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Experiment 5 AAS

This laboratory report summarizes an experiment using high-performance liquid chromatography (HPLC) to determine the concentration of copper in samples. Standard solutions with known copper concentrations were used to generate a calibration curve of absorbance versus concentration. Unknown samples were then analyzed to determine their copper concentrations based on the calibration curve. The results showed increasing absorbance with increasing standard solution concentration as expected. The goal of measuring copper concentration in samples was achieved. Recommendations included checking for errors in measurements and bubbles that could affect results.

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0% found this document useful (0 votes)
450 views15 pages

Experiment 5 AAS

This laboratory report summarizes an experiment using high-performance liquid chromatography (HPLC) to determine the concentration of copper in samples. Standard solutions with known copper concentrations were used to generate a calibration curve of absorbance versus concentration. Unknown samples were then analyzed to determine their copper concentrations based on the calibration curve. The results showed increasing absorbance with increasing standard solution concentration as expected. The goal of measuring copper concentration in samples was achieved. Recommendations included checking for errors in measurements and bubbles that could affect results.

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nn bb
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
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UNIVERSITI KUALA LUMPUR

MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING


TECHNOLOGY
LABORATORY REPORT SUBMISSION FORM
January Semester 2021

SECTION A – Filled up by Student


Subject & Code ANALYTICAL AND ORGANIC CHEMISTRY CLB 10803
Title of Experiment Experiment 5 – DETERMINATION OF COPPER USING AAS
Date of Experiment 26th April 2021 Section
Marks Jotter Notes Peer Evaluation Total
Group Members ID No.
(90%) (5%) (5%) (100%)
TM1) Ilyas Fikri b. Mohd Said 55213220037
TM2) Mohd Danish Zikry b. Mohd Hatta 55218119184
TM3) Mohd Adam b. Mohd Sofian 55218220016
TM4) Muhd Azizul Faiz b. Mohd Rozmi 55216220004
TM5)
Name of Lecturer Ms Norhayati Binti Mohd Idrus

SECTION B – Filled up by Lecturer


NOT VERY VERY
CRITERIA POOR GOOD EXCELLENT
Included POOR GOOD
1.0 INTRODUCTION (20%) – State the background or theory of the
0 4 8 12 16 20
experiment.
2.0 RESULTS (25%) – Results are presented a deemed suitable with
0 5 10 15 20 25
complete label & units. (Table/Graph/Figure etc.)
3.0 DISCUSSION (30%) – (i) Explanations of the referred table and
figure are presented after the table and figure.
0 6 12 18 24 30
(ii) Discuss on the findings and the relations to the theory and
objectives of the experiment.
4.0 CONCLUSION & RECOMMENDATIONS (20%) – The conclusion
should begin with a restatement of the results. The results should
be compared with literature values/theory whenever possible. Any 0 4 8 12 16 20
possible sources of error should be identified. Suggest your
recommendation (s) for the improvement of the experiment.
5.0 REFERENCES (5%) 0 1 2 3 4 5
6.0 JOTTER NOTE (5%) – Prepare a summary on the methodology of
the experiment (flowchart, diagram etc). Submit the jotter note Refer to Individual Jotter Note
along with respective lab report.
7.0 PEER EVALUATION (5%) - Team work, submit the peer
Refer to Peer Evaluation Form
evaluation form along with respective lab report.

TOTAL PERCENTAGE (90%)


1.0 INTRODUCTION

High performance liquid chromatography (HPLC) is a type of chromatography which is very


similar to liquid chromatography. In HPLC, however, the stationary phase column is more tightly
packed than in other types of liquid chromatography. In this lab, the column is packed with C18
particles that are less than 10 μm in diameter. The small diameter of the particles allows
unprecedented resolution and high efficiency. Since the particles in the column are so small, it is
necessary to pump the mobile phase through the column at a very high pressure. The pump keeps a
precise flow rate so that the positions of the peaks in time can be used to identify the species in a
sample. This is done by comparing the chromatographs of prepared standards of the particular
species to be determined. The common peak is an indication of the standard.

