Analytica Chimica Acta 445 (2001) 269–275
Determination of residual carbon by inductively-coupled
plasma optical emission spectrometry with axial and
radial view configurations
Sandro T. Gouveia
a
, Fernando V. Silva
b,c
, Let´ ıcia M. Costa
b
,
Ana Rita A. Nogueira
c
, Joaquim A. Nóbrega
b,∗
a
Universidade Federal do Ceará, Fortaleza, CE, Brazil
b
Departamento de Qu´ ımica, Universidade Federal de São Carlos, P.O. Box 676, 13560-970 São Carlos, SP, Brazil
c
Embrapa Pecuária Sudeste, São Carlos, SP, Brazil
Received 8 February 2001; received in revised form 3 July 2001; accepted 3 July 2001
Abstract
In this work it was evaluated the performance of inductively-coupled plasma optical emission spectrometers (ICP-OESs)
with axial and radial view configurations for residual carbon content (RCC) determination. The effects of carbon compound
source (urea, l-cysteine, and glucose), sample medium, and internal standards on RCC determination were systematically
evaluated. All measurements were carried out with two ICP spectrometers using the carbon atomic emission lines: 247.857
and 193.025 nm. The results obtained using axial and radial configurations showed that both the carbon source and the
sample medium did not affect significantly the emission intensities. The sample medium only caused drastic influence
when H
2
SO
4
was employed probably due to transport interference that can be corrected employing Y as internal standard.
The sensitivity attained using axial view ICP-OES was 20-fold better than that reached using radial view ICP-OES based
on the slopes of the analytical curves at the most sensitive wavelength (193.025nm). Using radial and axial ICP-OESs,
high concentrations of Fe (>100 mg l
-1
) interfered at 247.857 nm wavelength. An addition-recovery experiment was made
by adding urea to an acid-digested sample and all recoveries were in the 100 ± 5% range for axial and radial measure-
ments. At this wavelength, R.S.D. <2.0% (n = 10) and detection limits of 33 and 34 g ml
-1
C, were measured for
ICP-OESs with radial and axial configurations, respectively. Biological samples were acid-digested using a closed-vessel
microwave-assisted procedure and RCC was determined using both ICP-OES configurations. © 2001 Elsevier Science
B.V. All rights reserved.
Keywords: Residual carbon content; Microwave-assisted digestion; Inductively-coupled plasma optical emission spectrometry; Radial and
axial configurations
∗
Corresponding author. Fax: +55-162608350.
E-mail address: djan@zaz.com.br (J.A. N´ obrega).
1. Introduction
Frequently instrumental techniques require com-
plete sample decomposition before measurements.
Usually acid wet digestion is implemented combin-
ing oxidant agents and heating for destroying the
0003-2670/01/$ – see front matter © 2001 Elsevier ScienceB.V. All rights reserved.
PII:S0003-2670(01)01255-7