In which of the following mass spectrometric techniques is the sample

introduced as a solution which is nebulized under an applied electrical

potential?
fast atom bombardment (FAB)
electrospray ionization (ESI)
matrix-assisted laser desorption ionization (MALDI)
electron ionization (EI)

In reversed-phase HPLC:
a hydrophobic stationary phase is combined with a polar mobile phase
a hydrophilic stationary phase is combined with a non-polar mobile phase
a hydrophilic stationary phase is combined with a polar mobile phase
a hydrophobic stationary phase is combined with a non-polar mobile phase

Deuteration of C2H2OH to C2H5OD:

has no effect on the absorption due to the OH/D stretch
dramatically alters all the absorptions in the IR spectrum of the compound
shifts the wavenumber of the OH/D stretch to lower value
shifts the wavenumber of the OH/D stretch to higher value

To compare the electronic absorption spectra of three iron(II)

complexes, you want to combine the three spectra in one plot. You
should plot:
Extinction coefficient against wavelength

Extinction coefficient against concentration

Absorbance against wavenumber
Absorbance against wavelength

Which of the following analytical methods would you choose to

investigate whether a compound is a monomer, dimer or trimer?
NMR spectroscopy
IR spectroscopy
ESI-MS
elemental analysis

WCl2F4 is octahedral. Which of the following statements about the 19F

NMR spectra of cis- and trans-isomers of WCl2F4 is correct? Ignore
coupling to 183W.
The spectrum of trans-WCl2F4 exhibits a singlet
The spectrum of cis-WCl2F4 exhibits two doublets
The spectrum of trans-WCl2F4 exhibits two doublets
The spectrum of cis-WCl2F4 exhibits two signals

Values of I (natural abundance) for 11B and 1H are 3/2 (80%)

and 1/2 (100%) respectively. The 11B NMR spectrum of NaBH4 shows:
a non-binomial 5-line signal
a binomial quartet
a 1 : 1 : 1 : 1 signal
a binomial quintet

You have prepared a sample of [Co(en)3]Br3 (en = H2NCH2CH2NH2).

Which technique is best suited to confirming that the metal ion is in an
octahedral environment in the solid state?
ESI MS
H NMR spectroscopy

Moessbauer spectroscopy
single crystal XRD

Which of the following compounds would be the most suitable for

making a stock solution of Pb2+ ions for calibration purposes in AAS?
PbCO3
PbCl2
Pb(NO3)2
PbSO4

The 1H NMR spectrum of SbMe5 contains one signal at 320 K in solution.

This suggests:
SbMe5 is stereochemically non-rigid in solution at 320 K on the NMR timescale
SbMe5 adopts a trigonal pyramidal structure which is stereochemically rigid in
solution on the NMR timescale at 320 K
SbMe5 adopts a square-based pyramidal structure which is stereochemically rigid
in solution on the NMR timescale at 320 K
SbMe5 adopts a pentagonal planar structure in solution

The 1H NMR spectrum of PMe3 is expected to show:

a triplet
a singlet
a binomial decet
a doublet

A routine way of detecting whether a sample of PEt3 has partially

oxidized to OPEt3 is to:
record the 1H NMR spectrum
record the EPR spectrum
record the UV-VIS spectrum
record the

P NMR spectrum

31

You are trying to distinguish between Ph2PH (compound A) and

Ph2PCH2PPh2 (compound B) using 31P NMR spectroscopy. You would:

not be able to distinguish the compounds by this method

see one signal for A and two signals for B in the
be able to easily identify A by comparing the

P spectrum

31

P and

31

see a doublet for A and two singlets for B in the

P{1H} NMR spectra

31

P spectrum

31

Which technique does the pharmaceutical industry routinely use to

screen for polymorphs of a compound?
mass spectrometry

solution NMR spectroscopy

solution electronic absorption spectroscopy
powder XRD

The presence of solvent in a crystalline sample of a compound could be

detected and quantified using:
ESI-MS
AAS
UV-VIS
TGA

Samples prepared for Moessbauer spectroscopy should be in which

phase?
Solid

Vapour
Any phase
Liquid

In which of the following sets of isotopes is there an

NMR inactive nucleus?
H;

F;

19

H;

P;

31

P;

31

195

11

Pt;

F;

19

31

12

B; 1H

10

EPR spectroscopy is often used to investigate copper(II) complexes but

not copper(I) complexes. This is because:
Cu2+ has an s2d7 configuration but Cu+ is d10
Cu2+ has a d9 configuration but Cu+ is d10
Cu2+ has a d9 configuration but Cu+ is s1d9
Cu2+ has an s1d8 configuration but Cu+ is d10

You are trying to find out if a thiocyanate ligand , [NCS]-, is bonded to a

metal ion through the N or S atom. Which technique would be MOST
useful to you?
IR spectroscopy

UV-VIS spectroscopy
mass spectrometry
C NMR spectroscopy

13

Elemental anaytical data for a new, monomeric compound X are a

requirement of publishing details of the compound in the literature,
even when crystallographic and spectroscopic data are available. This
is because:
elemental analysis confirms that the compound is a monomer and not a dimer or
higher oligomer
elemental analysis is a requirement purely for historical reasons
elemental analysis is the only method of confirming that the compound contains
no solvate
elemental analysis confirms the composition of the bulk sample