Carbon 45 (2007) 907912

www.elsevier.com/locate/carbon

Quantitative assessment of carbon nanotube dispersions

by Raman spectroscopy
Christoph G. Salzmann *, Bryan T.T. Chu, Gerard Tobias, Simon A. Llewellyn,
Malcolm L.H. Green
Inorganic Chemistry Laboratory, University of Oxford, South Parks Road, OX1 3QR Oxford, United Kingdom
Received 1 August 2006; accepted 18 January 2007
Available online 26 January 2007

Abstract
Aqueous dispersions of single wall carbon nanotubes (C-SWNTs), prepared using dierent dispersing agents, have been analysed by
Raman spectroscopy. Normalising the spectra with respect to the area of the water OH stretching transition eliminates the eects of
photon scattering and absorption on the way through the dispersion, and the dispersions can be assessed quantitatively by comparison
of the areas of the carbon nanotube G-band. The normalised G-band areas show linear concentration dependence according to Beers
law. The inuences of dierent dispersing agents and excitation wavelengths are discussed and the results are compared to the commonly
used UVVisible spectroscopic analysis. The method presented here is semi-quantitative and it is proposed to use the most eective dispersing agent found in this study, sodium dodecylbenzene sulfonate (SDBS), as a benchmark for future dispersion experiments.
2007 Elsevier Ltd. All rights reserved.

1. Introduction
Single wall carbon nanotubes (C-SWNTs) have emerged
as a material with highly remarkable electronic, thermal,
optical, mechanical, spectroscopic and chemical properties
[18]. However, a general problem associated with their
application is their inherent insolubility in most solvents.
The dispersion of carbon nanotubes in dierent solvents
is therefore an important step in, for example, their chemical functionalisation, preparation of composites, and also
their characterisation [4,610]. Much research has focused
on achieving the highest possible degree of dispersion without altering the properties of the C-SWNT themselves. For
the dispersion of C-SWNTs in aqueous media, two strategies have been developed. The rst involves a chemical
functionalisation of the C-SWNT by either creating hydrophilic functional groups on the sidewalls of the C-SWNTs
or by covalently binding hydrophilic molecules onto the

Corresponding author. Tel.: +44 1865 272641; fax: +44 1865 272690.
E-mail address: christoph.salzmann@chem.ox.ac.uk (C.G. Salzmann).

0008-6223/$ - see front matter 2007 Elsevier Ltd. All rights reserved.
doi:10.1016/j.carbon.2007.01.009

surface of the C-SWNTs [1115]. The second approach

does not involve chemical modication of the C-SWNTs.
Instead, C-SWNTs are dispersed by using surfactants,
wrapping of hydrophilic (bio)polymers, or charged nanoparticles [6,10,1625].
C-SWNT dispersions are commonly quantied or characterised by UVVisible absorption spectroscopy, near
infrared (NIR) absorption spectroscopy, uorescence spectroscopy, weighing after solvent removal, or just by visual
inspection of the darkness of the dispersions: In UVVis
absorption spectroscopy, the absorption value at 500 nm
is often chosen to quantify dierent C-SWNTs dispersions
[21,24,25]. However, this suers in general from the diculty of separating contributions from C-SWNTs and
other species (e.g. carbonaceous impurities or dispersing
agents). Also, ultrasonication time was found to increase
UVVis absorption at a constant C-SWNT concentration
[26]. In the NIR spectral range, the electronic interband
transitions of the C-SWNTs are observed [10,27]. Especially the intensity of the S22 interband transition near
1000 nm has been used for quantication of C-SWNT dispersions [13] and also for purity evaluation of C-SWNTs in