Figure 1: Schematic Diagram of High Performance Liquid Chromatography


2.0 RESULTS

Concentration of Standard Absorbance


Solutions ( ppm )
1 0.048
2 0.111
3 0.156
4 0.222
5 0.269
Unknown 1 0.046
Unknown 2 0.091

Table 1: Concentration standard solution results and absorbance results

Determination of Copper(cu) using AAS


0.3

0.25

0.2
Absorbance

0.15

0.1

0.05

0
1 2 3 4 5
Concentration of standard solution (ppm)

Series 1

Figure 1: Graph Determination of Copper (Cu) using AAS, Absorbance vs standard solution
concentrations

3.0 DISCUSSION
The objective of this experiment is to optimize the burner system by flame AAS using
standard solution, to check the performances (sensitivity) of the atomic absorption
spectroscopy using standard solutions, to prepare a serial dilution and generate a standard
calibration curve and to determine the amount of Cu in the unknown sample. AAS is used to
measure the concentration of gas-phase atoms with light absorbing ultraviolet light or visible
light that will excite an electron from a lower energy level to a higher energy level. Atomic
Absorption Spectrophotometer(AAS) will be analysed all elements of the participant in this
study will be analysed. Then, atomic absorption spectroscopy process involves two steps
atomized sample and absorbed radiation from a light source by free atoms. At the first stage
mechanism, the analyte atoms or ions must be burned in the flame or specifically furnace
graphics. The fire was marching in the light of appropriate wavelength. Atom will undergo a
transition from the ground state to the first excited state because of the fire. Then the atoms
moving their transition, they will absorb some of the light from the beam.

This experiment was started with preparation of 100 ppm of ferum standard solution.
Next, series of standard solution with concentration of 1.0 ppm, 2.0 ppm, 3.0 ppm, 4.0 ppm
and 5.0 ppm. These concentration was calculated using M1V1 = M2V2. Next, operating the
AAS to optimizing the burner system and checking the performance of characteristic
concentration. After that, creating a calibration curve and analysing the samples. Lastly, shut
down the instrument.

A calibration curve was used to determine the unknown concentration of an element


in a solution. The instrument was calibrated using several solutions of known concentrations.
The absorbance of each known solution was measured and then a calibration curve of
concentration vs. absorbance was plotted. From the calibration graph a linear relationship
formed. The calibration curve is always represented with the absorbance (y) and the
concentrations on the horizontal (x). The calibration curve is generally used when there is a
linear relationship between analytical signal (y) and concentration (x) taking precautions to
ensure that linearity in the experimental response is maintained over a wide range of
concentrations. Based on the graph, when the concentration of solution increased, the
absorbance increased. If the concentration of solution is increased, then there are more
molecules for the light to hit when it passes through.
Based on the results, the absorbance reading for 1.0 ppm, concentration of standard
solution until 5.0 ppm was slightly increased from 0.048 to 0.269. This is because if we relate
the result with the Characteristics Concentration formula, where the Known Concentration
Used multiply by 0.0044 and divide with Absorbance value for known concentration used.
The Concentration of Standard Solution must follow the order from 1.0 ppm, 2.0 ppm, 3.0
ppm, 4.0 ppm and 5.0 ppm. If not, the result will not be achieved in linear working range.
4.0 CONCLUSION AND RECOMMENDATIONS

The goal of this experiment was met when the Cu content in a sample was effectively
measured. This experiment was carried out using high-performance liquid chromatography
(HPLC). The highest peak area for this experiment, based on the results, is at 5 ppm with
0.269 µv.s. This suggests that the outcome was consistent with the hypothesis, which claims
that the higher the concentration, the larger the peak area, and that a larger concentration has
a stronger influence on the area. Form the result obtained, was erroneous owing to parallax
mistake or incorrectly measuring the titration solution, as well as the presence of bubbles in
the syringe injected into HPLC. The standard addition plots provided R2 values that were
near to 1, indicating that the procedure of standard addition was successful, notwithstanding
the comparison of computed and literature values of the examined concentrations.
5.0 REFERENCE
1. http://www1.lasalle.edu/~prushan/Intrumental%20Analysis_files/AAPerkin%20Elmer
%20guide%20to%20all!.pdf
2. https://www.scimed.co.uk/education/what-is-atomic-absorption-spectroscopy-aas/
6.0 JOTTER NOTES
7.0 Appendix
7.0 PEER EVALUATION

UNIVERSITI KUALA LUMPUR


MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING
TECHNOLOGY

PEER EVALUATION FORM: LAB REPORT


Analytical & Organic Chemistry (CLB 10803)
January Semester 2021

STUDENT NAME : ILYAS FIKRI BIN MOHD SAID


STUDENT ID : 55213220037

1. Rate your team members on the relative contribution that were made in preparing and submitting your group assignment.
2. In rating your peers, use to five point scale.
3. Every single group member is to fill in this form and be honest, do not favour anyone. Form is to be submitting along with the respective
submission.

