Practical Exercise 02
Practical Exercise 02
Practical Exercise 02
Quantitative Analysis
ead through the whole method before starting any practical work. Where appropriate, prepare a table
R
for your results in the space provided.
Show your working and appropriate significant figures in the final answer to each step of your calculations.
1
In this experiment you will determine the percentage by mass of an impure sample of
sodium hydrogencarbonate, NaHCO3.
You will do this by titration with hydrochloric acid, HCl. The impurity in the sample is X. X is a
sodium compound which does not react with HCl.
(a) Method
Preparing a solution of FB 1
Titration of FB 3
● arry out as many accurate titrations as you think necessary to obtain consistent results.
C
● Make sure any recorded results show the precision of your practical work.
● Record in a suitable form below all of your burette readings and the volume of FB 2 added
in each accurate titration.
II
III
IV
VI
VII
VIII
[8]
(b) F
rom your accurate titration results, obtain a suitable value for the volume of FB 2 to be used
in your calculations.
Show clearly how you obtained this value.
(c) Calculations
(i) Give your answers to (ii), (iii), (iv) and (v) to the appropriate number of significant figures.
[1]
(ii) Calculate the number of moles of hydrochloric acid, HCl, in the volume of FB 2 calculated
in (b).
(iii) Complete and balance the equation for the reaction of sodium hydrogencarbonate with
hydrochloric acid. Include state symbols.
Deduce the number of moles of sodium hydrogencarbonate that reacted with the number
of moles of HCl calculated in (ii).
(iv) Use your answer to (iii) to calculate the number of moles of sodium hydrogencarbonate in
the FB 1 that you weighed out.
[Total: 14]
2 You will determine the percentage by mass of NaHCO3 in FB 1 again, this time by thermal
decomposition.
(a) Method
While the crucible is cooling, you may wish to begin work on Question 3.
● Reweigh the crucible and contents with the lid on. Record the mass.
● Heat the crucible and contents strongly for a further two minutes, without the lid.
● Replace the lid and leave the crucible and residue to cool for at least five minutes.
● Reweigh the crucible and contents with the lid on. Record the mass.
● Calculate and record the starting mass of FB 1 and the mass of residue obtained.
II
III
IV
[5]
(b) Calculations
(i) Calculate the number of moles of carbon dioxide produced during the thermal decomposition
of FB 1 by using the formula below.
(ii) Use your answer to (i) and the equation on page 6 to calculate the mass of sodium
hydrogencarbonate in the FB 1 you used in this experiment.
(iii) For this experiment calculate the percentage by mass of NaHCO3 in FB 1.
(c) (i) E
xplain why the crucible and contents were heated for a further two minutes after the first
weighing of the crucible and residue.
..............................................................................................................................................
..............................................................................................................................................
........................................................................................................................................ [2]
(ii) What assumption did you make about the behaviour of X when you carried out the
calculation?
..............................................................................................................................................
........................................................................................................................................ [1]
(iii) A
student suggested that it would have been more accurate to carry out the thermal
decomposition with the lid on the crucible throughout the experiment.
State and explain whether or not you agree with this suggestion.
..............................................................................................................................................
........................................................................................................................................ [1]
(iv) Suggest which of the two procedures, titration or thermal decomposition, gives a more
accurate value for the percentage by mass of NaHCO3 in FB 1.
Explain your choice.
..............................................................................................................................................
..............................................................................................................................................
........................................................................................................................................ [1]
[Total: 13]
Qualitative Analysis
Where reagents are selected for use in a test, the name or correct formula of the element or compound
must be given.
At each stage of any test you are to record details of the following:
3 (a)
FB 4 has the same composition as the residue obtained in Question 2.
It contains two sodium compounds, one of which is X.
Both anions present in FB 4 are listed in the Qualitative Analysis Notes.
(i) To a small spatula measure of FB 4 in a test-tube, add dilute nitric acid slowly.
Record your observations. Keep the solution produced for use in (ii).