C.G. Salzmann et al. / Carbon 45 (2007) 907912

dispersion [28]. However, it was also shown that the intensity of the S22 peak increases with increasing surfactant
concentration. Also, C-SWNT debundling leads to blueshifting of the peak position and changes in the ne structure of the peak [29]. Band gap uorescence measured from
C-SWNT dispersions is a powerful tool for the determination of the chirality/diameter distribution present in a sample [6,10]. However, due to the quenching eect of metallic
C-SWNTs in a bundle, it is limited to the analysis of individually dispersed C-SWNTs [10]. Also the peak position
of the uorescence peaks is greatly aected by the surfactant used [18].
Here, we present a method for quantifying carbon nanotube dispersions by Raman spectroscopy. In this regard,
the Raman spectra are normalised with respect to the area
of a solvent peak, for example the m(OH) stretching transition of water, and analysed by the resulting G-band areas.
The eects of scattering and absorption of photons on their
way through the dispersion as well as changes in the
experimental parameters are thereby eliminated. The
normalised G-band areas show linear concentration behaviour in accordance with Beers law. Due to the resonance
enhanced Raman intensity of C-SWNTs [5,30], this
method probes exclusively the C-SWNTs present in the dispersion, whereas other carbonaceous species such as amorphous carbon or graphite particles are neglected.
2. Experimental methods
2.1. Preparation of the dispersions
Carbon nanotubes were supplied by Thomas Swan and Co. Ltd. CSWNTs in a wet cake form (ca. 95% water by weight). According to
TEM analysis, the C-SWNTs have an average diameter of 1.7 0.3 nm.
The water was removed at 60 C before use. Based on literature procedures [10,18,20,22], dierent carbon nanotube dispersions were prepared:
10 mg of C-SWNTs were combined with 10 mL of a 1 wt% SDBS solution
(sodium dodecylbenzene sulfonate Aldrich), a 1 wt% SDS solution
(sodium dodecyl sulfate Aldrich), a 0.1 wt% DNA solution (single
stranded Salmon DNA Nippon Chemical Feed Co. Ltd.), a suspension
of ZrO2 nanoparticles (5 mL of 20 wt% ZrO2 nanoparticles (size 510 nm,
NYACOL Nanotechnology) +5 mL water), and just water. The CSWNTs were then dispersed by ultrasonic agitation in a bath sonicator
(110 W) for 15 min. Additionally, a dispersion of 10 mg amorphous carbon (carbon nanopowder 99+%, 30 nm average particle size, Aldrich) in
a 10 mL solution of 1 wt% SDBS was prepared. All dispersions were centrifuged at 4000 r.p.m. for 30 min and the supernatant was used for further
analysis. A set of dispersions with concentrations (c/c0) of 1.00, 0.75, 0.50,
0.25, and 0.10 was prepared by diluting the original SDBS dispersion with
1 wt% SDBS solution. These dispersions were ultrasonicated for 15 min
before analysis.

40 mW argon-ion laser (514 nm) were used. The 1800 L/mm grating provides a resolution starting from 1.0 at 200 cm1 up to 0.5 cm1 at
3600 cm1 for the HeNe laser and from 1.5 cm1 at 200 cm1 up to
1.0 cm1 at 3600 cm1 for the argon-ion laser. The abscissa was calibrated
with the 520.7 cm1 peak of a silicon standard, and the sharp Raman shifts
are accurate within the limits of the resolution.
UVVisible absorbance spectra of the dispersions were recorded in
quartz cuvettes (light path length of 5 mm) on a GBC spectrometer (Cintra 10) in the range from 200 to 1000 nm with a scan rate of 500 nm min1
and a resolution of 0.427 nm.

3. Results and discussion

For the quantitative analysis of C-SWNTs in dispersions, a linear relationship between the concentration of
the C-SWNTs and the measured quantity has to be established. Fig. 1 shows the Raman spectra of C-SWNT dispersions in SDBS solutions with relative concentrations (c/c0)
of 1.00, 0.75, 0.50, 0.25, and 0.10.
The C-SWNT peaks are found at 2625 cm1, 1590 cm1
and 1324 cm1. The most intense feature is the G-band at
1590 cm1 which is associated with several tangential CC
stretching transitions of the C-SWNT carbon atoms [5,30].
The broad peak at 3300 cm1 arises from the OH
stretching transitions (m(OH)) of water [31]. Peak intensities in Raman spectroscopy are proportional to the concentration of a species but are also inuenced by experimental
parameters including, for example, laser output power and
frequency, laser alignment conditions, and the focus conditions [32]. To eliminate the inuences of experimental
parameters, the dispersions were measured on the same
day and the distance between the inner wall of the glass
and the focus was set to 200 lm for all measurements.
The peak areas of the m(OH) bands and the G-bands
for spectra (1)(5) in Fig. 1 are shown as a function of
the C-SWNT concentration (c/c0) in Fig. 2.

