Lab Skills and Notes
Lab Skills and Notes
Chemistry
9701
Name : . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Grade : . . . . . . .
Volumetric Analysis
Reading burettes
The last digit is recorded as follows:
23
24
| P ag e 2
The last digit is recorded as :
5 if between divisions. ( 22.15, 23.55, 27.35, …. and so on) if the line with bottom of
meniscus is mid-way between two divisions
23
24
| P ag e 3
Mean titre: choose either identical value or concordant (consistent) i.e those that
differ by no more than 0.10 cm3
In a titration with a sharp end-point, titres should be within 0.10 cm3.
What is the average titre of the following titres 23.80 cm3, 23.30 cm3 and
23.20 cm3?
Ans: The mean titre is the average of the 2nd and 3rd titres
which agree to within 0.1 cm3.
23.30 23.20
Ans : = 23.25 cm3
2
| P ag e 4
Errors in measuring the volume
Burettes
The maximum error (uncertainty) is half a division on either side of the
smallest unit on the scale.
2 0.05
% error = 100 for 2 readings ( initial & final burette readings)
Vtitre
meniscus
39.35 cm3
| P ag e 5
Individual errors are in opposite directions?
If the error on one burette reading is – 0.05 cm3 and + 0.05 on the other burette
reading is, or
| P ag e 6
Volumetric flasks
The tolerance (maximum error) for grade B 250cm3 volumetric graduated flask is 0.2 cm3.
The error is the same every time when the flask is filled correctly to the graduation mark.
The volume of the solution may be 250– 0.2 = 249.8 cm3 or 250.2 cm3
| P ag e 7
Measuring Cylinders
A measuring cylinder has a maximum error of half a division.
0.5
% error = 100
Vmeasured
0.5
Close up view % error = 100
43
= 1.16% for a single measurement.
| P ag e 8
How many significant figures should be used?
The result should contain the same number of significant figures as the measurement that
has the smallest number of significant figures.
For the significant figure analysis
You already know the rules for significant figures.
Multiplication and division: The result must have the same number of significant
figures as the smallest of the number of significant
figures for any value used in the calculation.
Addition and subtraction: The result will have a last significant digit in the same
place as the left-most of the last significant digits of all
the numbers used in the calculation.
If you add two measurements the result CANNOT be more precise than your measures.
Mass of empty container: 2.3 g
Mass of container with copper: 22.54 g
| P ag e 9
“Weighing by difference”.
Weigh an empty weighing bottle or a boiling tube.
Weigh the bottle + sample of solid
Transfer the weighed solid to a beaker and add about 100 cm3 of distilled water to
dissolve it completely.
Weigh the weighing bottle + any remaining solid.
[By subtraction, determine the amount of solid transferred to the beaker]
| P ag e 10
Preparation of a standard solution from a Solid ( by weighing)
A standard solution is one whose concentration is accurately known [to a very high level of
precision].
Weight out the mass of solute required accurately method
Dissolve the solid completely in a small amount of distilled water (use a glass rod to
stir).
Transfer the solution from the beaker to a volumetric flask via a funnel.
Rinse the beaker, the glass rod and the funnel with distilled water.
Add all the washings from the beaker, the funnel and the glass rod to the volumetric
flask.
Make up (top up) the solution to 1 cm below the etched mark on the neck of
the volumetric flask.
Use a dropper and carefully add distilled water until the bottom of the
meniscus is on the mark.
Stopper the flask and invert several times to ensure that the final solution is
homogeneous or well mixed.
A good primary standard acid is sulphamic acid (H2NSO3H) – whereas HCl and H2SO4 are
not suitable as they are not solids at room temperature.
| P ag e 11
Suggest why hydrochloric acid cannot be made up as an accurate (standard)
solution from pure hydrogen chloride.
Ans : Hydrogen chloride cannot be weighed as it is a gas
This means it is always lost due to evaporation or diffusion.
You are provided with a clean, dry weighing bottle containing 2.45 g of pure
anhydrous sodium carbonate, Na2CO3.
Describe how you would prepare exactly 250 cm3 of a standard solution containing
all of this sodium carbonate.
A chemist is required to make up accurately 500 cm3 of a 0.0500 mol dm–3 standard
solution from anhydrous sodium carbonate, Na2CO3
(a) What mass of anhydrous sodium carbonate Na2CO3 is required?
