Lab # 6 Crystallization
Lab # 7 Analytical Chemistry : Gravimetric
Gravimetric Analysis - percentage oxalate inin an unknown
sample
Lab # 8 Analytical Chemistry : Gravimetric
Gravimetric Analysis - Vitamin
Vitamin C Tablet
Lab# 9 Analytical Chemistry : Spectroscopy : UV/Vis
Lab# 10 Analytical Chemistry : Quantitative Titration
Lab# 11 Chromatography : Paper Chromatography Pigment in leaves
Lab# 12 Chromatography : Paper Chromatography Inks
Lab# 13 Solvent Extraction
Lab # 14 Plan Design: Environmental Chemistry
Lab # 15 Simple and Fractional Distillation
Lab # 16 Environmental Chemistry : Organic Compounds
Lab # 17 Plan Design: To determine the acidity / pH of a soil sample
Lab # 18 Analytical Chemistry Back Titration
Lab # 19 Environmental test for pollutants in water.
Lab # 20 Plan and Design : Analytical Chemistry (Gravimetric)

 Princes Town West Secondary Unit 2 Chemistry Labs 2|Page


Lab # 1 Skills O/R/
Assessed: R 
Date: M/M

A/I

P/D

Title : Organic Compounds

Aim : To determine which organic compound is contained in the bottles labelled A,


B, C and D.

1. Test Tu
Tubes 6 . 2,4 -
2. Boil
Boiliing Tube
Tubess dinitrophenyihydrazine
3. 250 ml Beaker
Beaker(La
(Label
belled
led Organi
Organicc 7. Aqueo
Aqueousus Silv
Silver
er Nitr
Nitrat
atee
Apparatus
Waste) 8. Aque
Aqueououss Sodi
Sodium
um
and :
4. Magn
Magnes esiu
ium
m Powde
Powderr or Turn
Turnin
ings
gs Hydroxide
Material
5. Sodi
Sodium
um Carb
Carbon
onat
atee 9. Aque
Aqueououss Ammo
Ammoni niaa
10. Acidified
Acidified Potassiu
Potassiumm
Dichromate

Aqueous solutions, A, B, C and D. Each solution contains one of the


following.

I. an alcohol
II.
II. an alde
aldehy
hyde
de
III. a carboxyli
carboxylicc acid
IV. a ketone
ketone

Procedure 1. You are to perform


perform the tests
tests below and
and from the results
results establish
establish
which type of organic compound is contained in each of A, B, C and
D.
: 2. After
After each test
test discard
discard the
the contents
contents of the the 250 cm3
the tubes into the
 beaker, labelled organic waste. Rinse and re-use the tubes for the
remaining tests.
3. Tests
Tests for
for gases
gases are
are at the
the end ofof this
this lab sheet
sheet..

 Princes Town West Secondary Unit 2 Chemistry Labs 3|Page


Place 1 cm depth of each of the solutions A, B, C and D into separate test-tubes.
Test (a) To each tube add a small quantity of magnesium powder or turnings.
Identify any gas given off and record the test you used to make the identification.

Place 1 cm depth of each of the solutions A, B, C and D into separate test-tubes.


Test (b) To each tube add a small quantity of powdered sodium carbonate.
Identify any gas given off and record the test you used to make the identification.

Place 1 cm depth of each of the solutions A, B, C and D into separate test-tubes.


Test (c)
To each tube add 1 cm depth of 2,4-dinitrophenylhydrazine reagent.

: Place 1 cm depth of each of the solutions A, B, C and D into separate test-tubes.


Place 2 cm depth of aqueous silver nitrate in a boiling-tube and add to it 1 cm
depth of aqueous sodium hydroxide. This will produce a precipitate of silver
oxide.
Test (d)
Use a dropping pipette to add dilute aqueous ammonia to this mixture until the
 precipit
 precipitate
ate of silve
silverr oxide
oxide just
 jus t dissolves.
Do not add an excess of aqueous ammonia.
To each of the tubes containing A, B, C and D add 1 cm depth of the silver-
containing solution you have just prepared.

Place 1 cm depth of each of the solutions A, B, C and D into separate boiling-tubes.


Test (e) To each tube add a few drops of acidified potassium dichromate(V1) to give a
yellow-orange solution. Warm the tube gently.

