Lab Manual PST594
Lab Manual PST594
Characterization Laboratory
PST594
Polymer Technology
School of Industrial Technology
Faculty of Applied Sciences
UiTM Shah Alam
Experiment 3: ULTRA-VIOLET
SPECTROPHOTOMETRY
Before starting the work in a laboratory, familiarize yourself with the following:
• The hazards of the materials in the lab, as well as appropriate safe handling, storage
and emergency protocol. Read labels and material safety data sheets (MSDS) before
moving, handling or opening chemicals. Never use a product from an unlabeled
container, and report missing labels to the laboratory technicians.
• The agents, processes and equipments in the laboratory. If you are unsure of any
aspect of a procedure, check with your instructor before proceeding.
• The locations and operation of safety and emergency equipments such as fire
extinguishers, eye was and shower, first aid and spill response kits, fire alarm pull
stations, telephone and emergency exits.
• Emergency spill response procedures for the materials you will handle.
• Emergency reporting procedures and telephone numbers.
• Designated and alternate escape route.
• Restrict laboratory access to authorized persons only. Children are not permitted in
labs
• Smoking, eating, drinking, storage food, beverages or tobacco, applying cosmetics or
lip balm and handling contact lenses are not permitted in laboratories.
• Wear lab coats (knee length) and safety glasses in laboratory employing chemicals,
biohazards, radioisotopes. Open shoes, such as sandals, should never be worn in the
lab.
• Tie back or otherwise restrain long hair when working with chemicals, biohazards,
radioisotopes.
• Keep workplace clean and free of unwanted chemicals.
• Reports accidents and dangerous incidents promptly to your instructor
• Wash your hand thoroughly before leaving the laboratory
1. LOG BOOK
Students are required to have a log book to record any chemicals used, weight,
volume, concentration and all observations made during the laboratory experiments.
Students must write the outline of the lab experiment before coming to lab session.
Students need to present the log book along with answer to Pre-Lab Questions to the
instructor before experimental work started.
2. COVER PAGE
i) Introduction
ii) Objective(s)
iii) Apparatus/chemical/procedure – must be written in passive form
iv) Results and Data
v) Discussion – refer appendix 1
vi) Conclusion – This section should be short and concise and should be related to
the objective(s) of the experiment.
vii) References.
INTRODUCTION:
Infra-red radiation is part of the electromagnetic radiation that encompasses all the
wavelength between the visible and microwave regions of the electromagnetic spectrum. The
IR region can be divided into smaller regions known as near-IR, mid-IR and far-IR. The
ranges of each region are summed up in the table below:
In order to absorb infrared radiation, a molecule must undergo a net change in dipole moment
as a consequence of its vibrational or rotational motion. Nearly all molecules containing
covalent bonds will show some degree of IR absorption. The only exceptions are the diatomic
molecules such as H2, N2, O2 etc. in which there is not net change in dipole moment when
they vibrate or rotate. The IR spectra of polyatomic covalent compounds are often
exceedingly complex, consisting of numerous narrow absorption bands.
OBJECTIVES:
MATERIALS:
Solid sample:
Thin film: Polyethylene terephthalate (PET)
Liquid sample:
INSTRUMENT:
SAMPLE PREPARATION:
Solid sample
1. Solid sample (in powder form) are grind with KBr in ration 1:9 (sample: KBr).
2. Mixture of sample is compress using hang presser to form KBr disc.
Note: make sure the thin film is thin as possible.
Liquid sample
Sample parameters
Sample parameters
Name : ______________________________________________
Student ID : ______________________________________________
INTRODUCTION:
Principles of FTIR
An ATR accessory operates by measuring the changes that occur in an internally reflected IR
beam when the beam comes into contact with a sample. An IR beam is directed onto an
optically dense crystal with a high refractive index at a certain angle. This internal reflectance
creates an evanescent wave that extends beyond the surface of the crystal into the sample
held in contact with the crystal.
In regions of the IR spectrum where the sample absorbs energy, the evanescent wave will be
attenuated. The attenuated beam returns to the crystal, then exits the opposite end of the
crystal and is directed to the detector in the IR spectrometer. The detector records the
attenuated IR beam as an interferogram signal, which can then be used to generate an IR
spectrum.
OBJECTIVES:
1. To carry out a qualitative analysis of polymer samples e.g.: PET (film),
2. To identify IR absorption peaks and the corresponding functional groups of the tested
samples.
MATERIALS:
Solid sample :
Thin film : Polyethylene terephthalate (PET)
Liquid sample :
Name : ______________________________________________
Student ID : ______________________________________________
ULTRA-VIOLET SPECTROPHOTOMETRY
INTRODUCTION:
Visible light is the name given to the narrow band of electromagnetic spectrum which
the pigment of our eyes can absorb and allow us to detect. Light itself can split into spectrum
of colours that we see in a rainbow, different colour signify different wavelengths and
therefore, different energies. A beam of light consisting of only one colour is called
monochromatic. The energy of a mole of photons of any one colour is given by the
relationship:
E=hv
Where E = energy, h = Plank’s constant and v = frequency of light ( remember that frequency
and wavelength of light are related by c=v9λ where c = velocity of light, v = frequency and λ
= wavelength. Red light has a longer wavelength than blue light and therefore lower
frequency and lower energy.
Light will be absorbed by an atom, ion or molecule when the energy of one quantum
of light matches the energy required to cause an electron in outer orbital to jump to a higher
energy level. Each absorption band is caused by the transition between a given pair of energy
level; because the energy level differences vary with the different electronic structures,
absorption spectra can be often used to identify the analyte atom, ion or molecule.
