1.

Titration simple mole ratio

The following experiment was carried out.

a) An indigestion tablet was weighed and
crushed.
b) The tablet was transferred into pre-weighed
beaker and then reweighed.
c) About 50cm
3
of water was used to dissolve
the tablet and the liquid from the resulting
saturated solution was filtered and
transferred into a 250 cm
3
volumetric flask.
d) The flask was filled to the mark with tap
water and labelled TD1.
e) 25cm
3
of the tablet solution TD1 was
pipetted into a conical flask.
f) Three drops of methyl orange indicator.
g) The solution was titrated against TD2
(Hydrochloric acid 0.05mol.dm
-3
) from the
burette until the solution went red and stayed
red for one minute. This process was
repeated to gain concordant results.

Results
Mass of Beaker = 72.00g, Mass of beaker + tablet = 73.97 g
Titration results
Initial Volume (cm
3
) Final Volume (cm
3
)
Trial 1 2.75 26.20
Trial 2 22.25 45.90
Trial 3 5.30 28.80

Questions
Some indigestion tablets are hydroxide compounds and some are carbonate compounds.
Assuming the tablet only has magnesium hydroxide as its neutralisation agent:
1) Calculate the mass of active ingredient in the tablet.



















2) Calculate the percentage of the tablet that is active ingredient (and not filler compounds).


2. Titration moderate mole ratio

MnO
4
-
(aq) + 8H
+
(aq) + 5Fe
2+
(aq) Mn
2+
(aq) + 4H
2
O (l) + 5Fe
3+
(aq)

TB1 is Fe(NH
4
)
2
(SO
4
)
2
.6H
2
O powder M
r
=
392.1
TB2 will be made by you.
TB3 is 1.0mol.dm
-3
sulfuric acid
TB4 is potassium manganate(VII) solution of
unknown concentration
The following procedure was carried out
a) 4.03 g of TB1 was weighed in a beaker,
dissolved in 100cm
3
of TB3, then transfer
to a 250cm
3
volumetric flask. The flask
was filled up to the mark with tap water
and thoroughly mixed. This was labelled
TB2.
b) 25.0 cm
3
of the TB2 solution was pipetted
into a clean conical flask.
c) The burette was filled with TB4 solution
and a titration was carried out until the first
pale pink colour remained for 15 seconds.

Titration results
Initial Volume (cm
3
) Final Volume (cm
3
)
Trial 1 6.10 28.50
Trial 2 1.20 23.10
Trial 3 3.05 25.00

Questions
1) Calculate the concentration of TB4.






















2) The concentration of TB4 should be 0.00956 mol dm
-3
. Calculate the percentage error in your
results.




3. Water of crystallisation in washing soda, Na
2
CO
3
.xH
2
O
The following procedure was carried out.
a) A burette was filled with the acid, TC2 (0.50
moldm
-3
HCl).
b) 40.65 cm
3
of TC2 was run into a 250 cm
3

volumetric flask and made up to the mark
with tap water then inverted a few times to
ensure thorough mixing; this was labelled
TC3.
c) 3.09 g of the washing soda TC1, was
weighed into a beaker.
d) Tap water was added to the beaker to
dissolve the crystals. The solution was
transferred to a 250 cm
3
volumetric flask
and made up to 250 cm
3
with tap water and
inverted several times to ensure thorough
mixing. This solution was labelled TC4.
e) 25.0 cm
3
of TC4 was pipetted into a conical
flask and a few drops of the indicator
provided was added.
f) TC4 was titrate against TC3 from a burette
until the end point was reached.

Titration results
Initial Volume (cm
3
) Final Volume (cm
3
)
Trial 1 3.25 34.80
Trial 2 7.25 38.65
Trial 3 4.25 35.70

Questions
1) Determine the value of x in Na
2
CO
3
.xH
2
O.
4. Part 1 The enthalpy change in the displacement reaction between zinc and copper(II)
sulphate.

**The specific heat capacity of any dilute salt solution is approximated to that of pure water**

Zn(s) + CuSO
4
(aq) ZnSO
4
(aq) + Cu(s)

The following procedure was carried out.

a) 50 cm
3
of 0.2 mol dm
-3
copper (II) sulphate
was poured into the polystyrene cup.

b) 1.00 g (an excess) of powdered zinc was
weighed out.
c) The initial temperature of the solution in the
cup was recorded as 19.5
o
C and then the
powdered zinc was added.
d) The solution was stirred gently and
constantly with the thermometer until the
temperature stopped changing. The final
temperature was recorded as 29.0
o
C.

