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Journal of Near Infrared Spectroscopy
Volume 16 Issue 2, Pages 121–128 (2008)
doi: 10.1255/jnirs.766

 
Estimation of hexenuronic acids and kappa number in kraft pulps of Eucalyptus globulus by Fourier transform near infrared spectroscopy and multivariate analysis
Mariel Monrroy,a,b Regis Mendonça,a,b Jaime Baeza,a,c José Ruiz,a André Ferrazd and Juanita Freera,b,*
aRenewable Resources Laboratory, Biotechnology Center, Universidad de Concepción, Casilla 160-C, Concepción, Chile. E-mail: jfreer@udec.cl
bFaculty of Forest Sciences, Universidad de Concepción, Casilla 160-C, Concepción, Chile
cFaculty of Chemical Sciences, Universidad de Concepción, Casilla 160-C, Concepción, Chile
dEscola de Engenharia de Lorena, Universidade de São Paulo, CP 116, 12602-810 Lorena, SP, Brazil
ABSTRACT:
Fourier transformed near infrared (FT-NIR) spectroscopy was evaluated as an analytical tool for monitoring residual lignin, kappa number and hexenuronic acids (HexA) content in kraft pulps of Eucalyptus globulus. Sets of pulp samples were prepared under different cooking conditions to obtain a wide range of compound concentrations that were characterised by conventional wet chemistry analytical methods. The sample group was also analysed using FT-NIR spectroscopy in order to establish prediction models for the pulp characteristics. Several models were applied to correlate chemical composition in samples with the NIR spectral data by means of PCR or PLS algorithms. Calibration curves were built by using all the spectral data or selected regions. Best calibration models for the quantification of lignin, kappa and HexA were proposed presenting R2 values of 0.99. Calibration models were used to predict pulp titers of 20 external samples in a validation set. The lignin concentration and kappa number in the range of 1.4–18% and 8–62, respectively, were predicted fairly accurately (standard error of prediction, SEP 1.1% for lignin and 2.9 for kappa). The HexA concentration (range of 5–71 mmol kg–1 pulp) was more difficult to predict and the SEP was 7.0 mmol kg–1 pulp in a model of HexA quantified by an ultraviolet (UV) technique and 6.1 mmol kg–1 pulp in a model of HexA quantified by anion-exchange chromatography (AEC). Even in wet chemical procedures used for HexA determination, there is no good agreement between methods as demonstrated by the UV and AEC methods described in the present work. NIR spectroscopy did provide a rapid estimate of HexA content in kraft pulps prepared in routine cooking experiments.

Keywords: multivariate regression, Eucalyptus globulus, kraft pulping, hexenuronic acid, kappa number, lignin