Observati : Aqueous B C
A D
ons and Solutions
Results (Ketone (Alde
(Alcohol) (Carboxylic Acid)
) hyde)

 No Pop with glowing splint ∴ H2 gas


Test (a) No Rxn No Rxn given off. Hence Compound D is
Rxn
the acid.
effervescence and gas bubbled
 No through Ca(OH)2 White ppt
Test (b) No Rxn No Rxn formed.
Rxn
Gas given off CO2. D is the
carboxylic Acid.
Test (c) No Visible Yellow Yello  No Visible Rxn
Rxn  brown/ w
(orange)  brown  No ppt formed
 No ppt  ppt /
formed formed (orang
∴ e) ppt

 Princes Town West Secondary Unit 2 Chemistry Labs 4|Page


forme
d∴
Aldehyd
Aldeh
e or
yde or
Ketone
Keton
e

Silver
 ppt
forme
d on
ring
of test
 No tube ∴
 No Visible
Visible silver
Rxn  No Visible Rxn
Test (d) Rxn mirror
 No ppt effect  No ppt formed
 No ppt
formed hence
formed
comp
ound
C is
the
Aldeh
yde

Green
soluti
on
forme
Green
d
solution
 No indica
formed
Visible ting  No Visible Rxn
indicating
Test (e) Rxn Cr 3+
Cr 3+ ions
ions
hence an
hence
alcohol or
an
aldehyde
alcoh
ol or
aldeh
yde

Discussion : • Test (a)


○ Compound D is the acid as H2 gas was given off and identified

 Princes Town West Secondary Unit 2 Chemistry Labs 5|Page


 by the pop with the glowing splint.
○ 2R-COOH(aq)+2Mg(s)yields 2R-COO-Mg+(aq)+ H2(g)

• Test (b)
○ Effervescence CO2 given off as confirmation with white ppt
forming in CaA(OH)2
○ 2R-COOH(aq)+Na2CO3(s)yields 2R-COO-Na+(aq)+
CO2g+H2O(l)
○ CO2g+Ca(OH)2 yields CaCO3(s)+H2O(l)
○ ∴ Substance D is the acid as no other reactions
were observed by the other substances.

• Test (c)
○ Yellow brown (or orange) ppt seen for B and C indication it’s a
carbonyl compound.
○ ∴ Substance B and C are either a ketone or
aldehyde
○ RCHO+ C6H3NO22.NHNH2yields RCH=NNC6H3NO22
s+H2Ol
○ RR'CO+ C6H3NO22.NHNH2yields R'RC=NNC6H3NO22
s+H2Ol

• Test (d)
○ 2Ag(NH3)2 (aq)++ RCHO(l)+3OH(aq)- yields 2Ag(s)+
RCOO(aq)-+ 4NH3 g+ 2H2Ol
○ Tollen’s reagent only reacts with aldehydes to give the silver
mirror effect ∴ substance C is the aldehyde.

• Test (e)
○ Substance A is an Alcohol because it reduces aqueous K 2Cr 2O7
to a green Cr 3+ but did not react with either Tollen’s reagent or
2,4,-dinitrophenylhydrazine reagents.
○ Substance B ∴ has to be the ketone by reason of
elimination and its reaction with 2,4 ,-
dinitrophenylhydrazine.

Conclusio
:
n

 Princes Town West Secondary Unit 2 Chemistry Labs 6|Page


 gas test and test result 

ammonia, NH3 turns damp red litmus paper blue


gives a white ppt. with limewater 
carbon dioxide, CO 2
(ppt. dissolves with excess CO 2)
chlorine, 012 bleaches damp litmus paper  

hydrogen, H2 'pops' with a lighted splint

oxygen, 02 relights a glowing splint


turns potassium dichromate(VI) (aq) from orange to
sulphur dioxide, 80 2
green

 Princes Town West Secondary Unit 2 Chemistry Labs 7|Page


Conclusion :

 Princes Town West Secondary Unit 2 Chemistry Labs 10 | P a g e


Lab # 3 Skills O/R/
Assessed: R 
Date: M/M

A/I

P/D 

Title : Plan and Design : Organic Chemistry

Aim :

Case You are provided with solutions VF  3, VF 4 and VF 5.

The solutions are:

1.0 mol dm –3 Propanone

1.0 mol dm –3 Propanal

0.5 mol dm –3 Propanoic Acid

You are to plan experiments that will enable you to identify the
solution that matches each of

: VF 3, VF 4 and VF 5.

You have available the following apparatus:

 –10 °C to 110 °C thermometer,

100 cm3 beaker, measuring cylinder, and the following reagents

LiAlH4, EDTA, Fehlings Reagent, 2,4 DNPH, and one of your choice.