(b) Describe the steps necessary to make up this standard solution.
(c) What volume of 0.080 mol dm–3 HCl would be required to react completely with
25.0 cm3 of the standard sodium carbonate solution?
Na2CO3 + 2HCl
2NaCl + CO2 + H2O
= 50 cm3
Therefore, dilute 50 cm3 of the conc. (2.0M) to a final volume of 500 cm3 [by adding 450 cm3
of distilled (de– ionised) water.
Fill a clean, dry burette with the more concentrated standard solution
Run the calculated volume of the more concentrated standard solution into a clean
volumetric flask.
C final V final
Vinitial =
Cinitial
| P ag e 12
Titration
Preparation of burette
A burette is washed with distilled water and then with the solution going into it
Rinse the burette thoroughly with distilled water to remove any previous impurities.
Using a funnel, add a few cm3 of the solution and run through the burette (to remove
any distilled water–which would alter the concentration of the solution)
Close the tap again, fill the burette with solution through a funnel, and remove the
funnel and run off a little of the solution through the tap to remove any air bubbles
[Hit the tip of the burette while the solution is flowing to remove any air bubbles]
Note the level of the bottom of the meniscus to the nearest 0.05cm3
Your eye must be level to the bottom of the meniscus & the burette must be vertical.
Accurate
st
Rough 1 2nd 3rd etc
Final burette Reading/ cm3
Final burette Reading/ cm3
Titre/cm3
| P ag e 13
T.A Aoudi 2012- 2013
How?
Quickly run the solution in the burette into the conical flask with constant swirling until the expected
permanent colour change is observed.
[go to the end – point quickly].
| P ag e 14
Accurate titration: Concordant titres
Add the solution from the burette until the end point is reached
Repeat (for accuracy)
P Pipette: Rinse out a pipette with one of the solutions and (using a pipette
filler)
Use the pipette to transfer the volume ( e.g 25.0 cm3) of aqueous
solution A (e.g HCl) into a clean conical flask.
I Indicator : Add 2-3 drops of an indicator (if necessary) and place on a white tile
under the burette
Rinse out the burette with the other solution and fill the burette.
T Techniques :Run quickly enough of solution B (e.g NaOH) from the burette to
the solution in the flask with swirling & rinsing in the drops solution
sticking to the sides & in the neck of the conical flask with distilled water.
Then dropwise when close to the end-point.
E End point: Add solution B from the burette one drop at a time UNTIL ONE
DROP causes a permanent colour change (lasts for 30 seconds).
C Consistency Repeat the titration at least 2-3 times till I get concordant
readings / or titres that agree to within 0.05 cm3 to 0.2 cm3
or better.
| P ag e 15
Conical flask preparation
A conical flask is washed with distilled water ONLY
Rinse the conical flask with distilled water.
The flask should NOT be washed with the solution that will go in it because . . .
This will increase the number of moles of solute inside the flask and the titre will less.
| P ag e 16
Preparation of pipette ( 10.0cm3, 25.0 cm3…etc)
A pipette is washed with distilled water and then with the solution going into it.
Any water in the pipette will change the concentration of the solutions measured out.
1. Use a safety pipette filler (bulb) to fill the pipette a little bit above the calibration
mark. [Make sure that there are no air bubbles].
2. Remove the bulb and immediately cover stem with finger.
3. Wipe off the tip and the stem to free it of adhering liquid.
4. Adjust the level of meniscus to the calibration mark.
5. Place the pipette tip well within the conical flask and allow the liquid to
drain freely.
6. Rest the tip against the inner wall of the conical flask (receiver) for 10 seconds.
2.
4.
6.
| P ag e 17
Typical human or Personal errors
In a titration of a strong base with a strong acid, the following procedure was used:
1. A burette was rinsed with water and then filled with the standard acid.
2. A pipette was rinsed with some base solution.
3. A conical flask was rinsed with some base solution.
4. A pipette was used to transfer a measured volume of base solution into the conical flask.
5. Indicator was added to the base sample and it was titrated to the endpoint with the acid.
| P ag e 18
Answered Basic Questions
Sulfuric acid H2SO4 reacts with sodium hydroxide (NaOH) to form sodium sulfate and water.
