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PRINCES TOWN WEST SECONDARY

CAPE UNIT 2
CHEMISTRY LABS
2011 - 2012

Princes Town West Secondary Unit 2 Chemistry Labs

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Lab # 1
Lab # 2
Lab # 3
Lab # 4
Lab # 5
Lab # 6
Lab # 7
Lab # 8
Lab# 9
Lab# 10
Lab# 11
Lab# 12
Lab# 13
Lab #
14
Lab #
15
Lab #
16
Lab #
17
Lab #
18
Lab #
19
Lab #
20

Title
Organic Compounds : To determine which organic compound is contained in the
bottles labelled A, B, C and D
Organic Compounds: To determine which organic compound is contained in the
bottles labelled P, Q, R and S.
Plan and Design : Organic Chemistry
Organic Chemistry: To investigate the relative acidities of alcohols, phenols and
carboxylic acids
Analytical Chemistry : The degree of uncertainty
Crystallization
Analytical Chemistry : Gravimetric Analysis - percentage oxalate in an unknown
sample
Analytical Chemistry : Gravimetric Analysis - Vitamin C Tablet
Analytical Chemistry : Spectroscopy : UV/Vis
Analytical Chemistry : Quantitative Titration
Chromatography : Paper Chromatography Pigment in leaves
Chromatography : Paper Chromatography Inks
Solvent Extraction
Plan Design: Environmental Chemistry

Skills

Simple and Fractional Distillation


Environmental Chemistry : Organic Compounds
Plan Design: To determine the acidity / pH of a soil sample
Analytical Chemistry Back Titration
Environmental test for pollutants in water.
Plan and Design : Analytical Chemistry (Gravimetric)

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Lab # 1

Skills
Assessed:

Date:

Title

Aim

Apparatu
s and
Material

O/R/
R
M/M
A/I
P/D

: Organic Compounds
:

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


B, C and D.

1. Test Tubes
6. 2,4-dinitrophenyihydrazine
2. Boiling Tubes
7. Aqueous Silver Nitrate
3. 250 ml Beaker(Labelled Organic
8. Aqueous Sodium Hydroxide
:
9. Aqueous Ammonia
Waste)
10. Acidified Potassium
4. Magnesium Powder or Turnings
5. Sodium Carbonate
Dichromate
Aqueous solutions, A, B, C and D. Each solution contains one of the
following.
I.
an alcohol
II.
an aldehyde
III.
a carboxylic acid
IV. a ketone

Procedure
:

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

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Test (a)

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


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.

Test (b)

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


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.

Test (c)

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


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)

Test (e)

Observati
ons and
Results

Use a dropping pipette to add dilute aqueous ammonia to this mixture until the
precipitate of silver oxide just 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 silvercontaining solution you have just prepared.
Place 1 cm depth of each of the solutions A, B, C and D into separate boiling-tubes.
To each tube add a few drops of acidified potassium dichromate(V1) to give a
yellow-orange solution. Warm the tube gently.

Aqueous
Solutions

A
(Alcohol)

B
(Ketone)

C
(Aldehyde)

Test (a)

No Rxn

No Rxn

No Rxn

Test (b)

No Rxn

No Rxn

No Rxn

Test (c)

No Visible
Rxn
No ppt
formed

Yellow
brown/
(orange) ppt

Yellow
brown/
(orange) ppt

Princes Town West Secondary Unit 2 Chemistry Labs

D
(Carboxylic
Acid)
Pop with glowing
splint H2 gas
given off. Hence
Compound D is
the acid.
effervescence and
gas bubbled
through Ca(OH)
White ppt formed.
Gas given off
CO2. D is the
carboxylic Acid.
No Visible Rxn
No ppt formed

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formed
Aldehyde or
Ketone

Test (d)

No Visible
Rxn
No ppt
formed

Test (e)

Green
solution
formed
indicating
Cr3+ ions
hence an
alcohol or
aldehyde

Discussion

No Visible
Rxn
No ppt
formed

No Visible
Rxn

formed
Aldehyde or
Ketone
Silver ppt
formed on
ring of test
tube silver
mirror effect
hence
compound C
is the
Aldehyde
Green
solution
formed
indicating
Cr3+ ions
hence an
alcohol or
aldehyde

No Visible Rxn
No ppt formed

No Visible Rxn

Test (a)
o Compound D is the acid as H2 gas was given off and identified
by the pop with the glowing splint.
+
Mg(aq) + H 2( g)

RCOO
o
2 RCOOH (aq) +2 Mg(s) yields 2

Test (b)
o Effervescence CO2 given off as confirmation with white ppt
forming in CaA(OH)2
+
Na(aq) +CO 2( g )+ H 2 O(l)
RCOO
o
2 RCOOH (aq) + Na 2 CO 3 (s) yields 2

CO2 ( g )+Ca(OH )2 yields CaCO3 (s) + H 2 O(l)

o Substance D is the acid as no other reactions


were observed by the other substances.
Test (c)
o Yellow brown (or orange) ppt seen for B and C indication its a
carbonyl compound.

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o Substance B and C are either a ketone or


aldehyde
o
RCHO+C 6 H 3 ( NO 2 )2 . NH NH 2 yields RCH =NN C6 H 3 ( NO 2 )2 (s )+ H 2 O(l )

o
'

'

R R CO+ C6 H 3 ( NO 2 )2 . NH NH 2 yields R RC =NN C 6 H 3 ( NO 2) 2( s) + H 2 O (l)

Test (d)
+4 NH 3 ( g) +2 H 2 O(l )

yields 2 Ag(s) + RCOO(aq)


o

Conclusio
n

++ RCHO(l) +3 OH (aq)
2 Ag( NH 3 )2(aq)

o Tollens reagent only reacts with aldehydes to give the silver


mirror effect substance C is the aldehyde.
Test (e)
o Substance A is an Alcohol because it reduces aqueous K2Cr2O7
to a green Cr3+ but did not react with either Tollens reagent or
2,4,-dinitrophenylhydrazine reagents.
o Substance B has to be the ketone by reason of
elimination and its reaction with 2,4,dinitrophenylhydrazine.

gas

test and test result

ammonia, NH3

turns damp red litmus paper blue

carbon dioxide, CO2

gives a white ppt. with limewater


(ppt. dissolves with excess CO2)

chlorine, 012

bleaches damp litmus paper

hydrogen, H2

'pops' with a lighted splint

oxygen, 02
sulphur dioxide, 802

relights a glowing splint


turns potassium dichromate(VI) (aq) from orange to
green

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Lab # 2

Skills
Assessed:

Date:

Title

Aim

Apparatus
and
Material

O/R/
R
M/M
A/I
P/D

: Organic Compounds
:

To determine which organic compound is contained in the bottles labelled P,


Q, R and S.

1. Test Tubes
6. 2,4-dinitrophenyihydrazine
2. Boiling Tubes
7. Aqueous Silver Nitrate
3. 250 ml Beaker(Labelled Organic
8. Aqueous Sodium Hydroxide
:
9. Aqueous Ammonia
Waste)
10. Acidified Potassium
4. Magnesium Powder or Turnings
5. Sodium Carbonate
Dichromate
You are provided with four organic substances P, Q, R and S.
Each belongs to one of the following classes of compounds:
I.
An aromatic alcohol
II.
An alkene
III.
An alkane
IV. An alkyl halide

Procedure

1. You are to perform the tests below and from the results establish
which type of organic compound is contained in each of P, Q, R and
S.
2. After each test discard the contents of the tubes into the 250 cm3
beaker, labelled organic waste. Rinse and re-use the tubes for the
remaining tests.
3. Gloves, eye protection and lab coats must be worn. The Fume hood
must be used where specified.

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Place 5 drops of each of the substances P, Q, R and S into separate dry


Test (a) test-tubes. Cover each test-tube completely with foil. In the fume
Test (b)

Test (c)

cupboard add 5 drops of bromine to each. Stopper for 5-10 minutes.