5- Always 4- Most of the time 3- Sometimes 2- Rarely 1-Never

Names: MOHAMAD Names: MOHD Names: MUHAMMAD Names:


DANISH ZIKRY BIN ADAM BIN MOHD AZIZUL FAIZ BIN
MOHD HATTA SOFIAN MOHD ROZMI
Criteria
ID:55218119184 ID:55218220016 ID:55216220004 ID:

(1) Quality of Technical Work: Work is


correct, clear, complete, and relevant to the 5 5 5
problem. Equations, graphs, and notes are
clear and intelligible.
(2) Commitment to Team / Project: Attends
5 5 5
all meetings. Arrives on time or early.
Prepared. Ready to work. Dependable,
faithful, reliable.
(3)Leadership: Takes initiative, makes
suggestions, provides focus. Creative? 5 5 5
Energetic? Brings energy and excitement to
the team. Has a “can do” attitude. Sparks
creativity in others.
(4) Responsibility: Gladly accepts work and 5 5 5
gets it done. Spirit of excellence.
(5)Has abilities the team needs. Makes the
most of these abilities. Gives fully, doesn’t 5 5 5
hold back.
(6) Communication: Communicates clearly
when he/she speaks and when she/he 5 5 5
writes. Understands the team’s direction.
(7) Personality. Positive attitudes,
5 5 5
encourages others. Seeks consensus. Fun to
deal with. Brings out best in others.
Peacemaker. Pours water, not gasoline on
fires.
TOTAL MARK (35%) 35 35 35
TOTAL MARK (5%) 5 5 5

Keep in mind that if you award high scores to everyone, regardless of their contribution, team members who have worked unduly hard or
provided extraordinary leadership will go unrecognized, as will those at the other end of the scale who need your corrective feedback.
UNIVERSITI KUALA LUMPUR
MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING
TECHNOLOGY

PEER EVALUATION FORM: LAB REPORT


Analytical & Organic Chemistry (CLB 10803)
January Semester 2021

STUDENT NAME : MOHAMAD DANISH ZIKRY BIN MOHD HATTA


STUDENT ID : 55218119184

4. Rate your team members on the relative contribution that were made in preparing and submitting your group assignment.
5. In rating your peers, use to five point scale.
6. Every single group member is to fill in this form and be honest, do not favour anyone. Form is to be submitting along with the respective
submission.

5- Always 4- Most of the time 3- Sometimes 2- Rarely 1-Never

Names: ILYAS FIKRI Names: MOHD Names: MUHAMMAD Names:


BIN MOHD SAID ADAM BIN MOHD AZIZUL FAIZ BIN
SOFIAN MOHD ROZMI
Criteria
ID:55213220037 ID:55218220016 ID:55216220004 ID:

(1) Quality of Technical Work: Work is


correct, clear, complete, and relevant to the 5 5 5
problem. Equations, graphs, and notes are
clear and intelligible.
(2) Commitment to Team / Project: Attends
5 5 5
all meetings. Arrives on time or early.
Prepared. Ready to work. Dependable,
faithful, reliable.
(3)Leadership: Takes initiative, makes
suggestions, provides focus. Creative? 5 5 5
Energetic? Brings energy and excitement to
the team. Has a “can do” attitude. Sparks
creativity in others.
(4) Responsibility: Gladly accepts work and 5 5 5
gets it done. Spirit of excellence.
(5)Has abilities the team needs. Makes the
most of these abilities. Gives fully, doesn’t 5 5 5
hold back.
(6) Communication: Communicates clearly
when he/she speaks and when she/he 5 5 5
writes. Understands the team’s direction.
(7) Personality. Positive attitudes,
5 5 5
encourages others. Seeks consensus. Fun to
deal with. Brings out best in others.
Peacemaker. Pours water, not gasoline on
fires.
TOTAL MARK (35%) 35 35 35
TOTAL MARK (5%) 5 5 5

Keep in mind that if you award high scores to everyone, regardless of their contribution, team members who have worked unduly hard or
provided extraordinary leadership will go unrecognized, as will those at the other end of the scale who need your corrective feedback.
UNIVERSITI KUALA LUMPUR
MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING
TECHNOLOGY

PEER EVALUATION FORM: LAB REPORT


Analytical & Organic Chemistry (CLB 10803)
January Semester 2021

STUDENT NAME : MOHD ADAM BIN MOHD SOFIAN


STUDENT ID : 55218220016

1. Rate your team members on the relative contribution that were made in preparing and submitting your group assignment.
2. In rating your peers, use to five point scale.
3. Every single group member is to fill in this form and be honest, do not favour anyone. Form is to be submitting along with the respective
submission.