Questions
1) Calculate the enthalpy change (kJmol
-1
) that took place with respect to CuSO
4
.
c = 4.18J.
o
C
-1
.g
-1
.





2) Show that zinc is indeed the reactant that is in excess.



Part 2: The enthalpy change reaction between citric acid and sodium hydrogen carbonate.

C
6
H
8
O
7
(aq) + 3NaHCO
3
(s) C
6
H
5
O
7
Na
3
(aq) + 3CO
2
(g) + 3H
2
O(l)

The following procedure was carried out.
a) 25 cm
3
of 1 mol dm
-3
citric acid was poured
into the polystyrene cup.
b) 8.15 g of sodium hydrogen carbonate (an
excess) was weighed onto a piece of paper.
c) The initial temperature of the solution in the
cup was recorded as 20.0
o
C and then the
powdered NaHCO
3
was added.
d) The reaction frothed up, so the powdered
solid was added slowly to prevent it coming
over the top of the cup.
e) The final temperature reached was 4.0
o
C.

Question
1) Calculate the enthalpy change (kJmol
-1
) that took place with respect to citric acid.
c = 4.18J.
o
C
-1
.g
-1
.






2) Show that NaHCO
3
is indeed the reactant that is in excess.



5. Measuring the enthalpy change of neutralisation

The following procedure was carried out.
a) A clean, dry Styrofoam cup was weighed at
5.70g.
b) 50cm
3
of hydrochloric acid solution (1
mol.dm
-3
) was added to the cup.
c) The initial temperature of the solution was
recorded at 18.0
o
C.
d) About 50cm
3
of sodium hydroxide solution
(1 mol.dm
-3
) was added to a small beaker.
e) The initial temperature of this solution was
recorded at 19.0
o
C..
f) The two solutions temperatures were
averaged.
g) The NaOH from the beaker was poured into
the HCl in the cup.
h) The highest temperature reached by the
solution was recorded at 25.5
o
C, and the
temperature change was calculated.
i) The cup was reweighed at 106.70g.
Calculate the mass of solution used.

Results
Average Initial Temperature =
Temperature change =
Mass of solution =
Questions
1) Calculate the value for AH for this reaction in kJmol
-1
for hydrochloric acid.









2) Explain why the value gained for the AH is unreliable by giving three reasons for errors
throughout this practical.




3) Explain why the value for AH for sodium hydroxide should be the same.



4) When a substance like ammonium chloride is put into water, the temperature decreases.
AH[NH
4
Cl(s) NH
4
Cl(aq)] = 44.9kJmol
-1
. M
r
(NH
4
Cl) = 53.5

Calculate the temperature decrease when 4.00g of NH
4
Cl is dissolved into 50cm
3
of water.




6. Titration Hard mole Ratio - Reaction of iodine with sodium thiosulphate


TE1 = unknown concentration potassium
iodate solution, 4.00gdm
-3
.
TE2 = 0.1mol.dm
-3
potassium iodide solution
TE3 = 1.0mol.dm
-3
sulfuric acid solution
TE4 = 0.0989mol.dm
-3
sodium thiosulfate
solution (standard solution)
Fresh starch solution (indicator)

The following procedure was followed
a) 25cm
3
of TE1 was pipetted into a flask.
b) To this flask excess TE2, (25cm
3
) and
excess TE3 (2cm
3
) was added.
c) The burette was filled with TE4 and the
initial volume recorded.
d) TE4 was titrated into the flask until the
solution in the flask was a pale yellow. At
this point a few drops of starch was added
to make the solution blue/black.
e) Titrating was continued until the colour of
the solution went colourless. The final
volume was recorded.
f) This titration was repeated until two
concordant titre values were determined

Titration results
Initial Volume (cm
3
) Final Volume (cm
3
)
Trial 1 1.25 22.80
Trial 2 6.30 27.70
Trial 3 5.00 26.45

Questions
M(KIO
3
) = 214 g.mol
-1
.
1) Calculate the concentration of TE1 (in g.dm
-3
).

















