ANALYTICAL AND ORGANIC CHEMISTRY

CLD 10803
SEMESTER JANUARY 2020

CLD 10803 – Lab Assignment 2 (8% of final grade)

EXPERIMENT 3 AND EXPERIMENT 4

All the components in this assignment need to submit on 7/5/2020.

____/100 marks

Background and Content:

The purpose of this assignment is to help you to understand the methods of Experiment 3 and
Experiment 4 through the videos related to the experiments. In addition, it also help you to explore
connections between the lecture class learning and the experiments. In order to accomplish these
goals, this assignment has 2 sections.

Section 1 – Experiment 3 (60 marks)

In Section 1, there are 3 parts to fulfil this assignment.

 Part 1 – Preparation of Ethyl Ethanoate (Ester) – VIDEO 1 (20 marks)

This part contains the specific questions to review the methodology, materials and
etc. of the preparation of ethyl ethanoate.

 Part 2 – Utilization of FTIR for sample analysis – VIDEO 2 (20 marks)

This part to assist your understanding on how to prepare the samples and conduct
the analysis using FTIR.

 Part 3 – Utilization of GC for sample analysis – VIDEO 3 (20 marks)

This part to help you to learn on how to analyse the samples using UV-vis.

Section 2 – Experiment 4 (40 marks)

In Section 2, there is 2 part in this assignment.

 Part 1 – Preparation the sample solutions and standard solutions (20 marks)
This part to ensure that you know how to calculate the concentration in order to
prepare the standard solutions and plotting the calibration curve.

 Part 2 – Analysis samples and standard solutions using HPLC – VIDEO 4 (20 marks)
This part to help you to understand the function of HPLC in the analysis.

Learning Outcomes:
The learning outcome (CLO) is CLO2 and will assess your cognitive domain on top of this CLO.

Grading:
The marks have been attributed to each parts.

Assignment submission:
All complete assignment need to submit through my email: nadiah_usm@yahoo.com with Microsoft
words or PDF format.

Other things to note:

Kindly put or paste your name, ID number and signature (e-signature) in your assignment documents.
This is individual assignment.

UNIVERSITI KUALA LUMPUR

(UNIKL MICET)
NNMY
 ANALYTICAL AND ORGANIC CHEMISTRY
CLD 10803
SEMESTER JANUARY 2020

Section 1 – Experiment 3 (60 marks)

Part 1 – Preparation of Ethyl Ethanoate (Ester) – VIDEO 1 (20 marks)

1. Suggest the precaution that we need to take before this experiment started.
(4 marks)
2. During this experiment, she put the round bottom flask in ice bath before adding the
concentrated of sulfuric acid, 98%. Give the reason.
(4 marks)
3. Give the differences between reflux and distillation process.
(6 marks)
4. Give the function of sodium carbonate (Na2CO3) and calcium chloride (CaCl) in this
experiment.
(4 marks)

Part 2 – Utilization of FTIR for sample analysis – VIDEO 2 (20 marks)

1. Give full name of ATR.

(2 marks)
2. In this video, it shows the FTIR instrumentation diagram. Summarize clearly the process inside
FTIR equipment by using the same diagram in this video. You may give your answer in points.
(10 marks)
3. In FTIR spectrum, what is the information that you can obtain?
(4 marks)
4. By using the samples produced in Part 1 which is ethyl ethanoate, suggest the possible
functional group in this compound.
(4 marks)

Part 3 – Utilization of UV-vis for sample analysis – VIDEO 3 (20 marks)

1. Give the comparison between stationary phase and mobile phase.

(8 marks)
2. Determine the type of gas used for this instrument.
(2 marks)
3. Draw the GC instrument diagram in order to understand the process in the instrument.
(10 marks)

UNIVERSITI KUALA LUMPUR

(UNIKL MICET)
NNMY
 ANALYTICAL AND ORGANIC CHEMISTRY
CLD 10803
SEMESTER JANUARY 2020

Section 2 – Experiment 4 (40 marks)

Part 1 – Preparation the sample solutions and standard solutions (20 marks)
In this part, you may refer any sources to answer the questions.

1. Show the calculation (with correct equation) of concentration of caffeine standards which are
2 M, 4 M, 6 M, 8 M and 10 M from caffeine stock solution which the concentration is 100 M.
You need to put all the answer after calculation in one table in Excel sheet.
E.g. (All calculation data need to put in table in Excel sheet)

Concentration Volume (after calculation)

2M
4M
6M
8M
10 M
(10 marks)
2. After analysis of caffeine standard solution and sample using HPLC instrument, the data can
be summarized as shown in Table 1. Plot the calibration curve (concentration (x-axis) vs area
(y-axis)) of caffeine standard solutions and determine the concentration of sample if the area
under the graph is 113698.

In the calibration curve, you need to:

a) Copy and paste the data in Table 1 in excel sheet.
b) Plot the graph by choosing SCATTER (points)

c) After the graph have been plot, right click and go to FORMAT TREADLINE, click set intercept,
display equation and display R2 value.
d) Then you can determine the concentration of sample.

Table 1: HPLC data for caffeine standard solutions

Concentration Area
2M 20356
4M 45638
6M 80123
8M 108963
10 M 124957
(10 marks)

UNIVERSITI KUALA LUMPUR

(UNIKL MICET)
NNMY
 ANALYTICAL AND ORGANIC CHEMISTRY
CLD 10803
SEMESTER JANUARY 2020

Part 2 – Analysis samples and standard solutions using HPLC – VIDEO 4 (20 marks)

1. State the volume of sample needed to analyse using HPLC instrument.

(2 marks)
2. Draw the HPLC diagram in order to understand the process in the instrument.
(10 marks)
3. There is one technique she use to avoid ‘something’ in syringe before her injecting the samples
or standard solutions in HPLC instrument. Identify what is ‘something’ refer to and state the
technique she used.
(8 marks)

ALL THE BEST

UNIVERSITI KUALA LUMPUR

(UNIKL MICET)
NNMY