Place 5 drops of each of the substances P, Q, R and S into separate dry
test-tubes. In the fume cupboard add 5 drops of bromine to each.
Expose
to bright
sunlight.
Place 5 drops
of each
of the substances P, Q, R and S into separate dry
test-tubes. Add 2% aqueous potassium manganate(VII) drop wise.
Observe any changes within five minutes.
Place 2 drops of each of the substances P, Q, R and S into separate dry

Test (d) test-tubes. To each tube add 1 cm depth of aqueous Iron(III) chloride
solution. Warm if necessary.
Test (e)

Place 2 drops of each of the substances P, Q, R and S into separate dry


test-tubes. To each tube add 1 cm depth of aqueous silver nitrate
solution. Warm if necessary.

Observatio
ns and
Results

Aqueous
Solutions

Test (a)
Test (b)
:
Test (c)
Test (d)
Test (e)

Discussion

Conclusio
n

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Lab # 3

Skills
Assessed:

Date:

Title

: Plan and Design : Organic Chemistry

Aim

O/R/
R
M/M
A/I
P/D

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

Case

The solutions are:


1.0 mol dm3 Propanone
1.0 mol dm3 Propanal
0.5 mol dm3 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
Apparatus
and
Material

1.
:

Procedure

2.

1.
2.
3.
4.
5.
6.

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Observatio
ns and
Results

Data
Analysis
and
:
Interpretati
on
Discussion :

Conclusion

Lab # 4

Skills
Assessed:

Date:

O/R/
R
M/M
A/I
P/D

Title

: Organic Chemistry

Aim

: To investigate the relative acidities of alcohols, phenols and carboxylic acids

Theory

: The relative acidities of alcohols, phenols and carboxylic acids depends on


the ease at which the molecule gives up a proton to water in an aqueous
solution. Strong acids are those which easily donate a proton and hence is
fully ionised in an aqueous solution.
Example:

HCl

H+ + Cl-

Alcohols do not give up H+ ions readily due to the presence of the OH


group, because the alkyl group donates electrons to the O atom, thereby
decreasing the tendency for the H atom to ionise.
ROH + H2O

RO- + H3O+

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Phenols tend to give up H+ more readily than alcohols because electrons


from the OH bond tends to be localized around the benzene ring, and thus
increases the tendency for the H atom to ionise.

Carboxylic acids are the strongest acid of all the three, and tends to give up
H+ more readily than alcohol and phenols. The carboxyl group
tends
to pull electrons away from the OH bond, hence weakening the OH bond
and making it easier for the H atom to ionise.
RCOOH + H2O
RCOO- + H3O+
Apparatus
and
Material
Procedure

Observatio
ns and
Results

Data
Analysis
and
Interpretati
on

1. Samples of Ethanol, Phenol and


Ethanoic acid.
2. Magnesium Ribbon
3. Solid Na2CO3
4. Test tubes

1. A piece of Magnesium Ribbon was added to 4 cm3 of ethanol in a


test tube and observations were recorded
2. Solid Na2CO3 was added to 4 cm3 of ethanol in a test tube and
observations were recorded
3. The pH meter was then used to find the pH of ethanol, and this value
was also recorded.
4. The above procedure was then repeated using phenol and ethanoic
acid.
Table 1:

5. Apparatus to test gas,


splint, litmus, Ca(OH)2(aq)
6. pH meter / pH paper
7. spatula
8. Glass rod

Ethanol

Observation table
Phenol

Ethanoic Acid

Magnesium Ribbon
Solid Na2CO3
pH

1. Which samples reacted with Mg? Write a balanced equation for any
reaction which occurred.
:

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2. Which samples reaction with Solid Na2CO3? Write a balanced equation for
any reaction that occurred.

3. Use the results of the experiment to deduce the order of increasing


acidities of the samples.
Discussion

Conclusion

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Skills Assessed:

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O/R/R

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Lab # 5

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 and
Material

Procedure

1. 50 cm3 burette (Class A)


2. 10 cm3 measuring cylinder (Class A)
3. Distilled water
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.
Table: 1

Observations and
Results

Graph
Data Analysis

Readings obtained from the burette and measuring cylinder respectively.


No. of Drops
25
50
75
Final Burette Reading / cm3
Initial Burette Reading / cm3
Total Vol of drops Burette / cm3
Vol in measuring cylinder / cm3
S.D. between Readings

100

125

150

200

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


:

1.
2.
3.
4.

From the graph determine when 4 cm3 of the burette is delivered the volume of measuring cylinder?
From the graph when 8.2 cm3 of water is delivered from the burette the reading in the measuring cylinder ?
Which instrument is considered to be accurate
Which instrument is considered to be precise

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5. Explain your answer for questions 3 and 4.


Discussion

Conclusion

Lab # NA

Skills Assessed:

Date:

Title

Analytical Chemistry : Measurements

Aim

Uncertainty of measurements of volumes and masses

1.
2.
3.
4.
5.
6.

Apparatus and
Material

Procedure
Part A

Burette, 50 mL, Class B


Graduated pipette, 10 mL, Class B
Volumetric flasks, 25 mL, Class A and B
Measuring cylinder, 10 mL
15 Vials and stoppers
Tissue

O/R/R
M/M
A/I
P/D

7. Top loading balance


8. Analytical balance
9. Unknown liquid, 200 mL. (0.789 g ml-1)
10. Distilled water
11. Pipette filler

:
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

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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 sample vial, again ensuring that no liquid
is spilled on the outside.
4. The empty volumetric flasks with their stoppers were reweighed.
5. Results were recorder in Table 1.

Part C

1. Using a top loading balance combined masses of 2, 4, 6, 8, and 10, 100 g weights were obtained.
2. A graph was plotted of mass versus number of weights to obtain a best fit line through the points.

Part D

1. The weight of two 100 g weights were measured using a top loading balance first by:
a. The individual masses and
b. The combined masses of two
2. This procedure was then repeated on an analytical balance.

Observations and
Results

Part A and B: Table 1: Uncertainty of Measurements of Volumetric Apparatus


Apparatus
1
2
3
Average
Loaded
19.1175
19.0251
18.9238
Burette
Empty
11.0893
11.0073
10.8985
Class B 0.06
Mass
8.0282
8.0178
8.0253
8.0238
Loaded
18.8871
18.9043
19.0629
Graduated Pipette
Empty
10.8947
10.8963
11.0264
Class B 0.06
Mass
7.9924
8.008
8.0365
8.0123

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Measuring Cylinder
Class B 0.1 @ 20C

Volumetric Flask A
Class B 0.02 @ 20C

Volumetric Flask B
Class B 0.04 @ 20C

Loaded
Empty
Mass
Loaded
Empty
Mass
Loaded
Empty
Mass

Part C
i. 100 g Weights
2
4
6
8
10
Slope

18.7994
11.0705
7.7289
21.9282
14.0295
7.8987
23.6678
15.7382
7.9296

18.7795
11.0494
7.7301
21.917
14.0325
7.8845
23.6576
15.7443
7.9133

7.7241
7.8895
7.9117

Mass (g)
200.04
400.07
600.1
800.14
1000.17
100.01625

ii. Mass (g) 10100 g Weights


Group 1

200.040

400.07

600.10

800.14

Group 2

200.065

400.17

600.24

800.14

Group 3
Group 4

200.03
200.06

400.17
400.12

600.12
600.17

800.11
800.22

Mass( g) Average

Average Masses
Part D
iii. Mass 1-100 g
Weight
A
B
Average Mass
Mass Both 100 g
Weights

18.9284
11.2151
7.7133
21.915
14.0296
7.8854
23.6485
15.7562
7.8923

1000.1
7
1000.3
6
1000.2
1000.0
7

100.016
100.037
100.021
100.001
100.019

Top Loading Balance

Analytical Balance

100.02
100.02
100.02

100.003
100.001
100.002

200.04

200.004

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Part C
Graph showing Mass versus number of 100 g weights
1200
1000
800

Graph

Mass(g)

600
400
200
0
2

10

Number of 100 g Weights

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Data Analysis

Standard Deviation and Gossett T-Function of Part A and B


Standard Deviation =
S.D.