(a) You are to identify, by the minimum number of practical


steps, which of the solutions contains Propanone

 Princes Town West Secondary Unit 2 Chemistry Labs 11 | P a g e


Apparatus 1. 2.
and :
Material

Procedure : 1.

2.

3.

4.

5.

6.

Observatio
ns and :
Results

Data
Analysis and
:
Interpretati
on

Discussion : •

Conclusion :

Lab # 4 Skills O/R/


Assessed: R 
Date: M/M

A/I 

 Princes Town West Secondary Unit 2 Chemistry Labs 12 | P a g e


Lab # 5 Skills O/R/ 
Assessed: R 
Date: M/M

A/I

P/D

Title : Analytical Chemistry : The degree of uncertainty

Aim : To determine the degree of uncertainty between a measuring cylinder and a


 burette.

Apparatus 1. 50 cm3 burette (Class A)


and : 2. 10 cm3 measuring cylinder (Class A)
Material 3. Distilled water 

Procedure : 1. The burette was filled to a known volume and record the volume

2. 25 drops of water was delivered drop wise into a measuring cylinder


and record both the measuring cylinder and new burette reading

3. This process was repeated in steps of 25 drops until 200 drops were
delivered.

4. The results were tabulated.

5. A graph was drawn vol of burette against vol in cylinder 

6. A best fit line was drawn

7. Calculate the Standard Deviation between volumes in the burette and


the measuring cylinder.

Observatio : Table: 1 Readings obtained from the burette and measuring cylinder respectively.

ns and  No. of Drops 25 50 75 100 125 150 200


Results
Final Burette Reading / cm 3

Initial Burette Reading / cm 3

Total Vol of drops Burette / cm3

Vol in measuring cylinder / cm 3

 Princes Town West Secondary Unit 2 Chemistry Labs 20 | P a g e


S.D. between Readings

Graph Draw a graph of volume of burette versus volume of measuring cylinder 

Data 1. From the graph determine when 4 cm3 of the burette is delivered the
:
Analysis volume of measuring cylinder?

2. From the graph when 8.2 cm3 of water is delivered from the burette
the reading in the measuring cylinder ?

3. Which instrument is considered to be accurate

4. Which instrument is considered to be precise

5. Explain your answer for questions 3 and 4.

Discussion : •

Conclusion :

Lab # NA Skills O/R/R 


Assessed:
Date: M/M 

A/I

P/D

 Princes Town West Secondary Unit 2 Chemistry Labs 21 | P a g e


Title : Analytical Chemistry : Measurements

Aim : Uncertainty of measurements of volumes and masses

1. Burette, 50 mL, Class B 7. Top loading balance


2. Graduated pipette, 10 mL, Class B 8. Analytical balance
Apparatu 3. Volumetric flasks, 25 mL, Class A 9. Unknown liquid, 200 mL.
s and : and B (0.789 g ml-1)
Material 4. Measuring cylinder, 10 mL 10. Distilled water 
5. 15 Vials and stoppers 11. Pipette filler 
6. Tissue

Procedur
:
e

Part A 1. All glassware was rinsed with distilled water, and then 2 mL of
unknown liquid provided.

2. The empty vials and the volumetric flasks were labelled

3. The mass of the empty dried sample vials with their stoppers in place
were weighed. Precaution was taken no to interchange stoppers among
vials.

4. The burette, graduated pipette, and measuring cylinder were used to


transfer 10 mL of the unknown liquid into different vials.

5. The vials were stoppered and their loaded weights were recorded.

6. This was repeated until a total of three (3) loaded sample vials for each
 piece of measuring equipment.

7. Results were recorded in Table 1.

Part B 1. Each volumetric flask was filled to the 25 mL mark with the unknown
liquid ensuring that no liquid is spilled on the outside.

2. The volumetric flasks were stoppered and there loaded weights were
recorded.

3. The unknown liquid in the flasks were completely transferred into a

 Princes Town West Secondary Unit 2 Chemistry Labs 22 | P a g e


Table 1 Mass of hydrated magnesium sulphate

Mass of test tube and hydrated magnesium


sulphate / g
Mass of empty test tube /g

Mass of hydrated magnesium sulphate /g

Table 2 Mass of hydrated magnesium sulphate after


Observation heating
Mass of test tube and hydrated magnesium
s and :
sulphate after heating / g
Results

Mass of empty test tube /g

Mass of hydrated magnesium sulphate


after heating /g

Data : 1. Number of moles of anhydrous MgSO4 in the sample


Analysis
2. Determine the mass of water driven out of the sample
and
Interpretati 3. Number of moles of water driven out from the sample
on
4. Number of moles of water of crystallization in one mole of hydrated
MgSO4

= number of moles of water driven out from the samplenumber of


moles of anhydrous magnesium sulphate in the sample

5. Write an equation for the formation of anhydrous MgSO4 from


hydrated magnesium sulphate.

