Determination of the Concentration of
Single-Walled Carbon Nanotubes in Aqueous
Dispersions Using UV-Visible Absorption
Spectroscopy
S. Attal,
†
R. Thiruvengadathan,
†
and O. Regev*
,†,‡
Department of Chemical Engineering and The Ilse Katz Center for Meso and Nanoscale Science and Technology,
Ben-Gurion University of the Negev, Beer Sheva 84105, Israel
Stable, homogeneous, aqueous dispersions of single-
walled carbon nanotubes (SWNTs) are prepared by non-
specific physical adsorption of surfactants enhanced by
sonication. Upon centrifugation, supernatant and precipi-
tate phases are obtained. The initial weights of the SWNTs
and the surfactant are divided between these two phases,
and the respective SWNT concentration in each phase is
unknown. The focus of this work is on the determination
of the true concentration of raw, exfoliated HiPCO SWNTs
in the supernatant phase. A UV-visible absorption-based
approach is suggested for a direct measurement of the
SWNT and the surfactant concentration in the superna-
tant. UV-visible absorbance spectra of SWNTs-surfactant
dispersions and surfactants alone reveal that the intensity
of a certain peak, attributed to the π-plasmon resonance
absorption, is unaffected by the presence of most surfac-
tants. A calibration plot is then made by monitoring the
intensity of the peak as a function of the true concentration
of the exfoliated SWNTs. Thus, we are able to determine
the unknown concentration of surfactant-dispersed HiP-
CO SWNTs in the supernatant solution, simply by mea-
suring its optical absorbance. Moreover, we can now
calculate the surfactant efficiency in dispersing SWNTs.
Cryogenic-transmission electron microscopy and thermo-
gravimetric analysis techniques are used for the charac-
terization of these dispersions and to complement the
UV-visible measurements.
The discovery of carbon nanotubes
1
(CNTs) in the past decade
has immensely contributed to the advancement of nanoscience
and technology. The potential of CNTs as transistors, chemical
and biological sensors, field emission sources, and filler in polymer
matrixes is attributed to their exotic physical properties, such as
high aspect ratio, low density, high tensile strength, and aniso-
tropic electrical conductivity.
1-5
However, the as-synthesized
single-walled carbon nanotubes (SWNTs) are bundled,
6
preventing
their efficient use.
Several research groups have reported exfoliation of SWNT
bundles into individual ones either by their direct functionalization
7
or by treatment with superacids.
8-10
An alternative approach is
the use of dispersing agents, such as ionic surfactants (sodium
dodecyl sulfate, SDS),
11,12
sodium dodecylbenzenesulfonate (NaD-
DBS),
13
nonionic surfactant (Triton X-100
13
), or polysaccharides
(gum arabic).
14
Furthermore, DNA,
15
polyelectrolytes,
16-19
and
proteins
20,21
are also shown to exfoliate and stabilize SWNTs in
water.
Typically, the surfactant-dispersed SWNT solution is prepared
by mixing surfactant and SWNTs in water. The solution is then
sonicated and centrifuged. The grayish supernatant phase contains
* Corresponding author: (e-mail) oregev@bgu.ac.il.
†
Department of Chemical Engineering.
‡
Ilse Katz Center for Meso and Nanoscale Science and Technology.
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8098 Analytical Chemistry, Vol. 78, No. 23, December 1, 2006 10.1021/ac060990s CCC: $33.50 © 2006 American Chemical Society
Published on Web 10/24/2006