..............................................................................................................................................
..............................................................................................................................................
........................................................................................................................................ [2]
(ii) To a 1 cm depth of the solution obtained in (i) in a test‑tube, add a few drops of aqueous
silver nitrate, followed by aqueous ammonia.
Record your observations.
..............................................................................................................................................
..............................................................................................................................................
........................................................................................................................................ [1]
(iii) Give the equation for one reaction taking place in (i). State symbols are not required.
........................................................................................................................................ [1]
(b) Dissolve the remaining FB 4 in a 5 cm depth of distilled water in a boiling tube. This solution is
FB 5.
(i) Carry out the following tests and record your observations.
Use a 1 cm depth of FB 5 in a test-tube for each test.
test observations
Add several drops of
aqueous copper(II) sulfate,
then
add dilute sulfuric acid.
[6]
(ii) To a 1 cm depth of FB 5 in a boiling tube, add an equal volume of aqueous sodium hydroxide
and warm carefully, then add a small piece of aluminium foil to the mixture.
Record your observations.
[1]
........................................................................................................................................ [1]
(iv) What can you deduce about FB 4 from the observation when methyl orange indicator was
added to FB 5?
........................................................................................................................................ [1]
[Total: 13]
reaction with
ion
NaOH(aq) NH3(aq)
ammonium, no ppt.
–
NH4+(aq) ammonia produced on heating
calcium,
white ppt. with high [Ca2+(aq)] no ppt.
Ca2+(aq)
green ppt. turning brown on contact green ppt. turning brown on contact
iron(II),
with air with air
Fe2+(aq)
insoluble in excess insoluble in excess
off-white ppt. rapidly turning brown off-white ppt. rapidly turning brown
manganese(II),
on contact with air on contact with air
Mn2+(aq)
insoluble in excess insoluble in excess
2 Reactions of anions
ion reaction
sulfate, gives white ppt. with Ba2+(aq) (insoluble in excess dilute strong acids)
SO42–(aq)
sulfite, gives white ppt. with Ba2+(aq) (soluble in excess dilute strong acids)
SO3 (aq) 2–
H He
hydrogen helium
Key 1.0 4.0
3 4 atomic number 5 6 7 8 9 10
Li Be atomic symbol B C N O F Ne
lithium beryllium name boron carbon nitrogen oxygen fluorine neon
6.9 9.0 relative atomic mass 10.8 12.0 14.0 16.0 19.0 20.2
11 12 13 14 15 16 17 18
Na Mg Al Si P S Cl Ar
sodium magnesium aluminium silicon phosphorus sulfur chlorine argon
23.0 24.3 3 4 5 6 7 8 9 10 11 12 27.0 28.1 31.0 32.1 35.5 39.9
19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
potassium calcium scandium titanium vanadium chromium manganese iron cobalt nickel copper zinc gallium germanium arsenic selenium bromine krypton
39.1 40.1 45.0 47.9 50.9 52.0 54.9 55.8 58.9 58.7 63.5 65.4 69.7 72.6 74.9 79.0 79.9 83.8
37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54
12
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
rubidium strontium yttrium zirconium niobium molybdenum technetium ruthenium rhodium palladium silver cadmium indium tin antimony tellurium iodine xenon
85.5 87.6 88.9 91.2 92.9 95.9 – 101.1 102.9 106.4 107.9 112.4 114.8 118.7 121.8 127.6 126.9 131.3
9701/34/O/N/18
55 56 57–71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86
lanthanoids
Cs Ba Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
caesium barium hafnium tantalum tungsten rhenium osmium iridium platinum gold mercury thallium lead bismuth polonium astatine radon
132.9 137.3 178.5 180.9 183.8 186.2 190.2 192.2 195.1 197.0 200.6 204.4 207.2 209.0 – – –
87 88 89–103 104 105 106 107 108 109 110 111 112 114 116
actinoids
Fr Ra Rf Db Sg Bh Hs Mt Ds Rg Cn Fl Lv
