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37 Analytical Techniques: Analysis - Cie A-Level Chemistry
37 Analytical Techniques: Analysis - Cie A-Level Chemistry
AS
◦ If you’re starting in September 2020 with Year 12, then you’ll need to use the old syllabus for the AS in
May/June 2021.
◦ Only start this syllabus with AS in September 2020 if your students will take ALL the exams (AS & A2) at the
end of two years (May/June 2022).
A2
◦ Year 13 September 2020 old syllabus examined in 2021
◦ Year 13 September 2021 new (this) syllabus examined in 2022
Mastery learning information for the teacher:
There are increasingly more mastery learning definitions however they are all centred on the idea that students must achieve a defined proficiency
in a given unit of work before proceeding.
Repetition and practice are critical to mastery of different concepts as students proceed through the course. We need also to be mindful of retention
of the information to maintain mastery as a student works through the course over the 8 or 9 months before the examinations.
Mastery learning develops a growth mindset as the implication is that all students will understand all of the work. The variable is the time it takes
to master the different concepts.
In these A2 slide decks, mastery is encouraged by different styles of questioning, practice questions and relies of constant formative assessment by
the teacher. Only move on once everyone in the class is getting over 80% of the problems correct.
There are some more detailed suggestions on the website of how to use these presentations but arguably one of the most effective and the intended
approach is to use the flipped classroom model. It is advised to prepare additional practice as you progress through your own worksheets,
homeworks and extension activities, these can then be made available for those who work more quickly.
Retention is enhanced through spaced repetition in the starter activities and the allocation of complete A2 past paper questions.
The notes section of each slide provides links back to mastery learning ideas to provide the teacher with a rationale of what this slide is aiming to
achieve or test. It also includes answers and/or explanation of problems and questions for the teacher to consider as their students progress.
For additional support of questions related to mastery learning please email me at: content@chemcatalyst.co.uk
Starter 1: Retrieval Questions
What did you learn last lesson?
What did you learn last week?
What did you learn through an activity you organised yourself?
◦ independent reading, additional questions, research?
Starter 2: Amino acids
LINK
Thin Layer Chromatography
TLC is similar to paper chromatography which you
have almost certainly done earlier at school
Rather than using chromatography/filter paper the
stationary phase is a thin uniform layer (usually
silica gel) coated on a piece of plastic, metal or glass
The mobile phase is a liquid which acts as a solvent
for the substances you are trying to separate or
analyse
paper chromatography
Thin Layer Chromatography 1
1. A base line is drawn in pencil across the plate and dots of the substances are placed along the
linepeated application is used to increase the concentration
2. The plate is placed in a beaker of the solvent such that the level of the solvent is below the line and
the solvent moves up the plate.
3. A lid is placed to ensures that the atmosphere in the tank is saturated with the often volatile solvent
which climbs up the plate causing the mixture to separate
1 2 3
Thin Layer Chromatography 2
4 5 6
4. As the solvent front moves up the plate the purple mixture separates into a
fast moving red spot and a slower moving blue spot
5. The solvent reaches near to the top of the plate and the plate is removed
6. The solvent front (4) is noted and the solvent is left to evaporate
Rotating the sheet
This method can be developed into two dimensional chromatography
The sheet is rotated through 90° and a second solvent is used to further split the different components if
they initially overlap
rotated
through
90°
Calculating Rf
Assuming the following distances
◦ Base line to solvent front: 6 cm
◦ Base line to blue chemical: 2 cm
◦ Base line to red chemical: 5 cm
Rf = 2/6 = 0.33
Rf = 5/6 = 0.83
Providing the temperature and solvent is the same these R f values will remain the same if the experiment is
repeated
Calculating Rf
Once you have calculated the Rf value you can compare to a data source and identify which protein or
chemical substance you are dealing with
LINK
GLC
37.2 GAS / LIQUID CHROMATOGRAPHY
Gas-liquid
chromatography
A gas chromatography oven,
open to show a capillary
column
Gas-liquid chromatography 1
In GLC a long column is often filled with a polysiloxane liquid compound
In thinner tubes, the stationary phase is coated to the inside surface of the tube
The sample is vaporised and pushed through the column by an inert carrier gas (most often helium)
Gas-liquid chromatography 2
Depending on the solubility of the different compounds in the stationary liquid phase, their boiling
points and the temperature of the column, the different compounds will travel through the GLC column
at different speeds
The length of time a compound remains in the column is known as the retention time
It is calculated from the time the sample is injected until the maximum peak height for that
compound is observed on the display/chromatogram
Gas-liquid chromatography
LINK
Example results
In this example gas/liquid chromatogram we can see 3
peaks
Each peak corresponds to a different compound in the
sample and we can observe that they arrive at the detector in
sequence
They have different retention times
Proportion of components
C Remember the area of a triangle
The area under the peaks ◦ = ½ x base x height
can be used to calculate • Peak C
the composition of the Peak A
◦ Height: 17mm • Height: 110mm
mixture • Width: 5mm
◦ Width: 9mm
◦ Area: 76.5mm2 • Area: 225mm2
Peak B
B ◦ Height: 50mm
◦ Width: 4mm
A
◦ Area: 100mm2
96mm2 92mm2
time
NMR Spectroscopy
37.3 CARBON-13 NMR SPECTROSCOPY
NMR Spectroscopy
The nucleus’ of carbon and hydrogen atoms have magnetic
properties
Chemists use this property to determine information about
the structure and chemical environment of molecules
which contain the carbon and hydrogen atoms
NMR stands for
nuclear
magnetic
resonance
The other atoms attached to a carbon-13 atom mean that a slightly different magnetic field will need to
be applied to cause the resonance condition to occur in the carbon-13 nucleus
This can be used to work out the carbon atom's environment in the molecule
13
C-NMR Propan-1-ol
• In this 13C-NMR we can
see three peaks
• Is this what we would
expect?