A= abc or A=ϵbc
Two types of analysis can be done with the visible absorption measurements.
OBJECTIVES:
MATERIALS:
Standard KMnO₄ with the concentration of 1000 ppm and an unknown concentration of an
unknown concentration of KMnO₄.
INSTRUMENTS
During this laboratory experiment you will make a series of dilutions, and then take the
absorbance of the dilutions at λmax. The permanganate ion absorbs at 534 nm and it is at this
wavelength that we will determine the absorbance values for the solutions. In this
experiment, an initial permanganate stock solution is prepared and the solutions to be
measured are diluted from a dilution of the stock. Once the absorbance values are taken,
generate a Beer’s Law plot for KMnO₄ and determine the concentration of the unknown
solution.
1. Weigh accurately 0.01 g of KMnO₄ to the nearest mg, on a weighing paper. Record
the reading. Using a funnel, transfer the solid to a 100 mL volumetric flask.
2. Dissolve the solid with a few mL of distilled water. Stopper and shake the flask. Add
distilled water to the mark, using a medicine dropper to add the last few drops.
Stopper the flask and shake several times to homogenize the solution.
3. Pour the ‘stock’ solution into a beaker. Label the beaker as ‘100 ppm’.
4. Pipet 5.00 mL of the ‘stock’ solution and dilute with distilled water in a 100 mL
volumetric flask.
5. Transfer into a beaker and label as it as ‘5 ppm’.
6. Repeat Step 4, using a 10 mL, 15 mL and 20 mL stock solution and transfer into small
beakers.
7. Label the beakers as ’10 ppm’, ’15 ppm’, and ’20 ppm’, respectively.
1. Pipet between 5.00 to 20.00 ml of the 'stock' KMnO₄ solution and dilute with distilled
water in a 100 mL volumetric flask.
2. Transfer into a beaker and label it as *Unknown'.
Take the absorbance reading of each of your samples in succession, starting with the least
concentrated and sequentially moving up to the most concentrated solution.
CAUTION - When using spectrophotometers, all of your data must be taken on the same
instrument, at the same time. If you need to change instruments you must start over and
take all of the data for the spectrum again.
Remember that your blank is always the same as the solvent, in this case, distilled water.
Each spectrophotometer will need one cuvette for the blank, and each student will need one
cuvette for the sample. In order to 'clean' the cuvette so that a sample is at the appropriate
concentration, add a small amount of the 'new' solution using a medicine dropper and rinse
the sides of the cuvette with the solution. Rinse the cuvette three separate times in this way,
and then only fill with the sample before taking the absorbance reading.
Name : ______________________________________________
2. What features of molecular structure does the UV absorber have which enable it to
absorb light in the UV region of the electromagnetic spectrum.
_____________________________________________________________________
_____________________________________________________________________
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INTRODUCTION:
The thermal stability of a plastic varies with the type of plastic and concentration of additives.
It affects both processing and end use performance of the plastic part. It is important that
incoming materials are by equipment without thermal decomposition.
This hangdown balances have very high sensitivity up to 107 g. The main disadvantage of
this type of balance is the inconvenience in the placement of a temperature thermocouple in
contact with the sample compared to a horizontal balance which does not indirect contact
with sample except placing near sample.
• ANALYSED DATA by
• Taking temperature reading at 95% or 90% decomposition.
• Taking extrapolating tangent of step curves from obtained plateau.
• Taking of % of thermal decomposed during each decomposition step.
• Find % residue under graded species from % remains to 0%.
• Plot also the DTG or derivative data. Maximum decomposition rate is the peak in the
curve which is shown as steps in TG thermogram.
Name : ______________________________________________
1. What information can we get from TGA/DSC thermograms for polymer applications?
_____________________________________________________________________
_____________________________________________________________________
_____________________________________________________________________
2. Why the thermal decomposition must reach to high temperatures above 700°C to
complete the degradation for hydrocarbon-based polymers?
_____________________________________________________________________
_____________________________________________________________________
_____________________________________________________________________
4. How does derivative of TGA curve explain for its minima curve?
_____________________________________________________________________
_____________________________________________________________________
_____________________________________________________________________
INTRODUCTION:
In DSC, the difference in heat flow between a sample and inert reference is measured
as a function of time and temperature as both the sample and reference are subjected to a
controlled environment (pressure, purge gas). The degree of crystallinity, X is determined
from the ratio of the heat of fusion of a polymer sample, Als, and the enthalpy of fusion of a
100% crystalline sample AHc.
X = ΛHsc
ΛHsc
OBJECTIVE:
1. To determine glass transition temperature (Tg), melting temperature (Tm) and percent
of crystallinity of unknown sample
MATERIAL:
INSTRUMENT:
1. Weigh about 5-10 mg sample into the aluminum pan using an analytical balance.
Record the exact mass of the sample.
2. Placed the sample in the DSC sample holder on the left side. Another pan on the right
side is leaving empty for references.
3. Open the software (Jade DSC)
4. Open METHOD EDITOR P SAMPLE ~ FILE NAME b BROWSE ~ SAVE
5. Open the INITIAL STATE INFO, setting the parameter.
• Temperature range : 20 - 300°C
• Heat flow : 20°C/min
• Flow of nitrogen : 30mL/min
6. Click INSTRUMENT VIEW ˃ APPLY ˃ START BUTTON
7. Graph analysis
• Rescale the graph using display function
• On calculate function, click peak area
• Tick onset and end peak height
• Click calculate
Name : ______________________________________________
Sample name
Weight
Heating Rate
Tm (Melting temperature)
λ Hf (Heat of fusion)
Tc (Crystallization temperature)
Lecturer’s signature:
__________________________