G
Recorded intensity

908

O-H

G'

(1)

(2)

(3)
(4)

2.2. Characterisation of the dispersions

For recording Raman spectra, dispersions were pipetted into 2 mm
diameter quartz capillaries with 0.01 mm wall thickness (Hilgenberg company). The capillaries were sealed to prevent the evaporation of water. All
Raman spectra were recorded on a Jobin Yvon spectrometer (Labram 1B)
equipped with a microscope, through a 10 fold magnication objective
(Olympus company), by coadding four spectra with collection times of
40 s each. The distance between the wall of the capillary and the laser focus
was 200 lm for all measurements. A 20 mW HeNe laser (632 nm) and a

(5)

4000

3500

3000 2500 2000

-1
Raman shift / cm

1500

1000

Fig. 1. Raman spectra (k0 = 632 nm) recorded from a series of C-SWNT
dispersions in SDBS solution obtained upon diluting and ultrasonicating.
The C-SWNT concentrations (c/c0) are 1.00, 0.75, 0.5, 0.25, and 0.10 for
spectra (1)(5). Peaks arising from the C-SWNTs (D, G, and G 0 bands)
and water (m(OH)) are marked.

8x10

7x10

6x10

5x10

5x10

4x10

3x10

4x10

3x10

2x10

2x10

1x10

1x10

0
0.0

G-band
O-H

0.2

0.4
0.6
c / c0

0.8

0
1.0

Fig. 2. G-band and m(OH) peak areas (k0 = 632 nm) obtained upon
diluting the SDBS dispersion with starting concentration c0 and ultrasonication. Dashed lines are guides to the eye. Arrows indicate the
expected concentration dependencies.

The HOH bending transition (1640 cm1) overlaps

slightly with the carbon nanotube G-band on the higher frequency side of the G-band. The integration of this peak was
therefore carefully avoided. With increasing C-SWNT concentration, a signicant decrease of the m(OH) peak area is
observed. This behaviour is unexpected in the sense that the
concentration of water, as the solvent, would be expected to
be constant upon diluting the original C-SWNT dispersion
with SDBS solution. The expected behaviour is therefore
indicated by the horizontal arrow in Fig. 2. For the area
of the G-band, a linear trend is observed with increasing
C-SWNT concentration at low concentrations. However,
at higher C-SWNT concentrations, deviation from this linear behaviour is observed and the increase of G-band area
with concentration decreases signicantly. The expected linear behaviour according to Beers law is indicated by an
arrow at low concentrations. This nonlinearity represents
a major problem in the quantication of C-SWNT dispersions and was also observed by Itkis et al. in their study
on purity evaluation of C-SWNTs (cf. Fig. 10 in Ref.
[28]). They concluded that this behaviour originates from
photons undergoing secondary scattering or absorption
on their way out of the dispersion to the detector, thus
reducing the strength of the Raman signal. Scattering of
photons on their way through the dispersion seems indeed
likely as the wavelength of the Raman lasers have similar
orders of magnitude as the C-SWNT agglomerate sizes.
Upon diluting and ultrasonicating the C-SWNT dispersion,
a decrease in C-SWNT bundle size is expected [26] and
therefore secondary photon scattering should become less
likely. This is in accordance with the larger G-band area
increases with concentration at lower concentrations. For
C-SWNT dispersions, nonlinear transmittance behaviour
was observed at high laser powers which is thought to originate from the formation of microplasmas (cf. Fig. 4 in Ref.
[33]).
It can be assumed that photons arising from the G-band
and m(OH) Raman scattering processes experience very

909

similar amounts of secondary scattering and absorption

on their way through the dispersion. Also, as explained
above, the concentration of water is expected to remain
unchanged upon dilution. The Raman spectra are therefore
normalised in a next step with respect to the m(OH) areas so
that the m(OH) areas equal unity. Fig. 3 shows a plot of the
G-band areas, obtained by integration from the normalized
spectra, as a function of the C-SWNT concentration.
The normalised G-band areas show linear concentration
behaviour in accordance with Beers law. It is therefore
possible to use the normalised G-band areas for quantitative analysis of C-SWNT dispersions. By using this kind
of normalisation, it is furthermore possible to eliminate
the eects of changing experimental parameters, since the
sample and reference peaks are expected to be aected
equally.
We next use this quantication method to assess CSWNT dispersions using dierent dispersing agents in water
[10,18,20,22]. Fig. 4a shows the normalised Raman spectra
(HeNe laser) of dispersions using (1) SDBS, (2) SDS, (3)
DNA, (4) ZrO2 nanoparticles, (5) just water, and (6) a dispersion of amorphous carbon in SDBS solution.
The areas of the carbon nanotube G-bands at 1590 cm1
were determined next by integration from the normalised
spectra: (1) 0.288, (2) 0.156, (3) 0.126, (4) 0.059, (5) 0,
and (6) 0. These quantities can now be used for direct
quantitative comparison of the dierent C-SWNT dispersion. It is possible for example to conclude that SDBS is
almost twice as eective as SDS in dispersing C-SWNTs.
SDS and DNA show similar dispersing eects whereas
the dispersion prepared using ZrO2 nanoparticles is comparatively poor. The method presented here is semi-quantitative which means that the results are scored on an
arbitrary scale. For tests with potential dispersing agents,
we propose to use SDBS, the most eective dispersing
agent found here, as a benchmark.
The normalised G-band area of the C-SWNT dispersion
in pure water (5) is, as expected, zero as the C-SWNTs occulate immediately after ultrasonic agitation. The dispersion of amorphous carbon does not give a detectable