Discussion : •

 Princes Town West Secondary Unit 2 Chemistry Labs 30 | P a g e


Conclusion :

 Princes Town West Secondary Unit 2 Chemistry Labs 31 | P a g e


Lab # 7 Skills O/R/
Assessed: R 
Date: M/M

A/I 

P/D

Title : Analytical Chemistry : Gravimetric Analysis

Aim : Standardisation of a permanganate solution and determination of the


 percentage oxalate in an unknown sample

1. 4 – 250 mL conical flask  11. 2 spatulas


2. Burette and funnel 12. Analytical balance
3. Retort stand and clamp 13. K 2C2O4.H2O salt
4. 1 white tile 14. 3.0 M H2SO4
Apparatus
5. 2 sample vials with stoppers 15. ≈0.02 M KMnO4 solution
and :
6. Bunsen burner/ tripod / wire gauze 16. Distilled water 
Material
7. Thermometer  17. Unknown oxalate sample
8. 25 mL measuring cylinder  18. 250 mL volumetric flask 
9. 10 mL measuring cylinder  19. Laboratory cloth
10. 25 mL Pipette and pipette filler 

Procedure 1. ~1.5 grams of K 2C2O4.H2O salt (Potassium oxalate) was accurately


: weighed and dissolved properly into a 250 ml volumetric flask and
then made up to the mark.

2. 25 ml of K 2C2O4 standard was pipette into a conical flask and 15 mL


of 3.0 M H2SO4 was added.

3. The mixture was heated to about 85°C with a Bunsen burner and
ensuring it did not came to a boil temperature. The temperature was
monitored with a clean thermometer.

4. Using a laboratory cloth to hold the flask the solution was titrated
against permanganate with constant swirling until the pink colour of
the permanganate begins to take a few seconds to fade.

5. The temperature was ensured to be about 70 °C before continuing to


titrate drop-wise to reach the end point which was a pale pink

 Princes Town West Secondary Unit 2 Chemistry Labs 32 | P a g e


Conclusion : •

 Princes Town West Secondary Unit 2 Chemistry Labs 38 | P a g e


Lab# 9 Skills O/R/
Assessed: R 
Date: M/M 

A/I 

P/D

Title : Analytical Chemistry : Spectroscopy : UV/Vis

Aim : To determine the nitrate concentration in an unknown water sample using


UV/vis spectroscopy and the use of Beer Lamberts Law.

1. Evol
Evolut
utio
ion
n 600
600 UV-V
UV-Vis
is 5. 50 cm3 burette
Spectrophotometer) 6. Cadm
Cadmiuium
m redu
reduct
ctio
ion
n
Apparatus
2. 10 ppm KNO3solution (100 mg mixture
and :
dm3 anhydrous KNO3) 7. Test tu
tubes
Material
3. 5 – 50 cm3 volumetric flask  8. Stopwatch
4. Unkno
Unknownwn water
water samp
sample
le

Procedure 1. Using a burette


burette serial
serial dilution
dilutionss were
were made
made of the KNO
KNO3 Standard by
3
: transferring 10, 20, 30, 40, and 50 cm  of KNO3 into their respective
volumetric flask.

2. Each flask
flask was then made
made up to the
the mark
mark using disti
distilled
lled water
water and
labelled 2, 4, 6, 8, and 10 ppm respectively.

3. 5 cm3 of each standard was placed into a test tube and labelled,
together with the blank which was distilled water and labelled (0
 ppm) and the unknown sample.

4. A spatula
spatula of cadmium
cadmium reducti
reduction
on mixture
mixture was added to each
each test
test tube
and timed for 12 minutes for each reduction.

5. After the reductio


reduction
n the samples
samples were
were then
then measured
measured for Absorbance
Absorbance
on the UV/Vis spectrophotometer at λ= 530 nm.