When 0.1mol.dm–3 of sulfuric acid H2SO4 (aq) in a burette was titrated against 10.0cm3 of
sodium hydroxide in a flask, the following results were obtained.
Answer An average of these concordant results : 24.90 , 25.00 & 24.90 cm3 is
Since all agree to within 0.1 cm3.
| P ag e 19
3. A 1.62 g sample of impure sodium carbonate was dissolved in distilled water and then
made up to 250 cm3. 25.0 cm3 of this solution was put into a conical flask and three drops
of methyl orange indicator added. This was titrated against a 0.105 mol dm–3 solution of
hydrochloric acid until the end point was reached. The titration was repeated three more
times.
1 2 3 4
Burette reading (final) 25.30 25.30 25.85 25.95
Burette reading (at start) 0.00 0.50 0.75 1.25
Titre/cm3 25.30 24.80 25.10 24.70
....2.....T
...h..e..n...r..i.n..s..e...i.t..w
...i.t.h
....h..y..d..r..o..c..h..l.o..r..i.c...a..c.i.d............................................... [2]
(ii) Describe the colour change that tells when the end point has been reached.
......T
...h..e...s.o..l..u..t.i.o..n....w..i..l.l..g..o...f.r..o..m
....y..e..l.l.o..w
....t.o...o..r..a..n..g..e...(...p..e..a..c.h
...) ...................... [2]
(b) (i) Select the appropriate titres and calculate their mean.
(ii) Calculate the amount (in moles) of hydrochloric acid solution in the mean titre.
| P ag e 20
(iii) Calculate the amount (in moles) of pure sodium carbonate in 25.0 cm3 of solution.
Na2CO3 + 2HCl
(iv) Calculate the amount (in moles) of pure sodium carbonate in 250 cm3 of solution.
25.0 cm3 of 0.40 mol dm–3 samples of the sodium carbonate solution were titrated against aqueous
hydrochloric acid using methyl orange indicator.
Na2CO3 + 2HCl
2NaCl + H2O + CO2
The results of three titrations (in cm3) were: 29.10, 28.60 and 28.70.
| P ag e 21
1. Refer to the burette readings in Table below.
solution B, is aqueous M2CO3 of concentration 5.00 g dm–3 , where M is a Group 1 metal;
solution C, is aqueous hydrochloric acid of concentration 0.100 mol dm–3
M2CO3(aq) + 2HCl(aq)
2MCl(aq) + CO2(g) + H2O(l)
1 2 3 4
(a) List the numbers of the titrations that you will use to calculate the mean titre.
(c) Calculate the amount (number of moles) of hydrochloric acid in the mean titre.
(d) Calculate the amount (number of moles) of M2CO3 in 25.0 cm3 of solution B.
(e) Calculate the concentration of M2CO3 in solution B in mol dm–3 . Use this value
to calculate the relative molecular mass of M2CO3 and then identify M.
(f) When properly used, the pipette used in the experiment will deliver a volume of solution
B within 0.5% of 25.0 cm3. Suggest two techniques which a student should follow when
using the pipette to ensure that the volume delivered is within 0.5% of 25.0 cm3
| P ag e 22
Back titration
Back titration is used when the substance is unsuitable for direct titration. CaCO3 is not soluble in
water.
CaCO3 is made to react with excess acid. The titration (with alkali) then allows the amount of acid
which has not been used up reacting with the CaCO3 to be worked out.
n of HCl reacted
= n
total of HCl
(original)
– n ofreacted
excess HCl
with
with CaCO3
NaOH
4.0 g sample of dry CaCO3 and CaCl2 mixture was dissolved in 25.00 cm3 of 0.8 M HCl
solution. What was the percentage of CaCO3 in original sample, if 20.00 cm3 of 0.2 M
NaOH was used to titrate excess HCl?
Calculate the % of CaCO3(s) in the sample.
During titration n NaOH = 0.2 × 20.00 1000
= 4.0 × 10–3 mol
NaOH(aq) + HCl(aq)
NaOH(aq) + H2O(l)
CaCO3(s) + 2HCl(aq)
CaCl2(aq) + H2O (l) + CO2(g)
1 2
moles of CaCO3 (s) = 0.016 mol × ½
= 8.0 ×10–3 mol of CaCO3
So
Mass of CaCO3 (s) = n×M
= (8.0 ×10–3 ) × 100 g.mol–1
= 0.8 g
% CaCO3(s) = 0.8/4.0× 100
= 20%
| P ag e 23
A student carried out an experiment to find the percentage of calcium carbonate, CaCO3, in a
sample of limestone following his own plan. The student’s account of the experiment, results and
calculation of the mean titre are given below.
