CHEM2017 Analytical Chemistry Test 2012

Total marks = 45
Time allowed = 1 hour
Answer all questions in the booklet provided.
QUESTION 1
Nitrite (NO2-) was measured by gas chromatography in rainwater and unchlorinated drinking
water. The results standard deviation (number of samples in brackets) are given in the
following table.
Rainwater
Drinking water
(a)
(b)

0.069 0.005 mg/L (n=7)

0.076 0.007 mg/L (n=5)

Does the drinking water contain significantly more nitrite than the rainwater (at the 95%
confidence level)?
(5)
Would your answer to (a) change if a 90% confidence level was considered? And a
98% confidence level? Explain.
(3)
[8]

DATASHEET

t calc

t calc

ts

n
x1 x 2
spooled

d
sd

n1n 2
n1 n 2

x i x 2
n 1

s12(n1 1) s 2 2(n 2 1)

n1 n 2 2

spooled

sd

(di d )2
n 1

Values for Students t

Degrees of freedom
1
2
3
4
5
6
7
8
9
10
11
12

Confidence level
90%
95%
6.314
12.706
2.920
4.303
2.353
3.182
2.132
2.776
2.015
2.571
1.943
2.447
1.895
2.365
1.860
2.306
1.833
2.262
1.812
2.228
1.800
2.209
1.788
2.189
1.645
1.960
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QUESTION 2
A set of copper standards were prepared and analysed using flame atomic absorption
spectrometry. The calibration graph was plotted and is given below. A waste water sample
was analysed at the same time.
0.8

Absorbance

0.7
0.6
0.5

y = 0.0702x + 0.0033
R2 = 0.9993

0.4
0.3
0.2
0.1
0
0

10

12

Copper Concentration /ppm

(a)

(b)

(c)

A 2 mL sample was diluted to 100 mL and when the solution was analysed the
absorbance reading was 4.384 units. Estimate the concentration of copper in the
original waste water sample.
(4)
The sample from part (a) was then further diluted by taking 5 mL of the diluted solution
and making up the volume to 50 mL. When this solution was analysed the absorbance
reading was 0.492 units. Calculate the concentration of copper in the original waste
water sample.
(4)
Explain the why there is a difference in the results from (a) and (b).
(3)
[11]

QUESTION 3
Explain the terms below. You may use sketches to supplement your explanation where
necessary.
(a) Representative sample
(b) Detection limit
(c) Resolution
(d) Spectral interferences

(1)
(2)
(2)
(2)
[7]

QUESTION 4
In AAS, explain the function of:
(a) the nebuliser
(b) the monochromator

(1)
(2)
[3]

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QUESTION 5

Signal

Below is a gas chromatogram recorded for a standard sample of isopropanol.

(a)
(b)
(c)
(d)

Time /min

Calculate the number of theoretical plates for isopropanol on this column.

(3)
Calculate the height equivalent of a theoretical plate if this column was 25 cm long.
(1)
How would the chromatogram change if a 15 cm column of the same type were used
under the same conditions?
(2)
Explain how eddy diffusion causes band broadening gas chromatography.
(2)
[8]

QUESTION 6
In the analysis of crude aspirin, aspirin is titrated using an excess of NaOH. The unreacted
NaOH is then titrated using H2SO4.
OH

OCOCH3

+ CH 3CO 2Na + H 2O

+ 2NaOH
CO2H

CO2Na

A 0.5000 g crude aspirin sample was added to a particular volume of NaOH. The unreacted
NaOH was titrated with 13.05 ml of 0.200 M H2SO4. The same volume of NaOH (without
the addition of aspirin) was also titrated with 21.35 ml of 0.200 M H2SO4.
Calculate the percentage of aspirin in the sample.
[8]

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Page 4 of 5

CHEMISTRY DATA SHEET

Physical Constants
Gas constant

Boltzmann constant
k
Planck constant
h
Faraday constant
F
Avogadro constant
L or NA
Speed of light in vacuum
c
Mole volume of an ideal gas
Vm
Elementary charge
Rest mass of electron
Rest mass of proton
Rest mass of neutron
Permitivity of vacuum
Gravitational acceleration
(at sea level)
Conversion Factors
1W
1J
1 cal
1 eV
1 atm
1 atm
1 bar
1
1 ngstrom
1 micron ()
1 Poise
1 ppm

e
me
mp
mn
o
g

= 8.315 J K1 mol1
3 1
1
= 8.315 kPa dm K mol
3 1
1
= 8.315 Pa m K mol
2
1
1
= 8.206 x 10 atm K mol
23
1
= 1.381 x 10 J K
34
1
= 6.626 x 10 J K
4
1
= 9.649 x 10 C mol
23
1
= 6.022 x 10 mol
8
1
= 2.998 x 10 m s
1
= 22.41 mol (at 1 atm and 273.15 K)
1
= 22.71 mol (at 1 bar and 273.15 K)
19
= 1.602 x 10 C
31
= 9.109 x 10 kg
27
= 1.673 x 10 kg
27
= 1.675 x 10 kg
12 2 1 1
1
= 8.854 x 10 C J m (or F m )
2
= 9.807 m s

=1Js
= 0.2390 cal = 1 N m = 1 V C
2
= 1 Pa m3 = 1 kg m2 s
= 4.184 J
19
= 1.602 x 10 J
= 101.3 J
5
2
5
= 1.013 x 10 N m = 1.013 x 10 Pa = 760
mmHg
5
= 1 x 10 Pa
3 3
3
= 10 m = 1 dm
10
= 1 x 10 m = 0.1 nm = 100 pm
6
= 10 m = 1 m
2
= 0.1 Pa s = 0.1 N sm
1
1
= 1 g g = 1 mg kg
1
= 1 mg (dilute aq solutions only)

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