In the Laboratory
Chemical Characterization of Activated Carbon Fibers
and Activated Carbons
J. M. Valente Nabais* and P. J. M. Carrott
Centro de Química de Évora and Departamento de Química, Universidade de Évora, Rua Romão Ramalho,
nº59, 7000-671 Évora, Portugal; *jvn@uevora.pt
The objective of this laboratory is the chemical charac-
terization of carbon materials using several methods to ob-
tain information without using expensive instruments.
During this lab the students determine the potential of zero
charge (pzc) by mass titrations and quantify the acidic and
basic sites by acid–base titrations. This lab is useful in two
aspects:
• In specific disciplines about carbon materials, the
methods proposed in this article are important for the
chemical characterization of the materials. For instance,
the data are crucial to explain the results in studies of
liquid-phase adsorption, such as those previously pub-
lished in this Journal (1–3) or to analyze samples pro-
duced by chemical modification methods such as
oxidation in the liquid phase with nitric acid (4), sul-
furic acid (5), hydrogen peroxide (5), or by thermal
treatments under controlled atmosphere (6, 7).
• In general chemistry disciplines, the lab can interest
students in the basic acid–base concepts and titrations
as they are applied to materials that have a great im-
portance for environmental protection and a signifi-
cant number of daily life applications.
Figure 1. Activated carbon fiber from commercial textile acrylic
fibers (8).
436 Journal of Chemical Education • Vol. 83 No. 3 March 2006
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Activated carbons (AC) and activated carbon fibers
(ACF) are examined. Both activated products have well de-
veloped porosity and surface chemistry but also have some
interesting differences. A scanning electron micrograph clearly
shows that the ACF is in the form of filaments (Figure 1). In
this material the porosity is predominantly microporosity
(pore width, dp, < 2 nm) and opens directly to the exterior.
In AC, the microstructure is normally spherical and the po-
rosity decreases from macro (dp > 50 nm) to meso (2 nm <
dp < 50 nm) to microporosity from the external surface to-
wards the interior of the material (Figure 2).
These materials have a tremendous number of applica-
tions, which include antibacterial wound dressings, dispos-
able gas masks, methane storage, polarizable electrodes,
catalysis applications, SOx and NOx removal, gas separation,
cigarette filters, skin substitutes, and adsorption of pollut-
ants such as volatile organic compounds, hydrocarbons,
nickel, copper, lead, and mercury. The applications in the
gas phase are mainly due to the porous structure whereas the
applications in the liquid phase are mainly dependent on the
chemical structure of the materials. In this sense, the com-
plete characterization of the materials, including the chemi-
cal characterization, is of great importance.
Experimental Procedure
Materials
This lab has been applied to a variety of different car-
bon materials, which include commercial activated carbons
from Norit N.V. (Norit S51) and Merck (p.a., refª 2186) and
activated carbon fibers from Nipon Kynol Inc. (ACF-1603-
15) and samples produced in our laboratory from acrylic tex-
tile fibers.
Acid–Base Titrations
The carbon material, 300 mg, was equilibrated with 60.0
mL of 0.01 mol L᎑1 NaOH for 48 h with stirring at 25.0 ⬚C.
macropores
micropores
fiber surface
A B
Figure 2. Representation of the porous structure of activated car-
bon fibers (A) and activated carbons (B).
• www.JCE.DivCHED.org
 In the Laboratory

The suspension was filtered using Whatman #1 paper. The
concentrations of acidic sites were determined by back titra-
tion of the filtrate with 0.01 mol L᎑1 HNO3. The concentra-
tions of basic sites were determined in a similar manner. These
procedures should take place in a glove box under an inert
atmosphere to avoid carbonation of the NaOH solutions by
atmospheric CO2.
Mass Titrations
The curves were obtained by preparing three series of
suspensions with initial pH of 3, 6, and 11. The three initial
pH values were obtained by adjusting the pH of a solution
0.1 mol L᎑1 NaNO3 with NaOH or HNO3 solutions. For
each series, five suspensions of 50.0 mL of pH-adjusted so-
lutions with 0.05, 0.1, 2.0, 4.0, and 7.0% (w兾v) in carbon
material were prepared. The suspensions were placed in a tem-
perature-controlled bath with stirring (Grant Model SS40-
D) for 48 h at 25.0 ⬚C, and then filtered with Whatman #1
paper, and the equilibrium pH measured with a Crison po-
tentiometer (model 2002).
For didactic objectives it is preferable to determine the
complete curves although the pzc can also be obtained using
only the three suspensions with 7% (w兾v) (9).
tions (5–10% for carbons) the curve tends towards a plateau,
the corresponding pH value being independent of the initial
pH value of the aqueous phase. The analytical proof of this
principle can be found in ref 12.
In adsorption processes the surface of the carbon mate-
rials can be positive, neutral, or negatively charged depend-
ing on the pH at which the adsorption takes place. If the
adsorption pH is equal to pzc the surface will be neutral, but
if the adsorption pH is greater than the pzc the surface is
positively charged. On the other hand, if the pzc is greater
than the pH of the suspensions used in the adsorption pro-
cess the surface is negatively charged. The charge of the sur-
face can be important for understanding the adsorption of
ionic species. The graphics obtained for a commercial acti-
vated carbon from Merck and an activated carbon fiber from
Kynol are shown in Figure 3.
Acid–Base Titrations
By analysis of the titration curves using the first or the
second derivatives it is possible to perform the quantifica-
tion of the basic and acidic groups. We can assume that the
reaction of the acidic and basic groups present in the materi-