Gossetts T-Function
t= 4.302
2

Loaded

19.1175

19.0251

18.9238

Empty

11.0893

11.0073

10.8985

8.0282

8.0178

8.0253

0.000019
7

0.0000356

0.000002351

Loaded

18.8871

18.9043

19.0629

Empty

10.8947

10.8963

11.0264

7.9924

8.008

8.0365

0.000396

0.000018

0.000586

Loaded

18.7994

18.7795

18.9284

Empty

11.0705

11.0494

11.2151

7.7289

7.7301

7.7133

0.000023

0.000036

0.000117

Loaded

21.9282

21.917

21.915

Empty

14.0295

14.0325

14.0296

7.8987

7.8845

7.8854

0.000084

0.000025

0.000017

Loaded

23.6678

23.6576

23.6485

Empty

15.7382

15.7443

15.7562

Mass

7.9296

7.9133

7.8923

0.000319

0.000002

0.000378

Apparatus

Burette

Mass
2

( x x )

Graduated
Pipette

Mass

Average

2
(xx ) (xx )

2 =

sd t ( p ,n1)
n

8.0238
5.761E05

0.005
4

0.0133

1.000E-03

0.0224

0.0556

1.757E04

0.009
4

0.0233

1.264E04

0.008
0

0.0198

6.993E04

0.018
7

0.0465

8.0123

( x x )

Measuring
Cylinder

Mass

7.7241

( x x )

Volumetric
Flask A

Mass

7.8895

( x x )
Volumetric
Flask B

( x x )

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Part C

Pool Average Masses From Class


12
True Value
Accurate Measure
10
8
Frequency

6
4
2
0
99.99

100

100.01

100.02

100.03

100.04

Mass /g

Discussion
Part A

Part B

The analysis showed that the burette showed reliable results when compared to the other volumetric
instruments having the lowest deviation from the means and an acceptable confidence level of <0.05.
The pipette in this experiment was the least accurate, having highest deviation when comparing means and an
unacceptable confidence level. This result defies convention of the accuracy of the pipette and therefore the
results suggest human error may have resulted in this disparity.
The measuring cylinder provided a reasonable accurate measure of volume in the Laboratory.
Comparing the accuracy of various Classes of volumetric apparatus it was clearly seen that Class A apparatus
showed a high degree of accuracy when compared to Class B apparatus, which is expected by convention.
The confidence level for the Class A was less than that of the Class B indicating the reliability in the results.

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Part C

The accuracy of Group experiment showed that Group 1 was the closest to the accurate value whilst the rest
of the group even though were precise were not accurate.

Part D

When comparing the analytical balance to the top loading balance it was found the analytical balance was
more accurate in its measure of weights as expected by convention.

Conclusion

:
The experiment was conducted successfully. An understanding of measurements accuracy and precision was clearly
exemplified.

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Lab # 6

Skills Assessed:

Date:

O/R/R
M/M
A/I
P/D

Title

Crystallization

Aim

To determine the number of moles of water of crystallization in hydrated MgSO4.xH2O

Hydrated salts contain water of crystallization which can be removed by heating. The hydrated salt is heated and
weighed repeatedly until a constant mass is obtained. This loss in mass of the salt can then be used to calculate
the number of moles of water of crystallization.

Theory

Apparatus and
Material

Procedure

Observations and
Results

1. Hydrated Magnesium sulphate MgSO4.xH2O


2. Hard glass test tube and holder

3. Balance
4. Bunsen burner

1. The empty hard glass test tube was weighed and this value was recorded.
2. 6 g of hydrated magnesium sulphate was then placed in the test tube and reweighed. Readings were
recorded.
3. The test tube was then heated gently initially and then more strongly to remove any water that was
present. Heating was stopped if the salt started to decompose or emit white fumes.
4. The test tube was allowed to cool and then the tube and its contents were reweighed and this value was
recorded
5. The heating, cooling and weighing process was repeated until a constant mass was obtained. All the
readings were recorded.

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

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Table 2

Mass of hydrated magnesium sulphate after


heating
Mass of test tube and hydrated magnesium sulphate
after heating / g

Mass of empty test tube /g


Mass of hydrated magnesium sulphate after heating
/g
Data Analysis and
Interpretation

1.
2.
3.
4.

Number of moles of anhydrous MgSO4 in the sample


Determine the mass of water driven out of the sample
Number of moles of water driven out from the sample
Number of moles of water of crystallization in one mole of hydrated MgSO4
number of moles of water driven out

= the sample
number of moles of anhydrous magnesium sulphatethe sample

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

Discussion

Conclusion

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Lab # 7

Skills Assessed:

Date:

O/R/R
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


2. Burette and funnel
3. Retort stand and clamp
4. 1 white tile
5. 2 sample vials with stoppers
6. Bunsen burner/ tripod / wire gauze
7. Thermometer
8. 25 mL measuring cylinder
9. 10 mL measuring cylinder
10. 25 mL Pipette and pipette filler

Apparatus and
Material

Procedure

11. 2 spatulas
12. Analytical balance
13. K2C2O4.H2O salt
14. 3.0 M H2SO4
15. 0.02 M KMnO4 solution
16. Distilled water
17. Unknown oxalate sample
18. 250 mL volumetric flask
19. Laboratory cloth

1. ~1.5 grams of K2C2O4.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 K2C2O4 standard was pipette into a conical flask and 15 mL of 3.0 M H2SO4 was added.
3. The mixture was heated to about 85C 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 colouration that persists.
6. The titration was repeated twice more to ensure reliability of the titre value.
7. The mass of the unknown was accurately weighed and dissolved in 50 mL of distilled water in a 250 mL
Volumetric flask and then made up to the mark
8. 15 mL of 3M H2SO4 was added to the unknown oxalate solution and titrated with the standardised KMnO4
as outlined in procedure # 2 to 6.

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9. The mass of the unknown was repeatedly weighed until the mass produced a titre value close to
standardisation value of the permanganate.
Mass of K2C2O4.H2O salt used: ________ g
Table: 1

Standardisation of KMnO4.
Rough
1
2

Average

Final Burette Reading / cm3


Initial Burette Reading / cm3
Total Vol of Burette / cm3

Observations and
Results

Table: 2

Determination of the unknown concentration of oxalate.


Rough
1
2
Mass of unknown used /g
Final Burette Reading / cm3
Initial Burette Reading / cm3
Total Vol of Burette / cm3

Data Analysis

1. Calculation of the Molarity of the permanganate solution


2. Calculation of the percentage oxalate in the unknown mixture :
3. Why the unknown was repeatedly weighed to produce a titre value close to that of the permanganate.

Discussion

Conclusion

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Lab # 8

Skills Assessed:

Date:

Title

Analytical Chemistry : Gravimetric Analysis

Aim

To determine the Ascorbic Acid concentration in a commercially available Vitamin C Tablet.

Theory

VITAMIN C ANALYSIS

O/R/R
M/M
A/I
P/D

Step 1: Potassium iodate reacts with iodide to form the complex trihalide
+3 H 2 O
+ yields 3 I 3

+6 H
+8 I
: IO3
I 3

Anion

Step 2: The trihalide ion reacts with vitamin C :

++3 I
yields C6 H 6 O6 +2 H

C 6 H 8 O6 + I 3
Step 3: Remaining trihalide is determined with thiosulfate

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2
+ S4 O6
2 yields 3 I

+ 2 S2 O3
I 3

Apparatus and
Material

Procedure
:

1.
3.
5.
7.
9.
11.
13.
15.
17.
19.
21.
23.

