modern analytical techniques Flashcards

1
Q

what occurs in a mass spectrometer

A

sample introduced to spectrometer
low M weight samples vaporise in the vacuum of by heating
ionisation
ions are accelerated in an electric field so they have similar kinetic energy
by varying the magnetic field all ions are focused into detector
the ions are detected and the mass spectrum is plotted

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2
Q

what is the largest m/z value peak (furthest to the right) from

A

the parent ion

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3
Q

what is fragmentation

A

molecules may split into fragments when bombarded with fast moving electrons
only charges fragments are detected

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4
Q

what is the most abundant peak called

A

the base peak

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5
Q

what does high resolution mass spectroscopy do

A

measure the m/z values to enough accuracy to find the molecular formula

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6
Q

how does infrared spectroscopy work

A

all bonds vibrate at a characteristic frequency
frequency depends on mass of atoms in the bond,bond strength and type of vibration
frequencies are in the infra-red region of the electromagnetic spectrum
if infra-red light passed through compound, will absorb all or some of light at the frequency it’s bonds vibrate

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7
Q

what is IR light measured in

A

wave numbers (1/frequency) in cm

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8
Q

what is liquid or column chromatography used for

A

separating large quantities of soluble substances

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9
Q

what is the stationary phase of liquid chromatography

A

powder (silicon dioxide)

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10
Q

what is the mobile phase of liquid chromatography

A

liquid solvent

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11
Q

how does liquid chromatography work

A

mixture dissolved in solvent and placed at top of column
as solvent moves down through powder in column, substances in mixture move down the column at different rates
allows them to be collected separately

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12
Q

what does time taken to move down column (in liquid chromatography) depend on

A

balance between solubility of each substance in the mobile phase
and it’s retention in the stationary phase

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13
Q

HPLC high performance liquid chromatography advantages

A

use of fine particles increases surface area of stationary phase which results in greater separation
uses a pump to force mobile phase through column and provides higher resolution and faster analysis time
can be done at room temp- can be used to separate mixtures that would decompose on heating

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14
Q

how does HPLC work

A

eluent passes through a detector
(UV absorption is usually monitored)
detector indicates the presence of the substance of interest but cannot determine the concentration

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15
Q

what did early normal phase HPLC instruments use (and effect)

A

polar stationary phase
non polar solvent
more polar molecules absorbed more strongly to stationary phase
and take longer to appear in the eluent

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16
Q

what so reversed phase HPLC machines use (and effect)

A

column containing silica with attached long chain hydrocarbons making them non polar
polar solvent used
polar molecules pass through column more quickly

17
Q

what is gas liquid chromatography used to separate

A

mixtures of volatile liquids

18
Q

what is the stationary phase of gas liquid chromatography

A

powder coated with film of non volatile liquid

19
Q

what is the mobile phase of gas liquid chromatography

A

unreactive gas (eg nitrogen)

20
Q

how does gas liquid chromatography work

A

powder packed into coiled tube
tube heated in oven
vaporises volatile liquids
continuous flow of unreactive gas passes through column
sample injected into column
substances are separated depending on their affinity for stationary and mobile phases

21
Q

what does a gas liquid chromatogram show

A

time taken for each substance to pass through the column
size of signal proportional to amount of substance in the mixture

22
Q

RF value equation

A

distance travelled by spot
—————————————
distance travelled by solvent