Topic 19 Anaylytical Techniques Flashcards

(32 cards)

1
Q

What is a use for NMR spectroscopy in medicine?

A

MRI scan

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2
Q

State the region of electromagnetic spectrum used in 1H NMR spectroscopy

A

Radiowaves

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3
Q

Explain why CDCl3 is used as a solvent in 1H NMR spectroscopy.

A

No H atoms

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4
Q

How to determine the number of H/C environments from NMR spectrum? (Low res)

A

Number of peaks = number of environments

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5
Q

How to work out how many subpeaks there would be in a 1H NMR in High resolution?

A

(number of adjacent H atoms) + 1 rule

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6
Q

What does NMR stand for?

A

Nuclear Magnetic Resonance

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7
Q

What are nucleons?

A

proton + neutrons (things in nucleus)

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8
Q

What is multiplicity? How to name them?

A

The number of symmetrical peaks in High res NMR
singlet, doublet, triplet, quartet, quintet… or multiplet of 6 so on

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9
Q

Is there high resolution NMR for 13C and 1H?

A

No for 13C
Yes for 1H

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10
Q

What is chromatography used for?

A

Seperation

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11
Q

What are the types of chromatography (in spec)?

A
  • gas chromatography
  • HPLC
  • TLC
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12
Q

How does chromatography generally work?

A

2 phases: mobile phase and stationary phase
Since molecules have ‘an affinity’ for either phase
The retention time often helps identify

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13
Q

Why do molecules have an affinity for mobile or stationary phases in chromatography?

A

Relevant IMFs

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14
Q

What is the stationary phase of chromatography often made of?

A

Silica
it is polar

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15
Q

What does the retention time say about the component in a mixture?

A

more polar = higher affinity to polar Silica in stationary phase
= retarded = higher retention time

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16
Q

How does gas chromatography work?

A
  • inert carrier gas (mobile phase) in cylinder
  • pump allows sample inlet
  • long column lined with Silica as stationary phase - in oven
    to reach detection
17
Q

Do polar or nonpolar molecules take longer to get detected?

A

Polar
as have higher affinity to polar stationary phase

18
Q

What is retention time?

A

Time taken for samples to elute from the column

19
Q

What is HPLC?

A

High Performance Liquid Chromatography
- separate liquid/aqueous mixtures

20
Q

How does HPLC work?

A
  • Add mobile phase solvent to cover all silica beads
  • add test mixture to top of column
  • keep adding solvent to have constant supply of mobile phase
  • collect all eluted substances and test
21
Q

What is TLC? What is it made of?

A

Thin Layer Chromatography
Silica!

22
Q

How to do TLC?

A
  • scratch a line on the paper
  • dip in solvent (mobile phase)
  • allow run
  • draw solvent front line
  • calculate Rf value
23
Q

What does the movement of TLC indicate?

A
  • no movement = insoluble
  • closer to start line = higher affinity for stationary phase
  • further from start line = higher affinity for mobile phase
24
Q

How to do chromatography for α amino acids?

A

Dip one side in solvent 1
rotate 90°
Dip in solvent B
- separation after solvent 1 does not indicate number of amino acids present

25
What do 13C NMR peaks indicate?
number of carbon environments but proportion not representative of ratio of number of carbons in each environment
26
How to choose suitable solvent for recrystallisation?
Soluble in hot solvent and insoluble in cold solvent
27
Explain why X leaves the chromatography column after Y. (2 marks)
X has higher affinity to **stationary** phase Because it is more polar as… X has more positive charges or something that makes it more polar (As like dissolve like)
28
There are 3 amino acids present in a tripeptide. Give a reason why there is a lack of third spot in the TLC plate. (1 mark)
Two amino acids have the same Rf values
29
What reagent is used to locate amino acid spots on TLC? (1 MARK)
Ninhydrin
30
Give 2 reasons why 2 different amino acids have different Rf values. (2 marks)
-they have different ADSORPTION to stationary phase - they have different SOLUBILITY in mobile phase
31
Give 2 reasons why TMS is good to use as the standard for NMR.
- unreactive / inert - single peak as all H and C in same conditions - volatile, easily removed - non-toxic - TMS peak to the right - give strong signal so only small amount needed
32
What must be kept constant to measure change of pressure?
- temp AND volume of container AND initial amount of whatever involved