Analytical Flashcards

(39 cards)

1
Q

What is flight mass spectrometry

A

Where the elements in a compound are discovered via their mass

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2
Q

What are the stages of mass spec

A

Vaporisation
Ionisation
Acceleration
Time of Flight
Detection

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3
Q

What is vaporisation in mass spec

A

Dissolve the sample in a volatile solvent
Reduces pressure

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4
Q

What is ionisation in mass spec

A

Bombard sample with high energy elections, knocking off electrons to form 1+ charge
Fragmentation May also occur

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5
Q

What is acceleration in mass spec

A

Using the electric field to accelerate ions to give them equal kinetic energy

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6
Q

What is the equation for kinetic energy

A

Ke = 1/2 x m x v(squared)

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7
Q

What is time of flight in mass spec

A

Ions with different masses travel with different velocities

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8
Q

How does Carbon 13 NMR work

A

The difference in magnetic field between an atom with odd numbers of electrons and a large magnetic field can be measured by the absorption of radio waves to flip the nucleus

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9
Q

What atoms can be detected by NMR

A

H, C13

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10
Q

Why is a solvent used in NMR

A

To dissolve the organic substance without interfering with the spectrum

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11
Q

What are two commonly used NMR solvents

A

CCl4 (tetrachloromethane)
CDCl3 (deuterated brichloromethane)

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12
Q

How is NMR calibrated

A

The use of tetramethylsilane (TMS) creates a single peak at 0, so all other peaks are positioned relative to it

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13
Q

Why is TMS used

A

Generates a single peak in C13 and H NMR
Peak lies to right hand side of spectrum
Unreactive
Low boiling point so easy to remove from sample
Non toxic

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14
Q

What is the formula of TMS

A

C4H12Si

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15
Q

What does the number of peaks in C13 NMR tell us

A

The number of different carbon environments

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16
Q

What affects the height of peaks in C13 NMR

A

The more C atoms in that environment, the higher the peak

17
Q

What does the position of peaks tell us in C13 NMR

A

The type of chemical environment

18
Q

What does the number of signals in proton NMR show us

A

The number of hydrogen environments

19
Q

What does the intensity of the peak show in proton NMR

A

The number of hydrogen atoms in the environment

20
Q

What does the chemical shift(position of peak) show

A

The type of chemical environment

21
Q

What is the reference chemical for proton NMR

22
Q

What does the shape of peaks show in proton NMR

A

The number of adjacent hydrogens

23
Q

How can high resolution NMR chemical shift be calculated

A

Field for TMS - field of sample/ field for TMS x 10-6 ppm

24
Q

How does high resolution proton NMR differ from other NMR

A

Signals in high res H1 NMR are split, caused by the interactions of magnetic fields on hydrogen ions in neighbouring carbon atoms

25
What rule dictates the number of lines a signal is split into
Hydrogens on neighbouring atoms + 1
26
What determines retention time in gas chromatography
The higher the affinity for the stationary phase, the longer the retention time
27
What is the acidified dichromate test
Tests for alcohol
28
What is the result of the potassium dichromate test
Orange to green in presence of an alcohol
29
What alcohols turn green on the addition of potassium dichromate
Primary and Secondary
30
How does the Schiffs reagent test work
Warm the reaction mixture, then pass the vapours through cold Schiffs reagent
31
What are the results of Schiffs reagent
If Schiffs reagent turns magenta, it is a primary alcohol, if there’s no colour change it’s a secondary alcohol
32
What is the stationary phase for thin layer chromatography
Silica plate
33
What is the mobile phase for thin layer chromatography
Liquid solvent
34
What is the stationary phase for paper chromatography
High quality filter paper
35
What is the mobile phase for paper chromatography
Liquid solvent
36
What affects the rate at which a substance moves up the plate in TLC
Solubility of substance in solvent Attraction between solute and stationary phase
37
What is the use of a watch glass in TLC
Prevents evaporation of solvent
38
What must the pencil be in TLC
Insoluble so as not to affect the results
39
Where must the solvent level be in TLC
Solvent level below the pencil line to prevent washing off substance