2 White tiles
2 100 mL and 2 250 mL Beakers
2 sample vials with stoppers
1 250 mL, Volumetric flask
6 - 250 mL conical flasks
2 50 mL Burettes and 2 funnels
Cotton wool, tissue & lab cloth
3 Filter funnels
1 Mortar and pestle
2 Pasteur pipettes
2 Retort stands and clamps
1 Glass rod

2. 1 Wash bottle with distilled water


4. 2 Spatulas
6. 3 25 mL Pipettes and 3 pipette fillers

8. 2 25 mL, & 2 10 mL Measuring cylinders


10.
12.
14.
16.
18.
20.
22.

Analytical & top loading balances


1000 mg vitamin C tablet in vial
KIO3 solution (2.1526 g L-1)
M H2SO4
Sodium thiosulfate solution
10% KI solution
Starch

24. 1 Wash bottle with distilled water

PROCEDURE A: Standardization of Sodium Thiosulfate Solution Using Iodate Pipette 25 mL of the standard
potassium iodate solution provided into a 250 mL conical flask. Add 15 mL of 1 M sulfuric acid to the flask followed by 10
mL of 10% potassium iodide solution. Titrate the liberated iodine against the sodium thiosulfate solution until the solution
changes to a pale yellow. Then add 10 drops of starch solution and continue the titration until the blue colouration just
disappears.
PROCEDURE B: Determination of Ascorbic Acid content of Vitamin C Tablet Accurately weigh and record the mass of
one Vitamin C tablet. Using a mortar and pestle pulverize the entire tablet. Transfer 500 mg of the powder (accurately
weighed) to a 100 mL beaker and add 75 mL of 1M H2SO4. Agitate the mixture with a glass rod and gravity filter into a 250
mL volumetric flask. To filter the solution plug the stem of a funnel with a piece of cotton wool. Rinse the cotton with a
small volume of 1M H2SO4 ensuring that the flow rate is moderate before beginning to filter the Vitamin C H2SO4
mixture. Ensure that no solid material goes into the volumetric flask. If this happens you will need to re-filter. Make the
solution up to 250 mL with 1M H2SO4. Pipette 25 mL of the vitamin C solution into a conical flask and add 25 mL of
standard KIO3 solution by pipette. Add 10 mL of 10% KI solution to the mixture and titrate against the standardized
thiosulfate solution until the solution becomes a very pale yellow. Add 10 drops of starch solution and continue the titration
until the blue colouration just disappears. Repeat the experiment until a satisfactory average is obtained for the end point.

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Observations and
Results

Data Analysis

Using a Suitable Tables Record Your Results.

Use your average titre volume to calculate


1. The number of moles of 10; initially added to the solution

2. The number of moles of I; produced initially


3. The number of moles of I; which reacted with thiosulfate
4. The number of moles of I; which reacted with L-ascorbic acid

Discussion

Conclusion

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Lab# 9

Skills Assessed:

O/R/R
M/M
A/I
P/D

Date:

Title
Aim

Apparatus and
Material
Procedure

Observations and
Results

Analytical Chemistry : Spectroscopy : UV/Vis

To determine the nitrate concentration in an unknown water sample using UV/vis spectroscopy and the use of
Beer Lamberts Law.

1.
2.
3.
4.

Evolution 600 UV-Vis Spectrophotometer)


10 ppm KNO3solution (100 mg dm3 anhydrous KNO3)
5 50 cm3 volumetric flask
Unknown water sample

5.
6.
7.
8.

50 cm3 burette
Cadmium reduction mixture
Test tubes
Stopwatch

1. Using a burette serial dilutions were made of the KNO3 Standard by transferring 10, 20, 30, 40, and 50 cm3
of KNO3 into their respective volumetric flask.
2. Each flask was then made up to the mark using distilled 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 of cadmium reduction mixture was added to each test tube and timed for 12 minutes for each
reduction.
5. After the reduction the samples were then measured for Absorbance on the UV/Vis spectrophotometer at
= 530 nm.
6. The results were tabulated and a standard curve was drawn.
Table: 1

NO3 / ppm

Absorbance

Princes Town West Secondary Unit 2 Chemistry Labs

Absorbance values of nitrate ions standards and unknown


2
4
6
8
10
0.053

0.1157

0.2167

0.2309

0.2622

Unknown
0.1696

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Graph

1. Plot a graph of Absorbance versus concentration of

NO3

Data Analysis

2. From the graph infer the unknown concentration of the unknown sample
3. Using Beer-Lamberts Law A=cl determine the concentration of the unknown sample
4. When the c = 12 ppm A= ? l = 0.5 cm determine the Absorbance

Discussion

Conclusion

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Lab# 10

Skills Assessed:

Date:

Title

Analytical Chemistry : Quantitative Titration

To determine
the concentration of iron(II) ions in an unknown 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.
2.
3.
4.

Aim

Apparatus and
Material

O/R/R
M/M
A/I
P/D

Procedure

A is 0.02 mol dm-3 potassium manganate(VII), KMnO4


B is the unknown containing iron(II) ions, Fe2+,
C is an aqueous solution of a substance X.
Under acid conditions X oxidizes iron(II) to iron(III).

Experiment 1
1. Fill a burette with A, 0.02 mol dm-3 potassium manganate(VII), KMnO4.
2. Pipette 25.0 cm3 of B into a conical flask and add, using the measuring cylinder provided 10 cm3 of 1 mol dm3

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 your burette readings in Table 1.
5. Repeat the titrations as many times as you think necessary to obtain accurate results.
6. Make certain that the recorded results show the precision of your 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 dm3

sulphuric acid.
3. Add, from the second burette, 4.00 cm3 of X. This oxidizes some of the Fe2+ that has been pipetted into the
flask.
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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 Fe2+ 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.
Final burette reading/ cm3
Initial burette reading/ cm3
Volume of A used/ cm3
Observations and
Results

25.50
0.50

26.20
1.00

25.40
1.00

28.80
3.60

0.00

4.00

8.00

12.00

Final burette reading/ cm3

20.00

22.50

20.00

Initial burette reading/ cm3

0.05

6.50

8.05

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


Volume of X added/ cm3

Volume of A added/ cm3


Copy and fill out the titration values
Data Analysis

Experiment 1
(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.

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(c) Use the half equations for the reaction


2++ 4 H 2 O (l)
yields Mn( aq )

++5 e
+8 H (aq )
MnO4 ( aq)

3++ e
2+ yields Fe(aq)

Fe(aq)

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.
(b) Draw the best-fit straight line through the plotted points.
(c) From your graph find the volume of X that reacts with the Fe2+ present in 25.0 cm3 of B.
Graph
Discussion

Conclusion

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Lab# 11

Skills Assessed:

Date:

Title

Theory

O/R/R
M/M
A/I
P/D

Chromatography
In this activity you will be experimenting with a technique called chromatography which will allow you to
visually demonstrate that the pigment in leaves is a combination of several different coloured pigments.
This technique is useful in that it can separate and identify the various components of mixtures, such as those
contained in plant pigments. A pigment is a substance that absorbs light at specific wavelengths, chlorophyll is
one of these pigments. Its green-yellow in colour is due to the absorption of red, orange, blue, and violet
wavelengths and the reflection of the green and yellow wavelengths. This occurs when white light (containing all
of the light wavelengths, or the entire spectrum of colours) shines on the leaf surface, all of the wavelengths are
absorbed except for the ones you see, which are green-yellow, those are the portions of the spectrum being
reflected.
If the conditions are identical, the relative distance moved by a particular compound is the same from one mixture
to another. This is why chromatography can be used to identify a compound. The actual identification requires a
simple calculation as shown below:
Distance travelled by componet
Rf =
Distance travelled by mobile phase
It is important to remember that several factors can influence the reliability of the Rf value, these include
humidity, temperature, solvent, pigment extract preparation, and the amounts of the material present. Values are
comparable only when the extracts are prepared in the same way and the chromatograms are prepared identically
and developed together in the same container.
Acetone is flammable (even the amount found in nail polish remover), keep it away from sparks or open flames.
Wear eye protection, especially if using pure acetone.