2) Compare this value with that created with the impure KIO
3
and determine the percentage
purity of the solid potassium iodate.
IO
3

+ 5I
-
+ 6H
+
3I
2
+ 3H
2
O
3I
2
+ 6S
2
O
3
2-
3S
4
O
6
2-
+ 6I
-


7. The enthalpy change of solution for sodium hydroxide
In this experiment the temperature is measured over time and plotted on a graph; the regular method of
determining the maximum observable T rise is just an approximation. Extrapolation of the cooling curve will
give a correct value for the T rise. This makes an allowance for the heat loss to the surroundings.
The following procedure was carried out
1. A polystyrene cup was weighed at 2.77g.
2. Approximately 50cm
3
of water was
added to the cup the total mass was
recorded at 54.19g, and therefore mass
of water can be calculated.
3. The temperature of the water in the cup
was recorded for 2 minutes to determine
the baseline temperature.
4. 11 lumps of solid sodium hydroxide, from
the sealed container, was added to the
water at the 2 minute mark and stirred,
while continuing to time.
5. The cup was rewighed to determine the
mass of NaOH added.
6. Timing was continued but only once the
NaOH was all dissolved were the
temperatures recorded again.
7. The temperature of the water was
recorded over the next 10 minutes (total
of 12 minutes of timing).

Results
Mass of empty cup / g 2.77
Mass of cup plus water / g 54.19
Mass of cup, water and NaOH / g 54.72
Mass of water added / g
Mass of NaOH added / g

Time
period / s
Temperature /
o
C
temperature
/
o
C
0 29.5 0
30 29.5 0
60 29.5 0
90 29.5 0
120 29.5 0
150
180 42.5 13.0
210 42.0 12.5
240 42.0 12.5
270 42.0 12.5
300 41.5 12.0
330 41.5 12.0
360 41.0 11.5
390 41.0 11.5
420 41.0 11.5
450 40.5 11.0
480 40.5 11.0
510 40.0 10.5
540 40.0 10.5
570 40.0 10.5
600 39.5 10.0
630 39.5 10.0
660 39.5 10.0
690 39.0 9.5
720 39.0 9.5


Graphing
Plot a graph of temperature vs time.
There should be two distinct regions/lines to the
graph.
The cooling section of the graph needs to be
extrapolated back to the time at which the solid
was added to determine a corrected T for the
reaction.

Calculations
Find the enthalpy value for the reaction in kJmol
-1
.
8. The enthalpy change of solution for ammonium chloride

The following procedure was followed
a) 25cm
3
of water was pipetted into a small beaker.
b) The initial temperature was recorded.
c) 3.00g of MA1 was weighed out and added to the water.
d) The highest temperature (final temperature) was recorded.
e) The experiment was repeated using approximately 4.00, 5.00, 6.00, 7.00, 8.00 9.00 and 10.00
g of MA1.

Results
mass/g T change /
o
C
2.99 7.0
3.25 8.0
4.49 11.0
4.93 12.0
5.50 13.0
6.50 15.0

mass/g T change /oC
7.05 16.5
7.27 16.5
8.00 13.0
8.01 17.0
8.47 15.0
9.52 18.0
Questions
1) Plot a graph of T vs m for your data, and draw a trend line.
2) Determine (by extrapolation) the value for T when the mass of MA1 is 11.00g.

3) Determine the energy released when the mass of MA1 is 11.00g, where c = 4.18J
o
C
-1
K
-1
.




4) Calculate the H
r
(units kJmol
-1
) for ammonium chloride solid dissolving into water.

9. Determining the water of crystallisation by gravimetric analysis
Waters of crystallisation are water molecules trapped within the lattice of an ionic compound in a
set ratio. E.g. CuSO
4
.5H
2
O has five waters of crystallisation for every one CuSO
4
.
The mole ratio of the waters can be determined easily by the mass lost when a stable hydrated
ionic compound loses all of its water molecules to become anhydrous.
The following procedure was followed:
1. An empty crucible was weighed at 5.70 g.
2. 5.50 grams of hydrated magnesium sulphate were added.
3. The crucible was heated from beneath, carefully at first, then a little bit stronger for about a
minute.
4. The heat was removed and the crucible was allowed to cool a little bit, before being
weighed.
5. The crucible was reheated for another minute, cooled and reweighed.
6. This process was repeated until the mass dropped by less than 0.05g compared to the
previous heating. The final mass of the crucible and solid was 8.51 g.

Results draw an appropriate results table from the information above.