5- Always 4- Most of the time 3- Sometimes 2- Rarely 1-Never

Names: ILYAS FIKRI Names: MOHAMAD Names: MUHAMMAD Names:


BIN MOHD SAID DANISH ZIKRY BIN AZIZUL FAIZ BIN
MOHD HATTA MOHD ROZMI
Criteria
ID:55213220037 ID:55218119184 ID:55216220004 ID:

(1) Quality of Technical Work: Work is


correct, clear, complete, and relevant to the 5 5 5
problem. Equations, graphs, and notes are
clear and intelligible.
(2) Commitment to Team / Project: Attends
5 5 5
all meetings. Arrives on time or early.
Prepared. Ready to work. Dependable,
faithful, reliable.
(3)Leadership: Takes initiative, makes
suggestions, provides focus. Creative? 5 5 5
Energetic? Brings energy and excitement to
the team. Has a “can do” attitude. Sparks
creativity in others.
(4) Responsibility: Gladly accepts work and 5 5 5
gets it done. Spirit of excellence.
(5)Has abilities the team needs. Makes the
most of these abilities. Gives fully, doesn’t 5 5 5
hold back.
(6) Communication: Communicates clearly
when he/she speaks and when she/he 5 5 5
writes. Understands the team’s direction.
(7) Personality. Positive attitudes,
5 5 5
encourages others. Seeks consensus. Fun to
deal with. Brings out best in others.
Peacemaker. Pours water, not gasoline on
fires.
TOTAL MARK (35%) 35 35 35
TOTAL MARK (5%) 5 5 5

Keep in mind that if you award high scores to everyone, regardless of their contribution, team members who have worked unduly hard or
provided extraordinary leadership will go unrecognized, as will those at the other end of the scale who need your corrective feedback.
UNIVERSITI KUALA LUMPUR
MALAYSIAN INSTITUTE OF CHEMICAL BIOENGINEERING
TECHNOLOGY

PEER EVALUATION FORM: LAB REPORT


Analytical & Organic Chemistry (CLB 10803)
January Semester 2021

STUDENT NAME : MUHAMMAD AZIZUL FAIZ BIN MOHD ROZMI


STUDENT ID : 55216220004

1. Rate your team members on the relative contribution that were made in preparing and submitting your group assignment.
2. In rating your peers, use to five point scale.
3. Every single group member is to fill in this form and be honest, do not favour anyone. Form is to be submitting along with the respective
submission.

5- Always 4- Most of the time 3- Sometimes 2- Rarely 1-Never

Names: ILYAS FIKRI Names: MOHD Names: MOHAMAD Names:


BIN MOHD SAID ADAM BIN MOHD DANISH ZIKRY BIN
SOFIAN MOHD HATTA
Criteria
ID:55213220037 ID:55218220016 ID:55218119184
ID:
(1) Quality of Technical Work: Work is
correct, clear, complete, and relevant to the 5 5 5
problem. Equations, graphs, and notes are
clear and intelligible.
(2) Commitment to Team / Project: Attends
5 5 5
all meetings. Arrives on time or early.
Prepared. Ready to work. Dependable,
faithful, reliable.
(3)Leadership: Takes initiative, makes
suggestions, provides focus. Creative? 5 5 5
Energetic? Brings energy and excitement to
the team. Has a “can do” attitude. Sparks
creativity in others.
(4) Responsibility: Gladly accepts work and 5 5 5
gets it done. Spirit of excellence.
(5)Has abilities the team needs. Makes the
most of these abilities. Gives fully, doesn’t 5 5 5
hold back.
(6) Communication: Communicates clearly
when he/she speaks and when she/he 5 5 5
writes. Understands the team’s direction.
(7) Personality. Positive attitudes,
5 5 5
encourages others. Seeks consensus. Fun to
deal with. Brings out best in others.
Peacemaker. Pours water, not gasoline on
fires.
TOTAL MARK (35%) 35 35 35
TOTAL MARK (5%) 5 5 5

Keep in mind that if you award high scores to everyone, regardless of their contribution, team members who have worked unduly hard or
provided extraordinary leadership will go unrecognized, as will those at the other end of the scale who need your corrective feedback.

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