Aim

To separate the different pigments in plant leaves

Apparatus and
Material

1. Cone-type (size 4) coffee filter paper


(or Whatman #1 chromatography

Princes Town West Secondary Unit 2 Chemistry Labs

5. capillary tubes
6. fresh spinach
7. mortar and pestle
39 | P a g e

paper)
2. large glass jars
3. acetone
4. distilled water

8. clean sand

Procedure
:

1. Each lab group (or individual if not working in groups) will need 4 strips of filter paper, approximately 6
inches long and 1 inch wide, 2 chromatography development containers (500 ml beakers or large fruit jars
work well), 2 large rubber bands (able to stretch around the vessels from the mouth to the bottom of the
vessel), 2 solvents, water and either pure acetone, or nail polish remover.
2. Do the following with both fresh spinach leaves; tear leaf material and place in a glass container, cover with
acetone (this should be done the day before the actual lab activity). An alternative pigment extraction
technique is to use a
mortar and pestle. Place plant material the vessel, add a little clean sand, some acetone and then grind until a
dark green liquid appears. Both techniques yield very dark pigments with which to work. Be certain to keep
the pigments apart throughout the entire activity.
3. Place one of each solvents (water and acetone, or nail polish remover) in the chromatography vessels and
stretch a rubber band length-wise around each vessel. The rubber band will be the mechanism for hanging the
chromatography strips.
4. Make a pencil mark on each of the 2 chromatography strips, in the center, directly above the point of the strip,
about 1 inch from the tip of the paper. Using a capillary tube, or tooth pick, apply the plant pigment to each
filter paper strip. This is done by touching the tooth pick or capillary tube which has been dipped in the
pigment, to the pencil mark. Make an application, then wave the paper gently to dry it a little before the next
application. Be patient, you will need 12 to 15 applications.
5. By now you should have 2 strips with spinach pigment. Suspend one of each in each of the chromatography
development vessels. You can attach them with paper clips, or simply fold over a portion of the end and it
should hang in place. The tip of each strip should just touch the solvent.
6. Wait 20 to 30 minutes for the chromatograms to develop. Remove the chromatograms. Mark with a pencil

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(NOT a pen) where the solvent stopped as it moved up the chromatogram. This is called the solvent front.
Mark also where each pigment stopped moving up the chromatogram. Using the equation below, determine a
reference number for each pigment on the chromatograms. Depending on which chromatogram you are
viewing, you should see greens, yellow/yellow orange, and red. All measurements should be in mm. (Any
material which did not move from the
pencil dot is insoluble).

Observations and
Results

Data Analysis

Note: each pigment has a special name,


green = chlorophyll a or b
yellow/yellow orange = carotene
red = anthocyanin
brown = xanthophyll

1. Determine the Rf (ratio of fronts) value for each spot using the formula (remember there may be more than
one calculation per spot):
:

Rf =

Discussion

Conclusion

Distance travelled by componet


Distance travelled by mobile phase

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Lab# 12

Skills Assessed:

Date:

O/R/R
M/M
A/I
P/D

Title

Chromatography

Aim

To determine the various colours present in food colouring dye and ink pens using chromatography.

1.
2.
3.
4.
5.

Apparatus and
Material

Procedure

8" Aluminum pie plate


Toothpicks
Food coloring
Large Coffee filters
Pencil

6.
7.
8.
9.

Rubbing alcohol (70% Isopropyl Alcohol)


"Expresso" ink pens
Measuring cup
Ruler

1. Measure approximately 1cm from the edge of the coffee filter and mark eight evenly spaced lines around the
filter lightly with a pencil (do not use ink).
2. Use a toothpick to spot the four food colouring dyes on one-half of the coffee filter along the pencil mark. On
the other half, spot the filter using the pens. Allow each spot to dry and then re-spot two or three more times
3. After the coffee filter has been spotted, mark the top of each spot with your pencil. Below each spot, in pencil,
label the colour and if it is pen or food colouring. (Due to the small space below the spot, it may be easier to
label "p" for pen, "g" for green, etc.)
4. Place the spotted coffee filter "upside down" in the aluminium pie plate.
5. Fill the pie plate (the chromatographic chamber) with rubbing alcohol to a level just below the spots on the
filter.
6. Once the chromatogram has developed and the alcohol travels to the "top" of the coffee filter, remove the filter
from the plate. Using a pencil, mark the final position of the solvent. Click here to view a video of this
procedure.
7. Next place a pencil mark at the end of each colour. Note that some of the initial spots separated into multiple
colours- be sure to mark each colour
8. Allow the filter to air dry.
9. Determine and record the distance travelled by the mobile phase by measuring the distance (in mm) from the
top of each of the initial spots (original pencil marks) to the final position of the solvent

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10. Determine and record the distance travelled by each colour by measuring the distance (in mm) from the pencil
mark at the top of each of the initial spots to the mark indicating the end of each colour it produced.

Observations and
Results

Data Analysis

2. Determine the Rf (ratio of fronts) value for each spot using the formula (remember there may be more than
one calculation per spot):
:

Rf =

Discussion

Conclusion

Distance travelled by componet


Distance travelled by mobile phase

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Lab# 13

Skills Assessed:

Date:

Title

Solvent Extraction

Theory

Introduction:

O/R/R
M/M
A/I
P/D

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 acidbase titration. The dynamic equilibrium at the solvent boundary may be represented by eq. 2
CH
CH
[ 3 COOH ]ether eq .2
k1
[ 3 COOH ](aq)
k2

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),
CH
CH
k 2 [ 3 COOH ](ether ) eq .3
k 1 [ 3 COOH ](aq )=

and the equilibrium constant may then be defined in terms of solute concentrations or rate constants according to
eq. 4.

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CH
CH
[ 3 COOH ]( aq)=

k1
eq .4
k2

[ 3 COOH ](ether )

K =

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.

Apparatus and
Material

1.
2.
3.
4.
5.

Procedure

Observations and
Results

Aim

Graduated 100 cm3 measuring cylinder;


250 cm3 separating funnel;
Three 100 cm3 conical flasks;
10 cm3 pipette; 50 cm3 burette;
0.1 M sodium hydroxide solution;

6. Distilled water;
7. Diethyl ether;
8. 0.5 M aqueous ethanoic acid;
9. 0.125 M aqueous ethanoic acid;
10. Phenolphthalein indicator solution.

1. Using a measuring cylinder, add as accurately as possible 50 cm3 of 0.5 mol dm-3 aqueous ethanoic acid and 50 cm3 of
diethyl ether into a 250 cm3 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 cm3 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 cm3 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 cm3 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.

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Data Analysis

Treatment of Results
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 cm3 aliquot you titrated and, hence, evaluate the ethanoic 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

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Lab # 14

Skills Assessed:

Date:

Title

O/R/R
M/M
A/I
P/D

Plan Design: Analytical Chemistry

Contamination of drinking water supplies from industrial waste is a result of various types of industrial processes
and disposal practices. Industries that use large amounts of water for processing have the potential to pollute
waterways through the discharge of their waste into streams and rivers, or by run-off and seepage of stored wastes
into nearby water sources. From this information, is it possible to determine if effluents from ISPAT is sufficient to
cause adverse effects on the quality of drinking water.

Case

Hypothesis

Aim

Theory

Apparatus and
Material

Procedure

Variables

Expected
Observations and
Results

1.

2.

1.
2.
3.
4.

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Data Analysis

Precautions

1.
2.