Account
Equation
III The acidic solution in the beaker was filtered into a 250 cm3
volumetric flask. A small amount of solid impurity remained in the
filter paper. The solution in the volumetric flask was carefully made
up to 250 cm3 with distilled water.
Results
1 2 3
Burette reading (final) 14.90 15.40 30.25
Burette reading (at start) 0.00 0.05 15.40
Titre / cm3 14.90 15.35 14.85
| P ag e 24
(a) The accuracy of the student’s method was judged to be poor by his teacher. The
teacher suggested that the procedure in II could be improved and that the titres used to
calculate the mean were incorrectly chosen.
(i) Suggest, with a reason, one improvement to the student’s procedure in II.
Improvement...
.....U...s.e...p..i.p..e..t..t.e...o..r..b
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...d..e..r...
....
....O
...R
....U
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....v..a..l.i.d...m
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...g...o..r..a..c..i.d... s.p..r. ay.
Reason......
....A
....P...ip...e.t.t..e..i.s...m
...o..r.e...a..c..c.u...r.a..t.e.......................................................
..................................................................................................................... (2)
(i) Recalculate a value of the mean making clear which titres you choose and giving
your answer to an appropriate number of significant figures.
(b) (i) Using your answer to (a)(ii), calculate the amount (number of moles) of sodium
hydroxide in the mean titre.
14.90
0.100 × = 0.00149 mol (1)
1000
(ii) Hence state the amount (number of moles) of hydrochloric acid in a 25.0 cm3
portion of the acidic solution transferred in IV.
Number of moles HCl transferred = answer to (i) = 0.00149 mol
(1)
(iii) Hence calculate the amount (number of moles) of hydrochloric acid remaining
after the reaction in II.
Number of moles HCl remaining = answer above × 10 = 0.0149
(iv) Calculate the number of moles of hydrochloric acid transferred to the beaker in
II.
50
× 2.00 = 0.100 mol (1)
1000
(v) Hence calculate the amount (number of moles) of hydrochloric acid used in the
reaction in II.
Answer to (iv) - answer to (iii)
| P ag e 25
(vi) Hence calculate the amount (number of moles) of calcium carbonate and the
mass of calcium carbonate in the sample of limestone,
{Mr (CaCO3) = 100}.
Answer to (v) ÷ 2
0.08512 ÷2 = 0.0425
0.0425 × 100 = 4.25 g
(2)
(vii) Hence calculate the percentage of calcium carbonate by mass in the sample of
limestone.
Mass of CaCO3
× 100%
Mass of sample
(c) The burette used in the titrations had an uncertainty for each reading of ±0.05 cm3.
Suggest one reason why a student may obtain volumes outside the uncertainty of the
burette when carrying out a titration.
......m...i.s..s.i..n..g...e.n...d..-.p...o..i.n..t..o..r...l.e..a..k..i.n..g...t..a..p..,.............................................................................
not reading meniscus at eye-level or bubble below tap air lock below
...t.a..p
..../..f.u..n..n ...e.l...l.e..f.t..i.n....t.o..p...o..f..b...u..r..e.t..t.e.../..b..u..r..e..t.t..e..n
...o..t..v..e..r.t..i.c..a..l ....................................... (1)
An indigestion tablet was known to contain calcium carbonate, CaCO3, as the active
ingredient (to neutralise stomach acidity). The tablet of mass 1.23g was added to 25.0 cm3
of 1.50 mol .dm–3 hydrochloric acid (an excess).
After complete reaction, the mixture was transferred to a volumetric flask and distilled
water was added to make the volume 250cm3. When a 25.0cm3 portion of this solution was
titrated with 0.050M sodium hydroxide, 49.4cm3 of the NaOH solution was required to
reach the end-point.
| P ag e 26
FA 3 is crushed impure calcium carbonate, CaCO3.
FA 4 is 0.500 mol dm–3 hydrochloric acid
FA 5 is 0.280 mol dm–3 sodium hydroxide.