Questions
1. The formula for the hydrous magnesium sulphate is MgSO
4
.xH
2
O, Determine x from the
above data.




Answers
1. Titration

1. 2HCl + Mg(OH)
2
MgCl
2
+ 2H
2
O
2. E.g. (23.45 + 23.65 + 23.50) / 3 =
23.53cm
3
= 0.0235dm
3
.
3. n =cV = 0.05mol.dm
-3
x 0.0235dm
3
=
0.00118mol
4. Use the mole ratio. 0.00118mol / 2 =
0.000588mol
5. 0.000588mol per 25cm3, so times by
10 for the whole flask: 0.00588mol
6. m = nM = 0.00588mol x 58gmol
-1
=
0.34g
7. % = 0.35g / 1.97g x (100/1) = 17.4%

2. Titration.
1.
mol 0103 . 0
gmol 1 . 392
g 03 . 4
M
m
n
1
= = =


2. The total 250cm
3
flask has 0.0103mol, so the 25cm
3
pipette has a tenth of that: 0.00103mol
3. n(Fe
2+
) : n(MnO
4
-
) = 5:1. Divide by five.
mol 10 x 05 . 2
5
mol 00103 . 0
4
=

4.

3 3
cm 93 . 21 cm 925 . 21
2
) 95 . 21 90 . 21 (
titre Average = =
+
=
5.
mol 10 x 35 . 9
dm 02193 . 0
mol 10 x 05 . 2
V
n
c
3
3
4

= = =
.
6. % 20 . 2
1
100
00956 . 0
) 00935 . 0 00956 . 0 (
error % =
|
.
|

\
|

= .

3. Water of crystallisation
1.
3
3
3
3
moldm 0813 . 0
cm 250
cm 65 . 40
moldm 50 . 0

=
2. From titres that are concordant:
3 3
dm 03147 . 0 cm 47 . 31
3
45 . 31 40 . 31 55 . 31
= =
+ +

3. n=cV = 0.0813mol.dm
-3
x 0.03147dm
3
= 0.00256mol
4. Na
2
CO
3
:HCl = 1:2 so 0.00256mol /2 = 0.00128mol of sodium carbonate
5. 0.00128mol per 25cm
3
. Times by 10 for the 250cm
3
flask = 0.0128mol
6. m = nM = 0.0128mol x 106gmol
-1
= 1.36g
7. I added a total of 3.09g of hydrated sodium carbonate, and have just shown that 1.36g of it
is anhydrous sodium carbonate. The rest of the mass is water.
3.09g 1.36g = 1.70g of H
2
O.
First Second Third
Final reading / cm
3
28.50 23.10 25.00
Initial reading / cm
3
6.10 1.20 3.05
Titre / cm
3
22.40 21.90 21.95
8. mol 0944 . 0
gmol 18
g 70 . 1
O H mol 0128 . 0
gmol 106
g 36 . 1
CO Na
1
2
1
3 2
= = = =


O H 7 . CO Na therefore 7 36 . 7
mol 0128 . 0
mol 0944 . 0
O H 1
mol 0128 . 0
mol 0128 . 0
CO Na
2 3 2 2 3 2
= = = = =
Data booklets suggest that the actual value is 10 waters of crystallisation.

Experiment 4
Part 1
(1) E = mcT, m = 50g, c = 4.18, T= 9.5oC
E = 50 x 4.18 x 9.5
E = 1985.5 J
H = -E/n, n = cV n = 0.2 x 50/1000 = 0.01
mol
H = -1.9855kJ/0.01 mol
H = -198.55 kJ mol-1 or -200 kJ mol-1.
(2) n = m/M, M = 65.4 so n = 1/65.4
n = 0.015. As it is a 1:1 mole ratio and 0.015
> 0.01 then Zn is in excess.

Part 2
(1) E = mcT, m = 25g, c = 4.18, T= -16 oC
E = 25 x 4.18 x -16
E = -1672 J
H = -E/n, n = cV n = 1 x 25/1000 = 0.025
mol
H = -(-1.672)kJ/0.025 mol
H = 66.88 kJ mol-1 or 70 kJ mol-1.
(2) n = m/M, M = 23+1+12+48 = 84 so n =
8.15/84
n = 0.097. As it is a 3:1 mole ratio and
0.0977 > 3 x 0.025 then it is in excess.