francium radium rutherfordium dubnium seaborgium bohrium hassium meitnerium darmstadtium roentgenium copernicium flerovium livermorium
– – – – – – – – – – – – –
57 58 59 60 61 62 63 64 65 66 67 68 69 70 71
lanthanoids La Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
lanthanum cerium praseodymium neodymium promethium samarium europium gadolinium terbium dysprosium holmium erbium thulium ytterbium lutetium
138.9 140.1 140.9 144.4 – 150.4 152.0 157.3 158.9 162.5 164.9 167.3 168.9 173.1 175.0
89 90 91 92 93 94 95 96 97 98 99 100 101 102 103
actinoids Ac Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
actinium thorium protactinium uranium neptunium plutonium americium curium berkelium californium einsteinium fermium mendelevium nobelium lawrencium
– 232.0 231.0 238.0 – – – – – – – – – – –
Examinations Copyright Acknowledgements Booklet. This is produced for each series of examinations and is freely available to download at www.cie.org.uk after
To avoid the issue of disclosure of answer-related information to candidates, all copyright acknowledgements are reproduced online in the Cambridge International
2
Safety
Supervisors are advised to remind candidates that all substances in the examination should be treated
with caution.
Only those tests described in the Question Paper should be attempted.
In accordance with COSHH (Control of Substances Hazardous to Health) Regulations, operative in the
UK, a hazard appraisal of the examination has been carried out. The following codes are used where
relevant.
C corrosive MH moderate hazard
HH health hazard T acutely toxic
F flammable O oxidising
N hazardous to the aquatic environment
The attention of Supervisors is drawn to any local regulations relating to safety and first aid.
Hazard Data Sheets should be available from your chemical suppliers.
Before the examination
1 Access to the Question Paper is NOT permitted in advance of the examination.
2 Preparation of materials
here quantities are specified for each candidate, they are sufficient for the experiments described
W
in the Question Paper to be completed.
In preparing materials, the bulk quantity for each substance should be increased by 25%
as spare material should be available to cover accidental loss. More material may be supplied if
requested by candidates, without penalty.
All solutions should be bulked and mixed thoroughly before use to ensure uniformity.
Every effort should be made to keep the concentrations accurate.
If the concentrations differ slightly from those specified, the Examiners will make the necessary
allowance. They should be informed of the exact concentrations.
3 Labelling of materials
aterials must be labelled as specified in these Confidential Instructions. Materials with an FB code
M
number should be so labelled without the identities being included on the label. Where appropriate
the identity of an FB coded chemical is given in the Question Paper itself.
4 Identity of materials
It should be noted that descriptions of materials given in the Question Paper may not correspond
with the specifications in these Confidential Instructions. The candidates must assume the
descriptions given in the Question Paper.
5 Size of group
In view of the difficulty of the preparation of large quantities of solution of uniform concentration,
it is recommended that the maximum number of candidates per group be 30 and that separate
supplies of solutions be prepared for each group.
Apparatus
1 In addition to the fittings ordinarily contained in a chemical laboratory, the apparatus and materials
specified below will be necessary.
2 ipette fillers (or equivalent safety devices), suitable eye protection and disposable gloves should
P
be used where necessary.
1 × 25 cm3 pipette
1 × 50 cm3 burette
2 × 150 cm3 or 250 cm3 conical flask
1 × 250 cm3 volumetric (graduated) flask
1 × 100 cm3 beaker
1 × burette stand and clamp
1 × funnel (for filling burette)
1 × white tile
1 × spatula
2 × teat / dropping pipette
1 × glass rod
1 × 15 cm3 crucible and lid
1 × crucible tongs
1 × pipe-clay triangle
1 × tripod
1 × heatproof mat
1 × Bunsen burner
1 × stopwatch (or sight of clock)
2 × boiling tube*
6 × test-tube*
1 × test-tube rack
1 × test-tube holder
1 × wash bottle containing distilled water
1 × pen for labelling glassware
paper towels
access to balance weighing to at least 0.1 g
*Candidates are expected to rinse and reuse test-tubes and boiling tubes where possible.