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Lab # NA

Skills Assessed:

Date:

Title

Organic Chemistry

Aim

To distinguish between alkanes and alkenes

Theory

O/R/R
M/M
A/I
P/D

Alkanes are saturated compounds which are relatively inert. They undergo very few reactions which include
combustion, cracking and free radical substitution with halogens such as chlorine and bromine. Substitution
reaction requires the presence of UV light which is needed to split the inert halogens to from the reactive free
radicals.
Alkenes on the other hand, are unsaturated compounds which takes part in a wide range of addition reactions due
to the presence of the double bond in alkene molecules. The double bonds in alkenes are an electron rich centre
which allows it to undergo electrophilic reactions and react with oxidizing agents.
Alkenes decolorize a solution of bromine in 1, 1, 1 trichloroethane
CH3CCl3

:
C6H12 +
Hexene

Br2

reddish brown

C6H12Br2
colourless 1,2 dibromohexane

Alkenes decolorize an acidified solution of potassium manganate (VII)


KMnO4/H+

C6H12 +

Hexene

Apparatus and
Material

C6H12(OH)2
colourless hexane 1,2 - diol

1. 1 % bromine in 1,1,1 trichloroethane


2. 0.02 mol dm-3 KMnO4

Princes Town West Secondary Unit 2 Chemistry Labs

4. Samples of Hexane and Hexene labelled


A and B
49 | P a g e

3. Dilute H2SO4
Procedure

Observations and
Results

Data Analysis and


Interpretation

5. Test tubes

1. To 2 cm3 of sample A in a test tube, bromine was added drop by drop. Solution was stirred and
observations were made and recorded.
2. A few drops of dilute H2SO4 was added to 1 cm3 of KMnO4. The acidified KMnO4 was then added drop
by drop to another test tube containing 2 cm3 of sample A. The mixture was stirred and observations were
made and recorded.
3. Steps 1 and 2 were then repeated with sample B
Table 1
Observation table
Step
Sample A
On addition of Bromine
Solution turns colourless
On addition of acidified
Solution turns colourless
KMnO4.

Sample B
No visible reaction
No visible reaction

1. Deduce which sample is an alkane and which is an alkene


Sample A is an Alkene and Sample B is an Alkane.

2. Outline the mechanisms for any reactions which occurred.


Alkenes contain a double bond, which is an electron rich centre, and in the presence of bromine in 1, 1, 1trichloroethane, Br2 is added across the double bond, causing decolourization of the bromine solution
from brown to colourless, via an addition reaction.
CH3CCl3

C6H12 +
Hexene

Br2
reddish brown

C6H12Br2
colourless 1,2 dibromohexane

Alkenes react with potassium manganate(VII) solution. If the potassium manganate(VII) solution is

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acidified with dilute sulphuric acid, the purple solution becomes colourless. Manganate(VII) ions are a
strong oxidising agent, and they will oxidise the hexene to a diol, while the manganate(VII) ions are
reduced to manganese(II) ions.
Manganate (VII) ions are purple in solution whereas manganese(II) ions are colourless, and hence there
will be a colour change from purple to colourless in the presence of the alkene.
KMnO4/H+

C6H12 +

Hexene

C6H12(OH)2
colourless hexane 1,2 diol

Neither of these reactions will occur with the alkane, and so there will be no colour change in the
presence of the alkane.
Conclusion

Sample A is Hexene and Sample B is Hexane

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Lab # NA

Skills Assessed:

Date:

Title

Carbonyl Compounds

Aim

Investigating Carbonyl Compounds

O/R/R
M/M
A/I
P/D

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 Tollens and Fehlings reagents can oxidise aldehydes but not ketones. Hence this
reaction can be used to distinguish the both of them.
Tollens reagent forms a silver mirror on the wall of the test tube and Fehlings solution gives a red-brown
precipitate of Copper (I) Oxide.
Three samples are given, two of which are carbonyl compounds, one is an aldehye and the other is a ketone.

Apparatus and
Material
Procedure

1. Samples B, C and D
2. 2, 4 DNPH (dissolve 2 g of 2, 4- DNPH in 4 cm3 of
conc. H2SO4, 30 cm3 of methanol and 10 cm3 of water.

3.
4.
5.
6.

Fehlings reagent
Aqueous NH3 and AgNO3
Measuring cylinders
Test tubes

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.
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.

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Observations were recorded.


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

Observations and
Results

Data Analysis and


Interpretation

Table 1
Solution added
2,4- DNPH
AgNO3 and NH3

Sample B
Orange precipitate
formed
No visible reaction

Fehlings reagent

No visible reaction

Observations
Sample C
Orange precipitate
formed
Silver mirror formed
on test tube
Red-brown
precipitate

Sample D
No visible reaction
No visible reaction
No visible reaction

1. Deduce which of the samples are carbonyl compounds.


:

Sample B and Sample C are both Carbonyl compounds since they both reacted with 2, 4
dinitrophenylhydrazine to give an orange precipitate.
2. Deduce which of the samples is an aldehyde
Sample C is an aldehyde since it was oxidised by both Tollens 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:


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
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and Fehlings reagent.


These two tests are used to distinguish between an aldehyde and a ketone.
Discussion
:

Conclusion

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

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Lab # NA

Skills Assessed:

Date:

Title

Organic Compounds

Aim

To investigate the oxidation of alcohols

Theory

O/R/R
M/M
A/I
P/D

Primary alcohols are readily oxidised to carboxylic acids by a variety of oxidising agents such as acidified
potassium dichromate (VI).

Cr2O72- (aq) + 14H+(aq) + 6eOrange

2Cr3+ (aq) + 7H2O(l)


green

Primary alcohols are firstly oxidised to aldehydes and then to carboxylic acids. Secondary alcohols are oxidised
to ketones and tertiary alcohols are resistant to oxidation.
Apparatus and
Material

Procedure

1.
2.
3.
4.

Ethanol
5 g dm-3 Potassium dichromate (VI) solution
Test tubes
Water bath

5. Concentrated sulphuric acid


6. Measuring cylinders
7. Bunsen burner and tripod stand

1. 5 cm3 of ethanol was placed in a test tube.


2. To this tube, 2 cm3 of potassium dichromate (VI) solution was added, followed by 3-4 drops of
concentrated H2SO4
3. The tube containing this mixture was then placed in a water bath at 60 C and any colour change was recorded.
4. The mixture was then allowed to cool and the scent of vinegar was identified coming from the reaction
mixture.

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Observations and
Results

Table 1: Observations
On addition of potassium dichromate (VI)
solution
On addition of concentrated H2SO4 and heat

Solution in test tube turned orange colour


Colour change from orange

After cooling

Data Analysis and


Interpretation

Light green

yellow

blue

The scent of vinegar was noted and two layers


were present in the tube, one clear and the
other cloudy

1. Write equations for any reactions that occurred


An acidified dichromate ion readily accepts electrons and this makes it a powerful oxidising agent.
Cr2O72- (aq) + 14H+(aq) + 6eOrange

2Cr3+ (aq) + 7H2O(l)


green

Initially, the colour of the solution is orange due to the dichromate ions. On oxidation of ethanol, which is a
primary alcohol, an aldehyde is formed firstly.
Cr2O72-/H+

CH3CH2OH(aq)

CH3HC=O + 2H+ + 2e-

The aldehyde is further oxidised to a carboxylic acid, ethanoic acid.


CH3HC=O + H2O

CH3COOH + 2H+ + 2e-

2. Describe how this experiment can be scaled up to obtain a pure sample of ethanoic acid.

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Discussion

Discuss the principles on which the breathalyser test is based?.