Answers to Experiment 5

1) E = 101g x 4.2J
o
C
-1
g
-1
x 7
o
C = 2970J =
2.97kJ
2) n = cV = 1mol.dm
-3
x 0.050dm
3
=
0.05mol
3) DH = E / n = 2.97kJ / 0.05mol =
59.4kJmol
-1
.
4) Possible errors:
The measured volume of HCl was not
exactly 50cm3, so the molar amount is
wrong.
The total amount of HCl may not have
been fully neutralised, if there was
insufficient NaOH.
The temperature recorded to the nearest
half degree, over such a small
temperature rise has a large error.
5) If equal molar amounts of HCl and NaOH
were used, then the calculation is
identical.
6) mol
gmol
g
M
m
n 0748 . 0
5 . 53
00 . 4
1
= = =

J kJ n H E 3360 36 . 3 = = A =
C
g
J
mc
E
T
o
16
2 . 4 50
3360
=

= = A

Answers to Experiment 6

The working is as it should be, but the numbers are different to yours because your titration will
have gained different titre values.

1) From titres that are concordant:
3 3
dm 02147 . 0 cm 47 . 21
3
45 . 21 40 . 21 55 . 21
= =
+ +

2) n=cV = 0.0989mol.dm
-3
x 0.02147dm
3
= 0.00212mol of TE4
3) S
2
O
3
2-
: IO
3
-
= 6:1 = so 0.00212mol /6 = 0.000354mol of potassium iodate TE1
4) 0.000354mol per 25cm
3
.
3
3
dm . mol 0142 . 0
dm 025 . 0
mol 000354 . 0
V
n
c

= = =
5) 0.0142mol.dm
-3
x 214gmol
-1
= 3.03gdm
-3

6)
% 7 . 75
1
100
x
gdm 00 . 4
gdm 03 . 3
3
3
=
|
.
|

\
|

Experiment 7

Mass of empty cup / g 2.77
Mass of cup plus water / g 54.19
Mass of cup, water and NaOH / g 54.72
Mass of water added / g 51.42
Mass of NaOH added / g 0.53

Time period / s Temperature /
o
C
o
C
0 29.5 0
30 29.5 0
60 29.5 0
90 29.5 0
120 29.5 0
150
180 42.5 13
210 42 12.5
240 42 12.5
270 42 12.5
300 41.5 12
330 41.5 12
360 41 11.5
390 41 11.5
420 41 11.5
450 40.5 11
480 40.5 11
510 40 10.5
540 40 10.5
570 40 10.5
600 39.5 10
630 39.5 10
660 39.5 10
690 39 9.5
720 39 9.5

0
2
4
6
8
10
12
14
0 100 200 300 400 500 600 700 800


E = mcT = 51.42g x 4.18J g
-1

o
C
-1
x 13.4
o
C = 2880J = 2.88kJ
n = m/M = 0.53g / 40.0gmol
-1
= 0.013mol
H = E/n = 2.880kJ / 0.013mol = 217kJ

Experiment 8

mass/g
T
change
2.99 7.0
3.25 8.0
4.49 11.0
4.93 12.0
5.50 13.0
6.50 15.0
7.05 16.5
7.27 16.5
8.00 13.0
8.01 17.0
8.47 15.0
9.52 18.0

(2) 20.8 oC
(3) E = mcT
0.0
2.0
4.0
6.0
8.0
10.0
12.0
14.0
16.0
18.0
20.0
0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00
t
e
m
p

c
h
a
n
g
e
/
d
e
g

C
Mass/g
T change
Linear (T change)
E = 25 x 4.18 x 20.8
E = 2173.6 J released.
(4) n = m/M
n = 11.00/ 53.5
n = 0.206
(5) H = -E/n
H = -2.1736/0.206
H = -10.55 kJ mol-1 (-10.6)

Experiment 9
Results Table
Mass (g)
Crucible 5.70
Crucible + hydrous magnesium sulphate 11.20
Crucible + anhydrous magnesium sulphate 8.51

(1)
Mass of anhydrous magnesium sulphate = 8.51 5.70 = 2.81 g
Mass of water = 11.2 8.51 = 2.69g

(2) n(MgSO4) = m/M = 2.81/120.3 = 0.0233, n(H2O) = m/M = 2.69/18 = 0.1494

(3) Ratio = 0.0233/0.0233 : 0.1494/0.0233
= 1 : 6.4
MgSO4.6H2O.