Normalised G-band area

(O-H) area / cm

G-band area / cm

-1

6x10

-1

C.G. Salzmann et al. / Carbon 45 (2007) 907912

0.30
0.25
0.20
0.15
0.10
0.05
0.00
0.0

0.2

0.4

c / c0

0.6

0.8

1.0

Fig. 3. Concentration dependence of the normalised G-band area. The

linear t (dashed line) is forced through zero.

910

C.G. Salzmann et al. / Carbon 45 (2007) 907912

0 = 632 nm

A(O-H) = 1

G'

A(G-band) =
0.288

(1)
0.156

(2)

0.126

Normalised intensity

(3)

0.059

(4)
(5)
(6)

0 = 514 nm
A(O-H) = 1

A(G-band) =
0.0220

(1)

(2)
(3)

0.0139
0.0110

*
(4)
(5)

0.0041

(6)

4000

3500

3000 2500 2000

-1
Raman shift / cm

1500

1000

Fig. 4. Raman spectra of C-SWNT dispersions using (a) a HeNe laser

(632 nm) and (b) an argon-ion laser (514 nm). The dispersions were
prepared using (1) SDBS, (2) SDS, (3) DNA, (4) ZrO2 nanoparticles, (5)
and just water as dispersing agents. Spectrum (6) was recorded from a
dispersion of amorphous carbon in SDBS. Spectra were normalised by
dividing by the areas of the OH stretching transitions. The areas of Gbands are given in (a) and (b). The peaks arising from C-SWNTs (D, G,
and G 0 bands) are indicated in (a). Asterisks in (a) and (b) mark the peak
positions of acetic acid used for stabilisation of the ZrO2 nanoparticles.
Peaks marked by circles could arise from a small fraction of uorescing
nanoparticles.

G-band intensity in spectrum (6) which demonstrates the

poor Raman scattering properties of amorphous carbon
compared to C-SWNTs. In general, the Raman spectra
of C-SWNT samples are dominated by the spectral features
of the C-SWNTs and not by other carbonaceous impurities
such as amorphous carbon or graphitic particles [5]. For
the quantication method presented here, this is highly
advantageous as it allows for the quantication of CSWNTs alongside other carbonaceous impurities present
in the C-SWNT samples.
The high Raman intensity of the C-SWNTs arises from
a resonance Raman scattering process [30,34]. Depending
on the wavelength of the laser, C-SWNTs of dierent diameters and chiralities full the resonance conditions and contribute hence to the spectrum. Therefore, by using a specic
wavelength, only subsets of the carbon nanotube species

