XIAMEN UNIVERSITY MALAYSIA

Mark:

Course Code : CME430

Course Name : Pollution Sampling and Analysis
Lecturer : Dr Wong Kai Lun
Academic Session : 2020/04
Assessment Title : Individual Lab Report
Submission Due Date : 10th July 2020

Prepared by : Student ID Student Name

CME1709834 Soh Leong Sing
Date Received :

Feedback from Lecturer:

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Own Work Declaration

I/We hereby understand my/our work would be checked for plagiarism or other
misconduct, and the softcopy would be saved for future comparison(s).

I/We hereby confirm that all the references or sources of citations have been correctly
listed or presented and I/we clearly understand the serious consequence caused by any
intentional or unintentional misconduct.

This work is not made on any work of other students (past or present), and it has not
been submitted to any other courses or institutions before.

Signature: Soh Leong Sing

Date: 9-7-2020

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Determination Of Ferrocene Concentration In A Water Sample Using Ultraviolet-

Visible Spectrophotometry

1.0 Introduction

In this report, ferrocene or dicyclopentadienyl iron is an analyte that conducted in

experiment. It was firstly discovered by T.J. Kealy and P.L.Paulson in 1951. They
proposed that the structure of ferrocene is a carbon ring with attachment of an iron. In
1952, Wilkinson and R. B. Woodward deduced it as "sandwich compounds" because
the iron ion lied parallel to both anionic cyclopentadienyl rings that containing 6
delocalized π electrons. Ferrocene is an organometallic compound with chemical
structure C10H10Fe and molecular formula Fe(η5-C5H5)2 . It can be synthesised by
different methods in laboratory e.g. Grignard reagent, gas-metal reaction and alkali
cyclopentadienide. Ferrocene can be applied in many fields. For example, it is used as
an antiknock additive for gasoline. It can be transformed into variety of products like
coating material, lubricant, UV absorber, catalyst, and fuel oils. Ferrocene is known
as a flammable, irritant and toxic chemicals. It contains iron ion which may cause eye,
skin and respiractory tract irritation [1]. Not only that, it is categorised as combustible
solid by The National Institute for Occupational Safety and Health (NIOSH). To
prevent the exposure of ferrocene in laboratory, it is necessary to wear PPE like lab
coat, gloves, goggles when handling the chemicals. The chemicals must be stored
properly under fully sealed to prevent dust dispersion and fire hazard.

In analytical chemistry, quantity analysis is a effective measurement technique that is

used widely in a variety of chemical fields. The analysis helps to measure the
chemical composition by using absorption of light that occurs at different
wavelengths. Ferrocenes allow the use of a large variety of electrochemical detection
(ECD) techniques including amperometry, voltammetry and Mössbauer spectroscopy
[2]. In this virtual experiment, Ultraviolet-Visible Spectrophotometry is selected
because its quick analysis ability and easy to learn by a student. It can be directly
utilised to measure light intensity at different wavelengths. UV-vis instruments
generally analyse liquids and solutions efficiently. The theory of Beer-Lambert Law is
applied in this experiment. Beer’s Law, which describes there is a linear relationship
between absorbance and concentration, is the basis of a multitude of quantitative
analytical methods using this technique. The amount of energy absorbed by a sample

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is proportional to the molar absorptivity and the concentration of analyte. This can be

used to determine concentration of analyte from the photon absorption.

A=εcl

A= Absorbance

ε = Molar absorption coefficient /M-1cm-1

c= Molar concentration /M

l = optical path length cm

2.0 Objectives

1. To measure the absorbance of the ferrocene analyte from wavelengths 350 to 700
nm .
2. To determine the unknown concentration of the sample from calibration curve.
3. To verify the relationship of absorbance and concentration by applying Beer-
Lambert's Law.

3.0 Experimental Procedure

1. A blank cuvette was selected and placed in the spectrophotometer for

background. The lid was closed and it was ready to be tested. The cuvette was
ensured to be clean to ensure that no contamination affected the result. E.g.
The cuvette was wiped with tissue paper 
2. 0 ABS 100%T button was clicked and it was observed that the instrument
now read 0.00000 A.
3. A solution is selected with known concentration and absorbance was
measured between the wavelengths 350 nm to 700 nm. λmax was obtained
by looking at the maximum absorbance. UV spectrum was generated by using
Excel as shown in Table.
4. In second experiment, Absorbance values for each solution (0.02M, 0.04M,
0.06M, 0.08M, 0.1M) was read at the λmax in triplicates. The data was

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collected in the table 2. It was ensured that total 3 readings were obtained and
the average value was calculated.
5. The absorbance of sample with unknown concentration was measured in
spectrophotometer at λmax.
6. Calibration curve of absorbance vs. concentration plot was generated by using
Excel. A best fit line is draw by fitting the plots. Calibration equation is
obtained from the best fit line.
7. Concentration value for the unknown solution was predicted from the
calibration curve as shown diagram 2.