6. The results
results were tabulat
tabulated
ed and a standard
standard curve
curve was drawn.

 Princes Town West Secondary Unit 2 Chemistry Labs 39 | P a g e


 Table: 1 Absorbance values of nitrate ions standards and unknown

Observatio  NO3- / 0 2 4 6 8 10 Unknow


ns and :  ppm n
Results
Absorbanc 0 0.053 0.1157 0.216 0.230 0.2622 0.1696
e 7 9

Graph 1. Plot a graph


graph of Absorbance
Absorbance versus
versus concentratio
concentration
n of NO3-

Data 2. From the


the graph
graph infer
infer the unknown concentratio
concentration
n of the
the unknown
unknown
:
Analysis sample

3. Using Beer-L
Beer-Lambert
ambertss Law A=εcl
A=εcl determin
determinee the concentrat
concentration
ion of the
the
unknown sample

4. When the c = 12 ppm


ppm A=
A= ? l = 0.5 cm determ
determine
ine the
the Absorb
Absorbance
ance

Discussion : •

Conclusion : •

 Princes Town West Secondary Unit 2 Chemistry Labs 40 | P a g e


Lab# 10 Skills O/R/
Assessed: R 
Date: M/M

A/I 

P/D

Title : Analytical Chemistry : Quantitative Titration

Aim To determine
• the concentration of iron(II) ions in an unknown solution
solution and, by a
: graphical method,

• the volume of an aqueous solution of substance X that will oxidize


the iron(II) ions in 25 cm3 of the unknown.

1. A is 0.02 mol dm-3 potassium


manganate(VII), KMnO4
2. B is the unknown containing iron(II)
Apparatus
ions, Fe2+,
and :
3. C is an aqueous solution of a
Material
substance X.
4. Under
Under acid
acid condi
conditio
tions
ns X oxidiz
oxidizes
es
iron(II) to iron(III).

Procedure :  Experiment 1

1. Fill
Fill a bure
burett with A, 0.02 mol dm-3 potassium manganate(VII), KMnO4.
ttee with
2. Pipe
Pipett
ttee 25.
25.0 cm3 of B into a conical flask and add, using the measuring
0 cm
cylinder provided 10 cm3 of 1 mol dm-3 sulphuric acid.
3. Run A from the burette into the conical flask until the first permanent
 pale pink colour remains. This is the end point of the titration.
4. Record
Record your
your buret
burette
te readi
readings
ngs in
in Table
Table 1.
5. Repeat the titrations
titrations as many
many times
times as you think
think necessary
necessary to obtain
obtain
accurate results.
6. Make certain
certain that
that the recorded
recorded results show the
the precision
precision of
of your

 Princes Town West Secondary Unit 2 Chemistry Labs 41 | P a g e


practical work.

 Experiment 2

1. Fill the second burette with C, the aqueous solution of X.


2. Pipette 25.0 cm3 of B into a conical flask and add, using the measuring
cylinder provided, 10 cm3 of 1 mol dm-3 sulphuric acid.
3. Add, from the second burette, 4.00 cm 3 of X. This oxidizes some of
the Fe2+ that has been pipetted into the flask.
4. Titrate the remaining Fe2+ in the conical flask with A, potassium
manganate(VII) until the first permanent pale pink colour remains.
5. Record the volume of X added and your burette readings in table 2.
6. One accurate titration will be sufficient. Remember that the volume
added will be less than in  Experiment 1 as some of the Fe 2+ has been
oxidized by X.
7. Empty and rinse the conical flask.
8. Repeat Experiment 2, using the volumes of X shown in Table 2.
9. Record your results in Table 2.

Table 1: Titration of A, 0.02 mol dm-3 potassium manganate(VII),


KMnO4 with B, the unknown.

2 2 2
5 6 5
Final burette reading/
. . . 28.80
cm3
5 2 4
Observatio 0 0 0
ns and :
Results
0 1 1
Initial burette reading/
. . .  3.60
cm3
5 0 0
0 0 0

Volume of A used/ cm3

 Princes Town West Secondary Unit 2 Chemistry Labs 42 | P a g e


Table 2 Titration of B/X mixture with A, KMnO4

0 4 8
Volume of X added/ . . .
12.00
cm3 0 0 0
0 0 0

2 2
0 2
Final burette reading/
. . 20.00
cm3
0 5
0 0

0 6
Initial burette reading/
. . 8.05
cm3
0 5
5 0

Volume of A added/
cm3

↑ Copy and fill out the titration values

Data Experiment 1
:
Analysis

(a) 25.0 cm3 of B reacted with …………….. cm3 of A.