You are to determine the percentage purity of calcium carbonate by dissolving a measured
mass of FA 3 in a known volume of hydrochloric acid, which is in excess.
The hydrochloric acid remaining after all the calcium carbonate has dissolved can be
determined by titration with aqueous sodium hydroxide, FA 4.
You may assume that any impurity present in the calcium carbonate does not react with
hydrochloric acid.
(a) Method – Read through the instructions before starting any practical work.
• Weigh and record the mass of an empty boiling-tube.
• Add to the boiling-tube between 2.60 g and 2.80 g of FA 3.
• Reweigh the tube and its contents.
• In part (b) of the method you will tip the FA 3 into hydrochloric acid, then re-weigh
the tube and any residual FA 3.
In the space below record, in an appropriate form, all of the balance readings and the
mass of FA 3 used in the experiment.
Expected Answer
| P ag e 27
Titration
• Fill a burette with FA 5.
• Pipette 25.0 cm3 of FA 6 from the graduated flask into a conical flask.
• Add to the flask a few drops of the acid-base indicator provided.
• Place the flask on a white tile.
• Titrate the acid in the flask with FA 5.
You should perform a rough titration.
In the space below record your burette readings for this rough titration.
Run 1
Sample
Burette reading (final) /cm3 36.00
3
31.5 0 cm
The rough titre is ..............................................
• Carry out as many accurate titrations as you think necessary to obtain consistent results.
• Record in a suitable form below all of your burette readings and the volume of FA 5 added in
each titration.
• Make certain any recorded results show the precision of your practical work.
(c) From your titration results obtain a suitable value to be used in your calculation.
Show clearly how you have obtained this value.
Expected Answer
NOTE
Must be to nearest
0.05 cm3
29.70 + 29.60 + 29.70
Average titre = = 29.67 = 29.70 cm3
3
3 29.70 cm3 3
25.0 cm of FA 6 required .................................. cm of FA 5.
| P ag e 28
(d) Calculations
Show your working and appropriate significant figures in the final answer to each step
of your calculations.
(i) Calculate how many moles of sodium hydroxide are contained in the volume recorded in
(c).
Expected Answer
Moles of NaOH = C × V
= 0.280 × 29.70 1000
= 8.32 × 10–3 (3 s.f)
8.32 × 10–3
................................................................. mol of NaOH
(ii) Deduce how many moles of hydrochloric acid reacted with the sodium hydroxide in (i) and
calculate how many moles of hydrochloric acid were present in the 250 cm3 graduated flask
labelled FA6.
NaOH(aq) + HCl(aq)
NaOH(aq) + H2O(l)
Expected Answer
250
Moles of HCl present in the 250 cm3 flask FA6 = × 8.32 × 10–3 mol
25
8.32 × 10 –2 mol
.............................
(iii) Calculate how many moles of hydrochloric acid were present in 250 cm 3 of FA4.
250 cm3 of FA4 contained ....................................... mol HCl.
Moles of HCl = C × V
= 0.50 × 250 1000
= 0.125 mol
| P ag e 29
(iv) Calculate the following.
This is the amount of hydrochloric acid that reacted with the calcium carbonate in
the weighed sample of FA 3.
0..0
… 42..0...m
.… ...o..l...... mol of HCl reacted with the calcium carbonate in .....2....6..0 ..... g FA3.
(v) Use your answer to (iv) to calculate the mass of calcium carbonate that reacted
with hydrochloric acid.
This is the mass of pure CaCO3 in the weighed sample of FA3.
CaCO3(s) + 2HCl(aq)
CaCl2(aq) + CO2(g) + H2O(l)
= ½ × 0.0420 mol
= 0.021 mol
Mass of of CaCO3 = n × Mr
= 0.021 × 100
= 2.10 g
2.10 g
% of Pure CaCO3 = × 100 = 80.7%
2.60 g
| P ag e 30
(e) 6.25 g of pure calcium carbonate are required to neutralise all the hydrochloric acid in
250 cm3 of FA4.
You were instructed to measure a mass between 2.60 g and 2.80 g of FA3 in this
experiment.
What difficulties might you encounter if you used a mass of about 5.50 g of FA3 in this
experiment?