4.0 Results

Table 1 shows the wavelength and the corresponding absorbance.

λ (nm) Abs
530 0.3520
540 0.1797
550 0.0894
560 0.0441
570 0.0343
580 0.0249
590 0.0308
600 0.0119
610 0.0235
620 0.0170
630 0.0140
640 0.0224
650 0.0182
660 0.0133
670 0.0096
680 0.0162
690 0.0070
700 0.0067

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λ (nm) Abs
350 0.9317
360 0.5951
370 0.8204
380 1.4355
390 2.3241
400 3.3495
410 4.1965
420 4.8185
430 5.1722
440 5.2940
450 5.1647
460 4.8403
470 4.2696
480 3.4756
490 2.6342
500 1.8073
510 1.1206
520 0.6501

A graph of absorbance against wavelegth

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4
Absorbace/ A

0
350 400 450 500 550 600 650 700 750
Wavelength /nm

Diagram 1 shows the Ferrocene spectra.

Table 2 shows how the changing of concentration of sample effect on the absorbance.
λmax of Ferrocene: 440 nm

Particulars Trial 1 Trial 2 Trial 3 Mean

Absorbance at 0.02
M 5.2940 5.2940 5.2940 5.2940

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Absorbance at 0.04
M 10.5881 10.5881 10.5881 10.5881
Absorbance at 0.06
M 15.8821 15.8821 15.8821 15.8821
Absorbance at 0.08
M 21.1762 21.1762 21.1762 21.1762
Absorbance at 0.1
M 26.4702 26.4702 26.4702 26.4702

Table 3 shows the absorbance result for unknown sample.

Particular Trial 1 Trial 2 Trial 3 Mean

Absorbance of
unknown 1 1.8696 1.8696 1.8696 1.8696

A graph of absorbance against concentration

30

25 f(x) = 264.7 x − 0

20
Absorbace

15

10

0
0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08 0.09 0.1 0.11
Concentration /M

Diagram 2 shows a graph of absorbance against concentration of sample.

y=mx+c

M is obtained from the gradient of straight line.

C is obtained from the intercept of curve.

21.1762−5.2942
m= = 264.7 M −1
0.08−0.0

C = 5 ×10−3 A

y=264.7 x +3 ×10−5

For the absorbance of unknown concentration = 21.9748

21.8748 = x (264.7) + 3 ×10−5

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x = 0.08263 M

Molar adsorption coefficient calculation

1. Formula in eq.1

A=εcl

A (0.08−0.02)×1
ε= = =3.778 × 10−3 M-1cm-1
cl (21.1762−5.294 )

Discussion

From the diagram 1, it shows that the λmax is located at 440nm. This peak is
appeared due to the ferrocenyl group. In an experiment conducted by Fenzel et al.,
there is a peak shown in 335nm in ferrocene spectra [3]. Hence, the experiment shows
to be agree well with the other research’s studies because it supports the data
obtained.

For diagram 2, it shows that the absorbance increases linearly with concentration of
solution. The graph obtained from experiment is agree with the theoretical studies
from Beer-Lambert Law. Beer-Lambert law states that there is a linear relationship
between the concentration and the absorbance of the solution. After that, the unknown
concentration of a sample can be obtained from the calibration curve which is
0.08263M.

There are two methods to obtain the molar absorptivity coefficient. One is using Beer-
Lambert equation and another is obtained by best fit line in graph. The values
obtained by equation and graphical method are the same which is 3.778 ×10−3M-1cm-
1
.Therefore, it can be concluded that this experiment can be predicted well with Beer-
Lambert equation.

All three trial readings are the same in virtual experiment and this shows a perfectly
accuracy. However, this situation won’t be happened in the practical experiment.
There are many internal and external factors affecting on result. Firstly, the error

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maybe come from the undissolved ferrocene crystal in the solution. The sample will
scatter the light more than absorb the light and the data will be very skewed. To
improve the result, the solution must be well-stirred to form a homogeneous solution.
Other error can be obtained when the volatile ferrocene solution in cuvette is
evaporated under the room temperature. The decreasing of water content in the
solution lead to increase of the concentration. It is important to close the cuvette with
a lid to avoid both contamination and evaporation. Next, the cuvette must be wiped
with clean cloth before it is measured in spectrophotometer.

Conclusion

All objectives were completed successfully. The measurement for the absorbance of
the ferrocene analyte from wavelength 350 nm to 700 nm had been performed by
visual UV spectrophotometry in visual experiment. The wavelength with maximum
absorbance or peak in other word had been obtained. It is measured to be 440 nm.
After this, the calibration curve was obtained by different peak in different
concentration. This calibration curve was important for is to predict the concentration
of unknown sample. The calculated concentration of unknown sample was 0.08263
M. Observing from the graph obtained in diagram 2, It was concluded that the
absorbance and concentration of analyte are directly proportional to each other which
is described by Beer-Lambert.