Show which results you used to obtain this volume of A by placing a tick
under the readings in Table 1.

(b) Calculate how many moles of potassium manganate(VII) were


run from the burette into the conical flask during the titration of B
with A.

 Princes Town West Secondary Unit 2 Chemistry Labs 43 | P a g e


(c) Use the half equations for the reaction

MnO4aq- + 8Haq+ + 5e- yields Mnaq2+ + 4H2Ol

Fe(aq)2+ yields Fe(aq)3+ + e-

and your answer to (b) to calculate the concentration of Fe2+, in mol dm-3,
in B.

Experiment 2

(a) Plot the volume of A against the volume of X.


a. Your scale on the X axis should extend to 30.00 cm3.
(a) Draw the best-fit straight line through the plotted points.
(b) From your graph find the volume of X that reacts with the Fe2+
 present in 25.0 cm3 of B.

Graph

Discussion : •

Conclusion : •

 Princes Town West Secondary Unit 2 Chemistry Labs 44 | P a g e


Conclusion : •

 Princes Town West Secondary Unit 2 Chemistry Labs 50 | P a g e


Lab# 13 Skills O/R/
Assessed: R 
Date: M/M 

A/I 

P/D

Title : Solvent Extraction

Theory Introduction:

The aim of this experiment is to determine the equilibrium constant, K , for
the distribution of ethanoic acid (CH3COOH, also known as acetic acid)
 between two immiscible solvents, diethyl ether and water, using an acid-base
titration. The dynamic equilibrium  at the solvent boundary may be
represented by eq. 2

[CH3COOH](aq) k1⇋ k2 [CH3COOH]ether eq.2

: where k1 and k2 are the rate constants  of the forward and reverse processes.
At equilibrium the rates of the forward and reverse processes are equal (eq.
3),

k1[CH3COOH](aq)=k2[CH3COOH](ether) eq.3

and the equilibrium constant may then be defined in terms of solute


concentrations or rate constants  according to eq. 4.

K=[CH3COOH]ether[CH3COOH]aq=k1k2 eq.4

Aim To determine the equilibrium constant, K, for the distribution of ethanoic acid
: (CH COOH, also known as acetic acid) between two immiscible solvents, diethyl
3
ether and water, using an acid-base titration.

Apparatus : 1. Graduated 100 cm3 measuring 6. Distilled water;

 Princes Town West Secondary Unit 2 Chemistry Labs 51 | P a g e


cylinder; 7. Diethyl ether;
2. 250 cm3 separating funnel; 8. 0.5 M aqueous ethanoic acid;
and
3. Three 100 cm3 conical flasks; 9. 0.125 M aqueous ethanoic acid;
Material
4. 10 cm3 pipette; 50 cm3 burette; 10. Phenolphthalein indicator
5. 0.1 M sodium hydroxide solution; solution.

Procedure 1. Using a measuring cylinder, add as accurately as possible 50 cm 3 of 0.5 mol dm -
: 3
 aqueous ethanoic acid and 50 cm 3 of diethyl ether into a 250 cm 3 separating
funnel.
2. Allow the mixture to stand for at least twenty minutes, shaking occasionally
(remember to release the pressure after shaking by inverting the funnel, holding
on to the stopper and opening the tap).
3. Run off the lower (aqueous) phase into a clean 100 cm 3 conical flask, making
sure no ether is drained off. Now run off the interface portion and discard it and
leave the ether layer phase in the separating funnel.
4. Pipette 10 cm3 of each phase into separate 100 cm 3 conical flasks and add a few
drops of phenolphthalein indicator. Titrate both solutions with 0.1 mol dm -3
sodium hydroxide solution until the solution retains a permanent pink colour.
5. Repeat the titrations with two further 10 cm 3 aliquots.
6. Repeat steps 1-3 using 0.125 mol dm -3 aqueous ethanoic acid in place of the 0.5
mol dm-3 solution.

Observatio
ns and :
Results

Data Treatment of Results


Analysis 1. Write a balanced equation for the reaction between ethanoic acid and sodium
hydroxide.
2. From the volumes of sodium hydroxide solution required to neutralise the
ethanoic acid, calculate the number of moles of ethanoic acid in each 10 cm 3
: aliquot you titrated and, hence, evaluate the e thanoic acid concentration for each
solution.
3. Using the ethanoic acid concentrations you have determined, evaluate the
equilibrium constant, K, using eq. 4 for both initial ethanoic acid
concentrations.
4. Do the values of K obtained using 0.5 mol dm -3 and 0.125 mol dm -3 ethanoic
acid differ? Is this to be expected?