• The structure of propan-
1-ol is:
1 2 3
• Carbon ‘1’, ‘2’ and ‘3’ are all in different environments when you look at the atoms they are
attached to and also the atoms that are attached to them
13
C-NMR Propan-1-ol
• The value at around 63 corresponds to the carbon with the alcohol group
• The value at 11 is the leftmost carbon
• The value at 26 is the middle carbon which is shifted further downfield as it
is nearer the electronegative oxygen
The scale
The x-axis represents the chemical shift, δ
It is the frequency of the resonance relative to a standard compound which sets the scale at 0 ppm
downfield upfield
3 2
180 160 140 120 100 80 60 40 20 0
δ ppm
• Carbon ‘2’ and ‘4’ are all in the same environment when you look at the atoms they are attached
to and also the atoms that are attached to them
• Carbon ‘1’ and ‘3’ are in different environments
Calculating the number of peaks
How many peaks would a molecule of heptane have?
1 2 3 4 5 6 7
◦ 3,3-dimethylpentan-2-ol?
NMR Spectroscopy
37.4 PROTON ( 1 H) NMR SPECTROSCOPY
1
H-NMR
In the same way as a nucleus of carbon-13, hydrogen nuclei (a single proton) are affected by a
magnetic field
The magnetic spin can align with a magnetic field or against it in a higher energy state
The difference in energy between the two states once again corresponds to the energy of a specific
radio frequency
The size of energy gap between the two alignments depends on the environment of the hydrogen
atom
H-NMR Propan-1-ol
1
(1)
(2)
9 8 7 6 5 4 3 2 1 0
δ ppm
(1)
(2)
9 8 7 6 5 4 3 2 1 0
δ ppm
• (2), (1), (2) and (3) are relative areas and again are in line with our structure
• areas not to scale
H-NMR Propan-1-ol
1
9 8 7 6 5 4 3 2 1 0
δ ppm
Naming split signals
We classify the number of peaks a signal has with the following names:
Singlet
◦ 0 hydrogen neighbours = 1 peak
Doublet
◦ 1 hydrogen neighbour = 2 peaks
Triplet
◦ 2 hydrogen neighbours = 3 peaks
Quartet
◦ 3 hydrogen neighbours = 4 peaks
}
Quintet (Pentet)
◦ 4 hydrogen neighbours = 5 peaks
Sextet multiplets
◦ 5 hydrogen neighbours = 6 peaks
Septet
◦ 6 hydrogen neighbours = 7 peaks
1
H-NMR Propan-1-ol
If a proton has n neighbours
(protons attached to adjacent carbons) le t
It will split into n+1 lines , t rip
=3
n+1
2 ,
n= plet
t ri
= 3,
2 , n+1
n =
-OH
gro
ups
are
al way
s sing
l et s
n = 5, n+ 1 = 6,
sextet
-OH and –NH bonds
The hydrogen on the -OH or –NH always forms a singlet
They do not interact with other hydrogens to produce any splitting in their peak or the peaks of
neighbouring hydrogens
D2O is used to eliminate the peak from –OH and –NH bonds and allow more accurate analysis
Introducing D2O causes hydrogens on the –OH and -NH in the compound to be replaced by deuterium
due to proton exchange in the alcohol and amino groups
Peaks created by –OD and –ND bonds appear in a different region of the spectra and are not
displayed
Spectra Examples
Examples
Creating a baseline
In order to compare peaks tetramethylsilane is used as an internal standard for
calibrating chemical shift for 1H and 13C NMR
All four carbons atoms and all twelve hydrogen atoms (relative to each other) in a
tetramethylsilane molecule are equivalent so a strong peak is created
Creating a baseline
The peak appears to the far right of the spectra due to the silicon atom
◦ The electrons in the C-Si bond are closest here to the carbon atom and hence shield it the most effectively
from the magnetic field meaning a very large magnetic field (hence far right) is needed to create the resonance
condition in the carbon atoms in 13C-NMR
◦ For 1H-NMR twelve hydrogens creates a strong singlet which can be easily identified
• Assuming the device varies magnetic field, a peak at 80 means that the carbon atoms causing the peak need a
magnetic field 80 millionths less than the field needed by the TMS to create a resonance condition
Solvents
Solid molecules need to be dissolved into solution for the NMR to be run
Deuterated solvents such as CDCl3 are used
The hydrogen atom in this chloroform molecule has been replaced with an atom of deuterium, an
isotope of hydrogen
As such it doesn’t have any hydrogen to interfere with a 1H-NMR spectra
It does have carbon atoms but CDCl3 creates an easily identifiable peak which can be easily discounted
when analysing the spectra for 13C-NMR
Summary: Proton Nuclear Magnetic Resonance (NMR)
LINK
Homework task
Create a worksheet for another member of the
class
It should focus on one particular area of the
course
You should have an answer sheet so you can
assist and your colleague and mark their work
Paper Session Year Question
Past Paper
43 October 2017 6
42 October 2017 3
Questions
42 October 2017 8
43 May 2017 6
42 May 2017 2