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References

1.Bingham, E., Cohrssen, B. and Powell, C.H.
Encyclopaedia of Occupational Health and Safety. 4th edition, 
Geneva, Switzerland: International Labour Office, 1998,14 ,  15-63

2. Gerven, L.V. (Ed.), Nuclear Magnetic Resonance in Solids, NMR Studies of

Molecular Solids, Polymers and Glasses, Plenum Press 1997, 2(88), 131.

3Frenzel, J. N. and Hartley, G. F., Voltammetry and spectroscopic study of ferrocene

and hexacyanoferrate and the suitability of their redox couples as internal
standards in ionic liquids, Physical Chemistry Chemical Physics. 2017,19,
28841–28852. doi:10.1039/c7cp05483a.

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APPENDIX 1
CME430 LAB REPORT MARKING RUBRICS
Score and Descriptors
Criteria 3-4 1-2 0 Marks
Title Identifies the independent and/or Too long, or does not identify the No title, or too vague. e.g.
dependent variables, not too vague or independent and/or dependent variables. "Lab report"
too long, encapsulates the keywords Contains superfluous phrases, such as
of the report well. "An investigation into..." or "An
experiment on..."

Criteria 16-20 11-15 6-10 1-5 0 Marks

Introduction Clearly written, well Has included Has included Very short and Section
structured, with evidence of everything that was in everything that was skimpy, with no missing
relevant extra reading, flows the relevant handout, in the relevant attempt to completely.
well. Identifies the main and some evidence of handout, but include any
aims, and ends with a clear extra reading, but the elements are missing references to
outline of the study's structure is not very e.g. no justification relevant
hypotheses. Also has clear and appears for the study, no theoretical and
something novel in it, disjointed. Or it is well extra reading, poor empirical work.
compared to the handouts written, but shows no structure, no
that were supplied, and evidence of any extra hypotheses.
includes the rationale for reading.
performing the study.

Criteria 8-10 5-7 1-4 0 Marks

Objective(s) Purpose of the lab or the Purpose of the lab or the Purpose of the lab or the Section missing
question to be answered question to be answered question to be answered completely.
during the lab is clearly during the lab is partially during the lab is erroneous
identified and stated identified - vague or irrelevant

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Criteria 9-10 6-8 3-5 1-2 0 Marks

Procedure Contains all of the relevant Good structure, but Somewhat confused One or more Section
information about the some relevant and bits are missing sub-sections are missing
methods used; clearly and information has been within subsections. missing, completely.
systematically described in omitted. Parts have been confused, or
such a way that a naive included under the parts are
reader could replicate the wrong headings. included under
study from this description. the wrong sub-
section.
Correctly describes the
reagents, samples, Sentences are
independent variable(s) and not in passive
dependent variable(s) used in voice.
the experiment.
Verbs are not in
past tense.

Criteria 16-20 11-15 6-10 1-5 0 Marks

Results Logical and clear Standard deviations or Does not appear to Has graphs or Section
presentation of relevant standard errors have understood the tables, but missing
descriptive and inferential missing from tables or results. Only skimpy without any completely.
statistical results. Clear, well- graphs, figures/tables or inaccurate accompanying
labeled figures and tables, labeled incorrectly. explanations written
with a clear accompanying Does show some supplied. No graphs, explanation. Or
written description of what understanding, and has or irrelevant graphs, has some
they show, in the context of presented the or only with the raw writing, but no
the study. information in a data. tables or graphs.
logical format.

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Criteria 16-20 11-15 6-10 1-5 0 Marks

Discussion Clear summary of main Poor structure, but Poor structure, things Skimpy (e.g. Section
results, followed by a contains the essential in the wrong order, one paragraph) missing
successful attempt to relate elements. Or the shows little with no attempt completely.
the findings to relevant structure is good, but understanding of to relate results
previous theoretical and elements are missing. what the study was to relevant
empirical research. about, what the theoretical and
Intelligent evaluation of the results mean, or how empirical
strengths, weaknesses and they relate to research.
limitations of the study that previous work.
has been performed, and
sensible suggestions for
possible improvements and
extensions to it. Well
organized and clearly
written.

Criteria 5-8 1-4 0 Marks

Conclusion(s) Summary of key findings and relates A general overview of the Section missing completely.
them to the hypothesis. experimental results; does not relate to
the hypothesis.

Criteria 5-8 1-4 0 Marks

Reference(s) Complete references to sources used Incomplete references to sources used Section missing completely.
in report; with correct referencing in report; incorrect referencing style.
style.