Potassium dichromate, K2Cr2O7, is a yellow-orange compound. When alcohol vapour makes contact with the
yellow-coated crystals, the colour changes from yellow to green. The degree of the colour change is directly
related to the level of alcohol in the suspect's breath. The oldest breathalyzer models pass breath through a
solution of potassium dichromate, which oxidizes ethanol to acetic acid, changing color in the process
Cr6+

Orange
Conclusion

Cr3+
Green

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Lab # NA

Skills Assessed:

Date:

Title

Organic Compounds

Aim

To investigate the formation of esters

Theory

O/R/R
M/M
A/I
P/D

When an alcohol reacts with a carboxylic acid in the presence of concentrated sulphuric acid, an ester is formed.

RCOOH(l) + R OH(l)

RCOOR (l) + H2O (l)

The ester is recognised by its distinctive fruity smell.

Apparatus and
Material

Procedure

1.
2.
3.
4.
5.

Ethanol
Glacial ethanoic acid
Cold water
Bunsen burner and tripod
Boiling tube

1.
2.
3.
4.

5 cm3 of ethanol and 5 cm3 of ethanoic acid were placed in a boiling tube.
To this tube, 1 cm3 of concentrated H2SO4 was then added.
The tube containing this mixture was then placed in a water bath at 60 C and observations were made.
After heating the mixture in the water bath for 10 minutes, it was then poured into a beaker containing ice
cold water. Observations were made and recorded.

Princes Town West Secondary Unit 2 Chemistry Labs

6.
7.
8.
9.

Concentrated sulphuric acid


Measuring cylinders
Beaker
Water bath

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Observations and
Results

Data Analysis and


Interpretation

Table 1: Observations
On mixing ethanoic acid and ethanol
On addition of concentrated H2SO4 and heat
On pouring mixture in beaker containing
ice cold water

No visible reaction

No visible reaction
Two distinct layers were visible. The top layer
was insoluble and cloudy and a sweet fruity
smell was emitted.

1. Write equations for any reactions that occurred


Ethanol and Ethanoic acid react together to from an ester, ethyl ethanoate
:
CH3COOH(l)

+ CH3CH2OH(l)

CH3COOHCH2CH3(l)

+ H2O(l)

2. What is responsible for the smell obtained.


The formation of the ester, ethyl ethanoate, which has a fruity smell, is the compound that is responsible for the
fruity smell emitted during the reaction.

3. Why is the reaction mixture poured into cold water?

Discussion

Ethanoic acid + ethanol

ethyl ethanoate is a volatile ester with a characteristic fruity smell.


Ester formation is an example of a condensation reaction, where there is elimination of water, and
formation of the ester bond.

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Conclusion

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Lab # 15

Skills Assessed:

Date:

O/R/R
M/M
A/I
P/D

Title

Simple and Fractional Distillation

Aim

To compare the efficiency of separation of an ethanol- water mixture by simple and fractional distillation.

Simple distillation is used to separate volatile liquids from non- volatile ones with different boiling points. If the
boiling points difference between two liquids is less than 60 degrees, then fractional distillation is used instead.
Ethanol and water are miscible solvents whose boiling points are 78C and 100C respectively, and hence
fractional distillation is more appropriate for their separation.

Theory

Apparatus and
Material

Procedure
:

1. Simple and Fractional distillation apparatus


2. 50-50 mixture of ethanol and water
3. Thermometer

4. 50 cm3 measuring cylinder


5. Anti-bumping granules
6. Hot plate

1. The class was divided into two groups. One group carried out simple distillation and the other group
carried out fractional distillation. The information and data obtained by both groups were then shared
within the two groups.
2. The distillation apparatus was set up, using a measuring cylinder as the collecting vessel.
3. 50 cm3 of ethanol- water mixture together with some anti-bumping granules were added to the distilling
flask. The flask was then attached to the rest of the apparatus.
4. The distilling flask was placed on a hot plate
5. The temperature was recorded when the first drop of distillate came out.
6. The temperature was recorded for every 3 cm3 of distillate that came out
7. Distillation was stopped when there was about 5 cm3 of mixture in the distilling flask.

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Table 1 : Temperature readings for distillate collected during fractional distillation


Volume of Distillate / cm3
Temperature / C
1st drop
03
06
09
12
15
18
21
24
27
30

Observations and
Results

Table 2 : Temperature readings for distillate collected during simple distillation


Volume of Distillate / cm3
Temperature / C
03
06
09
12
15
18
21
24
27
30

1. Plot graph of temperature of distillate against volume of distillate for simple and fractional distillation on
the same axes.

Graph
Data Analysis

1. Use your graph to deduce which type of distillation separates the mixture better
2. Explain graph

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Data Analysis and


Interpretation
Discussion

Conclusion

:
:

1. Write a balanced equation for the reaction between hydrochloric acid and sodium hydroxide

How would heating more rapidly affect distillation?


What effect would using a longer column have on fractional distillation?

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Lab # 16

Skills Assessed:

Date:

Title

Organic Compound

Aim

To analyse substance X4

Theory

Sample X4 is an organic compound which contains four Carbon atoms.

Apparatus and
Material

Procedure

Observations and
Results

1.
2.
3.
4.

Sample X4
Bromine solution
Solid Na2CO3
Test tubes and test tube racks

O/R/R
M/M
A/I
P/D

5. 2, 4 DNPH
6. Bench reagents : AgNO3(aq), NH3(aq),
NaOH(aq), I2(aq)
7. Measuring cylinder

Bromine solution was added dropwise to 3 cm3 of sample X4 and observations were made and recorded
Solid Na2CO3 was added to 3 cm3 of sample X4 and observations were made and recorded
2, 4 DNPH was added dropwise to 3 cm3 of sample X4 and observations were made and recorded
Ammonia solution was added dropwise to 4 cm3 of AgNO3 until the precipitate that formed just re
dissolved. (Tollens Reagent). A few drops of Sample X4 was then added to this reagent. Any observations
made were recorded.
5. 2 cm3 of Iodine solution was added to 3 cm3 of sample X4 . NaOH was then added dropwise while gently
shaking. Any observations made were recorded.
1.
2.
3.
4.

Table 1: Observations and Inferences made during the experiment


Tests
Observations
Inferences
On addition of Bromine
solution
On addition of Solid
Na2CO3
On addition of 2,4
DNPH

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On addition of Tollens
Reagent
On addition of Iodine
Solution
Discussion

Conclusion

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Lab # 17

Skills Assessed:

Date:

O/R/
R
M/M
A/I
P/D

Title

: Plan Design: To determine the acidity / pH of a soil sample

Case

Soil pH is a measure of hydronium ion (H3O+, or more commonly the H+) activity
in the soil solution. Soil pH influences many facets of crop production and soil
chemistry, including availabilities of nutrients and toxic substances, activities and
nature of microbial populations, and activities of certain pesticides. Soils with pH
values below 7 are referred to as "acid" and those with pH values above 7 as
"alkaline"; soils at pH 7 are referred to as "neutral." Most crops grow best if the
: soil pH is between 6.0 and 7.5.
Mr. Smith, a farmer, wants to increase his yield of vegetables, but of lately, he
finds that his plants are not thriving well. His neighbour tells him that his soil
may be too acidic for the plants to grow well, and suggests that he test the pH of
his soil to confirm.
Plan and Design an experiment to test for the pH of the soil, using a pH meter.

Apparatus
and
Material
Procedure

1.
2.
3.
4.

pH meter
Electronic balance
Paper cups
Standard buffer solutions of pH 2, 4, 7
and 9 for calibrating pH meter

5.
6.
7.
8.

Pipettes
Soil sample
Deionized water
Stirrer

1. Calibrate the pH meter over the appropriate range using the standard
buffer solutions.
2. Weigh 5 g of sieved, air dried soil sample and place into a paper cup.
3. Add 5 ml deionized water to the sample of soil in the paper cup
4. Stir the sample for a minute, and then leave to settle for 30 minutes to
form a slurry

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5. After formation of slurry, place electrodes of the pH meter into the slurry
and read the pH, ensuring that the electrodes tips are in the slurry.
6. Repeat the above procedure at least twice for accuracy.