Discussion : •

Conclusion : •

 Princes Town West Secondary Unit 2 Chemistry Labs 52 | P a g e


Lab # NA Skills O/R/
Assessed: R 
Date: M/M

A/I 

P/D

Title : Carbonyl Compounds

Aim : Investigating Carbonyl Compounds

Theory Aldehydes and ketones are carbonyl compounds which contains the

carbonyl group . Aldehydes have a single alkyl or acyl group attached


to the carbon atom whilst ketones have two. They both react with 2, 4
dinitrophenylhydrazine (2,4 – DNPH) to give orange precipitates.

: Mild oxidising agents such as Tollen’s and Feh ling’s reagents can oxidise
aldehydes but not ketones. Hence this reaction can be used to distinguish the
 both of them.

Tollen’s reagent forms a silver mirror on the wall of the test tube and
Fehlings solution gives a red-brown precipitate of Copp er (I) Oxide.

Three samples are given, two of which are carbonyl compounds, one is an
aldehye and the other is a ketone.

1. Samples B, C and D 3. Fehling’s reagent


Apparatus 2. 2, 4 – DNPH (dissolve 2 g of 2, 4- 4. Aqueous NH3 and
and : DNPH in 4 cm3 of conc. H2SO4, 30 AgNO3
Material cm3 of methanol and 10 cm3 of 5. Measuring cylinders
water. 6. Test tubes

Procedure 1. 3 cm3 of 2,4 – DNPH was added to a few drops of sample B in a test
:
tube and observations were made and recorded.

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2. To 3 cm3 of AgNO3 in a test tube, ammonia solution was then added
dropwise, while shaking the solution until the precipitate formed re-
dissolved. A few drops of sample B was then added to this tube
(Tollens Test) and observations were made and recorded.

3. A few drops of sample B was added to Fehlings reagent in a test tube


and the tube was gently heated. Observations were recorded.

4. Steps 1-3 was then repeated for Sample C and D.

Table 1 Observations

Solution added Sample B Sample C Sample D

2,4- DNPH Orange Orange  No visible reaction


 precipitate  precipitate
Observation formed formed
s and :
AgNO3 and NH3  No visible Silver  No visible reaction
Results
reaction mirror
formed on
test tube

Fehlings reagent No visible Red-  No visible reaction


reaction  brown
 precipitate

Data 1. Deduce which of the samples are carbonyl compounds.


Analysis
and : Sample B and Sample C are both Carbonyl compounds since they
Interpretati  both reacted with 2, 4 dinitrophenylhydrazine to give an orange
on  precipitate.

2. Deduce which of the samples is an aldehyde

Sample C is an aldehyde since it was oxidised by both Tollen’s


reagent and Fehlings reagent where it formed a silver mirror and a
red- brown precipitate respectively. Mild oxidising agents can
oxidise aldehydes, but not ketones.

Tollens Test:
CH3CHO(l) + 2Ag+(aq) + H2O(l) CH3COOH (aq) + 2Ag(s) + 2H+(aq)

Fehlings reagent gives a red brown precipitate of copper (I) Oxide:

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CH3CHO(l) + 2Cu2+(aq) + 2H2O(l) CH3COOH (aq) + Cu2O(s) + 4H+(aq)

3. Deduce which sample is a ketone:

Sample B is the ketone, since it gave an orange precipitate with 2, 4


dinitrophenylhydrazine, which means that it is a carbonyl compound,
 but it showed no reaction with the weak oxidising agents Tollens
reagent and Fehlings reagent.

These two tests are used to distinguish between an aldehyde and a


ketone.

Discussion • Tollens reagent and Fehlings reagent are weak oxidising agents
• Can be used to distinguish between aldehydes and ketones
:
• Shows not reaction with ketones
• Gives a silver mirror test and red-brown precipitate with aldehydes

Conclusion : Sample B is the ketone and Sample C is an aldehyde.

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 Princes Town West Secondary Unit 2 Chemistry Labs 78 | P a g e
Lab # 19 Skills O/R/
Assessed: R 
Date: M/M 

A/I 

P/D

Title : Environmental

Aim : To test for pollutants in water 

Theory Pollutants found in water include cyanide, lead (II) ions, nitrates and
 phosphates. Cyanide is converted to thiocyanate when it reacts with sulphur.
This ion is found in effluents from mining and industrial factories. Certain
 pesticides also contain thiocyanate ion as the main ingredient. Phosphates are
nitrates are present in fertilizers and detergents, and these can also pollute the
waterways.
:
Carry out the following procedure to test for S CN-, NO3-, PO43- and Pb2+.