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..o
...u..l.d...b..e...t.o
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...R
...n
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..r...t.h..e...t.i.t..r.a..t.i.o
..n
.........
too fast effervescence(fizzing) or the acid is lost as it sprays
................................................................................................................................... [1]
The balance used in the experiment displays the mass to ...........2..............decimal places.
(ii) Calculate the maximum percentage error in the mass of FA3 measured in (a).
0.02
The maximum error in the mass of FA 3 is ...........................
× .........
100 .... %. [2]
2.60
(g) (i) The percentage of calcium carbonate in the weighed sample of FA3 can also be
found by investigating the thermal decomposition of the compound into calcium
oxide and carbon dioxide.
Write a balanced equation, including state symbols, for this thermal decomposition.
Answer
CaCO3(s)
heat
CaO(s) + CO2(g)
| P ag e 31
(ii) Briefly outline the key measurements to be made in order to find the percentage
of calcium carbonate in FA 3 by this method.
1.
....W
...e
..i.g
..h...a
..n
..d
...r.e
..c..o
..r.d
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..-.t.u
..b
..e
..........................................
2.
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...w
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..b
..e
................................
3.
...R
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..w
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...a..s..s..o
..f..t.h
..e
...b
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....C..a..C
...O
...3.(.s..)........
4.
....H
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...t.h
..e
...b
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..m
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..a
..C
...O
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5.
....R
...e..h..e..a..t.,..c..o..o..l.a
..n
..d
...r..e..w
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..m
...p
..o
..s..i.t.i.o..n...i.s...c.o
..m
...p..l.e..t.e...................
6. .....i...e...t.o...c.o
..n
..s..t.a
..n
..t..m
...a..s..s...........................................................................................
(You do not have to use all of the numbered steps in your answer) [2]
[Total: 14]
| P ag e 32
June 2009/ 32
You are provided with the following.
FB1 is 0.023 mol dm–3 potassium manganate(VII), KMnO4.
FB2 is aqueous ethanedioic acid, H2C2O4, made by dissolving the hydrated salt,
H2C2O42H2O.
Dilution of FB2
(a) By using a burette, measure between 42.50 cm3 and 43.00 cm3 of FB2 into the 250 cm3
graduated flask, labelled FB3.
Record your burette readings and the volume of FB 2 added to the flask in the space
below.
Make up the contents of the flask to the 250 cm3 mark with distilled water. Place the
stopper in the flask and mix the contents thoroughly by slowly inverting the flask a
number of times.
Titration
Pipette 25.0 cm3 of FB3 into a conical flask. Use the measuring cylinder provided to
add to the flask 25 cm3 of 1.0 mol dm–3 sulfuric acid and 40 cm3 of distilled water.
Put the thermometer in the flask and heat the solution until the temperature is just over
65 °C.
Carefully remove the thermometer and place the hot flask under the burette. If the neck
of the flask is too hot to hold safely, use a folded paper towel to hold the flask.
| P ag e 33
Run in 1 cm3 of FB1. Swirl the flask until the colour of the potassium manganate(VII)
has disappeared then continue the titration as normal until a permanent pale pink colour
is obtained. This is the end-point.
If a brown colour appears during the titration, reheat the flask to 65°C. The brown
colour should disappear and the titration can be completed as above.
If the brown colour does not disappear on reheating, discard the solution and start
the titration again.
Perform a rough (trial) titration and sufficient further titrations to obtain reliable
results.
Record your titration results in the space below. Make certain that your recorded results
show the precision of your working.
Burette reading (final) / cm3 33.50 26.95 29.10 at least two titres
within 0.1 cm3
Burette reading (initial) /cm3 8.50 3.55 5.60
(b) From your titration results obtain a volume of FB1 to be used in your calculations. Show
clearly how you obtained this volume. [1]
23.40 + 23.50
Average titre of FB1 = = 23.45 cm3
2
Calculations
Show your working and appropriate significant figures in the final answer to each step of
your calculations.
(c) Calculate how many moles of KMnO4 were run from the burette into the conical flask.
n = C × Vaverage
= 5.40 × 10–4
–4
5.40 × 10
………………… mol of KMnO4 were run from the burette into the conical flask.
| P ag e 34
Put the correct number of electrons into each of the following half-equations to balance
the electrical charges.