Observatio
ns and
Results

Discussion

Table 1 : Recorded pH of soil sample


Samples
Sample 1
Sample 2
Sample 3

Conclusion

pH

Which type of water (distilled, deionized, tap water) is preferred, and give
reasons why?
Theoretically, if the pH of a soil sample is 2, and you want to obtain the
optimum pH for best growth of crop, that is, a pH between 6.0 and 7.5,
what procedures can be done to this soil sample in order to achieve this
optimum pH?
Give two precautions that should be undertaken when carrying out your
experiment?

Lab # NA

Skills Assessed:

Date:

O/R/
R
M/M
A/I
P/D

Title

: Plan Design: To purify a sample of rock salt

Case

: Rock salt, also known as halite, or impure NaCl, is typically formed by the
evaporation of salty sea water which contains dissolved Na+ and Cl- ions, as well
as other impurities such as potassium and sulphates. Rock salt is also applied to

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road beds in cold climates to help reduce the freezing point of water on the road,
and since saline has a lower freezing point that water, putting rock salt on ice will
cause it to melt.
Table salt is essential for human life. A large amount of the commercially mined
rock salt is prepared for human consumption. Plan and design an experiment to
obtain pure NaCl, or table salt, from a sample of impure rock salt. Include how
you would be able to find the percentage of mass of salt crystals recovered from
the sample of rock salt.
Apparatus
and
Material

Procedure

Observatio
ns and
Results

1.
2.
3.
4.

Sample of rock salt


Balance / Scale
Filter paper and funnel
Bunsen burner

5.
6.
7.
8.

Conical flasks
Distilled water
Ice bath
Beakers

1. Weigh 10 g of the rock salt using the electronic balance


2. Place this sample in a beaker, and then dissolve it in a small amount of hot
water, while stirring the mixture
3. Weigh a sheet of filter paper and record this value
4. After dissolving the sample of rock salt, then filter the mixture, collecting
the filtrate in a conical flask
5. Allow the filtrate in the conical flask to cool by placing in into an ice
bath, to recrystallize the NaCl
6. Filter the crystals with distilled water to allow for any soluble impurities
to be removed
7. Wash, dry and weigh the crystals within the filter paper.

Table 1 : Mass of rock salt


Mass of rock salt / g
Table 2 : Mass of purified salt
Mass of filter paper and crystals / g
Mass of filter paper / g

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Mass of crystals / g

Data
Analysis

1. Mass of purified crystals (g)


= mass of filter paper and crystals (g) mass of filter
paper (g)
:

Discussion
Conclusion

:
:

2. Percentage by mass of salt crystals recovered from the sample of rock salt
mass of purified crystals(g)
=
x 100
mass of rock salt (g)

Lab # 18

Skills Assessed:

Date:

Title
Aim

Theory

O/R/
R
M/M
A/I
P/D

: Analytical Chemistry Back Titration


:

To determine the mass of 2-ethanoylhydroxy-benzoic acid in a commercial brand


of an aspirin tablet by back titration

: Aspirin is an analgesic compound which has to ability to reduce inflammation and


hence acts as both a pain killer and a fever reducer. The active ingredient in
aspirin tablet is 2-ethanoylhydroxy-benzoic acid (acetylsalicylic acid), the ester
linkage in aspirin is hydrolyzed/broken by alkalis to form ethanoate ions and 2-

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hydroxybenzoate (salicylate) ions.


CH3COOC6H4COOH + 2OH-

CH3COO- + HOC6H4COO- + H2O

An aspirin tablet can be hydrolyzed with excess sodium hydroxide and then back
titrated with hydrochloric acid. The amount of alkali used for the hydrolysis can
then be calculated and from this information, the mass of 2-ethanoylhydroxybenzoic acid in an aspirin tablet can be determined.

Apparatus
and
Material

Procedure
:

1.
2.
3.
4.

Aspirin tablets
Standard 0.2 mol dm-3 NaOH
Standard 0.1 mol dm-3 HCl
50 cm3 burette

5.
6.
7.
8.

25 cm3 pipette
3 conical flasks
Bunsen burner
Phenolphthalein indicator

1. 25 cm3 of NaOH was pipetted into a conical flask and one aspirin tablet
was added to this flask. The solution was then warmed gently to allow the
tablet to dissolve.
2. The solution was then cooled, and three drops of Phenolphthalein
indicator was then added to it.
3. This solution was then titrated with hydrochloric acid.
4. Steps 1 to 3 were then repeated until accurate results were obtained.

Table 1: Volume of HCl used in the titration


Observation
s and
Results

Final burette reading / cm3


Initial burette reading / cm3
Volume of HCl used / cm3

Rough
8.6
0.0
8.6

17.2
8.6
8.6

Accurate
25.8
34.3
17.2
25.8
8.6
8.5

25 cm3 of aspirin and NaOH required 8.6 cm3 of HCl in the titration.

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Discussion

1. Write a balanced equation for the reaction between hydrochloric acid and
sodium hydroxide
2. Calculate the number of moles of NaOH in the 25 cm3 of alkali used.
3. F ind the number of moles of HCl used in the titration
4. How many moles of NaOH reacted with HCl in the titration
5. How many moles of NaOH reacted with the 2-ethanoylhydroxy-benzoic
acid in one aspirin tablet.
6. Calculate the number of moles of 2-ethanoylhydroxy-benzoic acid in one
aspirin tablet.
7. Determine the mass of 2-ethanoylhydroxy-benzoic acid in one aspirin
tablet.

Conclusion

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Lab # 19

Skills Assessed:

Date:

Title

Environmental

Aim

To test for pollutants in water

Theory

O/R/R
M/M
A/I
P/D

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 SCN-, 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.

Apparatus and
Material

Procedure
:

1.
2.
3.
4.
5.
6.

Samples of Polluted water P, Q and R


0.1 mol dm-3 iron (III) nitrate solution
0.1 mol dm-3 ammonium molybdate
Solid iron (II) sulphate
Bunsen burner
spatula

7. Conc. H2SO4
8. Conc. HNO3
9. Bench HCl and H2SO4
10. Test tubes
11. Water bath

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

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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

Observations and
Results

Data Analysis and


Interpretation
:

Conclusion

Table 1 : Observations made during the experiment for all three samples P, Q
and R
Observations with:
2+
Fe(NO
)
Fe
/conc.
H2SO4
(NH4)2MoO4(aq)
HCl (aq)
3 3(aq)
(aq)
Sample
s
P
Q
R

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


Thiocyanate ions
Nitrate ions
Phosphate ions
Lead (II) ions
Justify your answers.

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Lab # NA

Skills Assessed:

Date:

O/R/R
M/M
A/I
P/D

Title

Plan and Design : Organic Chemistry

Aim

Organic

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.

Case

Apparatus and
Material

Procedure

Observations and
Results

Data Analysis and


Interpretation
Discussion

1.

2.

1.
2.
3.
4.
5.
6.

:
:

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Conclusion

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Lab # 20

Skills Assessed:

Date:

Title

Aim

O/R/R
M/M
A/I
P/D

Plan and Design : Analytical Chemistry (Gravimetric)

Caesium nitrate, CsNO3, decomposes on heating.

Case

The decomposition is represented by one of the following equations.


4CsNO3(s) 2Cs2O(s) + 4NO2(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, Vm, is 24.0 dm3 mol1 under room conditions.
Nitrogen dioxide, NO2, a toxic gas, is soluble in water.
Oxygen, O2, is not soluble in water.
[Ar; Cs, 133.0; N, 14.0; O, 16.0.]

Apparatus and
Material

Procedure

1.

2.

1.
2.

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3.
4.
5.
6.
Diagram

Observations and
Results

Data Analysis and


Interpretation
Discussion

Conclusion

:
:

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