present in dispersion are probed. In order to assess the

selectivity of a dispersing agent towards dispersing CSWNTs of certain diameters or chiralities, the Raman spectra of the dispersions were recorded using a dierent laser
wavelength. Fig. 4b shows the spectra of the dierent dispersions using an argon-ion laser (514 nm). The spectra
were again normalised with respect to the area of the O
H stretching transition, as described above. The areas of
G-bands in the normalised spectra are: (1) 0.0220, (2)
0.0139, (3) 0.0110, (4) 0.0041, (5) 0, and (6) 0. All G-band
areas in Fig. 4b are smaller when compared with the spectra in Fig. 4a. The reasons for this could be i.a. that the resonance conditions are met less accurately using the argonion laser (514 nm), that the concentration of C-SWNTs in
resonance is lower, or that the Raman scattering intensities
of the C-SWNTs in resonance are weaker. However, the
sequence of the normalised G-band areas is the same as
found for the HeNe laser in Fig. 1a. A plot of the normalised G-band areas, obtained using the HeNe laser,
against the values found for the argon-ion laser shows a
linear trend with a slope of 12.6 0.8 (R = 0.993) (not
shown). This implies that the C-SWNTs in resonance at
632 nm or 514 nm are dispersed very similarly by the dierent dispersing agents. It should be emphasised that the
slope of 12.6 0.8 is expected to change if dierent carbon
nanotube samples with dierent diameter distributions
were used.
Spectra (1), (2), (4), and (5) in Fig. 4b show broad peaks
centred at 2200 cm1. These features possibly arise from
a small fraction of uorescing nanoparticles present in the
dispersions. Such particles could be isolated from a CSWNT sample by electrophoresis [35] and from the supernatant of a SDS dispersion [36]. Also, very recently, we
have isolated uorescing carbonaceous fragments in high
concentrations from a C-SWNT sample after nitric acid
treatment [37] and we have shown that uorescence of
these fragments is quenched by adsorption onto the CSWNTs. The uorescence detected here could therefore
originate from similar fragments in the dispersion after
desorption from the C-SWNTs. The HeNe laser
(632 nm) is most probably too low in energy to excite uorescence as these broad features are not observed in Fig. 4a.
For quantitative analysis presented here it is necessary
that the Raman spectroscopic properties of the G-band
are not signicantly altered by using dierent dispersing
agents. This was previously stated in Refs. [18,38] and we
also nd that the peak positions and relative intensities of
the G, D, and G 0 -bands remain unchanged in spectra (1
4) in Fig. 4a or b. We have shown furthermore that, despite
progressive debundling of the C-SWNTs (cf. above), a linear behaviour between normalised G-band area and CSWNT concentration is found. To investigate further the
inuence of a surfactant on the Raman spectroscopic properties of the G-band, a SDS dispersion with c/c0 = 1 was
diluted with the same volume of a 1 wt% SDBS solution
and ultrasonicated for 5 min. This is thought to produce
an at least statistic mixture of SDS and SDBS surfactant

C.G. Salzmann et al. / Carbon 45 (2007) 907912

Absorbance

illustrates the advantage of the quantitative measurements

presented here using Raman spectroscopy as varying
amounts of dispersed amorphous carbon could obscure
the results obtained by UVVisible spectroscopy.

(6)

(1)

911

(2)

Acknowledgments
1

(3)
(4)

(5)

400

600
800
Wavelength / nm

1000

The authors thank Thomas Swan Co. Ltd. for supplying

the C-SWNT samples used in this study. We acknowledge
the nancial support provided through the Austrian
Science Funds (FWF; project J2446) (C.G.S.) and the 6th
European Community Framework Programme (Marie
Curie Intra-European Fellowship; MEIF-CT-2006024542) (G.T.).
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Fig. 5. UVVisible absorption spectra (upper) and photographs (lower) of

C-SWNT dispersion using (1) SDBS, (2) SDS, (3) DNA, (4) ZrO2
nanoparticles, (5) just water, and (6) a dispersion of amorphous carbon in
SDBS solution.

molecules in the C-SWNT micelle. Due to the p-stacking

capability of SDBS, it can be argued that SDBS is probably
enriched at the surfaces of the C-SWNTs. The C-SWNT
concentration after this procedure is c/c0 = 0.5. The normalised G-band area was found to halve as a consequence
of this experiment. This shows that the Raman scattering
properties of the C-SWNT G-band are not signicantly
aected by the substitution of SDS with SDBS.
Finally, we compare the results obtained here by Raman
spectroscopy with that obtained by UVVisible absorption
spectroscopy which is the method most commonly used to
analyse carbon nanotube dispersions [21,24,25]. Fig. 5
shows the UVVisible absorption spectra of the dierent
dispersions.
The absorptions at 500 nm are 1.152, 0.974, 0.659,
0.307, 0, and 3.19 for the dispersions using (1) SDBS, (2)
SDS, (3) DNA, (4) ZrO2 nanoparticles, (5) just water,
and (6) a dispersion of amorphous carbon in SDBS. The
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the dispersion of amorphous carbon in a solution of SDBS
(6) are very dierent. In UVVisible absorption, this dispersion gives an absorbance of 3.19 at 500 nm which is
the highest absorbance value of all samples. Also, visually,
this sample is one of the darkest dispersions (cf. Fig. 5(bottom)). With Raman spectroscopy on the other hand, amorphous carbon did not contribute to the spectrum. This

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