Hazards
No chemicals or procedures used by students present any A
12
significant hazards. The stock solutions of nitric acid and so-
dium hydroxide (0.01 mol L᎑1) and solid potassium bromide
are irritating and thus require proper eye and skin protec- 10

tion. Sodium nitrate is harmful if swallowed and irritating

for eyes and skin. Its contact with combustible material may
8
cause fire and thus the powder should be kept away from
pH

heat and sources of ignition and requires eye and skin pro-
tection. 6

Results and Discussion initial pH = 11

4
initial pH = 7
Potential of Zero Charge initial pH = 3
The functional groups on the surface of the carbon ma- 2
terials can be represented using a very simple model with two 0 2 4 6 8
kinds of functional groups, one basic (B) and one acidic (HA) Mass Concentration (%)
(10). These groups can suffer ionization determined by the B
respective pKa or pKb (11) and suspension pH but indepen- 12

dently from each other.

10
HA (s) + H2O (l) A−(s) + H3O+ (aq) (1)
8
pH

B(s) + H2O(l) BH+(s) + OH−(aq) (2)

6

A common indicator of the surface acidity is the value

of the potential of zero charge (pzc) defined as the value of 4
pX at which the net surface charge is zero. X is the ionic spe-
cies that determines the surface charge of the materials. For
carbon materials pX is the value of pH (or pOH). In the 2
0 2 4 6 8
mass titration method the pH of various aqueous suspensions
of adsorbent, with increasing mass兾volume percentages of ad- Mass Concentration (%)
sorbent, in acid, base, or neutral solutions, are plotted as a Figure 3. Mass titrations of an activated carbon from Merck (A)
function of the mass of adsorbent. For high mass concentra- and an activated carbon fiber from Kynol (B).

www.JCE.DivCHED.org • Vol. 83 No. 3 March 2006 • Journal of Chemical Education 437

 In the Laboratory
als with NaOH and HNO3, respectively, have stoichiometry
1:1 (eqs 3 and 4).
− +
HA(s) + NaOH (aq) A Na (s) + H2O(l) (3)
B(s) + HNO3(aq) BH+NO3−(s) (4)
With these data it is possible to determine the concentration
of the acidic and basic groups expressed as mmol兾(g of car-
bon material)
Summary
The execution of this lab allows the study of some as-
pects of acid–base chemistry, like back titrations and acid–
base titrations, in a more fashionable way by applying these
techniques to a novel system (carbon materials). Also, the stu-
dents have chance to learn about a different kind of titra-
tion, mass titration, where the solid acts as the titrant because
it will, for each initial pH, react with the H3O+ present us-
ing the equilibria in eqs 1 and 2. When the “titrant” is added
in excess the suspension pH will be determined by the solid
characteristics and be equal to the pzc value.
The mass titration curves can be obtained theoretically
by numeric simulations using a simple model and algorithm
(10). This can be useful in discipline where the use of the
computer is introduced to execute some kind of calculations.
Acknowledgments
The authors thank the students who performed the lab
during the 2001–2002 and 2002–2003 terms and Norit N.V.
and Nipon Kynol Inc. for the carbon samples.
438 Journal of Chemical Education • Vol. 83 No. 3 March 2006
W
Supplemental Material
Notes for the instructor are available in this issue of JCE
Online.
Literature Cited
1. Lynam, M. M.; Kilduff, J. E.; Weber, W. J. J. Chem. Educ.
1995, 72, 80–84.
2. Rybolt, R. T.; Burrell, E. D.; Shults, J. M.; Kelley, K. A. J.
Chem. Educ. 1988, 65, 1009–1010.
3. Turk, A.; Karamitsos, H.; Mahmood, K.; Mozaffari, J.; Loewi,
R.; Tola, V. J. Chem. Educ. 1992, 69, 929–932.
4. Noh, J. S.; Schwarz, J. A. Carbon 1990, 28, 675–682.
5. Pradhan, B.; Sandle, N. Carbon 1999, 37, 1323–1332.
6. Menéndez, J. A.; Carrott, P. J. M.; Valente Nabais, J. M.;
Ribeiro Carrott, M. M. L. Process for the Manufacture of
Carbon Molecular Sieves. Spanish Patent Application Num-
ber P200302133, 2003.
7. Carrott, P. J. M.; Valente Nabais, J. M.; Ribeiro Carrott, M.
M. L.; Menéndez, J. A. Carbon 2004, 42, 227–229.
8. Carrott, P. J. M.; Nabais, J. M. V.; Ribeiro Carrott, M. M. L.;
Pajares, J. A. Fuel Proc. Tech. 2002, 77–78, 381–387.
9. Carrott, P. J. M.; Nabais, J. M. V.; Ribeiro Carrott, M. M. L.;
Menendez, J. A. Mic. Mes. Mat. 2001, 47, 243–252.
10. Carrott, P. J. M.; Ribeiro Carrott, M. M. L.; Candeias, A. J.
E.; Ramalho, J. P. P. J. Chem. Soc. Faraday Trans. 1995, 91,
2179–2184.
11. Leon y Leon, C.; Radovic, L. R. Interfacial Chemistry and
Electrochemistry of Carbon Surfaces. In Chemistry and Phys-
ics of Carbon; Thrower, P., Ed.; Marcel Dekker: New York,
1994; Vol. 24, pp 236–237.
12. Noh, J. S.; Schwarz, J. A. J. Coll. Int. Science 1989, 130, 157–
164.
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