Additional tubes should be available.
Where balance provision is limited, some candidates should be instructed to start the examination
with different questions. See the current syllabus for balance : candidate ratio.
1 It is especially important that great care is taken that the confidential information given below does not reach the candidates either directly or
indirectly.
2
It should be noted that descriptions of substances given in the Question Paper may not correspond with the specifications in these Confidential
Instructions.
3 Particular requirements
per notes
hazard label identity
candidate (hazards given in this column are for the raw materials)
A mixture containing 75.0% by mass of NaHCO3 and 25.0% by mass
impure sodium of NaCl. The two solids should be thoroughly ground together using
FB 1 6.4–6.6 g
hydrogencarbonate a mortar and pestle.
Each candidate will require 6.4–6.6 g in a stoppered container.
9701/34/CI/O/N/18
4
Dilute 52.5 cm3 of 2.00 mol dm–3 HCl in each dm3 of solution.
A mixture containing 75.0% by mass of Na2CO3 [MH] and 25.0% by
mixture of anhydrous
mass of NaCl. The two solids should be thoroughly ground together
[MH] FB 4 1.0–1.2 g sodium carbonate and
using a mortar and pestle. Each candidate will require 1.0–1.2 g in a
sodium chloride
stoppered container.
aqueous
[C][N] 5 cm3 0.2 mol dm–3 copper(II) sulfate Dissolve 49.9 g of CuSO4.5H2O [MH][N][C] in each dm3 of solution.
copper(II) sulfate
[T][C]
[N][F] methyl orange
10 cm3 methyl orange indicator See preparation instructions in the current syllabus.
[MH] indicator
[HH]
4 The reagents below should also be provided. Unless otherwise stated, each candidate should require no more than 10 cm3 of any of these
© UCLES 2018
reagents. If necessary, they may be made available from a communal supply: however, the attention of the Invigilators should be drawn to the
fact that such an arrangement may lead to contamination of reagents and enhance the opportunity for malpractice between candidates.
[C][MH]
aqueous ammonia
[N]
–3
or
0.1 mol dm–3 barium nitrate
5
0.05 mol dm–3 silver nitrate
[MH] limewater
acidified aqueous
[MH]
potassium manganate(VII)
red and blue litmus papers, aluminium foil for testing nitrate/nitrite, wooden splints and the apparatus normally used in the Centre for use with
limewater in testing for carbon dioxide
[Turn over
Cambridge International AS and A Level Chemistry 9701 syllabus Practical assessment
Details of the specific requirements for apparatus and materials for a particular examination are given in the
Confidential Instructions which are sent to Centres several weeks prior to the examination. Centres should
contact Cambridge if they believe the Confidential Instructions have not been received.
Access to the question paper itself is not permitted in advance of the examination.
It is essential that absolute confidentiality be maintained in advance of the examination date: the contents of
the Confidential Instructions must not be revealed either directly or indirectly to candidates.
The Confidential Instructions describe information required by the Examiners. This will include a set of
numerical results for the experiments, which the Supervisor should obtain out of sight of the candidates.
A Supervisor’s Report Form is included in the Confidential Instructions. Centres must complete this form
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the apparatus available, enquiries should be sent to the Product Manager for Chemistry at Cambridge, using
either email ([email protected]), fax (+44 1223 553558) or telephone (+44 1223 553554).
Detailed guidance on preparing the standard bench reagents and indicators will not be given in the
Confidential Instructions. The Confidential Instructions will refer Supervisors to the following guidance notes
in this syllabus document. The following hazard codes are used where relevant.
The attention of Centres is drawn to any local regulations relating to safety, first-aid and disposal of
chemicals. ‘Hazard Data Sheets’ should be available from your chemical supplier.
Guidance for the preparation of reagents for qualitative analysis and indicators