MnO 4– + 8H+ 5 e–
+ ……
Mn2+ + 4H2O
C2O42–
2CO2 2 e–
+ ……
Calculate how many moles of ethanedioate ions, C2O 2–, reacted with the KMnO run
4 4
from the burette.
2MnO4– + 5 C2O4 2– . . . .
etc
5.40 × 10–4 ?
5
Amount of C2O42– = 5.40 × 10–4 × = 1.35 × 10–3 mol
2
1.35 × 10–3
………………… mol of ethanedioate ions reacted with the KMnO4 run from the burette.
1.35×10–3
C= = 0.0540 mol.dm– 3
25.0 1000
The concentration of C O 2– 5.40 × 10–2 –3
2 4 in FB3 is ……………………….. mol dm .
? 42.5 cm3
250 cm3
0.054 × = 0.32 mol.dm– 3
42.5 cm3
FB 2 contains ………4…
0.…
3 …… g dm–3 H2C2O42H2O.
| P ag e 35
9701/34/O/N/09
1 Read through question 1 before starting any practical work.
The formula of hydrated copper(II) sulfate is CuSO4xH2O where x shows the number of
molecules of water of crystallisation present.
(a) Method 1
Expected Answer
[3]
| P ag e 36
(b) Calculate the mass of water lost and the mass of copper(II) sulfate that remained after
heating.
mH O
2 = 33.85 – 32.90= 0.95 g
0…
mass of water lost = …… .95…… g
1…
mass of copper(II) sulfate remaining = …… .70…… g
[1]
Mass of remaining CuSO4(s) = 32.90 – 31.20
= 1.70 g
159.6
(c) Use your answer to (b) to calculate how many moles of water were lost and the moles of
copper(II) sulfate, CuSO4, remaining after heating.
Show all of your working. [Ar : Cu, 63.5; H, 1.0; O, 16.0; S, 32.1]
0.95
Amount of H2O = = 0.052
18
and …………0…
.01
…1…………… mol of CuSO4. [2]
(d) Use your answer to (c) to determine the value of x in the formula of hydrated copper(II)
sulfate, CuSO4.xH2O.
x = ………5..........................[2]
| P ag e 37
(e) Method 2
• Pipette 25.0 cm3 of FB2 into a conical flask and use a measuring cylinder to add
10 cm3 of FB 4.
• Titrate this solution with FB 3 from the burette until the mixture becomes yellow brown.
Do not add too much FB 3 at this stage.
• An off-white precipitate is also present in the flask and this will mask the colour of
the solution.
• Continue the titration until the blue-black colour of the complex just disappears
leaving the off-white precipitate.
• Record your titration results in the space below. Make certain that your recorded
results show the precision of your working.
Burette reading (final) / cm3 33.50 25.95 28.65 29.10 at least two titres
within 0.1 cm3
Burette reading (initial) /cm3 9.35 4.55 7.15 7.60
21…
25.0 cm3 of FB 2 reacted with ……… .5.…
0 …. cm3 of FB3.
Show which results you used to obtain the value of the volume of FB 3 by placing a tick (✓)
under the readings used in your results. [11]
| P ag e 38
(f) (i) In Method 1 a student was advised to carry out all weighings using the same
balance. What type of error might be introduced if more than one balance was
used?
D
..i.f.f.e
..r.e
..n
..t..b
..a
..l.a..n..c..e..s...h..a..v..e...d..if.f.e
..r..e..n..t..s.y..s..t.e..m
...a..t.i.c...e..r.r.o..r..e....g...............................................
.n..o..n..–..c..o..n..s.i.s..t.e..n..t..z..e..r.o....o..r..d
..i.f.f.e..r.e
..n
..t..p
..r.e
...c.i.s..i.o..n...o..f..b..a..l.a..n..c.e.......................................... [1]
Assume that the measuring cylinder used could be read to 0.5 cm3.
Calculate the percentage error in the measurement of this volume.
0.5 cm3
% error = × 100
10 cm3
(g) Method 1 is usually less accurate than Method 2 for finding the value of x in the
formula of hydrated copper(II) sulfate, CuSO4.xH2O.
A group of students carried out Method 1 correctly but calculated a value of 4 for x.
The true value for x is 5.
Suggest an error in the practical procedure of the experiment that could account for this
difference.
