chapter 29 Flashcards

1
Q

what is a TLC?

A

quick and inexpensive analytical technique used to indicate how many components there are in a mixture

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2
Q

how does TLC work?

A

capillary tube spots small sample of solution
baseline drawn in pencil
substances mixture forms weak bonds with silica surface (adsorption)
different components in different mixtures have different affinities for adsorbent so bind with different strengths
placed in beaker with solvent and cover lid
separation occurs as solvent carries components to different extents
may need UV lamp to see

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3
Q

how do you calculate Rf value?

A

distance dot travelled / distance solvent travelled

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4
Q

what is gas chromatography useful for?

A

separating and identifying volatile organic compounds present in mixture

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5
Q

what is the mobile phase in gas chromatography?

A

inert carrier gas

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6
Q

what is the stationary phase in gas chromatography?

A

high boiling point liquid absorbed onto inert solid support

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7
Q

what does separation depend on in gas chromatography?

A

depends on differing solubility of components in liquid stationary phase

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8
Q

how does gas chromatography work?

A

small amount of volatile mixture injected into apparatus
mobile carrier gas carries components through column which contains liquid stationary phase
more soluble a liquid is in stationary phase the slower it passes through
different components reach detector at different times

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9
Q

what is retention time?

A

time taken for each component to travel through column

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10
Q

what can retention times be used for?

A

to identify compounds present by comparing known values

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11
Q

what can peak integrations be used for (area under each peak)?

A

to determine concentrations of components in each sample

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12
Q

what can relative peak areas be used for?

A

give relative proportions of different compounds

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13
Q

what are calibration curves needed for?

A

to turn peak area into concentration

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14
Q

test for alkene?

A

add bromine water drop wise
orange colour disappears

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15
Q

test for haloalkane?

A

aqueous silver nitrate solution and ethanol
water bath 50 degrees
C - white
B - cream
I - yellow

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16
Q

test for carbonyl group?

A

add 2,4-DNP (Brady’s reagent)
orange precipItate will form

17
Q

what is the test for aldehydes?

A

add Tollen’s reagent
warm in water bath
produces silver mirror

18
Q

how do you test for primary and secondary alcohols and aldehydes?

A

add acidified dichromate
warm in water bath
colour change orange to green

19
Q

how do you test for phenols?

A

test with pH paper
pH shows phenol is weak acid
add sodium carbonate solution
no reaction shows its a phenol
or
add bromine water drop wise
if it becomes decolourised and white precipitate forms then it is a phenol

20
Q

how does a nuclei have non-zero nuclear spin?

A

if it has an odd number of nucleons
gives them magnetic moment

21
Q

what is NMR?

A

extremely powerful analytical tool
gives information on number and type of different carbon or hydrogen environment in a molecule

22
Q

how does NMR work?

A

sample dissolved in solvent
placed in NMR tube
placed inside strong external magnetic field and spun
C13 or H2 align with or against external magnetic field
energy difference between two possibilities
radio frequency applied to sample nuclei
can absorb radiation and flip between two spin states (resonance)

23
Q

why do H1 and C13 in different environments need different frequencies?

A

electrons surrounding nucleus shift energy and radio frenquency

24
Q

why is TMS used for standard reference chemical in chemical shift scale?

A

inert
non-toxic
produces single peak in NMR spectrum

24
what is frequency shifted measured on?
scale called chemical shift relative to standard reference chemical tetramethylsilane (TMS)
25
what is the deuterated solvent used in the chemical shift scale?
deuterium produces no NMR signal in frequency range used
26
what does carbon-13 NMR provide information on?
number of peaks chemical shift values
27
what do the number of peaks mean in a carbon-13 NMR?
number of different carbon environments
28
what do the chemical shift values mean in a carbon-13 NMR?
types of carbon environment
29
why do different carbon atoms absorb different chemical shifts?
have different environments
30
why might chemical shift values may be outside of range?
depends on solvent, concentration and substituents or carbon bonded to two 'shifting groups'
31
what does number of peaks mean in a proton NMR?
number of different proton environments
32
what does the chemical shift value mean in a proton NMR?
types of proton environments present
33
what does the peak area relate to?
number of protons responsible for that peak
34
what does the ratio of relative areas under each peak relate to?
number of protons responsible for each peak
35
how do you calculate name for splitting pattern?
n = number of protons attached to adjacent carbons n+1 = assigned name
36
how do you identify NH or OH peaks after proton spectrum has run?
sample shaken with D2O deuterium exchanges and replaces OH and NH protons when spectrum is retaken the peaks disappear