SCN- gives a blood red colour on addition of aqueous iron (III) nitrate.


PO43- gives a bright yellow precipitate when warmed with ammonium
molybdate
 NO3- is identified via the brown ring test
A white precipitate is formed with Pb2+ on addition of hydrochloric acid.

1. Samples of Polluted water P, Q and 7. Conc. H2SO4


R  8. Conc. HNO3
2. 0.1 mol dm-3 iron (III) nitrate 9. Bench HCl and H2SO4
Apparatus
solution 10. Test tubes
and :
3. 0.1 mol dm-3 ammonium molybdate 11. Water bath
Material
4. Solid iron (II) sulphate
5. Bunsen burner
6. spatula

Procedure : 1. Iron (III) Nitrate was added drop by drop to 2 cm3 of sample P in a
test tube. Observations were made and recorded.

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2. 2 cm3 of sample P in a test tube was acidified with dilute H2SO4. Half
a spatula of solid iron (II) sulphate was then add ed to the acidified
sample.

3. To this acidified sample of P, 0.5 cm3 of Conc. H2SO4 was then


carefully added, by letting it flow down the side of the test tube. The
mixture was then left undisturbed until two separate layers were
formed within the test tube. Observations were made ad recorded.

4. 2 cm3 of sample P in a test tube was acidified with Conc. HNO3. A


little amount of ammonium molybdate was then added and the tube
was then gently warmed in a water bath. Observations were made and
recorded.

5. Dilute HCl was added to 2 cm3 of sample P in a test tube. The


mixture was then heated for one minute and then allowed to cool.
Any observations were recorded.

6. Steps 1-5 were then repeated for both sample Q and R 

Table 1 : Observations made during the experiment for all three samples P, Q
and R 
Observations with:
Observatio Sample Fe(NO3)3(aq) Fe2+(aq)/conc. (NH4)2 HCl (aq)
ns and : H2SO4 MoO4(a
s
Results q)

Data : 1. Deduce which of the samples of water are polluted with:


Analysis and • Thiocyanate ions
Interpretati •  Nitrate ions
on • Phosphate ions
• Lead (II) ions

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Lab # NA Skills O/R/
Assessed: R 
Date: M/M 

A/I 

P/D

Title : Plan and Design : Organic Chemistry

Aim : Organic

Case Mr. Smith wants to buy a new car. He has a choice of vehicles which run on
leaded gasoline, unleaded gasoline, compressed natural gas, and diesel. His
: environmentally conscious friend suggests he buys a car which contributes to
the least amount of pollution. Suggest which fuel is most environmentally
friendly and plan and design an experiment to test your suggestion.

Apparatus 1. 2.
and :
Material

Procedure : 1.

2.

3.

4.

5.

6.

Observatio
ns and :
Results

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Data
Analysis and
:
Interpretati
on

Discussion : •

Conclusion :

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Lab # 20 Skills O/R/
Assessed: R 
Date: M/M 

A/I 

P/D

Title : Plan and Design : Analytical Chemistry (Gravimetric)

Aim :

Case Caesium nitrate, CsNO 3, decomposes on heating.

The decomposition is represented by one of the following equations.

4CsNO3(s)  2Cs2O(s) + 4NO 2(g) + O2(g)

2CsNO3(s)  2CsNO2(s) + O2(g)

 You are to devise a method of heating the solid


nitrate, collecting the gas given off and measuring its
volume.
:
From the experimental results you are to determine
which is the correct equation for the decomposition.

Information that may be used to prove your plan and design.

The molar volume of gas, V m, is 24.0 dm 3 mol –1 under room conditions.

Nitrogen dioxide, NO 2, a toxic gas, is soluble in water.

Oxygen, O2, is not soluble in water.

[ Ar; Cs, 133.0; N, 14.0; O, 16.0.]

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Apparatus 1. 2.
and :
Material

Procedure : 1.

2.

3.

4.

5.

6.

Diagram :

Observatio
ns and :
Results

Data
Analysis and
:
Interpretati
on

Discussion : •

Conclusion :

 Princes Town West Secondary Unit 2 Chemistry Labs 85 | P a g e

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