.T..h..e...M
...a..s..s..l.o
..s..s...i.s...t.o..o...lo
..w
....a..s...h..e..a..t.i.n..g...t.h..e...is...i.n..s..u..f.f.i.c.i.e..n..t...o..r...............................................
The solid reabsorbs moisture on cooli ng ...................................................................
................................................................ [1]
(h) Suggest a modification that could be made to the practical procedure in Method 1 to
reduce this error.
Explain why this modification should give an answer nearer to 5.
modification ......H..e..a..t.i.n..g...t.o...c..o..n..s..t.a..n..t..m
..a
..s..s....&
...c..o
..o
..l.i.n..g...w
..i.t.h
...l.i.d...o..n...c..r.u..c..i.b.l.e
..........................
........................................................................................................................................
explanation .....T..h..e...m
...a..s..s...lo
..s..s...i.s...t.o..o...lo
..w
....a..n..d...t.h..e...m
...o..d..i.f.i.c.a
..t.i.o..n...w
...i.ll..r.e
..d
..u
..c..e...t.h
..i.s.................
................................................................................................................................... [2]
[Total: 24]
| P ag e 39
9701/33/M/J/11
(a) Method
In the space below, record, in an appropriate form, all your weighings and include the
mass of FA4 used and the mass of water that was lost. [5]
NOTE
Records all weighings consistently to at least 1 decimal place .
| P ag e 40
(b) Calculations
Show your working and express your answers to three significant figures.
(i) Using the mass of water that was lost on heating, calculate the mass of
MgSO47H2O was present in the initial sample of FA 4.
[Ar: H, 1.0; O, 16.0; Mg, 24.3; S, 32.1]
246.4 g 7 ×18g
? 0.65 g
1.27
= ×100
1.45
(c) Suggest an improvement to the practical procedure that would give a more accurate
value for the percentage by mass of MgSO47H2O in FA 4.
........................................................................................................................................
....................................................................................................................................[1]
[Total: 8]
| P ag e 41
The thermal decomposition of group 2 carbonates
hard-glass test tube
Metal
Carbonate
Limewater
place about 1cm depth of metal(II) carbonate MCO3 in a dry test tube.
Strongly heat the carbonate (e.g CaCO3) for several(10 –15) minutes.
Note how rapidly gas is evolved and
Record the time for which lime water becomes milky.
Remove the tube from limewater as soon as heating is stopped.
Repeat the same procedure with the other carbonate e.g BaCO3(s) & compare.
| P ag e 42
Miscellaneous
XCO3(s)
XO(s) + CO2(g)
(a) Explain why it was necessary to heat the carbonate until there was no further change in mass.
To make sure the decomposition is complete and all the CO2(g) has been given off.
(b) (i) Calculate the mass of carbon dioxide gas given off.
(ii) Calculate the amount (moles) of carbon dioxide gas given off.
(iii) Use the answer from (ii) to state the amount (moles) of XCO3 in 5.75 g of the solid.
...M
...o..l.e..s...o..f...X..C
...O..3..(.g..)...=...0.....0..5...m
...o
...l.......................[...1...:...1..] ...........................(1)
5.75
M= = 115 g.mol–1
0.05
(v) Use your answer from (iv) and the relative atomic masses of carbon and oxygen to calculate the
relative atomic mass of X in XCO3.
X + 12 + 3 ×16 = 115
X = 55
| P ag e 43
(c) All measurements of mass have some uncertainty. In this case, this leads to an error of ±0.91 % in
the molar mass of XCO3.
(i) Use this information and your answer to (b)(iv) to calculate the error in the molar mass of XCO3.
0.91
Molar mass error = × 115 = 1.05 or 1.0
100
(ii) Hence suggest the range of possible values for the molar mass of XCO3.
...a..n..g..e..i.s...:..1..1..5...–...1...=
.........R ....1..1..4...t..o....1..1..5...+...1....0....=...1..1..6...............................................
(iii) Hence give the range of possible values of the relative atomic mass of X.
X = 54 or X = 56
(iv) Use the Periodic Table and your answer to (c)(iii) to suggest possible identities
of metal X.
.......X.....c..o..u..l.d...b
..e
....M
...n...o
...r..F
...e.....................................................................................
...............................................................................................................................
| P ag e 44